
data_global
_journal_name_full               Org.Biomol.Chem.
#==========================================================

_journal_coden_Cambridge         0177

_publ_contact_author_name        'Prof Koji Araki'
_publ_contact_author_address     
;
Institute of Industrial Science
University of Tokyo
4-6-1
Komaba
Meguro-ku
Tokyo
153-8505
JAPAN
;

_publ_contact_author_email       araki@iis.u-tokyo.ac.jp
_publ_contact_author_fax         +81-3-5452-6363

_publ_section_title              
;
Use of an adjustable soft segment as an effective
molecular design for crystal engineering of hydrogen-bonded tape motifs
;
loop_
_publ_author_name
'Koji Araki'
'Ryoichi Takasawa'
'Isao Yoshikawa'

#========================================================
data_1a+MeOH
_database_code_depnum_ccdc_archive 'CCDC 225956'
#========================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
2',3',5'-O-tris(tert-buthyldiphenylsilyl)-guanosine
;
_chemical_name_common            
2',3',5'-O-tris(tert-buthyldiphenylsilyl)-guanosine
_chemical_melting_point          ?
_chemical_formula_moiety         'C59 H71 N5 O6 Si3'
_chemical_formula_sum            'C59 H71 N5 O6 Si3'
_chemical_formula_weight         1030.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   p21

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   13.365(4)
_cell_length_b                   11.036(4)
_cell_length_c                   19.880(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.05(2)
_cell_angle_gamma                90.00
_cell_volume                     2924.9(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      12.5
_cell_measurement_theta_max      14.4

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.120
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1064
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.7470
_exptl_absorpt_correction_T_max  0.9997
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.70930
_diffrn_radiation_type           ?
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       ω-2θ
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 150
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        -18.88
_diffrn_reflns_number            7372
_diffrn_reflns_av_R_equivalents  0.0048
_diffrn_reflns_av_sigmaI/netI    0.0075
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.56
_diffrn_reflns_theta_max         27.44
_reflns_number_total             7074
_reflns_number_gt                4718
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1242P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(16)
_refine_ls_number_reflns         7074
_refine_ls_number_parameters     648
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0525
_refine_ls_wR_factor_ref         0.1792
_refine_ls_wR_factor_gt          0.1492
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      0.997
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C2 C 0.8726(3) 0.4783(4) 0.0591(2) 0.0417(9) Uani 1 1 d . . .
C4 C 0.8804(3) 0.2906(4) 0.09950(19) 0.0381(8) Uani 1 1 d . . .
C5 C 0.9493(3) 0.2520(4) 0.0558(2) 0.0406(9) Uani 1 1 d . . .
C6 C 0.9848(3) 0.3353(4) 0.0082(2) 0.0430(10) Uani 1 1 d . . .
C8 C 0.9194(3) 0.0992(4) 0.1165(2) 0.0427(9) Uani 1 1 d . . .
H8 H 0.9198 0.0217 0.1348 0.051 Uiso 1 1 calc R . .
C10 C 0.7951(3) 0.1805(4) 0.19260(19) 0.0351(8) Uani 1 1 d . . .
H10 H 0.8015 0.0990 0.2119 0.042 Uiso 1 1 calc R . .
C11 C 0.8105(3) 0.2733(4) 0.24911(19) 0.0370(8) Uani 1 1 d . . .
H11 H 0.8219 0.3536 0.2299 0.044 Uiso 1 1 calc R . .
C13 C 0.7079(3) 0.2703(4) 0.27844(18) 0.0363(8) Uani 1 1 d . . .
H13 H 0.6956 0.3423 0.3055 0.044 Uiso 1 1 calc R . .
C15 C 0.6392(3) 0.2648(4) 0.2133(2) 0.0399(9) Uani 1 1 d . . .
C17 C 0.6100(3) 0.3865(5) 0.1841(2) 0.0468(10) Uani 1 1 d . . .
H17A H 0.6693 0.4362 0.1804 0.056 Uiso 1 1 calc R . .
H17B H 0.5770 0.3767 0.1394 0.056 Uiso 1 1 calc R . .
C20 C 1.0851(4) 0.1755(5) 0.2626(3) 0.0561(12) Uani 1 1 d . . .
C21 C 1.1819(4) 0.1993(8) 0.2409(4) 0.085(2) Uani 1 1 d . . .
H21 H 1.2069 0.2780 0.2427 0.102 Uiso 1 1 calc R . .
C22 C 1.2388(7) 0.1082(11) 0.2172(5) 0.118(3) Uani 1 1 d . . .
H22 H 1.3025 0.1253 0.2038 0.142 Uiso 1 1 calc R . .
C23 C 1.2028(8) -0.0096(10) 0.2128(5) 0.120(3) Uani 1 1 d . . .
H23 H 1.2409 -0.0702 0.1945 0.144 Uiso 1 1 calc R . .
C24 C 1.1102(7) -0.0367(7) 0.2359(5) 0.097(2) Uani 1 1 d . . .
H24 H 1.0868 -0.1161 0.2349 0.117 Uiso 1 1 calc R . .
C25 C 1.0523(5) 0.0557(6) 0.2604(3) 0.0690(15) Uani 1 1 d . . .
H25 H 0.9899 0.0371 0.2758 0.083 Uiso 1 1 calc R . .
C26 C 1.0083(4) 0.4418(5) 0.2541(2) 0.0510(11) Uani 1 1 d . . .
C27 C 1.0657(4) 0.4645(7) 0.1995(3) 0.0698(16) Uani 1 1 d . . .
H27 H 1.1088 0.4046 0.1857 0.084 Uiso 1 1 calc R . .
C28 C 1.0604(6) 0.5735(9) 0.1653(4) 0.098(3) Uani 1 1 d . . .
H28 H 1.1000 0.5870 0.1294 0.118 Uiso 1 1 calc R . .
C29 C 0.9960(9) 0.6616(7) 0.1847(4) 0.106(3) Uani 1 1 d . . .
H29 H 0.9932 0.7356 0.1623 0.127 Uiso 1 1 calc R . .
C30 C 0.9359(8) 0.6423(6) 0.2369(4) 0.103(3) Uani 1 1 d . . .
H30 H 0.8924 0.7025 0.2497 0.123 Uiso 1 1 calc R . .
C31 C 0.9406(6) 0.5331(6) 0.2699(3) 0.0743(17) Uani 1 1 d . . .
H31 H 0.8976 0.5191 0.3039 0.089 Uiso 1 1 calc R . .
C32 C 1.0495(4) 0.3069(5) 0.3921(2) 0.0540(12) Uani 1 1 d . . .
C33 C 1.1610(4) 0.3386(9) 0.3995(3) 0.088(2) Uani 1 1 d . . .
H33A H 1.1720 0.4138 0.3769 0.132 Uiso 1 1 calc R . .
H33B H 1.1988 0.2755 0.3797 0.132 Uiso 1 1 calc R . .
H33C H 1.1824 0.3463 0.4464 0.132 Uiso 1 1 calc R . .
C34 C 1.0294(6) 0.1889(7) 0.4273(3) 0.086(2) Uani 1 1 d . . .
H34A H 0.9589 0.1711 0.4223 0.129 Uiso 1 1 calc R . .
H34B H 1.0502 0.1958 0.4744 0.129 Uiso 1 1 calc R . .
H34C H 1.0661 0.1248 0.4077 0.129 Uiso 1 1 calc R . .
C35 C 0.9918(6) 0.4067(9) 0.4270(3) 0.095(2) Uani 1 1 d . . .
H35A H 0.9214 0.3881 0.4234 0.143 Uiso 1 1 calc R . .
H35B H 1.0027 0.4831 0.4056 0.143 Uiso 1 1 calc R . .
H35C H 1.0151 0.4112 0.4737 0.143 Uiso 1 1 calc R . .
C37 C 0.7231(4) 0.2181(5) 0.4594(2) 0.0505(11) Uani 1 1 d . . .
C38 C 0.7155(5) 0.3440(6) 0.4611(3) 0.0670(15) Uani 1 1 d . . .
H38 H 0.6830 0.3839 0.4246 0.080 Uiso 1 1 calc R . .
C39 C 0.7541(5) 0.4109(7) 0.5146(3) 0.0771(17) Uani 1 1 d . . .
H39 H 0.7456 0.4945 0.5147 0.093 Uiso 1 1 calc R . .
C40 C 0.8146(5) 0.2329(7) 0.5681(3) 0.0761(17) Uani 1 1 d . . .
H40 H 0.8471 0.1940 0.6049 0.091 Uiso 1 1 calc R . .
C41 C 0.8058(6) 0.3549(7) 0.5685(3) 0.0794(18) Uani 1 1 d . . .
H41 H 0.8340 0.4002 0.6044 0.095 Uiso 1 1 calc R . .
C42 C 0.7762(4) 0.1655(6) 0.5143(3) 0.0627(14) Uani 1 1 d . . .
H42 H 0.7861 0.0821 0.5147 0.075 Uiso 1 1 calc R . .
C43 C 0.7233(4) -0.0334(5) 0.3966(2) 0.0511(11) Uani 1 1 d . . .
C44 C 0.8204(4) -0.0478(6) 0.3754(3) 0.0611(13) Uani 1 1 d . . .
H44 H 0.8532 0.0189 0.3588 0.073 Uiso 1 1 calc R . .
C45 C 0.8683(6) -0.1578(7) 0.3785(4) 0.086(2) Uani 1 1 d . . .
H45 H 0.9331 -0.1638 0.3646 0.103 Uiso 1 1 calc R . .
C46 C 0.8223(7) -0.2593(7) 0.4018(3) 0.088(2) Uani 1 1 d . . .
H46 H 0.8546 -0.3340 0.4034 0.105 Uiso 1 1 calc R . .
C47 C 0.7281(6) -0.2469(7) 0.4226(4) 0.085(2) Uani 1 1 d . . .
H47 H 0.6955 -0.3146 0.4383 0.102 Uiso 1 1 calc R . .
C48 C 0.6801(5) -0.1380(5) 0.4209(3) 0.0694(16) Uani 1 1 d . . .
H48 H 0.6162 -0.1333 0.4365 0.083 Uiso 1 1 calc R . .
C49 C 0.5233(4) 0.1229(6) 0.3917(3) 0.0627(14) Uani 1 1 d . . .
C50 C 0.4935(5) 0.0900(9) 0.4630(3) 0.100(3) Uani 1 1 d . . .
H50A H 0.5228 0.1472 0.4949 0.150 Uiso 1 1 calc R . .
H50B H 0.5173 0.0100 0.4745 0.150 Uiso 1 1 calc R . .
H50C H 0.4218 0.0922 0.4638 0.150 Uiso 1 1 calc R . .
C51 C 0.4770(5) 0.0331(8) 0.3408(4) 0.087(2) Uani 1 1 d . . .
H51A H 0.5015 -0.0468 0.3516 0.131 Uiso 1 1 calc R . .
H51B H 0.4949 0.0549 0.2964 0.131 Uiso 1 1 calc R . .
H51C H 0.4054 0.0344 0.3420 0.131 Uiso 1 1 calc R . .
C52 C 0.4834(5) 0.2495(7) 0.3734(4) 0.082(2) Uani 1 1 d . . .
H52A H 0.5125 0.3075 0.4050 0.123 Uiso 1 1 calc R . .
H52B H 0.4117 0.2504 0.3748 0.123 Uiso 1 1 calc R . .
H52C H 0.5008 0.2702 0.3288 0.123 Uiso 1 1 calc R . .
C54 C 0.5700(4) 0.6879(5) 0.1801(3) 0.0556(12) Uani 1 1 d . . .
C55 C 0.5906(5) 0.6994(7) 0.1139(3) 0.0786(18) Uani 1 1 d . . .
H55 H 0.5603 0.6457 0.0826 0.094 Uiso 1 1 calc R . .
C56 C 0.6541(5) 0.7862(7) 0.0912(3) 0.0824(18) Uani 1 1 d . . .
H56 H 0.6683 0.7884 0.0461 0.099 Uiso 1 1 calc R . .
C57 C 0.6958(6) 0.8689(8) 0.1357(4) 0.097(2) Uani 1 1 d . . .
H57 H 0.7353 0.9315 0.1209 0.116 Uiso 1 1 calc R . .
C58 C 0.6787(9) 0.8585(10) 0.2014(4) 0.141(5) Uani 1 1 d . . .
H58 H 0.7096 0.9123 0.2324 0.169 Uiso 1 1 calc R . .
C59 C 0.6172(7) 0.7711(9) 0.2235(4) 0.112(3) Uani 1 1 d . . .
H59 H 0.6067 0.7672 0.2692 0.135 Uiso 1 1 calc R . .
C60 C 0.3876(4) 0.5335(5) 0.1352(2) 0.0556(12) Uani 1 1 d . . .
C61 C 0.3509(4) 0.4169(6) 0.1261(3) 0.0628(13) Uani 1 1 d . . .
H61 H 0.3775 0.3546 0.1533 0.075 Uiso 1 1 calc R . .
C62 C 0.2743(5) 0.3918(7) 0.0764(3) 0.0781(18) Uani 1 1 d . . .
H62 H 0.2490 0.3135 0.0722 0.094 Uiso 1 1 calc R . .
C63 C 0.2370(5) 0.4783(9) 0.0351(3) 0.087(2) Uani 1 1 d . . .
H63 H 0.1862 0.4600 0.0023 0.104 Uiso 1 1 calc R . .
C64 C 0.2736(5) 0.5942(10) 0.0410(4) 0.098(3) Uani 1 1 d . . .
H64 H 0.2497 0.6539 0.0110 0.117 Uiso 1 1 calc R . .
C65 C 0.3461(4) 0.6221(7) 0.0917(3) 0.0721(16) Uani 1 1 d . . .
H65 H 0.3676 0.7019 0.0970 0.086 Uiso 1 1 calc R . .
C66 C 0.4124(4) 0.6113(6) 0.2820(3) 0.0602(12) Uani 1 1 d . . .
C67 C 0.4825(6) 0.6182(9) 0.3472(3) 0.093(2) Uani 1 1 d . . .
H67A H 0.5332 0.6785 0.3419 0.140 Uiso 1 1 calc R . .
H67B H 0.5138 0.5409 0.3557 0.140 Uiso 1 1 calc R . .
H67C H 0.4442 0.6397 0.3845 0.140 Uiso 1 1 calc R . .
C68 C 0.3579(6) 0.7324(7) 0.2699(4) 0.086(2) Uani 1 1 d . . .
H68A H 0.4059 0.7945 0.2617 0.129 Uiso 1 1 calc R . .
H68B H 0.3232 0.7533 0.3089 0.129 Uiso 1 1 calc R . .
H68C H 0.3106 0.7253 0.2314 0.129 Uiso 1 1 calc R . .
C69 C 0.3345(5) 0.5135(7) 0.2949(4) 0.0780(18) Uani 1 1 d . . .
H69A H 0.3677 0.4371 0.3024 0.117 Uiso 1 1 calc R . .
H69B H 0.2872 0.5074 0.2564 0.117 Uiso 1 1 calc R . .
H69C H 0.2999 0.5349 0.3339 0.117 Uiso 1 1 calc R . .
N1 N 0.9414(3) 0.4470(4) 0.01427(18) 0.0442(8) Uani 1 1 d . . .
H1 H 0.9590 0.5028 -0.0127 0.053 Uiso 1 1 calc R . .
N2 N 0.8372(3) 0.5920(4) 0.0553(2) 0.0554(10) Uani 1 1 d . . .
H2A H 0.7923 0.6150 0.0815 0.066 Uiso 1 1 calc R . .
H2B H 0.8595 0.6420 0.0267 0.066 Uiso 1 1 calc R . .
N3 N 0.8381(2) 0.4016(3) 0.10317(18) 0.0399(8) Uani 1 1 d . . .
N7 N 0.9739(3) 0.1310(3) 0.06666(18) 0.0431(8) Uani 1 1 d . . .
N9 N 0.8624(3) 0.1915(3) 0.13836(17) 0.0389(7) Uani 1 1 d . . .
O6 O 1.0455(3) 0.3152(3) -0.03453(17) 0.0560(9) Uani 1 1 d . . .
O12 O 0.8893(2) 0.2448(3) 0.29749(14) 0.0427(7) Uani 1 1 d . . .
O14 O 0.6980(2) 0.1624(3) 0.31471(14) 0.0445(7) Uani 1 1 d . . .
O16 O 0.6954(2) 0.1976(3) 0.16570(14) 0.0428(7) Uani 1 1 d . . .
O18 O 0.5444(2) 0.4428(3) 0.22698(16) 0.0507(8) Uani 1 1 d . . .
Si19 Si 1.00696(8) 0.29418(12) 0.30001(6) 0.0422(3) Uani 1 1 d . . .
Si36 Si 0.66582(8) 0.12116(12) 0.38944(6) 0.0424(3) Uani 1 1 d . . .
Si53 Si 0.48162(9) 0.56809(12) 0.20646(6) 0.0448(3) Uani 1 1 d . . .
O70 O 0.464(2) 0.067(3) 0.0994(13) 0.397(12) Uiso 1 1 d D . .
C71 C 0.407(2) -0.015(3) 0.0489(14) 0.321(14) Uiso 1 1 d D . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C2 N3 1.324(5) . ?
C2 N2 1.342(6) . ?
C2 N1 1.369(5) . ?
C4 N3 1.353(6) . ?
C4 N9 1.370(5) . ?
C4 C5 1.378(5) . ?
C5 N7 1.388(6) . ?
C5 C6 1.424(6) . ?
C6 O6 1.235(5) . ?
C6 N1 1.372(6) . ?
C8 N7 1.319(5) . ?
C8 N9 1.361(5) . ?
C10 O16 1.413(5) . ?
C10 N9 1.458(5) . ?
C10 C11 1.524(6) . ?
C11 O12 1.411(5) . ?
C11 C13 1.528(5) . ?
C13 O14 1.402(5) . ?
C13 C15 1.535(5) . ?
C15 O16 1.453(5) . ?
C15 C17 1.504(6) . ?
C17 O18 1.410(5) . ?
C20 C25 1.392(8) . ?
C20 C21 1.417(8) . ?
C20 Si19 1.863(6) . ?
C21 C22 1.364(11) . ?
C22 C23 1.387(16) . ?
C23 C24 1.383(13) . ?
C24 C25 1.390(10) . ?
C26 C27 1.397(7) . ?
C26 C31 1.405(9) . ?
C26 Si19 1.868(5) . ?
C27 C28 1.381(11) . ?
C28 C29 1.372(13) . ?
C29 C30 1.373(13) . ?
C30 C31 1.371(9) . ?
C32 C34 1.512(9) . ?
C32 C33 1.528(7) . ?
C32 C35 1.537(9) . ?
C32 Si19 1.884(5) . ?
C37 C42 1.387(7) . ?
C37 C38 1.394(8) . ?
C37 Si36 1.874(5) . ?
C38 C39 1.366(9) . ?
C39 C41 1.378(10) . ?
C40 C41 1.351(10) . ?
C40 C42 1.372(9) . ?
C43 C48 1.392(7) . ?
C43 C44 1.401(7) . ?
C43 Si36 1.872(6) . ?
C44 C45 1.372(9) . ?
C45 C46 1.373(11) . ?
C46 C47 1.360(11) . ?
C47 C48 1.362(10) . ?
C49 C51 1.518(10) . ?
C49 C52 1.531(10) . ?
C49 C50 1.542(8) . ?
C49 Si36 1.909(5) . ?
C54 C55 1.371(8) . ?
C54 C59 1.381(9) . ?
C54 Si53 1.872(5) . ?
C55 C56 1.376(9) . ?
C56 C57 1.362(10) . ?
C57 C58 1.348(11) . ?
C58 C59 1.360(10) . ?
C60 C61 1.384(8) . ?
C60 C65 1.393(8) . ?
C60 Si53 1.866(5) . ?
C61 C62 1.399(8) . ?
C62 C63 1.333(11) . ?
C63 C64 1.372(12) . ?
C64 C65 1.383(9) . ?
C66 C68 1.532(9) . ?
C66 C69 1.533(9) . ?
C66 C67 1.547(9) . ?
C66 Si53 1.881(5) . ?
O12 Si19 1.662(3) . ?
O14 Si36 1.640(3) . ?
O18 Si53 1.653(4) . ?
O70 C71 1.513(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 C2 N2 119.9(4) . . ?
N3 C2 N1 123.4(4) . . ?
N2 C2 N1 116.7(4) . . ?
N3 C4 N9 127.0(3) . . ?
N3 C4 C5 127.9(4) . . ?
N9 C4 C5 105.1(4) . . ?
C4 C5 N7 111.1(4) . . ?
C4 C5 C6 119.2(4) . . ?
N7 C5 C6 129.6(4) . . ?
O6 C6 N1 121.6(4) . . ?
O6 C6 C5 127.3(4) . . ?
N1 C6 C5 111.0(3) . . ?
N7 C8 N9 113.0(4) . . ?
O16 C10 N9 108.9(3) . . ?
O16 C10 C11 105.3(3) . . ?
N9 C10 C11 115.6(3) . . ?
O12 C11 C10 114.1(3) . . ?
O12 C11 C13 112.5(3) . . ?
C10 C11 C13 100.9(3) . . ?
O14 C13 C11 109.6(3) . . ?
O14 C13 C15 109.1(3) . . ?
C11 C13 C15 100.3(3) . . ?
O16 C15 C17 109.7(3) . . ?
O16 C15 C13 105.3(3) . . ?
C17 C15 C13 114.5(4) . . ?
O18 C17 C15 108.4(4) . . ?
C25 C20 C21 117.3(6) . . ?
C25 C20 Si19 119.7(4) . . ?
C21 C20 Si19 122.7(5) . . ?
C22 C21 C20 120.7(8) . . ?
C21 C22 C23 120.9(8) . . ?
C22 C23 C24 119.8(8) . . ?
C23 C24 C25 119.4(8) . . ?
C24 C25 C20 121.7(6) . . ?
C27 C26 C31 116.3(5) . . ?
C27 C26 Si19 124.1(5) . . ?
C31 C26 Si19 119.2(4) . . ?
C28 C27 C26 121.8(7) . . ?
C29 C28 C27 119.4(7) . . ?
C30 C29 C28 121.0(7) . . ?
C29 C30 C31 119.2(8) . . ?
C30 C31 C26 122.1(7) . . ?
C34 C32 C33 110.9(5) . . ?
C34 C32 C35 107.3(5) . . ?
C33 C32 C35 108.1(6) . . ?
C34 C32 Si19 109.5(4) . . ?
C33 C32 Si19 109.6(4) . . ?
C35 C32 Si19 111.4(4) . . ?
C42 C37 C38 115.6(5) . . ?
C42 C37 Si36 120.3(4) . . ?
C38 C37 Si36 124.1(4) . . ?
C39 C38 C37 122.3(6) . . ?
C38 C39 C41 120.2(7) . . ?
C41 C40 C42 121.1(6) . . ?
C40 C41 C39 118.8(7) . . ?
C40 C42 C37 122.0(6) . . ?
C48 C43 C44 115.2(5) . . ?
C48 C43 Si36 127.1(4) . . ?
C44 C43 Si36 117.7(4) . . ?
C45 C44 C43 121.8(6) . . ?
C46 C45 C44 121.2(7) . . ?
C47 C46 C45 117.8(7) . . ?
C46 C47 C48 121.8(7) . . ?
C47 C48 C43 122.3(6) . . ?
C51 C49 C52 108.6(5) . . ?
C51 C49 C50 109.9(6) . . ?
C52 C49 C50 109.0(6) . . ?
C51 C49 Si36 109.7(4) . . ?
C52 C49 Si36 109.6(4) . . ?
C50 C49 Si36 110.0(4) . . ?
C55 C54 C59 115.1(5) . . ?
C55 C54 Si53 120.5(4) . . ?
C59 C54 Si53 124.4(4) . . ?
C54 C55 C56 123.3(6) . . ?
C57 C56 C55 119.2(6) . . ?
C58 C57 C56 118.9(7) . . ?
C59 C58 C57 121.4(8) . . ?
C58 C59 C54 122.0(7) . . ?
C61 C60 C65 116.7(5) . . ?
C61 C60 Si53 120.1(4) . . ?
C65 C60 Si53 123.0(5) . . ?
C60 C61 C62 120.7(6) . . ?
C63 C62 C61 121.1(7) . . ?
C62 C63 C64 119.9(6) . . ?
C63 C64 C65 119.8(7) . . ?
C64 C65 C60 121.6(7) . . ?
C68 C66 C69 108.6(5) . . ?
C68 C66 C67 110.0(6) . . ?
C69 C66 C67 105.9(5) . . ?
C68 C66 Si53 110.5(4) . . ?
C69 C66 Si53 109.4(4) . . ?
C67 C66 Si53 112.2(4) . . ?
C2 N1 C6 126.3(4) . . ?
C2 N3 C4 112.2(3) . . ?
C8 N7 C5 103.7(3) . . ?
C8 N9 C4 107.1(3) . . ?
C8 N9 C10 124.2(3) . . ?
C4 N9 C10 128.7(3) . . ?
C11 O12 Si19 127.3(3) . . ?
C13 O14 Si36 137.9(3) . . ?
C10 O16 C15 109.8(3) . . ?
C17 O18 Si53 123.1(3) . . ?
O12 Si19 C20 108.2(2) . . ?
O12 Si19 C26 108.24(19) . . ?
C20 Si19 C26 113.2(2) . . ?
O12 Si19 C32 105.89(18) . . ?
C20 Si19 C32 107.5(2) . . ?
C26 Si19 C32 113.4(2) . . ?
O14 Si36 C43 100.93(19) . . ?
O14 Si36 C37 113.2(2) . . ?
C43 Si36 C37 108.6(2) . . ?
O14 Si36 C49 110.2(2) . . ?
C43 Si36 C49 114.3(3) . . ?
C37 Si36 C49 109.4(2) . . ?
O18 Si53 C60 108.6(2) . . ?
O18 Si53 C54 109.9(2) . . ?
C60 Si53 C54 109.7(2) . . ?
O18 Si53 C66 106.6(2) . . ?
C60 Si53 C66 108.4(2) . . ?
C54 Si53 C66 113.6(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.44
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.056

#===END

#========================================================
data_1a+2EA
_database_code_depnum_ccdc_archive 'CCDC 225957'
#========================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
2',3',5'-O-tris(tert-buthyldiphenylsilyl)-guanosine
;
_chemical_name_common            
2',3',5'-O-tris(tert-buthyldiphenylsilyl)-guanosine
_chemical_melting_point          ?
_chemical_formula_moiety         'C66 H83 N5 O9 Si3'
_chemical_formula_sum            'C66 H83 N5 O9 Si3'
_chemical_formula_weight         1174.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   20.698(2)
_cell_length_b                   28.908(3)
_cell_length_c                   11.4650(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6859.9(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    20
_cell_measurement_theta_min      1.5
_cell_measurement_theta_max      30

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2512
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       theta/2theta
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5855
_diffrn_reflns_av_R_equivalents  0.067
_diffrn_reflns_av_sigmaI/netI    0.0826
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.63
_diffrn_reflns_theta_max         59.98
_reflns_number_total             5014
_reflns_number_gt                4652
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'MXC(MAC Science)'
_computing_cell_refinement       'MXC(MAC Science)'
_computing_data_reduction        Crystan
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    maXus
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0742P)²+11.0564P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00060(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(7)
_refine_ls_number_reflns         5014
_refine_ls_number_parameters     724
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0807
_refine_ls_wR_factor_ref         0.2047
_refine_ls_wR_factor_gt          0.1978
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_restrained_S_all      1.159
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si19 Si 0.37228(12) 0.19496(8) 0.2929(2) 0.0699(7) Uani 1 1 d . . .
Si37 Si 0.62135(11) 0.17988(8) 0.1911(2) 0.0615(6) Uani 1 1 d . . .
Si54 Si 0.60208(14) 0.03165(9) 0.6054(2) 0.0739(7) Uani 1 1 d . . .
O6 O 0.2074(3) -0.0188(2) 0.3469(5) 0.0760(18) Uani 1 1 d . . .
O12 O 0.4355(3) 0.16586(18) 0.2463(5) 0.0635(15) Uani 1 1 d . . .
O14 O 0.5608(2) 0.14319(19) 0.2015(5) 0.0625(14) Uani 1 1 d . . .
O16 O 0.4953(3) 0.05190(17) 0.2115(5) 0.0618(14) Uani 1 1 d . . .
O18 O 0.5955(3) 0.0532(2) 0.4727(5) 0.0684(15) Uani 1 1 d . . .
N1 N 0.2842(3) 0.0077(2) 0.4751(5) 0.0598(18) Uani 1 1 d . . .
H1 H 0.2621 -0.0032 0.5324 0.072 Uiso 1 1 calc R . .
N2 N 0.3543(4) 0.0331(3) 0.6171(5) 0.078(2) Uani 1 1 d . . .
H2 H 0.3886 0.0474 0.6394 0.094 Uiso 1 1 calc R . .
H3 H 0.3292 0.0206 0.6679 0.094 Uiso 1 1 calc R . .
N3 N 0.3778(3) 0.0491(2) 0.4258(5) 0.0555(16) Uani 1 1 d . . .
N7 N 0.2953(3) 0.0231(3) 0.1589(5) 0.0648(19) Uani 1 1 d . . .
N9 N 0.3841(3) 0.0612(2) 0.2143(5) 0.0532(15) Uani 1 1 d . . .
C2 C 0.3399(4) 0.0302(3) 0.5017(6) 0.059(2) Uani 1 1 d . . .
C4 C 0.3562(3) 0.0434(3) 0.3155(6) 0.0506(18) Uani 1 1 d . . .
C5 C 0.3010(4) 0.0208(3) 0.2790(7) 0.058(2) Uani 1 1 d . . .
C6 C 0.2595(4) 0.0007(3) 0.3630(7) 0.062(2) Uani 1 1 d . . .
C8 C 0.3457(4) 0.0465(3) 0.1256(6) 0.060(2) Uani 1 1 d . . .
H4 H 0.3546 0.0527 0.0476 0.072 Uiso 1 1 calc R . .
C10 C 0.4452(3) 0.0839(3) 0.2014(6) 0.0501(18) Uani 1 1 d . . .
H5 H 0.4470 0.0971 0.1227 0.060 Uiso 1 1 calc R . .
C11 C 0.4590(3) 0.1231(2) 0.2896(6) 0.0495(17) Uani 1 1 d . . .
H6 H 0.4393 0.1161 0.3653 0.059 Uiso 1 1 calc R . .
C13 C 0.5320(4) 0.1208(3) 0.2981(7) 0.0532(18) Uani 1 1 d . . .
H7 H 0.5477 0.1334 0.3723 0.064 Uiso 1 1 calc R . .
C15 C 0.5450(4) 0.0687(3) 0.2878(7) 0.0570(19) Uani 1 1 d . . .
H8 H 0.5875 0.0635 0.2523 0.068 Uiso 1 1 calc R . .
C17 C 0.5406(4) 0.0426(3) 0.4027(7) 0.066(2) Uani 1 1 d . . .
H9 H 0.5014 0.0514 0.4435 0.079 Uiso 1 1 calc R . .
H10 H 0.5390 0.0096 0.3879 0.079 Uiso 1 1 calc R . .
C20 C 0.2978(5) 0.1581(3) 0.3039(11) 0.085(3) Uani 1 1 d . . .
C21 C 0.2749(6) 0.1412(4) 0.4106(13) 0.108(4) Uani 1 1 d . . .
H11 H 0.2972 0.1472 0.4794 0.129 Uiso 1 1 calc R . .
C22 C 0.2199(9) 0.1161(6) 0.412(2) 0.158(8) Uani 1 1 d . . .
H12 H 0.2046 0.1063 0.4842 0.189 Uiso 1 1 calc R . .
C23 C 0.1862(8) 0.1044(6) 0.319(3) 0.173(11) Uani 1 1 d . . .
H13 H 0.1492 0.0864 0.3252 0.207 Uiso 1 1 calc R . .
C24 C 0.2069(9) 0.1190(6) 0.214(2) 0.157(8) Uani 1 1 d . . .
H14 H 0.1837 0.1117 0.1470 0.188 Uiso 1 1 calc R . .
C25 C 0.2638(6) 0.1457(4) 0.2061(15) 0.120(5) Uani 1 1 d . . .
H15 H 0.2786 0.1551 0.1332 0.145 Uiso 1 1 calc R . .
C26 C 0.3884(4) 0.2184(3) 0.4406(8) 0.071(2) Uani 1 1 d . . .
C27 C 0.4505(6) 0.2217(4) 0.4843(10) 0.091(3) Uani 1 1 d . . .
H16 H 0.4845 0.2096 0.4409 0.109 Uiso 1 1 calc R . .
C28 C 0.4636(8) 0.2421(5) 0.5892(12) 0.116(4) Uani 1 1 d . . .
H17 H 0.5059 0.2443 0.6157 0.139 Uiso 1 1 calc R . .
C29 C 0.4140(11) 0.2594(7) 0.6550(15) 0.159(7) Uani 1 1 d . . .
H18 H 0.4233 0.2739 0.7254 0.191 Uiso 1 1 calc R . .
C30 C 0.3522(10) 0.2557(6) 0.6204(15) 0.145(6) Uani 1 1 d . . .
H19 H 0.3184 0.2657 0.6675 0.174 Uiso 1 1 calc R . .
C31 C 0.3408(6) 0.2364(4) 0.5107(14) 0.115(4) Uani 1 1 d . . .
H20 H 0.2985 0.2356 0.4836 0.138 Uiso 1 1 calc R . .
C33 C 0.3665(6) 0.2443(3) 0.1845(10) 0.089(3) Uani 1 1 d . . .
C34 C 0.3056(7) 0.2728(5) 0.2130(15) 0.145(6) Uani 1 1 d . . .
H81 H 0.3075 0.2831 0.2926 0.218 Uiso 1 1 calc R . .
H82 H 0.2679 0.2540 0.2020 0.218 Uiso 1 1 calc R . .
H83 H 0.3035 0.2992 0.1622 0.218 Uiso 1 1 calc R . .
C35 C 0.3635(7) 0.2275(5) 0.0574(10) 0.128(5) Uani 1 1 d . . .
H84 H 0.3256 0.2089 0.0464 0.193 Uiso 1 1 calc R . .
H85 H 0.4012 0.2094 0.0403 0.193 Uiso 1 1 calc R . .
H86 H 0.3619 0.2537 0.0060 0.193 Uiso 1 1 calc R . .
C36 C 0.4268(7) 0.2733(4) 0.1974(14) 0.123(5) Uani 1 1 d . . .
H87 H 0.4301 0.2842 0.2762 0.185 Uiso 1 1 calc R . .
H88 H 0.4247 0.2992 0.1452 0.185 Uiso 1 1 calc R . .
H89 H 0.4640 0.2549 0.1789 0.185 Uiso 1 1 calc R . .
C38 C 0.6004(5) 0.2164(3) 0.0638(8) 0.072(3) Uani 1 1 d . . .
C39 C 0.5519(6) 0.2030(4) -0.0096(9) 0.107(4) Uani 1 1 d . . .
H30 H 0.5272 0.1774 0.0105 0.129 Uiso 1 1 calc R . .
C40 C 0.5380(9) 0.2256(5) -0.1106(12) 0.150(7) Uani 1 1 d . . .
H31 H 0.5067 0.2138 -0.1607 0.180 Uiso 1 1 calc R . .
C41 C 0.5703(8) 0.2662(5) -0.1394(12) 0.136(6) Uani 1 1 d . . .
H32 H 0.5590 0.2828 -0.2059 0.163 Uiso 1 1 calc R . .
C42 C 0.6185(9) 0.2812(4) -0.0686(12) 0.125(5) Uani 1 1 d . . .
H33 H 0.6414 0.3080 -0.0866 0.150 Uiso 1 1 calc R . .
C43 C 0.6334(6) 0.2559(4) 0.0317(10) 0.097(4) Uani 1 1 d . . .
H34 H 0.6670 0.2660 0.0789 0.117 Uiso 1 1 calc R . .
C44 C 0.6288(4) 0.2146(3) 0.3299(8) 0.070(2) Uani 1 1 d . . .
C45 C 0.6153(6) 0.2618(4) 0.3309(11) 0.105(4) Uani 1 1 d . . .
H35 H 0.6021 0.2762 0.2623 0.126 Uiso 1 1 calc R . .
C46 C 0.6209(8) 0.2875(5) 0.4306(14) 0.129(5) Uani 1 1 d . . .
H36 H 0.6103 0.3188 0.4295 0.155 Uiso 1 1 calc R . .
C47 C 0.6416(8) 0.2680(6) 0.5303(15) 0.127(5) Uani 1 1 d . . .
H37 H 0.6478 0.2860 0.5966 0.153 Uiso 1 1 calc R . .
C48 C 0.6538(7) 0.2208(6) 0.5337(12) 0.118(4) Uani 1 1 d . . .
H38 H 0.6658 0.2067 0.6033 0.142 Uiso 1 1 calc R . .
C49 C 0.6480(5) 0.1951(4) 0.4333(9) 0.087(3) Uani 1 1 d . . .
H39 H 0.6574 0.1636 0.4357 0.104 Uiso 1 1 calc R . .
C50 C 0.6976(5) 0.1476(4) 0.1560(10) 0.087(3) Uani 1 1 d . . .
C51 C 0.6856(7) 0.1179(5) 0.0459(13) 0.138(6) Uani 1 1 d . . .
H90 H 0.6517 0.0961 0.0611 0.207 Uiso 1 1 calc R . .
H91 H 0.7245 0.1015 0.0259 0.207 Uiso 1 1 calc R . .
H92 H 0.6733 0.1376 -0.0178 0.207 Uiso 1 1 calc R . .
C52 C 0.7523(5) 0.1824(5) 0.1302(13) 0.130(5) Uani 1 1 d . . .
H93 H 0.7389 0.2031 0.0693 0.195 Uiso 1 1 calc R . .
H94 H 0.7903 0.1660 0.1059 0.195 Uiso 1 1 calc R . .
H95 H 0.7617 0.1998 0.1994 0.195 Uiso 1 1 calc R . .
C53 C 0.7226(6) 0.1152(5) 0.2547(12) 0.120(4) Uani 1 1 d . . .
H96 H 0.6898 0.0930 0.2740 0.180 Uiso 1 1 calc R . .
H97 H 0.7328 0.1333 0.3225 0.180 Uiso 1 1 calc R . .
H98 H 0.7607 0.0993 0.2286 0.180 Uiso 1 1 calc R . .
C55 C 0.5426(5) 0.0601(3) 0.6998(8) 0.079(3) Uani 1 1 d . . .
C56 C 0.5070(5) 0.0999(3) 0.6618(10) 0.083(3) Uani 1 1 d . . .
H49 H 0.5136 0.1115 0.5870 0.099 Uiso 1 1 calc R . .
C57 C 0.4632(6) 0.1212(4) 0.7348(12) 0.101(4) Uani 1 1 d . . .
H50 H 0.4411 0.1471 0.7075 0.121 Uiso 1 1 calc R . .
C58 C 0.4507(8) 0.1062(5) 0.8446(13) 0.124(5) Uani 1 1 d . . .
H51 H 0.4182 0.1194 0.8899 0.149 Uiso 1 1 calc R . .
C59 C 0.4883(10) 0.0707(6) 0.8857(14) 0.165(7) Uani 1 1 d . . .
H52 H 0.4856 0.0627 0.9642 0.198 Uiso 1 1 calc R . .
C60 C 0.5297(8) 0.0466(4) 0.8154(11) 0.130(5) Uani 1 1 d . . .
H53 H 0.5500 0.0204 0.8449 0.156 Uiso 1 1 calc R . .
C61 C 0.5871(6) -0.0321(4) 0.5959(10) 0.092(3) Uani 1 1 d . . .
C62 C 0.5429(9) -0.0534(7) 0.6588(18) 0.169(7) Uiso 1 1 d . . .
H54 H 0.5217 -0.0364 0.7160 0.203 Uiso 1 1 calc R . .
C63 C 0.5244(12) -0.1039(8) 0.644(2) 0.195(8) Uiso 1 1 d . . .
H55 H 0.4902 -0.1179 0.6829 0.234 Uiso 1 1 calc R . .
C64 C 0.5616(10) -0.1253(8) 0.5705(19) 0.170(8) Uiso 1 1 d . . .
H56 H 0.5587 -0.1574 0.5684 0.204 Uiso 1 1 calc R . .
C65 C 0.6019(8) -0.1062(5) 0.5005(18) 0.158(8) Uani 1 1 d . . .
H57 H 0.6220 -0.1231 0.4419 0.189 Uiso 1 1 calc R . .
C66 C 0.6146(6) -0.0593(4) 0.5151(13) 0.117(4) Uani 1 1 d . . .
H58 H 0.6445 -0.0457 0.4650 0.141 Uiso 1 1 calc R . .
C67 C 0.6862(6) 0.0452(4) 0.6531(10) 0.092(3) Uani 1 1 d . . .
C68 C 0.6943(7) 0.0971(5) 0.6670(14) 0.131(5) Uani 1 1 d . . .
H99 H 0.6631 0.1085 0.7218 0.196 Uiso 1 1 calc R . .
H100 H 0.6879 0.1119 0.5929 0.196 Uiso 1 1 calc R . .
H101 H 0.7370 0.1037 0.6950 0.196 Uiso 1 1 calc R . .
C69 C 0.7361(6) 0.0273(6) 0.5663(14) 0.140(5) Uani 1 1 d . . .
H102 H 0.7315 -0.0055 0.5579 0.210 Uiso 1 1 calc R . .
H103 H 0.7787 0.0344 0.5942 0.210 Uiso 1 1 calc R . .
H104 H 0.7295 0.0420 0.4921 0.210 Uiso 1 1 calc R . .
C70 C 0.7010(8) 0.0222(6) 0.7742(12) 0.151(6) Uani 1 1 d . . .
H105 H 0.6969 -0.0108 0.7676 0.226 Uiso 1 1 calc R . .
H106 H 0.6709 0.0334 0.8313 0.226 Uiso 1 1 calc R . .
H107 H 0.7442 0.0298 0.7979 0.226 Uiso 1 1 calc R . .
C71 C 0.268(2) 0.147(2) 0.745(4) 0.26(3) Uiso 0.62(3) 1 d PD A 1
C72 C 0.2189(18) 0.133(2) 0.833(3) 0.23(2) Uiso 0.62(3) 1 d PD A 1
O19 O 0.231(2) 0.1357(16) 0.935(3) 0.33(2) Uiso 0.62(3) 1 d PD A 1
O20 O 0.1634(13) 0.1124(10) 0.798(3) 0.198(12) Uiso 0.62(3) 1 d PD A 1
C73 C 0.1096(19) 0.1131(14) 0.870(4) 0.25(2) Uiso 0.62(3) 1 d PD A 1
C74 C 0.0724(19) 0.0696(14) 0.876(4) 0.24(2) Uiso 0.62(3) 1 d PD A 1
C75 C 0.0338(16) 0.1151(11) 0.432(3) 0.224(16) Uiso 0.70(2) 1 d PD B 2
C76 C 0.0201(17) 0.0674(13) 0.477(5) 0.34(3) Uiso 0.70(2) 1 d PD B 2
O21 O 0.0596(15) 0.0445(11) 0.529(3) 0.325(19) Uiso 0.70(2) 1 d PD B 2
O22 O -0.0440(15) 0.0698(12) 0.504(4) 0.325(18) Uiso 0.70(2) 1 d PD B 2
C77 C -0.063(2) 0.1159(15) 0.521(7) 0.35(3) Uiso 0.70(2) 1 d PD B 2
C78 C -0.135(2) 0.115(2) 0.494(8) 0.43(5) Uiso 0.70(2) 1 d PD B 2
C79 C 0.2690(19) 0.136(2) 0.787(5) 0.144(18) Uiso 0.38(3) 1 d PD A 3
C80 C 0.198(2) 0.124(2) 0.807(4) 0.141(17) Uiso 0.38(3) 1 d PD A 3
O23 O 0.180(3) 0.116(2) 0.906(4) 0.29(3) Uiso 0.38(3) 1 d PD A 3
O24 O 0.169(2) 0.105(2) 0.713(4) 0.29(3) Uiso 0.38(3) 1 d PD A 3
C81 C 0.109(3) 0.084(2) 0.725(7) 0.30(5) Uiso 0.38(3) 1 d PD A 3
C82 C 0.060(2) 0.112(3) 0.796(8) 0.26(4) Uiso 0.38(3) 1 d PD A 3
C83 C -0.072(4) 0.0260(17) 0.602(9) 0.40(9) Uiso 0.30(2) 1 d PD B 4
C84 C -0.046(3) 0.0749(19) 0.617(7) 0.51(14) Uiso 0.30(2) 1 d PD B 4
O25 O 0.000(2) 0.0894(19) 0.562(5) 0.22(2) Uiso 0.30(2) 1 d PD B 4
O26 O -0.099(2) 0.1015(19) 0.636(4) 0.22(3) Uiso 0.30(2) 1 d PD B 4
C85 C -0.111(4) 0.134(2) 0.547(6) 0.21(4) Uiso 0.30(2) 1 d PD B 4
C86 C -0.107(3) 0.112(3) 0.425(5) 0.24(4) Uiso 0.30(2) 1 d PD B 4


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si19 O12 1.645(6) . ?
Si19 C26 1.854(10) . ?
Si19 C20 1.878(10) . ?
Si19 C33 1.896(10) . ?
Si37 O14 1.646(5) . ?
Si37 C38 1.852(10) . ?
Si37 C50 1.877(11) . ?
Si37 C44 1.887(10) . ?
Si54 O18 1.650(6) . ?
Si54 C55 1.834(10) . ?
Si54 C67 1.867(12) . ?
Si54 C61 1.871(11) . ?
O6 C6 1.230(10) . ?
O12 C11 1.417(9) . ?
O14 C13 1.414(9) . ?
O16 C10 1.395(9) . ?
O16 C15 1.434(9) . ?
O18 C17 1.425(10) . ?
N1 C2 1.359(9) . ?
N1 C6 1.398(10) . ?
N2 C2 1.359(10) . ?
N3 C2 1.292(9) . ?
N3 C4 1.351(9) . ?
N7 C8 1.299(10) . ?
N7 C5 1.384(10) . ?
N9 C8 1.360(9) . ?
N9 C4 1.394(9) . ?
N9 C10 1.431(8) . ?
C4 C5 1.381(10) . ?
C5 C6 1.416(11) . ?
C10 C11 1.547(10) . ?
C11 C13 1.515(10) . ?
C13 C15 1.537(11) . ?
C15 C17 1.520(11) . ?
C20 C25 1.370(17) . ?
C20 C21 1.400(16) . ?
C21 C22 1.35(2) . ?
C22 C23 1.32(3) . ?
C23 C24 1.34(3) . ?
C24 C25 1.41(2) . ?
C26 C31 1.373(15) . ?
C26 C27 1.382(14) . ?
C27 C28 1.368(16) . ?
C28 C29 1.37(2) . ?
C29 C30 1.34(2) . ?
C30 C31 1.40(2) . ?
C33 C36 1.512(15) . ?
C33 C35 1.538(17) . ?
C33 C34 1.540(16) . ?
C38 C39 1.366(14) . ?
C38 C43 1.379(13) . ?
C39 C40 1.360(16) . ?
C40 C41 1.392(18) . ?
C41 C42 1.358(19) . ?
C42 C43 1.399(17) . ?
C44 C49 1.372(13) . ?
C44 C45 1.394(14) . ?
C45 C46 1.369(16) . ?
C46 C47 1.34(2) . ?
C47 C48 1.39(2) . ?
C48 C49 1.375(16) . ?
C50 C52 1.544(14) . ?
C50 C51 1.547(16) . ?
C50 C53 1.558(16) . ?
C55 C60 1.406(15) . ?
C55 C56 1.436(13) . ?
C56 C57 1.380(14) . ?
C57 C58 1.356(18) . ?
C58 C59 1.37(2) . ?
C59 C60 1.367(18) . ?
C61 C62 1.32(2) . ?
C61 C66 1.342(15) . ?
C62 C63 1.52(3) . ?
C63 C64 1.30(3) . ?
C64 C65 1.28(2) . ?
C65 C66 1.391(19) . ?
C67 C68 1.519(16) . ?
C67 C69 1.523(17) . ?
C67 C70 1.570(16) . ?
C71 C72 1.489(19) . ?
C72 O19 1.203(19) . ?
C72 O20 1.349(19) . ?
O20 C73 1.386(19) . ?
C73 C74 1.48(2) . ?
C75 C76 1.50(2) . ?
C76 O21 1.21(2) . ?
C76 O22 1.36(2) . ?
O22 C77 1.40(2) . ?
C77 C78 1.52(2) . ?
C79 C80 1.52(2) . ?
C80 O23 1.22(2) . ?
C80 O24 1.34(2) . ?
O24 C81 1.40(2) . ?
C81 C82 1.52(2) . ?
C83 C84 1.52(2) . ?
C84 O25 1.22(2) . ?
C84 O26 1.36(2) . ?
O26 C85 1.40(2) . ?
C85 C86 1.53(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O12 Si19 C26 109.9(4) . . ?
O12 Si19 C20 112.6(4) . . ?
C26 Si19 C20 107.1(5) . . ?
O12 Si19 C33 102.8(4) . . ?
C26 Si19 C33 109.6(5) . . ?
C20 Si19 C33 114.7(5) . . ?
O14 Si37 C38 104.3(4) . . ?
O14 Si37 C50 109.6(4) . . ?
C38 Si37 C50 108.1(5) . . ?
O14 Si37 C44 110.1(3) . . ?
C38 Si37 C44 112.4(4) . . ?
C50 Si37 C44 112.1(5) . . ?
O18 Si54 C55 108.7(4) . . ?
O18 Si54 C67 105.5(4) . . ?
C55 Si54 C67 111.1(5) . . ?
O18 Si54 C61 107.7(4) . . ?
C55 Si54 C61 111.3(5) . . ?
C67 Si54 C61 112.2(5) . . ?
C11 O12 Si19 127.2(5) . . ?
C13 O14 Si37 132.3(5) . . ?
C10 O16 C15 111.1(5) . . ?
C17 O18 Si54 120.3(5) . . ?
C2 N1 C6 125.9(7) . . ?
C2 N3 C4 112.3(6) . . ?
C8 N7 C5 104.5(7) . . ?
C8 N9 C4 105.3(6) . . ?
C8 N9 C10 125.6(6) . . ?
C4 N9 C10 128.4(6) . . ?
N3 C2 N1 124.5(7) . . ?
N3 C2 N2 119.8(7) . . ?
N1 C2 N2 115.7(7) . . ?
N3 C4 C5 127.9(7) . . ?
N3 C4 N9 126.6(6) . . ?
C5 C4 N9 105.4(6) . . ?
C4 C5 N7 110.4(7) . . ?
C4 C5 C6 119.4(7) . . ?
N7 C5 C6 130.2(7) . . ?
O6 C6 N1 121.7(7) . . ?
O6 C6 C5 128.2(8) . . ?
N1 C6 C5 110.1(7) . . ?
N7 C8 N9 114.3(7) . . ?
O16 C10 N9 110.2(6) . . ?
O16 C10 C11 107.1(5) . . ?
N9 C10 C11 115.5(6) . . ?
O12 C11 C13 113.8(6) . . ?
O12 C11 C10 110.3(6) . . ?
C13 C11 C10 101.2(6) . . ?
O14 C13 C11 110.5(6) . . ?
O14 C13 C15 108.3(6) . . ?
C11 C13 C15 102.3(6) . . ?
O16 C15 C17 108.5(6) . . ?
O16 C15 C13 104.6(6) . . ?
C17 C15 C13 114.2(7) . . ?
O18 C17 C15 109.5(6) . . ?
C25 C20 C21 116.8(10) . . ?
C25 C20 Si19 121.0(10) . . ?
C21 C20 Si19 122.2(9) . . ?
C22 C21 C20 118.9(16) . . ?
C23 C22 C21 125(2) . . ?
C22 C23 C24 118.4(18) . . ?
C23 C24 C25 119.7(19) . . ?
C20 C25 C24 121.2(16) . . ?
C31 C26 C27 115.4(10) . . ?
C31 C26 Si19 122.9(9) . . ?
C27 C26 Si19 121.5(8) . . ?
C28 C27 C26 122.1(12) . . ?
C29 C28 C27 119.6(15) . . ?
C30 C29 C28 121.5(15) . . ?
C29 C30 C31 117.3(15) . . ?
C26 C31 C30 123.9(13) . . ?
C36 C33 C35 107.5(12) . . ?
C36 C33 C34 111.0(10) . . ?
C35 C33 C34 109.8(11) . . ?
C36 C33 Si19 107.5(8) . . ?
C35 C33 Si19 112.7(8) . . ?
C34 C33 Si19 108.4(9) . . ?
C39 C38 C43 115.7(10) . . ?
C39 C38 Si37 119.8(7) . . ?
C43 C38 Si37 124.5(8) . . ?
C40 C39 C38 123.0(11) . . ?
C39 C40 C41 120.4(13) . . ?
C42 C41 C40 118.7(12) . . ?
C41 C42 C43 119.0(12) . . ?
C38 C43 C42 123.0(12) . . ?
C49 C44 C45 117.0(10) . . ?
C49 C44 Si37 122.3(7) . . ?
C45 C44 Si37 120.7(8) . . ?
C46 C45 C44 121.4(13) . . ?
C47 C46 C45 120.6(14) . . ?
C46 C47 C48 119.6(14) . . ?
C49 C48 C47 119.5(14) . . ?
C44 C49 C48 121.8(11) . . ?
C52 C50 C51 108.9(11) . . ?
C52 C50 C53 106.7(10) . . ?
C51 C50 C53 108.2(10) . . ?
C52 C50 Si37 109.5(8) . . ?
C51 C50 Si37 108.5(8) . . ?
C53 C50 Si37 115.0(8) . . ?
C60 C55 C56 114.3(10) . . ?
C60 C55 Si54 124.0(9) . . ?
C56 C55 Si54 121.6(7) . . ?
C57 C56 C55 120.7(10) . . ?
C58 C57 C56 123.1(13) . . ?
C57 C58 C59 116.8(13) . . ?
C60 C59 C58 122.3(14) . . ?
C59 C60 C55 122.2(13) . . ?
C62 C61 C66 113.5(14) . . ?
C62 C61 Si54 122.9(12) . . ?
C66 C61 Si54 123.1(10) . . ?
C61 C62 C63 124(2) . . ?
C64 C63 C62 112(2) . . ?
C65 C64 C63 126(2) . . ?
C64 C65 C66 117.9(18) . . ?
C61 C66 C65 125.0(16) . . ?
C68 C67 C69 109.2(12) . . ?
C68 C67 C70 107.7(11) . . ?
C69 C67 C70 107.7(11) . . ?
C68 C67 Si54 109.9(9) . . ?
C69 C67 Si54 111.8(8) . . ?
C70 C67 Si54 110.6(9) . . ?
O19 C72 O20 120(3) . . ?
O19 C72 C71 120(3) . . ?
O20 C72 C71 120(3) . . ?
C72 O20 C73 120(3) . . ?
O20 C73 C74 116(3) . . ?
O21 C76 O22 125(4) . . ?
O21 C76 C75 123(3) . . ?
O22 C76 C75 102(2) . . ?
C76 O22 C77 110(3) . . ?
O22 C77 C78 103(3) . . ?
O23 C80 O24 122(3) . . ?
O23 C80 C79 119(3) . . ?
O24 C80 C79 114(3) . . ?
C80 O24 C81 120(3) . . ?
O24 C81 C82 114(3) . . ?
O25 C84 O26 121(4) . . ?
O25 C84 C83 123(4) . . ?
O26 C84 C83 105(3) . . ?
C84 O26 C85 114(3) . . ?
O26 C85 C86 113(3) . . ?

_diffrn_measured_fraction_theta_max 0.887
_diffrn_reflns_theta_full        59.98
_diffrn_measured_fraction_theta_full 0.887
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.056

#===END

#========================================================
data_1b
_database_code_depnum_ccdc_archive 'CCDC 225958'
#========================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
2',3',5'-O-tris(triisopropylsilyl)-guanosine
;
_chemical_name_common            2',3',5'-O-tris(triisopropylsilyl)-guanosine
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H73 N5 O5 Si3'
_chemical_formula_sum            'C37 H73 N5 O5 Si3'
_chemical_formula_weight         752.27

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   9.8080(5)
_cell_length_b                   10.9010(4)
_cell_length_c                   21.4960(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.211(2)
_cell_angle_gamma                90.00
_cell_volume                     2288.79(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    19180
_cell_measurement_theta_min      4.13
_cell_measurement_theta_max      73.19

_exptl_crystal_description       plate-like
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             824
_exptl_absorpt_coefficient_mu    1.282
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.5670
_exptl_absorpt_correction_T_max  0.8572
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'MacScience DIPLabo'
_diffrn_measurement_method       IP
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19180
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_av_sigmaI/netI    0.0143
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         4.13
_diffrn_reflns_theta_max         73.19
_reflns_number_total             5625
_reflns_number_gt                5202
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'MacScience Xpress'
_computing_cell_refinement       Scalepack
_computing_data_reduction        'Denzo and Scalepack'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    maXus
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.41(9)
_refine_ls_number_reflns         5625
_refine_ls_number_parameters     463
_refine_ls_number_restraints     377
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.1089
_refine_ls_wR_factor_ref         0.3936
_refine_ls_wR_factor_gt          0.3720
_refine_ls_goodness_of_fit_ref   1.981
_refine_ls_restrained_S_all      1.970
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N -0.9400(5) -0.4264(4) -0.0245(2) 0.0740(10) Uani 1 1 d . . .
H1 H -0.9700 -0.4865 -0.0020 0.089 Uiso 1 1 calc R . .
C2 C -0.8751(6) -0.4565(5) -0.0756(2) 0.0760(11) Uani 1 1 d . . .
N2 N -0.8583(6) -0.5770(4) -0.0870(2) 0.0837(11) Uani 1 1 d . . .
H2 H -0.8136 -0.6003 -0.1187 0.100 Uiso 1 1 calc R . .
H3 H -0.8920 -0.6323 -0.0628 0.100 Uiso 1 1 calc R . .
N3 N -0.8236(5) -0.3757(4) -0.1126(2) 0.0734(10) Uani 1 1 d . . .
C4 C -0.8451(5) -0.2579(5) -0.0961(2) 0.0698(10) Uani 1 1 d . . .
C5 C -0.9098(5) -0.2194(4) -0.0437(2) 0.0679(10) Uani 1 1 d . . .
C6 C -0.9621(5) -0.3072(5) -0.0055(2) 0.0705(10) Uani 1 1 d . . .
O6 O -1.0236(4) -0.2890(4) 0.04266(16) 0.0801(9) Uani 1 1 d . . .
N7 N -0.9137(5) -0.0922(4) -0.04298(19) 0.0715(9) Uani 1 1 d . . .
C8 C -0.8570(5) -0.0565(5) -0.0918(2) 0.0719(10) Uani 1 1 d . . .
H4 H -0.8481 0.0272 -0.1031 0.086 Uiso 1 1 calc R . .
N9 N -0.8106(4) -0.1528(4) -0.12591(17) 0.0677(8) Uani 1 1 d . . .
C10 C -0.7579(5) -0.1419(6) -0.1866(2) 0.0763(12) Uani 1 1 d . A .
H5 H -0.7300 -0.0549 -0.1929 0.092 Uiso 1 1 calc R . .
C11 C -0.6409(6) -0.2245(6) -0.1986(3) 0.0824(13) Uani 1 1 d D . .
H6 H -0.6509 -0.3053 -0.1775 0.099 Uiso 0.56(2) 1 calc PR A 1
H7 H -0.6614 -0.3060 -0.1802 0.099 Uiso 0.44(2) 1 calc PR A 2
C12 C -0.6565(9) -0.2406(9) -0.2674(3) 0.105(2) Uani 1 1 d . A .
H8 H -0.6091 -0.3157 -0.2812 0.126 Uiso 1 1 calc R . .
C13 C -0.8150(9) -0.2506(9) -0.2781(3) 0.106(2) Uani 1 1 d D . .
H9 H -0.8431 -0.2142 -0.3200 0.128 Uiso 0.513(13) 1 calc PR A 5
H10 H -0.8478 -0.2225 -0.3212 0.128 Uiso 0.487(13) 1 calc PR A 6
O12 O -0.8656(5) -0.1729(5) -0.23311(17) 0.0945(13) Uani 1 1 d . A .
O11 O -0.5147(12) -0.1654(13) -0.1741(5) 0.082(3) Uani 0.56(2) 1 d PD A 1
Si1 Si -0.3921(8) -0.2355(6) -0.1304(4) 0.0855(16) Uani 0.56(2) 1 d PD A 1
C15 C -0.4593(12) -0.2942(11) -0.0593(6) 0.085(3) Uiso 0.56(2) 1 d PD A 1
H11 H -0.5355 -0.3515 -0.0735 0.103 Uiso 0.56(2) 1 calc PR A 1
C16 C -0.3603(14) -0.3682(13) -0.0138(7) 0.097(4) Uiso 0.56(2) 1 d PD A 1
H12 H -0.3214 -0.4360 -0.0363 0.145 Uiso 0.56(2) 1 calc PR A 1
H13 H -0.4102 -0.4010 0.0200 0.145 Uiso 0.56(2) 1 calc PR A 1
H14 H -0.2865 -0.3145 0.0038 0.145 Uiso 0.56(2) 1 calc PR A 1
C17 C -0.5204(19) -0.2003(15) -0.0177(7) 0.105(5) Uiso 0.56(2) 1 d PD A 1
H15 H -0.5853 -0.1483 -0.0431 0.158 Uiso 0.56(2) 1 calc PR A 1
H16 H -0.4472 -0.1493 0.0027 0.158 Uiso 0.56(2) 1 calc PR A 1
H17 H -0.5683 -0.2427 0.0141 0.158 Uiso 0.56(2) 1 calc PR A 1
C18 C -0.3246(13) -0.3659(12) -0.1757(7) 0.108(4) Uiso 0.56(2) 1 d PD A 1
H18 H -0.3151 -0.3333 -0.2185 0.129 Uiso 0.56(2) 1 calc PR A 1
C19 C -0.4175(18) -0.4748(16) -0.1842(10) 0.123(5) Uiso 0.56(2) 1 d PD A 1
H19 H -0.5096 -0.4476 -0.1998 0.185 Uiso 0.56(2) 1 calc PR A 1
H20 H -0.4215 -0.5166 -0.1440 0.185 Uiso 0.56(2) 1 calc PR A 1
H21 H -0.3823 -0.5315 -0.2143 0.185 Uiso 0.56(2) 1 calc PR A 1
C20 C -0.1807(14) -0.4073(16) -0.1501(8) 0.109(4) Uiso 0.56(2) 1 d PD A 1
H22 H -0.1169 -0.3384 -0.1514 0.164 Uiso 0.56(2) 1 calc PR A 1
H23 H -0.1507 -0.4748 -0.1756 0.164 Uiso 0.56(2) 1 calc PR A 1
H24 H -0.1828 -0.4351 -0.1068 0.164 Uiso 0.56(2) 1 calc PR A 1
C21 C -0.2636(11) -0.1119(11) -0.1119(5) 0.090(4) Uiso 0.56(2) 1 d PD A 1
H25 H -0.1936 -0.1439 -0.0792 0.108 Uiso 0.56(2) 1 calc PR A 1
C22 C -0.3218(14) 0.0063(11) -0.0874(7) 0.096(4) Uiso 0.56(2) 1 d PD A 1
H26 H -0.3657 -0.0111 -0.0492 0.144 Uiso 0.56(2) 1 calc PR A 1
H27 H -0.3895 0.0405 -0.1190 0.144 Uiso 0.56(2) 1 calc PR A 1
H28 H -0.2476 0.0656 -0.0782 0.144 Uiso 0.56(2) 1 calc PR A 1
C23 C -0.1896(17) -0.079(2) -0.1700(7) 0.112(4) Uiso 0.56(2) 1 d PD A 1
H29 H -0.1547 -0.1539 -0.1881 0.168 Uiso 0.56(2) 1 calc PR A 1
H30 H -0.1131 -0.0235 -0.1579 0.168 Uiso 0.56(2) 1 calc PR A 1
H31 H -0.2540 -0.0384 -0.2010 0.168 Uiso 0.56(2) 1 calc PR A 1
O110 O -0.5152(14) -0.188(2) -0.1696(9) 0.104(7) Uani 0.44(2) 1 d PD A 2
Si10 Si -0.4034(12) -0.2489(11) -0.1159(6) 0.100(3) Uani 0.44(2) 1 d PD A 2
C150 C -0.4760(13) -0.2800(12) -0.0412(7) 0.076(3) Uiso 0.44(2) 1 d PD A 2
H32 H -0.5508 -0.3409 -0.0517 0.091 Uiso 0.44(2) 1 calc PR A 2
C160 C -0.380(2) -0.342(2) 0.0099(9) 0.106(5) Uiso 0.44(2) 1 d PD A 2
H33 H -0.3302 -0.4092 -0.0086 0.158 Uiso 0.44(2) 1 calc PR A 2
H34 H -0.4338 -0.3756 0.0422 0.158 Uiso 0.44(2) 1 calc PR A 2
H35 H -0.3143 -0.2821 0.0287 0.158 Uiso 0.44(2) 1 calc PR A 2
C170 C -0.543(2) -0.1774(17) -0.0103(8) 0.090(4) Uiso 0.44(2) 1 d PD A 2
H36 H -0.6073 -0.1359 -0.0408 0.135 Uiso 0.44(2) 1 calc PR A 2
H37 H -0.4730 -0.1190 0.0065 0.135 Uiso 0.44(2) 1 calc PR A 2
H38 H -0.5922 -0.2097 0.0238 0.135 Uiso 0.44(2) 1 calc PR A 2
C180 C -0.3386(18) -0.3946(17) -0.1527(11) 0.120(6) Uiso 0.44(2) 1 d PD A 2
H39 H -0.3244 -0.3746 -0.1971 0.144 Uiso 0.44(2) 1 calc PR A 2
C190 C -0.438(2) -0.4999(19) -0.1539(11) 0.115(6) Uiso 0.44(2) 1 d PD A 2
H40 H -0.5266 -0.4739 -0.1744 0.172 Uiso 0.44(2) 1 calc PR A 2
H41 H -0.4494 -0.5259 -0.1111 0.172 Uiso 0.44(2) 1 calc PR A 2
H42 H -0.4026 -0.5686 -0.1771 0.172 Uiso 0.44(2) 1 calc PR A 2
C200 C -0.2030(17) -0.442(3) -0.1220(13) 0.151(10) Uiso 0.44(2) 1 d PD A 2
H43 H -0.1353 -0.3760 -0.1193 0.227 Uiso 0.44(2) 1 calc PR A 2
H44 H -0.1704 -0.5097 -0.1470 0.227 Uiso 0.44(2) 1 calc PR A 2
H45 H -0.2159 -0.4722 -0.0799 0.227 Uiso 0.44(2) 1 calc PR A 2
C210 C -0.265(2) -0.129(2) -0.1120(12) 0.161(18) Uiso 0.44(2) 1 d PD A 2
H46 H -0.2006 -0.1454 -0.0739 0.193 Uiso 0.44(2) 1 calc PR A 2
C232 C -0.313(3) 0.004(2) -0.1098(14) 0.121(7) Uiso 0.44(2) 1 d PD A 2
H47 H -0.3752 0.0135 -0.0770 0.182 Uiso 0.44(2) 1 calc PR A 2
H48 H -0.3609 0.0265 -0.1503 0.182 Uiso 0.44(2) 1 calc PR A 2
H49 H -0.2336 0.0582 -0.1010 0.182 Uiso 0.44(2) 1 calc PR A 2
C230 C -0.181(3) -0.132(3) -0.1696(12) 0.134(8) Uiso 0.44(2) 1 d PD A 2
H50 H -0.1410 -0.2139 -0.1735 0.201 Uiso 0.44(2) 1 calc PR A 2
H51 H -0.1083 -0.0708 -0.1647 0.201 Uiso 0.44(2) 1 calc PR A 2
H52 H -0.2419 -0.1141 -0.2073 0.201 Uiso 0.44(2) 1 calc PR A 2
O13 O -0.6113(8) -0.1331(8) -0.2950(2) 0.124(2) Uani 1 1 d . . .
Si2 Si -0.5218(10) -0.1048(10) -0.3538(3) 0.154(3) Uani 0.696(14) 1 d PD A 3
C24 C -0.364(2) -0.196(3) -0.3465(14) 0.222(13) Uiso 0.696(14) 1 d PD A 3
H53 H -0.3349 -0.1929 -0.3008 0.267 Uiso 0.696(14) 1 calc PR A 3
C25 C -0.369(6) -0.334(3) -0.361(5) 0.47(6) Uiso 0.696(14) 1 d PD A 3
H301 H -0.4432 -0.3718 -0.3397 0.707 Uiso 0.696(14) 1 calc PR A 3
H302 H -0.2816 -0.3714 -0.3451 0.707 Uiso 0.696(14) 1 calc PR A 3
H303 H -0.3851 -0.3466 -0.4057 0.707 Uiso 0.696(14) 1 calc PR A 3
C26 C -0.241(4) -0.150(5) -0.376(4) 0.46(5) Uiso 0.696(14) 1 d PD A 3
H304 H -0.2321 -0.0617 -0.3689 0.695 Uiso 0.696(14) 1 calc PR A 3
H305 H -0.2523 -0.1670 -0.4208 0.695 Uiso 0.696(14) 1 calc PR A 3
H306 H -0.1593 -0.1921 -0.3570 0.695 Uiso 0.696(14) 1 calc PR A 3
C27 C -0.648(3) -0.149(3) -0.4221(10) 0.206(12) Uiso 0.696(14) 1 d PD A 3
H60 H -0.6769 -0.2354 -0.4141 0.247 Uiso 0.696(14) 1 calc PR A 3
C28 C -0.775(4) -0.073(6) -0.429(2) 0.34(3) Uiso 0.696(14) 1 d PD A 3
H307 H -0.8177 -0.0744 -0.3892 0.513 Uiso 0.696(14) 1 calc PR A 3
H308 H -0.8388 -0.1073 -0.4619 0.513 Uiso 0.696(14) 1 calc PR A 3
H309 H -0.7518 0.0111 -0.4390 0.513 Uiso 0.696(14) 1 calc PR A 3
C29 C -0.583(5) -0.151(7) -0.4849(14) 0.34(3) Uiso 0.696(14) 1 d PD A 3
H310 H -0.5006 -0.2020 -0.4809 0.516 Uiso 0.696(14) 1 calc PR A 3
H311 H -0.5596 -0.0675 -0.4963 0.516 Uiso 0.696(14) 1 calc PR A 3
H312 H -0.6492 -0.1855 -0.5173 0.516 Uiso 0.696(14) 1 calc PR A 3
C30 C -0.497(2) 0.0652(15) -0.3497(7) 0.142(5) Uiso 0.696(14) 1 d PD A 3
H300 H -0.5917 0.1009 -0.3538 0.171 Uiso 0.696(14) 1 calc PR A 3
C31 C -0.422(5) 0.127(3) -0.4002(16) 0.33(3) Uiso 0.696(14) 1 d PD A 3
H313 H -0.4607 0.0980 -0.4414 0.488 Uiso 0.696(14) 1 calc PR A 3
H314 H -0.3249 0.1057 -0.3943 0.488 Uiso 0.696(14) 1 calc PR A 3
H315 H -0.4332 0.2158 -0.3976 0.488 Uiso 0.696(14) 1 calc PR A 3
C32 C -0.431(4) 0.110(3) -0.2864(12) 0.223(15) Uiso 0.696(14) 1 d PD A 3
H316 H -0.4814 0.0781 -0.2528 0.335 Uiso 0.696(14) 1 calc PR A 3
H317 H -0.4321 0.2002 -0.2855 0.335 Uiso 0.696(14) 1 calc PR A 3
H318 H -0.3356 0.0816 -0.2807 0.335 Uiso 0.696(14) 1 calc PR A 3
Si20 Si -0.5747(15) -0.1125(15) -0.3689(5) 0.119(4) Uani 0.304(14) 1 d PD A 4
C240 C -0.416(3) -0.031(3) -0.3434(16) 0.135(11) Uiso 0.304(14) 1 d PD A 4
H74 H -0.3992 0.0121 -0.3830 0.162 Uiso 0.304(14) 1 calc PR A 4
C250 C -0.277(4) -0.091(5) -0.328(5) 0.30(5) Uiso 0.304(14) 1 d PD A 4
H319 H -0.2685 -0.1620 -0.3551 0.449 Uiso 0.304(14) 1 calc PR A 4
H320 H -0.2685 -0.1173 -0.2842 0.449 Uiso 0.304(14) 1 calc PR A 4
H321 H -0.2048 -0.0315 -0.3346 0.449 Uiso 0.304(14) 1 calc PR A 4
C260 C -0.424(5) 0.076(4) -0.301(2) 0.154(15) Uiso 0.304(14) 1 d PD A 4
H322 H -0.5066 0.1241 -0.3134 0.231 Uiso 0.304(14) 1 calc PR A 4
H323 H -0.3431 0.1281 -0.3028 0.231 Uiso 0.304(14) 1 calc PR A 4
H324 H -0.4281 0.0472 -0.2577 0.231 Uiso 0.304(14) 1 calc PR A 4
C270 C -0.699(3) -0.002(3) -0.4143(16) 0.176(19) Uiso 0.304(14) 1 d PD A 4
H81 H -0.6727 0.0821 -0.3993 0.212 Uiso 0.304(14) 1 calc PR A 4
C280 C -0.690(6) -0.002(5) -0.4833(18) 0.44(12) Uiso 0.304(14) 1 d PD A 4
H325 H -0.5941 0.0105 -0.4919 0.660 Uiso 0.304(14) 1 calc PR A 4
H326 H -0.7461 0.0648 -0.5023 0.660 Uiso 0.304(14) 1 calc PR A 4
H327 H -0.7225 -0.0804 -0.5009 0.660 Uiso 0.304(14) 1 calc PR A 4
C290 C -0.848(3) -0.021(4) -0.4007(17) 0.134(11) Uiso 0.304(14) 1 d PD A 4
H328 H -0.8547 -0.0184 -0.3555 0.201 Uiso 0.304(14) 1 calc PR A 4
H329 H -0.8813 -0.1000 -0.4173 0.201 Uiso 0.304(14) 1 calc PR A 4
H330 H -0.9049 0.0452 -0.4207 0.201 Uiso 0.304(14) 1 calc PR A 4
C300 C -0.552(3) -0.249(2) -0.4209(14) 0.146(12) Uiso 0.304(14) 1 d PD A 4
H88 H -0.5135 -0.2215 -0.4601 0.175 Uiso 0.304(14) 1 calc PR A 4
C310 C -0.464(4) -0.354(3) -0.3917(14) 0.19(2) Uiso 0.304(14) 1 d PD A 4
H331 H -0.3715 -0.3248 -0.3797 0.291 Uiso 0.304(14) 1 calc PR A 4
H332 H -0.4611 -0.4210 -0.4222 0.291 Uiso 0.304(14) 1 calc PR A 4
H333 H -0.5051 -0.3848 -0.3547 0.291 Uiso 0.304(14) 1 calc PR A 4
C320 C -0.694(3) -0.309(3) -0.4370(16) 0.132(10) Uiso 0.304(14) 1 d PD A 4
H334 H -0.7569 -0.2476 -0.4565 0.199 Uiso 0.304(14) 1 calc PR A 4
H335 H -0.7287 -0.3395 -0.3987 0.199 Uiso 0.304(14) 1 calc PR A 4
H336 H -0.6848 -0.3771 -0.4661 0.199 Uiso 0.304(14) 1 calc PR A 4
C14 C -0.877(3) -0.3733(17) -0.2770(13) 0.133(11) Uiso 0.513(13) 1 d PD A 5
H95 H -0.8677 -0.4020 -0.2331 0.159 Uiso 0.513(13) 1 calc PR A 5
H96 H -0.9758 -0.3643 -0.2896 0.159 Uiso 0.513(13) 1 calc PR A 5
O14 O -0.8259(12) -0.4688(11) -0.3145(5) 0.101(3) Uiso 0.513(13) 1 d PD A 5
Si3 Si -0.8973(11) -0.5986(8) -0.3358(3) 0.126(3) Uani 0.513(13) 1 d PD A 5
C33 C -1.0700(19) -0.572(3) -0.3731(12) 0.173(11) Uiso 0.513(13) 1 d PD A 5
H111 H -1.0894 -0.6453 -0.4007 0.207 Uiso 0.513(13) 1 calc PR A 5
C34 C -1.192(4) -0.564(9) -0.334(3) 0.39(7) Uiso 0.513(13) 1 d PD A 5
H337 H -1.1897 -0.6334 -0.3046 0.589 Uiso 0.513(13) 1 calc PR A 5
H338 H -1.2775 -0.5675 -0.3615 0.589 Uiso 0.513(13) 1 calc PR A 5
H339 H -1.1882 -0.4871 -0.3105 0.589 Uiso 0.513(13) 1 calc PR A 5
C35 C -1.084(3) -0.463(3) -0.4167(12) 0.164(9) Uiso 0.513(13) 1 d PD A 5
H340 H -1.0099 -0.4644 -0.4443 0.245 Uiso 0.513(13) 1 calc PR A 5
H341 H -1.0790 -0.3873 -0.3921 0.245 Uiso 0.513(13) 1 calc PR A 5
H342 H -1.1725 -0.4671 -0.4418 0.245 Uiso 0.513(13) 1 calc PR A 5
C36 C -0.899(2) -0.6978(17) -0.2629(7) 0.129(6) Uiso 0.513(13) 1 d PD A 5
H97 H -0.9631 -0.6589 -0.2349 0.155 Uiso 0.513(13) 1 calc PR A 5
C37 C -0.761(2) -0.708(2) -0.2271(10) 0.129(6) Uiso 0.513(13) 1 d PD A 5
H343 H -0.7263 -0.6258 -0.2164 0.193 Uiso 0.513(13) 1 calc PR A 5
H344 H -0.6982 -0.7501 -0.2527 0.193 Uiso 0.513(13) 1 calc PR A 5
H345 H -0.7694 -0.7549 -0.1887 0.193 Uiso 0.513(13) 1 calc PR A 5
C38 C -0.953(3) -0.827(2) -0.2795(13) 0.165(10) Uiso 0.513(13) 1 d PD A 5
H346 H -1.0436 -0.8211 -0.3028 0.248 Uiso 0.513(13) 1 calc PR A 5
H347 H -0.9607 -0.8741 -0.2410 0.248 Uiso 0.513(13) 1 calc PR A 5
H348 H -0.8899 -0.8688 -0.3052 0.248 Uiso 0.513(13) 1 calc PR A 5
C39 C -0.773(2) -0.661(3) -0.3891(10) 0.173(10) Uiso 0.513(13) 1 d PD A 5
H104 H -0.7146 -0.7235 -0.3647 0.208 Uiso 0.513(13) 1 calc PR A 5
C40 C -0.676(4) -0.567(4) -0.414(2) 0.25(2) Uiso 0.513(13) 1 d PD A 5
H349 H -0.6258 -0.5242 -0.3792 0.378 Uiso 0.513(13) 1 calc PR A 5
H350 H -0.7290 -0.5080 -0.4407 0.378 Uiso 0.513(13) 1 calc PR A 5
H351 H -0.6106 -0.6093 -0.4389 0.378 Uiso 0.513(13) 1 calc PR A 5
C41 C -0.840(5) -0.726(5) -0.4474(17) 0.25(2) Uiso 0.513(13) 1 d PD A 5
H352 H -0.9062 -0.7867 -0.4350 0.375 Uiso 0.513(13) 1 calc PR A 5
H353 H -0.7691 -0.7682 -0.4690 0.375 Uiso 0.513(13) 1 calc PR A 5
H354 H -0.8864 -0.6658 -0.4755 0.375 Uiso 0.513(13) 1 calc PR A 5
C140 C -0.8648(18) -0.3866(12) -0.2670(7) 0.084(4) Uiso 0.487(13) 1 d PD A 6
H118 H -0.8023 -0.4311 -0.2360 0.101 Uiso 0.487(13) 1 calc PR A 6
H119 H -0.9594 -0.3894 -0.2544 0.101 Uiso 0.487(13) 1 calc PR A 6
O140 O -0.8566(17) -0.4295(14) -0.3279(6) 0.122(4) Uiso 0.487(13) 1 d PD A 6
Si30 Si -0.8774(15) -0.5743(14) -0.3443(7) 0.229(10) Uani 0.487(13) 1 d PD A 6
C330 C -0.910(4) -0.592(3) -0.4297(10) 0.26(3) Uiso 0.487(13) 1 d PD A 6
H140 H -1.0036 -0.5564 -0.4389 0.306 Uiso 0.487(13) 1 calc PR A 6
C340 C -0.824(7) -0.519(5) -0.4723(18) 0.30(3) Uiso 0.487(13) 1 d PD A 6
H355 H -0.8089 -0.4360 -0.4555 0.448 Uiso 0.487(13) 1 calc PR A 6
H356 H -0.8716 -0.5143 -0.5142 0.448 Uiso 0.487(13) 1 calc PR A 6
H357 H -0.7352 -0.5598 -0.4744 0.448 Uiso 0.487(13) 1 calc PR A 6
C350 C -0.925(5) -0.719(4) -0.4566(17) 0.23(2) Uiso 0.487(13) 1 d PD A 6
H373 H -0.8395 -0.7425 -0.4740 0.350 Uiso 0.487(13) 1 calc PR A 6
H374 H -1.0002 -0.7202 -0.4898 0.350 Uiso 0.487(13) 1 calc PR A 6
H375 H -0.9440 -0.7768 -0.4237 0.350 Uiso 0.487(13) 1 calc PR A 6
C360 C -0.718(2) -0.663(3) -0.3141(11) 0.182(12) Uiso 0.487(13) 1 d PD A 6
H120 H -0.7294 -0.7478 -0.3309 0.218 Uiso 0.487(13) 1 calc PR A 6
C370 C -0.586(3) -0.616(6) -0.3341(19) 0.25(2) Uiso 0.487(13) 1 d PD A 6
H361 H -0.5916 -0.6119 -0.3798 0.370 Uiso 0.487(13) 1 calc PR A 6
H362 H -0.5117 -0.6711 -0.3189 0.370 Uiso 0.487(13) 1 calc PR A 6
H363 H -0.5682 -0.5336 -0.3168 0.370 Uiso 0.487(13) 1 calc PR A 6
C380 C -0.708(4) -0.673(3) -0.2426(11) 0.182(13) Uiso 0.487(13) 1 d PD A 6
H364 H -0.7945 -0.7044 -0.2295 0.273 Uiso 0.487(13) 1 calc PR A 6
H365 H -0.6884 -0.5925 -0.2239 0.273 Uiso 0.487(13) 1 calc PR A 6
H366 H -0.6337 -0.7302 -0.2287 0.273 Uiso 0.487(13) 1 calc PR A 6
C390 C -1.026(2) -0.628(3) -0.3024(14) 0.215(17) Uiso 0.487(13) 1 d PD A 6
H133 H -1.0095 -0.6041 -0.2575 0.259 Uiso 0.487(13) 1 calc PR A 6
C400 C -1.055(5) -0.766(3) -0.306(3) 0.34(4) Uiso 0.487(13) 1 d PD A 6
H376 H -0.9778 -0.8111 -0.2844 0.506 Uiso 0.487(13) 1 calc PR A 6
H377 H -1.0677 -0.7921 -0.3496 0.506 Uiso 0.487(13) 1 calc PR A 6
H378 H -1.1384 -0.7842 -0.2855 0.506 Uiso 0.487(13) 1 calc PR A 6
C410 C -1.163(2) -0.572(3) -0.3295(12) 0.144(8) Uiso 0.487(13) 1 d PD A 6
H370 H -1.1553 -0.4822 -0.3297 0.216 Uiso 0.487(13) 1 calc PR A 6
H371 H -1.2359 -0.5961 -0.3037 0.216 Uiso 0.487(13) 1 calc PR A 6
H372 H -1.1851 -0.6013 -0.3723 0.216 Uiso 0.487(13) 1 calc PR A 6


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C2 1.359(7) . ?
N1 C6 1.385(6) . ?
C2 N3 1.318(7) . ?
C2 N2 1.349(7) . ?
N3 C4 1.353(6) . ?
C4 N9 1.371(7) . ?
C4 C5 1.405(6) . ?
C5 N7 1.387(6) . ?
C5 C6 1.389(7) . ?
C6 O6 1.261(6) . ?
N7 C8 1.292(7) . ?
C8 N9 1.381(7) . ?
N9 C10 1.450(6) . ?
C10 O12 1.428(6) . ?
C10 C11 1.499(8) . ?
C11 O110 1.390(18) . ?
C11 O11 1.451(12) . ?
C11 C12 1.484(10) . ?
C12 O13 1.403(12) . ?
C12 C13 1.555(12) . ?
C13 O12 1.409(9) . ?
C13 C14 1.469(17) . ?
C13 C140 1.585(14) . ?
O11 Si1 1.645(9) . ?
Si1 C15 1.835(11) . ?
Si1 C21 1.862(10) . ?
Si1 C18 1.877(10) . ?
C15 C17 1.517(13) . ?
C15 C16 1.542(11) . ?
C18 C19 1.498(14) . ?
C18 C20 1.535(13) . ?
C21 C22 1.523(12) . ?
C21 C23 1.543(11) . ?
O110 Si10 1.658(13) . ?
Si10 C150 1.846(14) . ?
Si10 C210 1.880(16) . ?
Si10 C180 1.909(14) . ?
C150 C170 1.483(16) . ?
C150 C160 1.540(15) . ?
C180 C190 1.505(18) . ?
C180 C200 1.523(17) . ?
C210 C232 1.535(19) . ?
C210 C230 1.546(18) . ?
O13 Si2 1.634(9) . ?
O13 Si20 1.675(11) . ?
Si2 C24 1.832(17) . ?
Si2 C30 1.869(15) . ?
Si2 C27 1.894(16) . ?
C24 C26 1.497(19) . ?
C24 C25 1.53(2) . ?
C27 C28 1.49(2) . ?
C27 C29 1.540(19) . ?
C30 C31 1.52(2) . ?
C30 C32 1.536(18) . ?
Si20 C240 1.832(17) . ?
Si20 C300 1.889(17) . ?
Si20 C270 1.915(17) . ?
C240 C260 1.496(19) . ?
C240 C250 1.517(19) . ?
C270 C280 1.49(2) . ?
C270 C290 1.53(2) . ?
C300 C310 1.53(2) . ?
C300 C320 1.547(19) . ?
C14 O14 1.433(17) . ?
O14 Si3 1.625(11) . ?
Si3 C33 1.829(16) . ?
Si3 C39 1.880(16) . ?
Si3 C36 1.906(14) . ?
C33 C35 1.514(19) . ?
C33 C34 1.53(2) . ?
C36 C37 1.499(18) . ?
C36 C38 1.537(18) . ?
C39 C40 1.53(2) . ?
C39 C41 1.534(19) . ?
C140 O140 1.400(15) . ?
O140 Si30 1.626(13) . ?
Si30 C330 1.846(17) . ?
Si30 C390 1.875(17) . ?
Si30 C360 1.899(16) . ?
C330 C350 1.500(15) . ?
C330 C340 1.525(19) . ?
C360 C370 1.49(2) . ?
C360 C380 1.536(19) . ?
C390 C400 1.53(2) . ?
C390 C410 1.545(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N1 C6 124.2(5) . . ?
N3 C2 N2 118.7(5) . . ?
N3 C2 N1 124.0(5) . . ?
N2 C2 N1 117.2(5) . . ?
C2 N3 C4 113.5(4) . . ?
N3 C4 N9 128.3(4) . . ?
N3 C4 C5 125.9(5) . . ?
N9 C4 C5 105.9(4) . . ?
N7 C5 C6 132.0(5) . . ?
N7 C5 C4 108.9(4) . . ?
C6 C5 C4 119.0(4) . . ?
O6 C6 N1 119.2(4) . . ?
O6 C6 C5 127.4(5) . . ?
N1 C6 C5 113.4(4) . . ?
C8 N7 C5 106.1(4) . . ?
N7 C8 N9 112.9(5) . . ?
C4 N9 C8 106.3(4) . . ?
C4 N9 C10 127.7(4) . . ?
C8 N9 C10 125.2(4) . . ?
O12 C10 N9 108.0(4) . . ?
O12 C10 C11 105.4(4) . . ?
N9 C10 C11 116.5(5) . . ?
O110 C11 O11 10.3(11) . . ?
O110 C11 C12 119.2(10) . . ?
O11 C11 C12 114.9(7) . . ?
O110 C11 C10 114.3(10) . . ?
O11 C11 C10 108.2(7) . . ?
C12 C11 C10 103.4(5) . . ?
O13 C12 C11 108.3(7) . . ?
O13 C12 C13 110.2(7) . . ?
C11 C12 C13 99.6(5) . . ?
O12 C13 C14 111.4(10) . . ?
O12 C13 C12 105.4(5) . . ?
C14 C13 C12 118.0(14) . . ?
O12 C13 C140 109.0(7) . . ?
C14 C13 C140 9.4(16) . . ?
C12 C13 C140 111.1(9) . . ?
C13 O12 C10 109.8(5) . . ?
C11 O11 Si1 123.7(10) . . ?
O11 Si1 C15 109.8(7) . . ?
O11 Si1 C21 103.4(6) . . ?
C15 Si1 C21 111.2(6) . . ?
O11 Si1 C18 109.2(7) . . ?
C15 Si1 C18 109.7(7) . . ?
C21 Si1 C18 113.2(6) . . ?
C17 C15 C16 103.9(10) . . ?
C17 C15 Si1 116.5(8) . . ?
C16 C15 Si1 117.3(9) . . ?
C19 C18 C20 109.9(12) . . ?
C19 C18 Si1 115.1(10) . . ?
C20 C18 Si1 113.1(9) . . ?
C22 C21 C23 107.5(11) . . ?
C22 C21 Si1 114.7(8) . . ?
C23 C21 Si1 110.8(9) . . ?
C11 O110 Si10 134.4(16) . . ?
O110 Si10 C150 113.3(9) . . ?
O110 Si10 C210 100.5(11) . . ?
C150 Si10 C210 115.0(10) . . ?
O110 Si10 C180 105.6(10) . . ?
C150 Si10 C180 112.2(9) . . ?
C210 Si10 C180 109.1(9) . . ?
C170 C150 C160 106.3(13) . . ?
C170 C150 Si10 118.2(10) . . ?
C160 C150 Si10 116.2(11) . . ?
C190 C180 C200 106.6(16) . . ?
C190 C180 Si10 113.7(13) . . ?
C200 C180 Si10 114.5(13) . . ?
C232 C210 C230 103.3(18) . . ?
C232 C210 Si10 115.8(16) . . ?
C230 C210 Si10 112.5(16) . . ?
C12 O13 Si2 134.3(7) . . ?
C12 O13 Si20 128.0(8) . . ?
Si2 O13 Si20 20.6(5) . . ?
O13 Si2 C24 109.8(11) . . ?
O13 Si2 C30 103.1(8) . . ?
C24 Si2 C30 115.6(11) . . ?
O13 Si2 C27 101.2(10) . . ?
C24 Si2 C27 114.3(12) . . ?
C30 Si2 C27 111.3(10) . . ?
C26 C24 C25 105(2) . . ?
C26 C24 Si2 119.1(19) . . ?
C25 C24 Si2 120(2) . . ?
C28 C27 C29 109(2) . . ?
C28 C27 Si2 114(2) . . ?
C29 C27 Si2 113.2(18) . . ?
C31 C30 C32 107.2(19) . . ?
C31 C30 Si2 118.1(17) . . ?
C32 C30 Si2 113.7(17) . . ?
O13 Si20 C240 91.8(14) . . ?
O13 Si20 C300 120.2(14) . . ?
C240 Si20 C300 114.5(12) . . ?
O13 Si20 C270 112.7(12) . . ?
C240 Si20 C270 109.5(14) . . ?
C300 Si20 C270 107.4(13) . . ?
C260 C240 C250 107(2) . . ?
C260 C240 Si20 118(2) . . ?
C250 C240 Si20 125(2) . . ?
C280 C270 C290 110(2) . . ?
C280 C270 Si20 115(2) . . ?
C290 C270 Si20 113.4(19) . . ?
C310 C300 C320 104(2) . . ?
C310 C300 Si20 116.2(17) . . ?
C320 C300 Si20 108.1(17) . . ?
O14 C14 C13 119.2(16) . . ?
C14 O14 Si3 128.8(12) . . ?
O14 Si3 C33 110.2(10) . . ?
O14 Si3 C39 101.6(10) . . ?
C33 Si3 C39 114.6(11) . . ?
O14 Si3 C36 107.4(7) . . ?
C33 Si3 C36 111.8(10) . . ?
C39 Si3 C36 110.5(11) . . ?
C35 C33 C34 105(2) . . ?
C35 C33 Si3 115.0(16) . . ?
C34 C33 Si3 121(2) . . ?
C37 C36 C38 109.1(17) . . ?
C37 C36 Si3 112.8(13) . . ?
C38 C36 Si3 111.0(13) . . ?
C40 C39 C41 105(2) . . ?
C40 C39 Si3 115.4(19) . . ?
C41 C39 Si3 114(2) . . ?
O140 C140 C13 97.3(11) . . ?
C140 O140 Si30 120.7(12) . . ?
O140 Si30 C330 108.9(13) . . ?
O140 Si30 C390 106.7(13) . . ?
C330 Si30 C390 111.9(13) . . ?
O140 Si30 C360 109.5(12) . . ?
C330 Si30 C360 110.5(13) . . ?
C390 Si30 C360 109.2(12) . . ?
C350 C330 C340 107(2) . . ?
C350 C330 Si30 119(2) . . ?
C340 C330 Si30 119(2) . . ?
C370 C360 C380 110(2) . . ?
C370 C360 Si30 116(2) . . ?
C380 C360 Si30 111.0(15) . . ?
C400 C390 C410 103(2) . . ?
C400 C390 Si30 115.8(19) . . ?
C410 C390 Si30 112.5(16) . . ?

_diffrn_measured_fraction_theta_max 0.863
_diffrn_reflns_theta_full        73.19
_diffrn_measured_fraction_theta_full 0.863
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.076

#===END

#========================================================
data_3c
_database_code_depnum_ccdc_archive 'CCDC 225959'
#========================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
2'-deoxy-3',5'-O-bis(tert-butyldimethylsilyl)-guanosine
;
_chemical_name_common            
2'-deoxy-3',5'-O-bis(tert-butyldimethylsilyl)-guanosine
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H41 N5 O4 Si2'
_chemical_formula_sum            'C22 H41 N5 O4 Si2'
_chemical_formula_weight         495.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   31.5910(6)
_cell_length_b                   10.8750(2)
_cell_length_c                   17.0050(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.0920(10)
_cell_angle_gamma                90.00
_cell_volume                     5732.97(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    25256
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      73.14

_exptl_crystal_description       plate-like
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.82
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2144
_exptl_absorpt_coefficient_mu    1.399
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.5458
_exptl_absorpt_correction_T_max  0.8022
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'MacScience DIPLabo'
_diffrn_measurement_method       IP
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25256
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.65
_diffrn_reflns_theta_max         73.14
_reflns_number_total             10061
_reflns_number_gt                9874
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'MacScience Xpress'
_computing_cell_refinement       Scalepack
_computing_data_reduction        'Denzo and Scalepack'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    maXus
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
We assumed that a disorder at disorder group3 and group4 take place
not independently but with the disorder group sets, 3-4* and 3*-4.
We fixed occupancy of these parts to be 0.5.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1544P)²+3.9891P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0026(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.22(4)
_refine_ls_number_reflns         10061
_refine_ls_number_parameters     652
_refine_ls_number_restraints     571
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0768
_refine_ls_wR_factor_ref         0.2138
_refine_ls_wR_factor_gt          0.2123
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.74829(10) -0.4958(3) 0.45084(15) 0.0451(6) Uani 1 1 d . . .
H1 H 0.7363 -0.5519 0.4767 0.054 Uiso 1 1 calc R . .
C1 C 0.75853(12) -0.5292(3) 0.37954(18) 0.0448(7) Uani 1 1 d . . .
N2 N 0.74819(13) -0.6434(3) 0.35422(16) 0.0577(8) Uani 1 1 d . . .
H2 H 0.7536 -0.6685 0.3080 0.069 Uiso 1 1 calc R . .
H3 H 0.7360 -0.6936 0.3838 0.069 Uiso 1 1 calc R . .
N3 N 0.77696(10) -0.4544(2) 0.33439(15) 0.0443(6) Uani 1 1 d . . .
C2 C 0.78465(11) -0.3416(3) 0.36884(18) 0.0423(6) Uani 1 1 d . . .
C3 C 0.77381(11) -0.2985(3) 0.43769(18) 0.0426(6) Uani 1 1 d . . .
C4 C 0.75531(11) -0.3806(3) 0.48600(17) 0.0439(7) Uani 1 1 d . . .
O1 O 0.74470(10) -0.3608(2) 0.55136(13) 0.0574(6) Uani 1 1 d . . .
N4 N 0.78693(10) -0.1772(2) 0.45207(16) 0.0474(6) Uani 1 1 d . . .
C5 C 0.80582(12) -0.1507(3) 0.3924(2) 0.0513(8) Uani 1 1 d . . .
H4 H 0.8185 -0.0730 0.3862 0.062 Uiso 1 1 calc R . .
N5 N 0.80561(9) -0.2468(2) 0.33891(16) 0.0465(6) Uani 1 1 d . . .
C6 C 0.83224(11) -0.2577(3) 0.2786(2) 0.0512(7) Uani 1 1 d . A .
H5 H 0.8268 -0.3393 0.2513 0.061 Uiso 1 1 calc R . .
C7 C 0.82666(13) -0.1567(4) 0.2156(2) 0.0571(8) Uani 1 1 d . A .
H6 H 0.8040 -0.1781 0.1688 0.068 Uiso 1 1 calc R . .
H7 H 0.8194 -0.0771 0.2380 0.068 Uiso 1 1 calc R . .
C8 C 0.87089(16) -0.1531(4) 0.1936(3) 0.0696(11) Uani 1 1 d D . .
H8 H 0.8774 -0.0730 0.1696 0.083 Uiso 0.485(12) 1 calc PR A 1
H9 H 0.8769 -0.0693 0.1742 0.083 Uiso 0.515(12) 1 calc PR A 2
C9 C 0.90043(15) -0.1807(4) 0.2718(3) 0.0752(12) Uani 1 1 d D A .
H10 H 0.9245 -0.2335 0.2605 0.090 Uiso 0.50 1 calc PR B 3
H11 H 0.9242 -0.2341 0.2602 0.090 Uiso 0.50 1 calc PR B 4
O2 O 0.87567(9) -0.2519(3) 0.3187(2) 0.0736(8) Uani 1 1 d . . .
O3 O 0.8814(3) -0.2573(5) 0.1500(4) 0.0651(18) Uiso 0.485(12) 1 d PD A 1
Si1 Si 0.8990(3) -0.2279(8) 0.0663(5) 0.081(2) Uani 0.485(12) 1 d PD A 1
C10 C 0.8556(5) -0.1527(17) -0.0098(10) 0.131(6) Uiso 0.485(12) 1 d PD A 1
H12 H 0.8480 -0.0731 0.0108 0.197 Uiso 0.485(12) 1 calc PR A 1
H13 H 0.8300 -0.2057 -0.0200 0.197 Uiso 0.485(12) 1 calc PR A 1
H14 H 0.8661 -0.1401 -0.0598 0.197 Uiso 0.485(12) 1 calc PR A 1
C11 C 0.9454(4) -0.1150(13) 0.0894(8) 0.082(3) Uiso 0.485(12) 1 d PD A 1
H15 H 0.9348 -0.0363 0.1059 0.123 Uiso 0.485(12) 1 calc PR A 1
H16 H 0.9578 -0.1028 0.0415 0.123 Uiso 0.485(12) 1 calc PR A 1
H17 H 0.9675 -0.1476 0.1329 0.123 Uiso 0.485(12) 1 calc PR A 1
C12 C 0.9157(3) -0.3780(9) 0.0326(6) 0.093(4) Uiso 0.485(12) 1 d PD A 1
C13 C 0.8775(5) -0.4664(15) 0.0260(13) 0.136(6) Uiso 0.485(12) 1 d PD A 1
H18 H 0.8530 -0.4338 -0.0125 0.204 Uiso 0.485(12) 1 calc PR A 1
H19 H 0.8695 -0.4751 0.0786 0.204 Uiso 0.485(12) 1 calc PR A 1
H20 H 0.8857 -0.5469 0.0077 0.204 Uiso 0.485(12) 1 calc PR A 1
C14 C 0.9534(4) -0.4286(15) 0.0930(9) 0.122(5) Uiso 0.485(12) 1 d PD A 1
H21 H 0.9779 -0.3722 0.0976 0.183 Uiso 0.485(12) 1 calc PR A 1
H22 H 0.9615 -0.5093 0.0750 0.183 Uiso 0.485(12) 1 calc PR A 1
H23 H 0.9450 -0.4369 0.1453 0.183 Uiso 0.485(12) 1 calc PR A 1
C15 C 0.9287(6) -0.3644(19) -0.0491(8) 0.141(7) Uiso 0.485(12) 1 d PD A 1
H24 H 0.9044 -0.3310 -0.0878 0.211 Uiso 0.485(12) 1 calc PR A 1
H25 H 0.9366 -0.4451 -0.0675 0.211 Uiso 0.485(12) 1 calc PR A 1
H26 H 0.9534 -0.3085 -0.0444 0.211 Uiso 0.485(12) 1 calc PR A 1
O4 O 0.8678(2) -0.2415(5) 0.1296(3) 0.0499(14) Uiso 0.515(12) 1 d PD A 2
Si2 Si 0.9001(2) -0.2602(9) 0.0654(4) 0.0707(15) Uani 0.515(12) 1 d PD A 2
C16 C 0.8669(4) -0.2188(12) -0.0344(6) 0.091(3) Uiso 0.515(12) 1 d PD A 2
H27 H 0.8587 -0.1319 -0.0344 0.136 Uiso 0.515(12) 1 calc PR A 2
H28 H 0.8408 -0.2697 -0.0449 0.136 Uiso 0.515(12) 1 calc PR A 2
H29 H 0.8837 -0.2331 -0.0763 0.136 Uiso 0.515(12) 1 calc PR A 2
C17 C 0.9492(3) -0.1618(12) 0.0878(7) 0.076(3) Uiso 0.515(12) 1 d PD A 2
H30 H 0.9661 -0.1838 0.1405 0.113 Uiso 0.515(12) 1 calc PR A 2
H31 H 0.9407 -0.0752 0.0879 0.113 Uiso 0.515(12) 1 calc PR A 2
H32 H 0.9667 -0.1748 0.0468 0.113 Uiso 0.515(12) 1 calc PR A 2
C18 C 0.9172(3) -0.4266(9) 0.0714(6) 0.081(3) Uiso 0.515(12) 1 d PD A 2
C19 C 0.8770(4) -0.5059(13) 0.0696(9) 0.104(4) Uiso 0.515(12) 1 d PD A 2
H33 H 0.8559 -0.4883 0.0207 0.156 Uiso 0.515(12) 1 calc PR A 2
H34 H 0.8644 -0.4873 0.1166 0.156 Uiso 0.515(12) 1 calc PR A 2
H35 H 0.8851 -0.5930 0.0704 0.156 Uiso 0.515(12) 1 calc PR A 2
C20 C 0.9510(5) -0.4539(18) 0.1452(10) 0.133(6) Uiso 0.515(12) 1 d PD A 2
H36 H 0.9764 -0.4025 0.1450 0.199 Uiso 0.515(12) 1 calc PR A 2
H37 H 0.9592 -0.5408 0.1452 0.199 Uiso 0.515(12) 1 calc PR A 2
H38 H 0.9392 -0.4360 0.1933 0.199 Uiso 0.515(12) 1 calc PR A 2
C21 C 0.9377(8) -0.457(2) -0.0024(12) 0.182(10) Uiso 0.515(12) 1 d PD A 2
H39 H 0.9166 -0.4411 -0.0517 0.273 Uiso 0.515(12) 1 calc PR A 2
H40 H 0.9464 -0.5433 -0.0005 0.273 Uiso 0.515(12) 1 calc PR A 2
H41 H 0.9631 -0.4045 -0.0015 0.273 Uiso 0.515(12) 1 calc PR A 2
C22 C 0.9199(3) -0.0607(8) 0.3085(7) 0.065(3) Uiso 0.50 1 d PD A 3
H42 H 0.9442 -0.0791 0.3531 0.078 Uiso 0.50 1 calc PR A 3
H43 H 0.9313 -0.0130 0.2676 0.078 Uiso 0.50 1 calc PR A 3
O5 O 0.8883(5) 0.0115(12) 0.3381(12) 0.093(6) Uani 0.50 1 d PD A 3
Si3 Si 0.9021(2) 0.1458(8) 0.3775(5) 0.121(3) Uani 0.50 1 d PD A 3
C23 C 0.8620(5) 0.1841(16) 0.4451(9) 0.114(4) Uiso 0.50 1 d PD A 3
H44 H 0.8642 0.1223 0.4876 0.171 Uiso 0.50 1 calc PR A 3
H45 H 0.8326 0.1842 0.4132 0.171 Uiso 0.50 1 calc PR A 3
H46 H 0.8686 0.2655 0.4691 0.171 Uiso 0.50 1 calc PR A 3
C24 C 0.9568(5) 0.143(3) 0.4455(14) 0.181(10) Uiso 0.50 1 d PD A 3
H47 H 0.9572 0.0805 0.4869 0.272 Uiso 0.50 1 calc PR A 3
H48 H 0.9627 0.2241 0.4708 0.272 Uiso 0.50 1 calc PR A 3
H49 H 0.9789 0.1244 0.4140 0.272 Uiso 0.50 1 calc PR A 3
C25 C 0.8974(5) 0.2632(13) 0.2977(8) 0.119(5) Uiso 0.50 1 d PD A 3
C26 C 0.8519(5) 0.2450(19) 0.2457(11) 0.135(6) Uiso 0.50 1 d PD A 3
H50 H 0.8300 0.2608 0.2782 0.203 Uiso 0.50 1 calc PR A 3
H51 H 0.8490 0.1604 0.2255 0.203 Uiso 0.50 1 calc PR A 3
H52 H 0.8479 0.3024 0.2004 0.203 Uiso 0.50 1 calc PR A 3
C27 C 0.9364(7) 0.230(3) 0.2617(16) 0.191(12) Uiso 0.50 1 d PD A 3
H53 H 0.9628 0.2424 0.3019 0.287 Uiso 0.50 1 calc PR A 3
H54 H 0.9371 0.2828 0.2153 0.287 Uiso 0.50 1 calc PR A 3
H55 H 0.9344 0.1438 0.2448 0.287 Uiso 0.50 1 calc PR A 3
C28 C 0.9038(9) 0.3916(17) 0.3366(16) 0.179(10) Uiso 0.50 1 d PD A 3
H56 H 0.8807 0.4076 0.3665 0.269 Uiso 0.50 1 calc PR A 3
H57 H 0.9029 0.4541 0.2948 0.269 Uiso 0.50 1 calc PR A 3
H58 H 0.9318 0.3949 0.3733 0.269 Uiso 0.50 1 calc PR A 3
C29 C 0.9212(3) -0.0802(10) 0.3341(8) 0.073(3) Uiso 0.50 1 d PD A 4
H59 H 0.9251 -0.1122 0.3895 0.088 Uiso 0.50 1 calc PR A 4
H60 H 0.9495 -0.0534 0.3235 0.088 Uiso 0.50 1 calc PR A 4
O6 O 0.8907(4) 0.0196(9) 0.3222(11) 0.082(4) Uani 0.50 1 d PD A 4
Si4 Si 0.89462(16) 0.1692(6) 0.3429(4) 0.0867(15) Uani 0.50 1 d PD A 4
C30 C 0.8494(5) 0.2130(18) 0.3964(11) 0.133(6) Uiso 0.50 1 d PD A 4
H61 H 0.8503 0.1597 0.4432 0.200 Uiso 0.50 1 calc PR A 4
H62 H 0.8216 0.2030 0.3598 0.200 Uiso 0.50 1 calc PR A 4
H63 H 0.8529 0.2989 0.4139 0.200 Uiso 0.50 1 calc PR A 4
C31 C 0.9470(5) 0.189(2) 0.4205(11) 0.149(7) Uiso 0.50 1 d PD A 4
H64 H 0.9458 0.1373 0.4673 0.224 Uiso 0.50 1 calc PR A 4
H65 H 0.9502 0.2753 0.4372 0.224 Uiso 0.50 1 calc PR A 4
H66 H 0.9716 0.1644 0.3968 0.224 Uiso 0.50 1 calc PR A 4
C32 C 0.8954(3) 0.2652(10) 0.2561(6) 0.093(3) Uiso 0.50 1 d PD A 4
C33 C 0.8557(5) 0.2305(19) 0.1934(10) 0.138(6) Uiso 0.50 1 d PD A 4
H67 H 0.8295 0.2488 0.2143 0.207 Uiso 0.50 1 calc PR A 4
H68 H 0.8566 0.1426 0.1814 0.207 Uiso 0.50 1 calc PR A 4
H69 H 0.8555 0.2781 0.1444 0.207 Uiso 0.50 1 calc PR A 4
C34 C 0.9346(4) 0.2375(17) 0.2207(10) 0.122(5) Uiso 0.50 1 d PD A 4
H70 H 0.9607 0.2602 0.2591 0.183 Uiso 0.50 1 calc PR A 4
H71 H 0.9332 0.2847 0.1712 0.183 Uiso 0.50 1 calc PR A 4
H72 H 0.9354 0.1494 0.2088 0.183 Uiso 0.50 1 calc PR A 4
C35 C 0.8944(6) 0.4008(12) 0.2796(12) 0.133(6) Uiso 0.50 1 d PD A 4
H73 H 0.8685 0.4170 0.3017 0.200 Uiso 0.50 1 calc PR A 4
H74 H 0.8940 0.4523 0.2322 0.200 Uiso 0.50 1 calc PR A 4
H75 H 0.9201 0.4200 0.3200 0.200 Uiso 0.50 1 calc PR A 4
N6 N 0.75630(10) 0.3277(2) 0.05099(15) 0.0435(6) Uani 1 1 d . . .
H76 H 0.7626 0.3873 0.0201 0.052 Uiso 1 1 calc R . .
C36 C 0.75497(11) 0.3570(3) 0.12863(17) 0.0414(6) Uani 1 1 d . . .
N7 N 0.76429(12) 0.4731(3) 0.15103(16) 0.0532(7) Uani 1 1 d . . .
H77 H 0.7645 0.4958 0.2008 0.064 Uiso 1 1 calc R . .
H78 H 0.7702 0.5269 0.1161 0.064 Uiso 1 1 calc R . .
N8 N 0.74594(9) 0.2754(2) 0.18173(14) 0.0404(5) Uani 1 1 d . . .
C37 C 0.73869(10) 0.1622(3) 0.14994(16) 0.0374(6) Uani 1 1 d . . .
C38 C 0.73973(11) 0.1237(3) 0.07289(17) 0.0404(6) Uani 1 1 d . . .
C39 C 0.74856(11) 0.2116(3) 0.01634(16) 0.0423(6) Uani 1 1 d . . .
O7 O 0.74936(10) 0.1952(2) -0.05508(13) 0.0545(6) Uani 1 1 d . . .
N9 N 0.72905(10) 0.0005(2) 0.06404(15) 0.0466(6) Uani 1 1 d . . .
C40 C 0.72208(12) -0.0345(3) 0.13373(19) 0.0461(7) Uani 1 1 d . . .
H79 H 0.7145 -0.1161 0.1454 0.055 Uiso 1 1 calc R . .
N10 N 0.72687(9) 0.0600(2) 0.18858(14) 0.0397(5) Uani 1 1 d . . .
C41 C 0.72087(12) 0.0560(3) 0.27162(18) 0.0455(7) Uani 1 1 d . D .
H80 H 0.7466 0.0924 0.3075 0.055 Uiso 1 1 calc R . .
C42 C 0.68018(14) 0.1203(4) 0.2855(3) 0.0609(9) Uani 1 1 d . D .
H81 H 0.6866 0.1752 0.3328 0.073 Uiso 1 1 calc R . .
H82 H 0.6671 0.1696 0.2381 0.073 Uiso 1 1 calc R . .
C43 C 0.65063(11) 0.0181(4) 0.2995(2) 0.0580(8) Uani 1 1 d D . .
H83 H 0.6355 -0.0086 0.2451 0.070 Uiso 0.34 1 calc PR C 5
H84 H 0.6328 -0.0073 0.2469 0.070 Uiso 0.33 1 calc PR C 6
H85 H 0.6277 -0.0037 0.2523 0.070 Uiso 0.33 1 calc PR C 7
C44 C 0.68226(12) -0.0857(4) 0.3307(2) 0.0521(8) Uani 1 1 d . D .
H86 H 0.6927 -0.0757 0.3897 0.063 Uiso 1 1 calc R . .
O8 O 0.71733(9) -0.0695(2) 0.29051(15) 0.0523(6) Uani 1 1 d . . .
O9 O 0.6190(3) 0.0234(10) 0.3462(5) 0.057(3) Uiso 0.34 1 d PD D 5
Si5 Si 0.5871(2) 0.1409(6) 0.3478(4) 0.0917(19) Uani 0.34 1 d PD D 5
C45 C 0.6173(7) 0.2730(19) 0.4091(13) 0.110 Uiso 0.34 1 d PD D 5
H87 H 0.6394 0.3054 0.3813 0.165 Uiso 0.34 1 calc PR D 5
H88 H 0.6311 0.2425 0.4620 0.165 Uiso 0.34 1 calc PR D 5
H89 H 0.5969 0.3385 0.4153 0.165 Uiso 0.34 1 calc PR D 5
C46 C 0.5679(5) 0.2096(16) 0.2471(8) 0.073(4) Uiso 0.34 1 d PD D 5
H90 H 0.5927 0.2366 0.2248 0.110 Uiso 0.34 1 calc PR D 5
H91 H 0.5493 0.2804 0.2519 0.110 Uiso 0.34 1 calc PR D 5
H92 H 0.5515 0.1481 0.2115 0.110 Uiso 0.34 1 calc PR D 5
C47 C 0.5474(5) 0.0854(15) 0.4044(9) 0.109(6) Uiso 0.34 1 d PD D 5
C48 C 0.5319(9) -0.038(2) 0.3671(17) 0.129(8) Uiso 0.34 1 d PD D 5
H93 H 0.5567 -0.0938 0.3700 0.194 Uiso 0.34 1 calc PR D 5
H94 H 0.5181 -0.0263 0.3109 0.194 Uiso 0.34 1 calc PR D 5
H95 H 0.5111 -0.0745 0.3964 0.194 Uiso 0.34 1 calc PR D 5
C49 C 0.5683(9) 0.073(3) 0.4922(11) 0.144(9) Uiso 0.34 1 d PD D 5
H96 H 0.5791 0.1532 0.5132 0.216 Uiso 0.34 1 calc PR D 5
H97 H 0.5924 0.0147 0.4975 0.216 Uiso 0.34 1 calc PR D 5
H98 H 0.5471 0.0425 0.5225 0.216 Uiso 0.34 1 calc PR D 5
C50 C 0.5104(8) 0.177(2) 0.3981(17) 0.148(10) Uiso 0.34 1 d PD D 5
H99 H 0.5211 0.2541 0.4244 0.222 Uiso 0.34 1 calc PR D 5
H100 H 0.4879 0.1429 0.4243 0.222 Uiso 0.34 1 calc PR D 5
H101 H 0.4983 0.1928 0.3415 0.222 Uiso 0.34 1 calc PR D 5
O10 O 0.6225(3) 0.0548(13) 0.3514(6) 0.060(3) Uiso 0.33 1 d PD D 6
Si6 Si 0.57283(10) 0.1060(4) 0.3320(2) 0.0464(9) Uani 0.33 1 d PD D 6
C51 C 0.5302(4) -0.0073(13) 0.3307(9) 0.072(3) Uiso 0.33 1 d PD D 6
H102 H 0.5354 -0.0530 0.3813 0.108 Uiso 0.33 1 calc PR D 6
H103 H 0.5299 -0.0645 0.2861 0.108 Uiso 0.33 1 calc PR D 6
H104 H 0.5023 0.0347 0.3240 0.108 Uiso 0.33 1 calc PR D 6
C52 C 0.5640(5) 0.1720(17) 0.2276(8) 0.075(4) Uiso 0.33 1 d PD D 6
H105 H 0.5855 0.2359 0.2251 0.113 Uiso 0.33 1 calc PR D 6
H106 H 0.5350 0.2078 0.2142 0.113 Uiso 0.33 1 calc PR D 6
H107 H 0.5668 0.1065 0.1893 0.113 Uiso 0.33 1 calc PR D 6
C53 C 0.5749(4) 0.2282(11) 0.4110(8) 0.075(4) Uiso 0.33 1 d PD D 6
C54 C 0.6096(5) 0.3300(15) 0.3970(11) 0.083(4) Uiso 0.33 1 d PD D 6
H108 H 0.6010 0.3654 0.3433 0.125 Uiso 0.33 1 calc PR D 6
H109 H 0.6381 0.2914 0.4020 0.125 Uiso 0.33 1 calc PR D 6
H110 H 0.6110 0.3951 0.4372 0.125 Uiso 0.33 1 calc PR D 6
C55 C 0.5871(6) 0.1717(18) 0.4919(9) 0.095(5) Uiso 0.33 1 d PD D 6
H111 H 0.6136 0.1237 0.4948 0.142 Uiso 0.33 1 calc PR D 6
H112 H 0.5638 0.1176 0.5015 0.142 Uiso 0.33 1 calc PR D 6
H113 H 0.5919 0.2366 0.5326 0.142 Uiso 0.33 1 calc PR D 6
C56 C 0.5328(5) 0.3010(18) 0.4002(11) 0.086(5) Uiso 0.33 1 d PD D 6
H114 H 0.5276 0.3418 0.3479 0.129 Uiso 0.33 1 calc PR D 6
H115 H 0.5349 0.3629 0.4427 0.129 Uiso 0.33 1 calc PR D 6
H116 H 0.5089 0.2449 0.4032 0.129 Uiso 0.33 1 calc PR D 6
O11 O 0.6350(4) 0.0514(12) 0.3714(5) 0.073(3) Uiso 0.33 1 d PD D 7
Si7 Si 0.58975(19) 0.0713(6) 0.4011(4) 0.1104(18) Uani 0.33 1 d PD D 7
C57 C 0.5949(11) 0.059(3) 0.5122(9) 0.156(11) Uiso 0.33 1 d PD D 7
H117 H 0.6055 -0.0236 0.5297 0.234 Uiso 0.33 1 calc PR D 7
H118 H 0.5666 0.0719 0.5265 0.234 Uiso 0.33 1 calc PR D 7
H119 H 0.6153 0.1206 0.5386 0.234 Uiso 0.33 1 calc PR D 7
C58 C 0.5516(10) -0.054(3) 0.355(2) 0.180(16) Uiso 0.33 1 d PD D 7
H120 H 0.5464 -0.0471 0.2965 0.270 Uiso 0.33 1 calc PR D 7
H121 H 0.5241 -0.0456 0.3734 0.270 Uiso 0.33 1 calc PR D 7
H122 H 0.5643 -0.1345 0.3712 0.270 Uiso 0.33 1 calc PR D 7
C59 C 0.5692(6) 0.2296(15) 0.3753(13) 0.139(10) Uiso 0.33 1 d PD D 7
C60 C 0.6016(9) 0.317(3) 0.427(2) 0.172(16) Uiso 0.33 1 d PD D 7
H123 H 0.6301 0.3086 0.4128 0.258 Uiso 0.33 1 calc PR D 7
H124 H 0.6037 0.2970 0.4840 0.258 Uiso 0.33 1 calc PR D 7
H125 H 0.5917 0.4026 0.4179 0.258 Uiso 0.33 1 calc PR D 7
C61 C 0.5273(6) 0.249(2) 0.4076(13) 0.098(6) Uiso 0.33 1 d PD D 7
H126 H 0.5049 0.1934 0.3795 0.147 Uiso 0.33 1 calc PR D 7
H127 H 0.5177 0.3341 0.3987 0.147 Uiso 0.33 1 calc PR D 7
H128 H 0.5327 0.2305 0.4651 0.147 Uiso 0.33 1 calc PR D 7
C62 C 0.5633(12) 0.247(3) 0.2846(14) 0.190(16) Uiso 0.33 1 d PD D 7
H129 H 0.5907 0.2312 0.2676 0.286 Uiso 0.33 1 calc PR D 7
H130 H 0.5539 0.3311 0.2705 0.286 Uiso 0.33 1 calc PR D 7
H131 H 0.5415 0.1889 0.2576 0.286 Uiso 0.33 1 calc PR D 7
C63 C 0.66651(16) -0.2157(4) 0.3131(2) 0.0823(15) Uani 1 1 d D . .
H132 H 0.6908 -0.2663 0.3021 0.099 Uiso 0.358(4) 1 calc PR D 8
H133 H 0.6577 -0.2497 0.3615 0.099 Uiso 0.358(4) 1 calc PR D 8
H134 H 0.6901 -0.2747 0.3321 0.099 Uiso 0.642(4) 1 calc PR D 9
H135 H 0.6425 -0.2336 0.3411 0.099 Uiso 0.642(4) 1 calc PR D 9
O12 O 0.6316(2) -0.2266(8) 0.2477(5) 0.076(2) Uiso 0.358(4) 1 d PD D 8
Si8 Si 0.61099(11) -0.3594(3) 0.2306(3) 0.0742(14) Uani 0.358(4) 1 d PD D 8
C64 C 0.5752(6) -0.3929(19) 0.3050(10) 0.102(5) Uiso 0.358(4) 1 d PD D 8
H136 H 0.5537 -0.3272 0.3029 0.153 Uiso 0.358(4) 1 calc PR D 8
H137 H 0.5928 -0.3974 0.3591 0.153 Uiso 0.358(4) 1 calc PR D 8
H138 H 0.5604 -0.4716 0.2916 0.153 Uiso 0.358(4) 1 calc PR D 8
C65 C 0.6511(5) -0.4876(14) 0.2384(11) 0.076(4) Uiso 0.358(4) 1 d PD D 8
H139 H 0.6700 -0.4742 0.1998 0.114 Uiso 0.358(4) 1 calc PR D 8
H140 H 0.6358 -0.5659 0.2266 0.114 Uiso 0.358(4) 1 calc PR D 8
H141 H 0.6684 -0.4899 0.2927 0.114 Uiso 0.358(4) 1 calc PR D 8
C66 C 0.5783(4) -0.3344(12) 0.1288(7) 0.082(4) Uiso 0.358(4) 1 d PD D 8
C67 C 0.5492(5) -0.2215(15) 0.1370(11) 0.081(5) Uiso 0.358(4) 1 d PD D 8
H142 H 0.5673 -0.1518 0.1592 0.122 Uiso 0.358(4) 1 calc PR D 8
H143 H 0.5294 -0.2421 0.1728 0.122 Uiso 0.358(4) 1 calc PR D 8
H144 H 0.5326 -0.1992 0.0841 0.122 Uiso 0.358(4) 1 calc PR D 8
C68 C 0.5501(5) -0.4379(15) 0.0916(11) 0.086(4) Uiso 0.358(4) 1 d PD D 8
H145 H 0.5677 -0.5117 0.0899 0.129 Uiso 0.358(4) 1 calc PR D 8
H146 H 0.5361 -0.4151 0.0371 0.129 Uiso 0.358(4) 1 calc PR D 8
H147 H 0.5280 -0.4546 0.1236 0.129 Uiso 0.358(4) 1 calc PR D 8
C69 C 0.6104(7) -0.309(2) 0.0733(12) 0.126(7) Uiso 0.358(4) 1 d PD D 8
H148 H 0.6288 -0.2393 0.0940 0.189 Uiso 0.358(4) 1 calc PR D 8
H149 H 0.5945 -0.2901 0.0193 0.189 Uiso 0.358(4) 1 calc PR D 8
H150 H 0.6284 -0.3821 0.0712 0.189 Uiso 0.358(4) 1 calc PR D 8
O13 O 0.65198(17) -0.2276(4) 0.2274(2) 0.0657(11) Uiso 0.642(4) 1 d PD D 9
Si9 Si 0.62996(6) -0.34747(15) 0.17322(12) 0.0616(6) Uani 0.642(4) 1 d PD D 9
C70 C 0.6561(3) -0.4900(8) 0.2164(6) 0.074(2) Uiso 0.642(4) 1 d PD D 9
H151 H 0.6871 -0.4861 0.2161 0.111 Uiso 0.642(4) 1 calc PR D 9
H152 H 0.6434 -0.5605 0.1845 0.111 Uiso 0.642(4) 1 calc PR D 9
H153 H 0.6518 -0.4991 0.2717 0.111 Uiso 0.642(4) 1 calc PR D 9
C71 C 0.6407(3) -0.3238(9) 0.0690(5) 0.085(2) Uiso 0.642(4) 1 d PD D 9
H154 H 0.6268 -0.2476 0.0466 0.128 Uiso 0.642(4) 1 calc PR D 9
H155 H 0.6291 -0.3934 0.0351 0.128 Uiso 0.642(4) 1 calc PR D 9
H156 H 0.6719 -0.3179 0.0713 0.128 Uiso 0.642(4) 1 calc PR D 9
C72 C 0.5706(2) -0.3520(8) 0.1735(5) 0.083(2) Uiso 0.642(4) 1 d PD D 9
C73 C 0.5504(4) -0.4666(12) 0.1273(9) 0.121(4) Uiso 0.642(4) 1 d PD D 9
H157 H 0.5651 -0.5406 0.1514 0.181 Uiso 0.642(4) 1 calc PR D 9
H158 H 0.5534 -0.4606 0.0712 0.181 Uiso 0.642(4) 1 calc PR D 9
H159 H 0.5197 -0.4712 0.1300 0.181 Uiso 0.642(4) 1 calc PR D 9
C74 C 0.5502(8) -0.2392(19) 0.1280(15) 0.199(13) Uiso 0.642(4) 1 d PD D 9
H160 H 0.5620 -0.1646 0.1563 0.298 Uiso 0.642(4) 1 calc PR D 9
H161 H 0.5189 -0.2414 0.1244 0.298 Uiso 0.642(4) 1 calc PR D 9
H162 H 0.5567 -0.2391 0.0739 0.298 Uiso 0.642(4) 1 calc PR D 9
C75 C 0.5610(4) -0.3662(12) 0.2570(6) 0.108(3) Uiso 0.642(4) 1 d PD D 9
H163 H 0.5750 -0.4409 0.2818 0.162 Uiso 0.642(4) 1 calc PR D 9
H164 H 0.5298 -0.3724 0.2537 0.162 Uiso 0.642(4) 1 calc PR D 9
H165 H 0.5721 -0.2946 0.2895 0.162 Uiso 0.642(4) 1 calc PR D 9


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.363(4) . ?
N1 C4 1.388(4) . ?
C1 N3 1.327(4) . ?
C1 N2 1.334(4) . ?
N3 C2 1.360(4) . ?
C2 C3 1.365(4) . ?
C2 N5 1.375(4) . ?
C3 N4 1.391(4) . ?
C3 C4 1.413(4) . ?
C4 O1 1.240(4) . ?
N4 C5 1.305(4) . ?
C5 N5 1.385(4) . ?
N5 C6 1.452(4) . ?
C6 O2 1.412(5) . ?
C6 C7 1.520(5) . ?
C7 C8 1.515(6) . ?
C8 O3 1.427(5) . ?
C8 O4 1.440(4) . ?
C8 C9 1.501(8) . ?
C9 O2 1.446(6) . ?
C9 C22 1.524(6) . ?
C9 C29 1.574(12) . ?
O3 Si1 1.656(8) . ?
Si1 C12 1.841(6) . ?
Si1 C10 1.883(11) . ?
Si1 C11 1.892(10) . ?
C12 C14 1.518(7) . ?
C12 C13 1.529(7) . ?
C12 C15 1.529(7) . ?
O4 Si2 1.644(8) . ?
Si2 C17 1.864(10) . ?
Si2 C16 1.870(10) . ?
Si2 C18 1.885(11) . ?
C18 C20 1.512(14) . ?
C18 C19 1.530(12) . ?
C18 C21 1.553(14) . ?
C22 O5 1.436(5) . ?
O5 Si3 1.630(11) . ?
Si3 C25 1.848(12) . ?
Si3 C24 1.885(14) . ?
Si3 C23 1.913(12) . ?
C25 C27 1.521(15) . ?
C25 C28 1.542(15) . ?
C25 C26 1.549(14) . ?
C29 O6 1.440(5) . ?
O6 Si4 1.664(9) . ?
Si4 C32 1.812(9) . ?
Si4 C30 1.896(12) . ?
Si4 C31 1.919(12) . ?
C32 C34 1.509(11) . ?
C32 C35 1.530(11) . ?
C32 C33 1.529(11) . ?
N6 C36 1.367(4) . ?
N6 C39 1.396(4) . ?
C36 N7 1.335(4) . ?
C36 N8 1.336(4) . ?
N8 C37 1.346(4) . ?
C37 N10 1.379(4) . ?
C37 C38 1.382(4) . ?
C38 N9 1.383(4) . ?
C38 C39 1.421(4) . ?
C39 O7 1.233(4) . ?
N9 C40 1.303(4) . ?
C40 N10 1.376(4) . ?
N10 C41 1.461(4) . ?
C41 O8 1.411(4) . ?
C41 C42 1.522(5) . ?
C42 C43 1.500(5) . ?
C43 O9 1.393(5) . ?
C43 O10 1.424(5) . ?
C43 O11 1.449(5) . ?
C43 C44 1.533(5) . ?
C44 O8 1.420(4) . ?
C44 C63 1.509(6) . ?
O9 Si5 1.631(9) . ?
Si5 C47 1.824(13) . ?
Si5 C46 1.859(11) . ?
Si5 C45 1.918(14) . ?
C47 C49 1.518(16) . ?
C47 C50 1.523(16) . ?
C47 C48 1.528(15) . ?
O10 Si6 1.639(9) . ?
Si6 C51 1.823(11) . ?
Si6 C53 1.882(11) . ?
Si6 C52 1.885(11) . ?
C53 C55 1.488(15) . ?
C53 C56 1.527(14) . ?
C53 C54 1.609(14) . ?
O11 Si7 1.621(9) . ?
Si7 C59 1.862(14) . ?
Si7 C57 1.870(14) . ?
Si7 C58 1.888(15) . ?
C59 C62 1.528(16) . ?
C59 C61 1.541(16) . ?
C59 C60 1.548(16) . ?
C63 O12 1.414(3) . ?
C63 O13 1.448(3) . ?
O12 Si8 1.587(8) . ?
Si8 C66 1.857(11) . ?
Si8 C65 1.871(12) . ?
Si8 C64 1.889(12) . ?
C66 C68 1.498(14) . ?
C66 C69 1.538(15) . ?
C66 C67 1.556(14) . ?
O13 Si9 1.669(5) . ?
Si9 C70 1.842(8) . ?
Si9 C72 1.878(8) . ?
Si9 C71 1.885(8) . ?
C72 C75 1.514(11) . ?
C72 C74 1.526(15) . ?
C72 C73 1.544(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C4 125.3(3) . . ?
N3 C1 N2 119.4(3) . . ?
N3 C1 N1 123.8(3) . . ?
N2 C1 N1 116.7(3) . . ?
C1 N3 C2 111.4(3) . . ?
N3 C2 C3 128.7(3) . . ?
N3 C2 N5 125.1(3) . . ?
C3 C2 N5 106.2(3) . . ?
C2 C3 N4 111.2(3) . . ?
C2 C3 C4 118.8(3) . . ?
N4 C3 C4 129.8(3) . . ?
O1 C4 N1 119.6(3) . . ?
O1 C4 C3 128.7(3) . . ?
N1 C4 C3 111.7(3) . . ?
C5 N4 C3 103.8(3) . . ?
N4 C5 N5 113.5(3) . . ?
C2 N5 C5 105.4(3) . . ?
C2 N5 C6 125.9(3) . . ?
C5 N5 C6 126.6(3) . . ?
O2 C6 N5 107.2(3) . . ?
O2 C6 C7 106.2(3) . . ?
N5 C6 C7 115.7(3) . . ?
C8 C7 C6 101.8(3) . . ?
O3 C8 O4 21.2(3) . . ?
O3 C8 C9 97.7(5) . . ?
O4 C8 C9 118.5(5) . . ?
O3 C8 C7 115.2(4) . . ?
O4 C8 C7 103.8(4) . . ?
C9 C8 C7 102.8(3) . . ?
O2 C9 C8 106.6(4) . . ?
O2 C9 C22 116.8(6) . . ?
C8 C9 C22 109.0(6) . . ?
O2 C9 C29 101.5(6) . . ?
C8 C9 C29 124.4(6) . . ?
C22 C9 C29 17.6(5) . . ?
C6 O2 C9 109.6(3) . . ?
C8 O3 Si1 116.3(5) . . ?
O3 Si1 C12 105.1(5) . . ?
O3 Si1 C10 110.7(7) . . ?
C12 Si1 C10 112.7(7) . . ?
O3 Si1 C11 108.7(6) . . ?
C12 Si1 C11 112.6(6) . . ?
C10 Si1 C11 107.1(7) . . ?
C14 C12 C13 109.0(10) . . ?
C14 C12 C15 109.7(10) . . ?
C13 C12 C15 109.9(10) . . ?
C14 C12 Si1 110.2(8) . . ?
C13 C12 Si1 108.2(8) . . ?
C15 C12 Si1 109.9(9) . . ?
C8 O4 Si2 128.6(5) . . ?
O4 Si2 C17 113.0(6) . . ?
O4 Si2 C16 105.2(6) . . ?
C17 Si2 C16 110.3(7) . . ?
O4 Si2 C18 106.9(6) . . ?
C17 Si2 C18 108.7(6) . . ?
C16 Si2 C18 112.7(6) . . ?
C20 C18 C19 110.8(10) . . ?
C20 C18 C21 107.0(12) . . ?
C19 C18 C21 109.8(12) . . ?
C20 C18 Si2 112.5(9) . . ?
C19 C18 Si2 108.1(8) . . ?
C21 C18 Si2 108.6(11) . . ?
O5 C22 C9 111.1(8) . . ?
C22 O5 Si3 119.0(10) . . ?
O5 Si3 C25 109.9(9) . . ?
O5 Si3 C24 112.4(11) . . ?
C25 Si3 C24 113.2(10) . . ?
O5 Si3 C23 106.6(8) . . ?
C25 Si3 C23 108.8(8) . . ?
C24 Si3 C23 105.6(10) . . ?
C27 C25 C28 109.7(15) . . ?
C27 C25 C26 118.3(15) . . ?
C28 C25 C26 113.0(14) . . ?
C27 C25 Si3 100.1(12) . . ?
C28 C25 Si3 109.0(12) . . ?
C26 C25 Si3 105.4(10) . . ?
O6 C29 C9 104.4(8) . . ?
C29 O6 Si4 133.3(10) . . ?
O6 Si4 C32 113.7(8) . . ?
O6 Si4 C30 108.3(8) . . ?
C32 Si4 C30 112.1(7) . . ?
O6 Si4 C31 105.9(8) . . ?
C32 Si4 C31 110.6(7) . . ?
C30 Si4 C31 105.7(8) . . ?
C34 C32 C35 110.9(11) . . ?
C34 C32 C33 107.4(11) . . ?
C35 C32 C33 111.4(11) . . ?
C34 C32 Si4 110.5(9) . . ?
C35 C32 Si4 109.8(9) . . ?
C33 C32 Si4 106.8(9) . . ?
C36 N6 C39 125.7(3) . . ?
N7 C36 N8 120.0(3) . . ?
N7 C36 N6 116.7(3) . . ?
N8 C36 N6 123.3(3) . . ?
C36 N8 C37 112.2(2) . . ?
N8 C37 N10 125.9(2) . . ?
N8 C37 C38 128.6(3) . . ?
N10 C37 C38 105.4(2) . . ?
C37 C38 N9 110.3(3) . . ?
C37 C38 C39 118.8(3) . . ?
N9 C38 C39 130.8(3) . . ?
O7 C39 N6 120.7(3) . . ?
O7 C39 C38 127.9(3) . . ?
N6 C39 C38 111.4(2) . . ?
C40 N9 C38 105.3(3) . . ?
N9 C40 N10 112.5(3) . . ?
C40 N10 C37 106.4(2) . . ?
C40 N10 C41 128.0(3) . . ?
C37 N10 C41 125.6(2) . . ?
O8 C41 N10 106.2(2) . . ?
O8 C41 C42 107.7(3) . . ?
N10 C41 C42 114.0(3) . . ?
C43 C42 C41 104.7(3) . . ?
O9 C43 O10 14.9(7) . . ?
O9 C43 O11 27.2(6) . . ?
O10 C43 O11 18.8(6) . . ?
O9 C43 C42 126.6(6) . . ?
O10 C43 C42 111.8(7) . . ?
O11 C43 C42 105.8(6) . . ?
O9 C43 C44 108.9(5) . . ?
O10 C43 C44 115.7(6) . . ?
O11 C43 C44 101.3(6) . . ?
C42 C43 C44 102.5(3) . . ?
O8 C44 C63 106.2(3) . . ?
O8 C44 C43 105.0(3) . . ?
C63 C44 C43 116.9(3) . . ?
C41 O8 C44 109.4(3) . . ?
C43 O9 Si5 123.7(7) . . ?
O9 Si5 C47 103.9(7) . . ?
O9 Si5 C46 113.1(7) . . ?
C47 Si5 C46 119.0(8) . . ?
O9 Si5 C45 110.5(9) . . ?
C47 Si5 C45 106.4(9) . . ?
C46 Si5 C45 103.8(9) . . ?
C49 C47 C50 108.2(15) . . ?
C49 C47 C48 111.9(16) . . ?
C50 C47 C48 111.6(16) . . ?
C49 C47 Si5 109.5(13) . . ?
C50 C47 Si5 110.0(13) . . ?
C48 C47 Si5 105.5(13) . . ?
C43 O10 Si6 131.1(8) . . ?
O10 Si6 C51 116.8(8) . . ?
O10 Si6 C53 101.3(6) . . ?
C51 Si6 C53 114.2(6) . . ?
O10 Si6 C52 106.4(6) . . ?
C51 Si6 C52 105.7(7) . . ?
C53 Si6 C52 112.5(7) . . ?
C55 C53 C56 112.9(12) . . ?
C55 C53 C54 111.0(12) . . ?
C56 C53 C54 103.2(12) . . ?
C55 C53 Si6 109.6(10) . . ?
C56 C53 Si6 111.8(10) . . ?
C54 C53 Si6 108.1(9) . . ?
C43 O11 Si7 139.5(9) . . ?
O11 Si7 C59 109.8(8) . . ?
O11 Si7 C57 113.2(11) . . ?
C59 Si7 C57 105.4(11) . . ?
O11 Si7 C58 107.8(12) . . ?
C59 Si7 C58 113.8(12) . . ?
C57 Si7 C58 106.9(13) . . ?
C62 C59 C61 113.4(17) . . ?
C62 C59 C60 116.1(19) . . ?
C61 C59 C60 103.5(16) . . ?
C62 C59 Si7 108.6(16) . . ?
C61 C59 Si7 108.9(13) . . ?
C60 C59 Si7 105.9(15) . . ?
O12 C63 O13 31.9(4) . . ?
O12 C63 C44 114.4(5) . . ?
O13 C63 C44 108.2(3) . . ?
C63 O12 Si8 116.8(6) . . ?
O12 Si8 C66 99.9(5) . . ?
O12 Si8 C65 114.7(6) . . ?
C66 Si8 C65 115.0(7) . . ?
O12 Si8 C64 109.3(7) . . ?
C66 Si8 C64 110.8(7) . . ?
C65 Si8 C64 107.1(8) . . ?
C68 C66 C69 106.5(12) . . ?
C68 C66 C67 108.5(11) . . ?
C69 C66 C67 112.6(13) . . ?
C68 C66 Si8 117.6(10) . . ?
C69 C66 Si8 106.4(10) . . ?
C67 C66 Si8 105.3(9) . . ?
C63 O13 Si9 130.0(4) . . ?
O13 Si9 C70 109.2(4) . . ?
O13 Si9 C72 109.2(3) . . ?
C70 Si9 C72 110.4(4) . . ?
O13 Si9 C71 106.3(3) . . ?
C70 Si9 C71 110.0(4) . . ?
C72 Si9 C71 111.5(4) . . ?
C75 C72 C74 114.7(12) . . ?
C75 C72 C73 104.9(9) . . ?
C74 C72 C73 107.3(12) . . ?
C75 C72 Si9 112.6(6) . . ?
C74 C72 Si9 107.5(11) . . ?
C73 C72 Si9 109.6(7) . . ?

_diffrn_measured_fraction_theta_max 0.938
_diffrn_reflns_theta_full        73.14
_diffrn_measured_fraction_theta_full 0.938
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.081

#===END

#========================================================
data_2c+AcOH
_database_code_depnum_ccdc_archive 'CCDC 225960'
#========================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
2',3'-O-bis(tert-butyldimethylsilyl)-guanosine
;
_chemical_name_common            
2',3'-O-bis(tert-butyldimethylsilyl)-guanosine
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H45 N5 O7 Si2'
_chemical_formula_sum            'C24 H45 N5 O7 Si2'
_chemical_formula_weight         571.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   17.3260(4)
_cell_length_b                   11.3690(3)
_cell_length_c                   17.3950(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.838(2)
_cell_angle_gamma                90.00
_cell_volume                     3057.38(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11879
_cell_measurement_theta_min      4.83
_cell_measurement_theta_max      73.19

_exptl_crystal_description       plate-like
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1232
_exptl_absorpt_coefficient_mu    1.455
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.6398
_exptl_absorpt_correction_T_max  0.8407
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'MacScience DIPLabo'
_diffrn_measurement_method       IP
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11879
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_sigmaI/netI    0.0199
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.83
_diffrn_reflns_theta_max         73.19
_reflns_number_total             3592
_reflns_number_gt                3581
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'MacScience Xpress'
_computing_cell_refinement       Scalepack
_computing_data_reduction        'Denzo and Scalepack'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    maXus

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0918P)²+4.6277P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.23(4)
_refine_ls_number_reflns         3592
_refine_ls_number_parameters     344
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0533
_refine_ls_wR_factor_ref         0.1415
_refine_ls_wR_factor_gt          0.1414
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C4 C 1.0812(2) 0.9033(3) 0.93131(19) 0.0195(7) Uani 1 1 d . . .
C2 C 1.1209(2) 1.0901(3) 0.9697(2) 0.0213(7) Uani 1 1 d . . .
C8 C 1.0830(2) 0.7121(3) 0.9092(2) 0.0205(7) Uani 1 1 d . . .
H8 H 1.0633 0.6338 0.8930 0.025 Uiso 1 1 calc R . .
C6 C 1.2340(2) 0.9440(3) 0.9930(2) 0.0201(7) Uani 1 1 d . . .
C5 C 1.1641(2) 0.8632(3) 0.9581(2) 0.0205(7) Uani 1 1 d . . .
C11 C 0.88943(19) 0.7558(4) 0.77127(19) 0.0213(7) Uani 1 1 d . . .
H11 H 0.9260 0.6971 0.7598 0.026 Uiso 1 1 calc R . .
C14 C 0.8435(2) 0.6452(4) 0.8598(2) 0.0249(7) Uani 1 1 d . . .
H14 H 0.7980 0.6543 0.8798 0.030 Uiso 1 1 calc R . .
C10 C 0.9356(2) 0.7982(3) 0.8651(2) 0.0207(7) Uani 1 1 d . . .
H10 H 0.9118 0.8764 0.8699 0.025 Uiso 1 1 calc R . .
C16 C 0.8695(3) 0.5183(4) 0.8676(3) 0.0372(10) Uani 1 1 d . . .
H16A H 0.9022 0.4964 0.9292 0.045 Uiso 1 1 calc R . .
H16B H 0.8174 0.4679 0.8411 0.045 Uiso 1 1 calc R . .
C13 C 0.8093(2) 0.6962(3) 0.7689(2) 0.0231(7) Uani 1 1 d . . .
H13 H 0.7880 0.6324 0.7246 0.028 Uiso 1 1 calc R . .
C30 C 0.4871(2) 0.8810(5) 0.6456(3) 0.0480(12) Uani 1 1 d . . .
H30A H 0.4679 0.8346 0.5926 0.072 Uiso 1 1 calc R . .
H30B H 0.4579 0.9576 0.6321 0.072 Uiso 1 1 calc R . .
H30C H 0.4726 0.8391 0.6866 0.072 Uiso 1 1 calc R . .
C21 C 0.8435(3) 0.8048(4) 0.5409(2) 0.0332(9) Uani 1 1 d . . .
C29 C 0.6161(3) 0.9709(5) 0.7681(3) 0.0462(12) Uani 1 1 d . . .
H29A H 0.6785 0.9844 0.7923 0.069 Uiso 1 1 calc R . .
H29B H 0.6034 0.9276 0.8099 0.069 Uiso 1 1 calc R . .
H29C H 0.5858 1.0466 0.7553 0.069 Uiso 1 1 calc R . .
C28 C 0.5857(2) 0.8994(4) 0.6856(2) 0.0347(9) Uani 1 1 d . . .
C26 C 0.6069(3) 0.6617(5) 0.6101(3) 0.0432(11) Uani 1 1 d . . .
H26A H 0.6198 0.7044 0.5683 0.065 Uiso 1 1 calc R . .
H26B H 0.5447 0.6459 0.5849 0.065 Uiso 1 1 calc R . .
H26C H 0.6387 0.5872 0.6248 0.065 Uiso 1 1 calc R . .
C27 C 0.6167(3) 0.6705(5) 0.7888(3) 0.0446(12) Uani 1 1 d . . .
H27A H 0.6348 0.7177 0.8413 0.067 Uiso 1 1 calc R . .
H27B H 0.6484 0.5959 0.8029 0.067 Uiso 1 1 calc R . .
H27C H 0.5545 0.6548 0.7642 0.067 Uiso 1 1 calc R . .
C19 C 0.8863(3) 1.0462(4) 0.6289(3) 0.0401(10) Uani 1 1 d . . .
H19A H 0.8240 1.0610 0.6049 0.060 Uiso 1 1 calc R . .
H19B H 0.9075 1.0751 0.5888 0.060 Uiso 1 1 calc R . .
H19C H 0.9165 1.0871 0.6842 0.060 Uiso 1 1 calc R . .
C20 C 1.0248(2) 0.8513(5) 0.6916(3) 0.0379(10) Uani 1 1 d . . .
H20A H 1.0333 0.7661 0.6998 0.057 Uiso 1 1 calc R . .
H20B H 1.0558 0.8911 0.7472 0.057 Uiso 1 1 calc R . .
H20C H 1.0470 0.8786 0.6520 0.057 Uiso 1 1 calc R . .
C31 C 0.6087(3) 0.9668(4) 0.6213(3) 0.0393(10) Uani 1 1 d . . .
H31A H 0.5884 0.9220 0.5676 0.059 Uiso 1 1 calc R . .
H31B H 0.6715 0.9770 0.6464 0.059 Uiso 1 1 calc R . .
H31C H 0.5806 1.0441 0.6093 0.059 Uiso 1 1 calc R . .
C23 C 0.7489(3) 0.8360(6) 0.5044(4) 0.0676(19) Uani 1 1 d . . .
H36 H 0.7278 0.8163 0.5465 0.101 Uiso 1 1 calc R . .
H37 H 0.7161 0.7915 0.4512 0.101 Uiso 1 1 calc R . .
H38 H 0.7414 0.9205 0.4919 0.101 Uiso 1 1 calc R . .
C24 C 0.8556(4) 0.6710(5) 0.5576(4) 0.0702(19) Uani 1 1 d . . .
H39 H 0.9171 0.6513 0.5815 0.105 Uiso 1 1 calc R . .
H40 H 0.8234 0.6286 0.5033 0.105 Uiso 1 1 calc R . .
H41 H 0.8338 0.6482 0.5986 0.105 Uiso 1 1 calc R . .
C22 C 0.8759(5) 0.8365(9) 0.4756(3) 0.102(3) Uani 1 1 d . . .
H42 H 0.9373 0.8160 0.4988 0.153 Uiso 1 1 calc R . .
H43 H 0.8685 0.9211 0.4638 0.153 Uiso 1 1 calc R . .
H44 H 0.8427 0.7928 0.4221 0.153 Uiso 1 1 calc R . .
C33 C 0.8736(2) 0.1886(4) 0.8259(2) 0.0291(8) Uani 1 1 d . . .
C32 C 0.7800(3) 0.2198(4) 0.7786(3) 0.0461(12) Uani 1 1 d . . .
H32A H 0.7568 0.2321 0.8200 0.069 Uiso 1 1 calc R . .
H32B H 0.7484 0.1558 0.7393 0.069 Uiso 1 1 calc R . .
H32C H 0.7734 0.2921 0.7455 0.069 Uiso 1 1 calc R . .
N7 N 1.16540(17) 0.7436(3) 0.94426(17) 0.0211(6) Uani 1 1 d . . .
N3 N 1.05500(17) 1.0153(3) 0.93479(17) 0.0207(6) Uani 1 1 d . . .
N9 N 1.02912(16) 0.8067(3) 0.89909(16) 0.0181(6) Uani 1 1 d . . .
N1 N 1.20546(18) 1.0574(3) 0.99865(18) 0.0214(6) Uani 1 1 d . . .
H1 H 1.2451 1.1121 1.0228 0.026 Uiso 1 1 calc R . .
N2 N 1.10435(19) 1.2040(3) 0.9788(2) 0.0264(7) Uani 1 1 d . . .
H2A H 1.0507 1.2276 0.9619 0.032 Uiso 1 1 calc R . .
H2B H 1.1472 1.2546 1.0018 0.032 Uiso 1 1 calc R . .
O6 O 1.31173(15) 0.9254(2) 1.01756(16) 0.0275(6) Uani 1 1 d . . .
O12 O 0.87009(16) 0.8507(3) 0.71476(15) 0.0290(6) Uani 1 1 d . . .
O14 O 0.74456(14) 0.7813(2) 0.75204(14) 0.0257(6) Uani 1 1 d . . .
O15 O 0.91764(15) 0.7151(3) 0.91451(14) 0.0265(6) Uani 1 1 d . . .
O17 O 0.9224(2) 0.5012(3) 0.8247(2) 0.0469(8) Uani 1 1 d . . .
H17 H 0.9374 0.4303 0.8288 0.070 Uiso 1 1 calc R . .
O34 O 0.93214(17) 0.2581(3) 0.83850(18) 0.0346(6) Uani 1 1 d . . .
O35 O 0.88765(17) 0.0804(3) 0.85404(18) 0.0316(6) Uani 1 1 d . . .
H35 H 0.9412 0.0679 0.8799 0.047 Uiso 1 1 calc R . .
Si25 Si 0.64019(6) 0.75252(10) 0.70927(6) 0.0274(3) Uani 1 1 d . . .
Si18 Si 0.90706(6) 0.88550(10) 0.64564(6) 0.0266(2) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C4 N3 1.362(5) . ?
C4 N9 1.370(4) . ?
C4 C5 1.372(5) . ?
C2 N3 1.330(4) . ?
C2 N2 1.352(5) . ?
C2 N1 1.369(4) . ?
C8 N7 1.323(4) . ?
C8 N9 1.383(4) . ?
C6 O6 1.233(4) . ?
C6 N1 1.399(5) . ?
C6 C5 1.420(5) . ?
C5 N7 1.383(5) . ?
C11 O12 1.395(4) . ?
C11 C13 1.529(5) . ?
C11 C10 1.535(4) . ?
C14 O15 1.443(4) . ?
C14 C16 1.499(6) . ?
C14 C13 1.531(5) . ?
C10 O15 1.404(4) . ?
C10 N9 1.456(4) . ?
C16 O17 1.433(5) . ?
C13 O14 1.408(4) . ?
C30 C28 1.541(5) . ?
C21 C23 1.509(6) . ?
C21 C22 1.519(6) . ?
C21 C24 1.546(8) . ?
C21 Si18 1.887(4) . ?
C29 C28 1.522(6) . ?
C28 C31 1.548(6) . ?
C28 Si25 1.870(5) . ?
C26 Si25 1.865(5) . ?
C27 Si25 1.859(4) . ?
C19 Si18 1.859(5) . ?
C20 Si18 1.864(4) . ?
C33 O34 1.225(5) . ?
C33 O35 1.305(5) . ?
C33 C32 1.493(5) . ?
O12 Si18 1.646(3) . ?
O14 Si25 1.648(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 C4 N9 126.6(3) . . ?
N3 C4 C5 127.9(3) . . ?
N9 C4 C5 105.5(3) . . ?
N3 C2 N2 118.9(3) . . ?
N3 C2 N1 123.4(3) . . ?
N2 C2 N1 117.7(3) . . ?
N7 C8 N9 111.9(3) . . ?
O6 C6 N1 119.9(3) . . ?
O6 C6 C5 128.7(4) . . ?
N1 C6 C5 111.4(3) . . ?
C4 C5 N7 111.4(3) . . ?
C4 C5 C6 119.4(3) . . ?
N7 C5 C6 129.2(3) . . ?
O12 C11 C13 113.4(3) . . ?
O12 C11 C10 110.5(3) . . ?
C13 C11 C10 101.5(3) . . ?
O15 C14 C16 109.2(3) . . ?
O15 C14 C13 106.6(3) . . ?
C16 C14 C13 114.8(3) . . ?
O15 C10 N9 108.1(3) . . ?
O15 C10 C11 106.7(3) . . ?
N9 C10 C11 113.8(3) . . ?
O17 C16 C14 108.7(3) . . ?
O14 C13 C11 109.3(3) . . ?
O14 C13 C14 112.1(3) . . ?
C11 C13 C14 102.5(3) . . ?
C23 C21 C22 109.1(5) . . ?
C23 C21 C24 109.8(5) . . ?
C22 C21 C24 108.1(6) . . ?
C23 C21 Si18 109.9(3) . . ?
C22 C21 Si18 110.8(3) . . ?
C24 C21 Si18 109.1(3) . . ?
C29 C28 C30 109.8(4) . . ?
C29 C28 C31 108.9(4) . . ?
C30 C28 C31 109.6(3) . . ?
C29 C28 Si25 110.1(3) . . ?
C30 C28 Si25 108.9(3) . . ?
C31 C28 Si25 109.4(3) . . ?
O34 C33 O35 122.8(4) . . ?
O34 C33 C32 123.4(4) . . ?
O35 C33 C32 113.8(4) . . ?
C8 N7 C5 104.3(3) . . ?
C2 N3 C4 112.5(3) . . ?
C4 N9 C8 106.8(3) . . ?
C4 N9 C10 128.8(3) . . ?
C8 N9 C10 124.3(3) . . ?
C2 N1 C6 125.3(3) . . ?
C11 O12 Si18 130.7(2) . . ?
C13 O14 Si25 124.5(2) . . ?
C10 O15 C14 110.1(2) . . ?
O14 Si25 C27 109.13(16) . . ?
O14 Si25 C26 110.21(17) . . ?
C27 Si25 C26 109.3(2) . . ?
O14 Si25 C28 105.32(17) . . ?
C27 Si25 C28 110.7(2) . . ?
C26 Si25 C28 112.1(2) . . ?
O12 Si18 C20 110.33(16) . . ?
O12 Si18 C19 103.85(19) . . ?
C20 Si18 C19 111.6(2) . . ?
O12 Si18 C21 109.80(17) . . ?
C20 Si18 C21 111.2(2) . . ?
C19 Si18 C21 109.8(2) . . ?

_diffrn_measured_fraction_theta_max 0.821
_diffrn_reflns_theta_full        73.19
_diffrn_measured_fraction_theta_full 0.821
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.059

#===END

#========================================================
data_4
_database_code_depnum_ccdc_archive 'CCDC 225961'
#========================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
2',3',5'-O-tris(tert-butyldimethylsilyl)-adenosine
;
_chemical_name_common            
2',3',5'-O-tris(tert-butyldimethylsilyl)-adenosine
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H55 N5 O4 Si3'
_chemical_formula_sum            'C28 H55 N5 O4 Si3'
_chemical_formula_weight         610.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   10.1680(8)
_cell_length_b                   8.0240(6)
_cell_length_c                   22.9470(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.000(4)
_cell_angle_gamma                90.00
_cell_volume                     1872.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    15080
_cell_measurement_theta_min      3.85
_cell_measurement_theta_max      73.03

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             664
_exptl_absorpt_coefficient_mu    1.447
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.9162
_exptl_absorpt_correction_T_max  0.9358
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'MacScience DIPLabo'
_diffrn_measurement_method       IP
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15080
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.85
_diffrn_reflns_theta_max         73.03
_reflns_number_total             3317
_reflns_number_gt                3174
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'MacScience Xpress'
_computing_cell_refinement       Scalepack
_computing_data_reduction        'Denzo and Scalepack'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    maXus
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0716P)²+5.1322P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0026(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(9)
_refine_ls_number_reflns         3317
_refine_ls_number_parameters     367
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0809
_refine_ls_wR_factor_ref         0.1964
_refine_ls_wR_factor_gt          0.1898
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N -0.8832(6) -0.5234(8) -0.4463(2) 0.0406(15) Uani 1 1 d . . .
C2 C -0.8215(7) -0.5548(11) -0.3955(3) 0.0407(18) Uani 1 1 d . . .
H1 H -0.7909 -0.6660 -0.3916 0.049 Uiso 1 1 calc R . .
N3 N -0.7959(6) -0.4582(8) -0.3499(3) 0.0425(15) Uani 1 1 d . . .
C4 C -0.8345(7) -0.3014(9) -0.3613(3) 0.0390(17) Uani 1 1 d . . .
C5 C -0.8973(7) -0.2469(9) -0.4107(3) 0.0339(16) Uani 1 1 d . . .
C6 C -0.9221(7) -0.3623(10) -0.4551(3) 0.0360(15) Uani 1 1 d . . .
N6 N -0.9835(6) -0.3269(8) -0.5053(3) 0.0419(15) Uani 1 1 d . . .
H2 H -0.9975 -0.4060 -0.5311 0.050 Uiso 1 1 calc R . .
H3 H -1.0099 -0.2244 -0.5124 0.050 Uiso 1 1 calc R . .
N7 N -0.9280(6) -0.0757(8) -0.4072(3) 0.0403(15) Uani 1 1 d . . .
C8 C -0.8858(7) -0.0353(10) -0.3563(3) 0.0405(17) Uani 1 1 d . . .
H4 H -0.8918 0.0752 -0.3416 0.049 Uiso 1 1 calc R . .
N9 N -0.8311(6) -0.1645(8) -0.3241(3) 0.0401(15) Uani 1 1 d . . .
C10 C -0.7665(7) -0.1411(10) -0.2687(3) 0.0370(16) Uani 1 1 d . A .
H5 H -0.8058 -0.0412 -0.2493 0.044 Uiso 1 1 calc R . .
C11 C -0.7726(8) -0.2895(10) -0.2254(3) 0.0420(18) Uani 1 1 d D . .
H6 H -0.8357 -0.3759 -0.2397 0.050 Uiso 0.503(7) 1 calc PR A 1
H7 H -0.8399 -0.3748 -0.2363 0.050 Uiso 0.497(7) 1 calc PR A 2
C13 C -0.6319(7) -0.3568(11) -0.2269(3) 0.0398(17) Uani 1 1 d D A .
H8 H -0.6229 -0.4321 -0.2614 0.048 Uiso 0.57(4) 1 calc PR B 3
H9 H -0.6200 -0.4404 -0.2588 0.048 Uiso 0.43(4) 1 calc PR B 4
C15 C -0.5531(8) -0.1992(10) -0.2384(3) 0.0408(18) Uani 1 1 d . . .
H10 H -0.5440 -0.1339 -0.2016 0.049 Uiso 1 1 calc R A .
O16 O -0.6298(5) -0.1084(7) -0.2790(2) 0.0409(13) Uani 1 1 d . A .
C17 C -0.4183(8) -0.2287(11) -0.2650(3) 0.049(2) Uani 1 1 d . A .
H11 H -0.3792 -0.1207 -0.2766 0.059 Uiso 1 1 calc R . .
H12 H -0.3599 -0.2808 -0.2357 0.059 Uiso 1 1 calc R . .
O12B O -0.8178(15) -0.220(2) -0.1724(6) 0.039(4) Uiso 0.503(7) 1 d PD A 1
Si1B Si -0.9667(5) -0.2369(7) -0.1502(2) 0.0483(16) Uani 0.503(7) 1 d P A 1
C20B C -1.033(2) -0.453(3) -0.1546(11) 0.081(7) Uiso 0.503(7) 1 d P A 1
H13 H -0.9795 -0.5271 -0.1306 0.122 Uiso 0.503(7) 1 calc PR A 1
H14 H -1.0313 -0.4907 -0.1952 0.122 Uiso 0.503(7) 1 calc PR A 1
H15 H -1.1242 -0.4537 -0.1404 0.122 Uiso 0.503(7) 1 calc PR A 1
C21B C -1.072(2) -0.095(3) -0.1980(10) 0.069(6) Uiso 0.503(7) 1 d P A 1
H16 H -1.0341 0.0177 -0.1980 0.103 Uiso 0.503(7) 1 calc PR A 1
H17 H -1.1614 -0.0911 -0.1826 0.103 Uiso 0.503(7) 1 calc PR A 1
H18 H -1.0729 -0.1383 -0.2379 0.103 Uiso 0.503(7) 1 calc PR A 1
C22B C -0.9647(16) -0.156(2) -0.0746(7) 0.049(4) Uiso 0.503(7) 1 d P A 1
C23B C -0.920(2) 0.023(3) -0.0709(10) 0.080(7) Uiso 0.503(7) 1 d P A 1
H19 H -0.8320 0.0336 -0.0881 0.120 Uiso 0.503(7) 1 calc PR A 1
H20 H -0.9167 0.0577 -0.0299 0.120 Uiso 0.503(7) 1 calc PR A 1
H21 H -0.9816 0.0945 -0.0922 0.120 Uiso 0.503(7) 1 calc PR A 1
C24B C -0.865(2) -0.269(4) -0.0385(11) 0.085(8) Uiso 0.503(7) 1 d P A 1
H22 H -0.8926 -0.3858 -0.0413 0.127 Uiso 0.503(7) 1 calc PR A 1
H23 H -0.8663 -0.2342 0.0025 0.127 Uiso 0.503(7) 1 calc PR A 1
H24 H -0.7765 -0.2563 -0.0543 0.127 Uiso 0.503(7) 1 calc PR A 1
C25B C -1.1031(19) -0.164(3) -0.0475(9) 0.067(5) Uiso 0.503(7) 1 d P A 1
H25 H -1.1297 -0.2806 -0.0432 0.101 Uiso 0.503(7) 1 calc PR A 1
H26 H -1.1657 -0.1059 -0.0729 0.101 Uiso 0.503(7) 1 calc PR A 1
H27 H -1.1019 -0.1102 -0.0091 0.101 Uiso 0.503(7) 1 calc PR A 1
O12A O -0.7898(15) -0.226(2) -0.1673(6) 0.041(4) Uiso 0.497(7) 1 d P A 2
Si1A Si -0.9053(5) -0.2560(6) -0.1167(2) 0.0408(14) Uani 0.497(7) 1 d P A 2
C20A C -0.823(2) -0.211(3) -0.0473(8) 0.057(5) Uiso 0.497(7) 1 d P A 2
H28 H -0.7466 -0.2850 -0.0428 0.085 Uiso 0.497(7) 1 calc PR A 2
H29 H -0.8842 -0.2292 -0.0151 0.085 Uiso 0.497(7) 1 calc PR A 2
H30 H -0.7930 -0.0948 -0.0470 0.085 Uiso 0.497(7) 1 calc PR A 2
C21A C -0.9610(19) -0.478(2) -0.1260(8) 0.056(5) Uiso 0.497(7) 1 d P A 2
H31 H -0.8854 -0.5527 -0.1219 0.085 Uiso 0.497(7) 1 calc PR A 2
H32 H -0.9999 -0.4919 -0.1648 0.085 Uiso 0.497(7) 1 calc PR A 2
H33 H -1.0267 -0.5045 -0.0962 0.085 Uiso 0.497(7) 1 calc PR A 2
C22A C -1.0535(16) -0.117(2) -0.1259(7) 0.049(4) Uiso 0.497(7) 1 d P A 2
C23A C -1.0101(18) 0.069(3) -0.1215(8) 0.059(5) Uiso 0.497(7) 1 d P A 2
H34 H -0.9700 0.0898 -0.0834 0.089 Uiso 0.497(7) 1 calc PR A 2
H35 H -1.0871 0.1416 -0.1263 0.089 Uiso 0.497(7) 1 calc PR A 2
H36 H -0.9460 0.0939 -0.1523 0.089 Uiso 0.497(7) 1 calc PR A 2
C24A C -1.112(2) -0.151(3) -0.1871(9) 0.069(6) Uiso 0.497(7) 1 d P A 2
H37 H -1.1333 -0.2702 -0.1906 0.104 Uiso 0.497(7) 1 calc PR A 2
H38 H -1.0477 -0.1208 -0.2170 0.104 Uiso 0.497(7) 1 calc PR A 2
H39 H -1.1922 -0.0853 -0.1923 0.104 Uiso 0.497(7) 1 calc PR A 2
C25A C -1.156(2) -0.157(4) -0.0769(11) 0.091(7) Uiso 0.497(7) 1 d P A 2
H40 H -1.1809 -0.2747 -0.0790 0.137 Uiso 0.497(7) 1 calc PR A 2
H41 H -1.2343 -0.0873 -0.0823 0.137 Uiso 0.497(7) 1 calc PR A 2
H42 H -1.1170 -0.1335 -0.0387 0.137 Uiso 0.497(7) 1 calc PR A 2
O14A O -0.5776(15) -0.4414(15) -0.1761(4) 0.031(3) Uiso 0.57(4) 1 d PD A 3
Si2A Si -0.5505(9) -0.6341(15) -0.1726(3) 0.047(4) Uani 0.57(4) 1 d P A 3
C27A C -0.423(3) -0.694(4) -0.2238(11) 0.080(8) Uiso 0.57(4) 1 d P A 3
H43 H -0.3410 -0.6349 -0.2141 0.119 Uiso 0.57(4) 1 calc PR B 3
H44 H -0.4499 -0.6637 -0.2634 0.119 Uiso 0.57(4) 1 calc PR B 3
H45 H -0.4080 -0.8140 -0.2215 0.119 Uiso 0.57(4) 1 calc PR B 3
C28A C -0.717(3) -0.750(3) -0.1936(10) 0.070(6) Uiso 0.57(4) 1 d P A 3
H46 H -0.7387 -0.7260 -0.2343 0.105 Uiso 0.57(4) 1 calc PR B 3
H47 H -0.7877 -0.7110 -0.1682 0.105 Uiso 0.57(4) 1 calc PR B 3
H48 H -0.7052 -0.8706 -0.1886 0.105 Uiso 0.57(4) 1 calc PR B 3
C30A C -0.386(3) -0.567(4) -0.0813(12) 0.087(8) Uiso 0.57(4) 1 d P B 3
H49 H -0.4110 -0.4489 -0.0821 0.130 Uiso 0.57(4) 1 calc PR B 3
H50 H -0.3196 -0.5880 -0.1113 0.130 Uiso 0.57(4) 1 calc PR B 3
H51 H -0.3499 -0.5946 -0.0430 0.130 Uiso 0.57(4) 1 calc PR B 3
C31A C -0.476(2) -0.862(3) -0.0888(8) 0.058(6) Uiso 0.57(4) 1 d P B 3
H70 H -0.4019 -0.8869 -0.1145 0.087 Uiso 0.43(4) 1 calc PR B 3
H71 H -0.5524 -0.9293 -0.1004 0.087 Uiso 0.43(4) 1 calc PR B 3
H72 H -0.4525 -0.8883 -0.0485 0.087 Uiso 0.43(4) 1 calc PR B 3
C32 C -0.6297(11) -0.6563(16) -0.0549(4) 0.082(3) Uani 1 1 d D B .
H88 H -0.6875 -0.7533 -0.0590 0.122 Uiso 1 1 calc R . .
H89 H -0.6774 -0.5553 -0.0663 0.122 Uiso 1 1 calc R . .
H90 H -0.6013 -0.6463 -0.0142 0.122 Uiso 1 1 calc R . .
O14B O -0.609(2) -0.428(2) -0.1716(6) 0.032(4) Uiso 0.43(4) 1 d PD A 4
Si2B Si -0.5535(13) -0.635(2) -0.1730(6) 0.060(6) Uani 0.43(4) 1 d P A 4
C27B C -0.394(2) -0.654(3) -0.2146(10) 0.043(6) Uiso 0.43(4) 1 d P A 4
H61 H -0.3284 -0.5798 -0.1973 0.064 Uiso 0.43(4) 1 calc PR B 4
H62 H -0.4087 -0.6229 -0.2554 0.064 Uiso 0.43(4) 1 calc PR B 4
H63 H -0.3627 -0.7694 -0.2127 0.064 Uiso 0.43(4) 1 calc PR B 4
C28B C -0.676(2) -0.760(3) -0.2027(9) 0.033(5) Uiso 0.43(4) 1 d P A 4
H64 H -0.6881 -0.7318 -0.2439 0.050 Uiso 0.43(4) 1 calc PR B 4
H65 H -0.7587 -0.7416 -0.1816 0.050 Uiso 0.43(4) 1 calc PR B 4
H66 H -0.6507 -0.8776 -0.1993 0.050 Uiso 0.43(4) 1 calc PR B 4
C29 C -0.5110(9) -0.6777(13) -0.0935(4) 0.058(2) Uiso 1 1 d D . .
C30B C -0.420(3) -0.540(3) -0.0669(10) 0.045(6) Uiso 0.43(4) 1 d P B 4
H67 H -0.3370 -0.5364 -0.0884 0.068 Uiso 0.43(4) 1 calc PR B 4
H68 H -0.4027 -0.5659 -0.0259 0.068 Uiso 0.43(4) 1 calc PR B 4
H69 H -0.4641 -0.4316 -0.0697 0.068 Uiso 0.43(4) 1 calc PR B 4
C31B C -0.429(3) -0.843(3) -0.0887(10) 0.056(7) Uiso 0.43(4) 1 d P B 4
H52 H -0.4823 -0.9372 -0.1018 0.084 Uiso 0.57(4) 1 calc PR B 4
H53 H -0.4023 -0.8605 -0.0481 0.084 Uiso 0.57(4) 1 calc PR B 4
H54 H -0.3500 -0.8341 -0.1132 0.084 Uiso 0.57(4) 1 calc PR B 4
O18 O -0.4285(5) -0.3352(7) -0.3150(2) 0.0487(14) Uani 1 1 d . . .
Si3 Si -0.3164(2) -0.3530(3) -0.36574(10) 0.0519(6) Uani 1 1 d . A .
C33 C -0.2740(10) -0.1440(15) -0.3948(4) 0.075(3) Uani 1 1 d . . .
H73 H -0.3534 -0.0904 -0.4101 0.113 Uiso 1 1 calc R A .
H74 H -0.2092 -0.1557 -0.4261 0.113 Uiso 1 1 calc R . .
H75 H -0.2369 -0.0755 -0.3635 0.113 Uiso 1 1 calc R . .
C34 C -0.1670(9) -0.4560(16) -0.3346(4) 0.071(3) Uani 1 1 d . . .
H76 H -0.1267 -0.3824 -0.3055 0.106 Uiso 1 1 calc R A .
H77 H -0.1038 -0.4782 -0.3659 0.106 Uiso 1 1 calc R . .
H78 H -0.1923 -0.5612 -0.3160 0.106 Uiso 1 1 calc R . .
C35 C -0.3956(9) -0.4898(14) -0.4218(4) 0.061(3) Uani 1 1 d . . .
C36 C -0.5115(9) -0.3955(16) -0.4503(4) 0.074(3) Uani 1 1 d . A .
H79 H -0.4788 -0.2939 -0.4690 0.111 Uiso 1 1 calc R . .
H80 H -0.5761 -0.3658 -0.4203 0.111 Uiso 1 1 calc R . .
H81 H -0.5532 -0.4670 -0.4796 0.111 Uiso 1 1 calc R . .
C37 C -0.4470(10) -0.6495(14) -0.3947(4) 0.070(3) Uani 1 1 d . A .
H82 H -0.3747 -0.7083 -0.3754 0.106 Uiso 1 1 calc R . .
H83 H -0.4844 -0.7207 -0.4252 0.106 Uiso 1 1 calc R . .
H84 H -0.5153 -0.6227 -0.3660 0.106 Uiso 1 1 calc R . .
C38 C -0.2956(10) -0.5307(18) -0.4700(4) 0.086(4) Uani 1 1 d . A .
H85 H -0.2632 -0.4269 -0.4874 0.129 Uiso 1 1 calc R . .
H86 H -0.3382 -0.5984 -0.5001 0.129 Uiso 1 1 calc R . .
H87 H -0.2217 -0.5928 -0.4533 0.129 Uiso 1 1 calc R . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C2 1.347(9) . ?
N1 C6 1.367(10) . ?
C2 N3 1.329(9) . ?
N3 C4 1.344(10) . ?
C4 C5 1.371(9) . ?
C4 N9 1.391(9) . ?
C5 C6 1.400(9) . ?
C5 N7 1.411(9) . ?
C6 N6 1.340(9) . ?
N7 C8 1.287(9) . ?
C8 N9 1.388(9) . ?
N9 C10 1.445(8) . ?
C10 O16 1.434(8) . ?
C10 C11 1.552(10) . ?
C11 O12B 1.415(13) . ?
C11 O12A 1.439(17) . ?
C11 C13 1.530(10) . ?
C13 O14B 1.411(13) . ?
C13 O14A 1.458(11) . ?
C13 C15 1.520(10) . ?
C15 O16 1.416(8) . ?
C15 C17 1.519(11) . ?
C17 O18 1.434(9) . ?
O12B Si1B 1.604(15) . ?
Si1B C22B 1.852(17) . ?
Si1B C20B 1.86(3) . ?
Si1B C21B 1.91(2) . ?
C22B C23B 1.51(3) . ?
C22B C25B 1.54(3) . ?
C22B C24B 1.59(3) . ?
O12A Si1A 1.669(16) . ?
Si1A C20A 1.837(19) . ?
Si1A C21A 1.88(2) . ?
Si1A C22A 1.885(18) . ?
C22A C24A 1.55(3) . ?
C22A C23A 1.56(3) . ?
C22A C25A 1.57(3) . ?
O14A Si2A 1.573(18) . ?
Si2A C27A 1.81(3) . ?
Si2A C29 1.892(11) . ?
Si2A C28A 1.99(3) . ?
C30A C29 1.58(3) . ?
C31A C29 1.52(2) . ?
C32 C29 1.507(11) . ?
O14B Si2B 1.76(2) . ?
Si2B C28B 1.74(3) . ?
Si2B C27B 1.89(2) . ?
Si2B C29 1.905(16) . ?
C29 C30B 1.56(2) . ?
C29 C31B 1.57(3) . ?
O18 Si3 1.635(6) . ?
Si3 C33 1.855(11) . ?
Si3 C34 1.872(10) . ?
Si3 C35 1.872(10) . ?
C35 C37 1.517(14) . ?
C35 C38 1.538(12) . ?
C35 C36 1.546(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N1 C6 116.1(6) . . ?
N3 C2 N1 131.6(8) . . ?
C2 N3 C4 109.5(6) . . ?
N3 C4 C5 126.6(7) . . ?
N3 C4 N9 127.7(7) . . ?
C5 C4 N9 105.4(6) . . ?
C4 C5 C6 118.3(7) . . ?
C4 C5 N7 111.5(6) . . ?
C6 C5 N7 130.1(6) . . ?
N6 C6 N1 117.6(7) . . ?
N6 C6 C5 124.7(7) . . ?
N1 C6 C5 117.7(6) . . ?
C8 N7 C5 102.8(6) . . ?
N7 C8 N9 115.3(7) . . ?
C8 N9 C4 104.7(6) . . ?
C8 N9 C10 123.5(6) . . ?
C4 N9 C10 130.9(6) . . ?
O16 C10 N9 108.6(5) . . ?
O16 C10 C11 106.5(6) . . ?
N9 C10 C11 116.5(6) . . ?
O12B C11 O12A 12.5(9) . . ?
O12B C11 C13 117.6(8) . . ?
O12A C11 C13 105.1(8) . . ?
O12B C11 C10 105.0(9) . . ?
O12A C11 C10 109.0(9) . . ?
C13 C11 C10 102.6(6) . . ?
O14B C13 O14A 13.9(8) . . ?
O14B C13 C15 113.8(8) . . ?
O14A C13 C15 109.1(7) . . ?
O14B C13 C11 106.1(10) . . ?
O14A C13 C11 120.0(9) . . ?
C15 C13 C11 101.7(7) . . ?
O16 C15 C17 108.3(6) . . ?
O16 C15 C13 104.6(6) . . ?
C17 C15 C13 114.6(7) . . ?
C15 O16 C10 109.4(5) . . ?
O18 C17 C15 110.4(6) . . ?
C11 O12B Si1B 123.1(10) . . ?
O12B Si1B C22B 104.9(7) . . ?
O12B Si1B C20B 114.0(10) . . ?
C22B Si1B C20B 112.4(10) . . ?
O12B Si1B C21B 107.0(9) . . ?
C22B Si1B C21B 109.5(9) . . ?
C20B Si1B C21B 108.7(11) . . ?
C23B C22B C25B 107.0(17) . . ?
C23B C22B C24B 108.8(17) . . ?
C25B C22B C24B 110.2(17) . . ?
C23B C22B Si1B 113.0(14) . . ?
C25B C22B Si1B 110.7(12) . . ?
C24B C22B Si1B 107.2(14) . . ?
C11 O12A Si1A 132.7(11) . . ?
O12A Si1A C20A 104.6(9) . . ?
O12A Si1A C21A 105.7(8) . . ?
C20A Si1A C21A 115.0(9) . . ?
O12A Si1A C22A 113.5(8) . . ?
C20A Si1A C22A 110.2(9) . . ?
C21A Si1A C22A 107.9(8) . . ?
C24A C22A C23A 109.7(16) . . ?
C24A C22A C25A 111.0(16) . . ?
C23A C22A C25A 109.7(17) . . ?
C24A C22A Si1A 107.6(13) . . ?
C23A C22A Si1A 109.5(12) . . ?
C25A C22A Si1A 109.4(14) . . ?
C13 O14A Si2A 124.4(9) . . ?
O14A Si2A C27A 110.6(11) . . ?
O14A Si2A C29 105.5(7) . . ?
C27A Si2A C29 114.8(10) . . ?
O14A Si2A C28A 107.4(9) . . ?
C27A Si2A C28A 109.2(12) . . ?
C29 Si2A C28A 109.0(9) . . ?
C13 O14B Si2B 114.7(12) . . ?
C28B Si2B O14B 108.9(11) . . ?
C28B Si2B C27B 111.8(12) . . ?
O14B Si2B C27B 111.0(12) . . ?
C28B Si2B C29 115.8(11) . . ?
O14B Si2B C29 102.9(8) . . ?
C27B Si2B C29 106.0(10) . . ?
C32 C29 C31A 104.7(11) . . ?
C32 C29 C30B 99.3(13) . . ?
C31A C29 C30B 121.4(13) . . ?
C32 C29 C31B 118.8(13) . . ?
C31A C29 C31B 18.8(12) . . ?
C30B C29 C31B 104.7(14) . . ?
C32 C29 C30A 118.5(15) . . ?
C31A C29 C30A 110.4(13) . . ?
C30B C29 C30A 19.3(12) . . ?
C31B C29 C30A 92.0(14) . . ?
C32 C29 Si2A 111.9(7) . . ?
C31A C29 Si2A 107.2(10) . . ?
C30B C29 Si2A 111.7(11) . . ?
C31B C29 Si2A 109.6(10) . . ?
C30A C29 Si2A 103.7(12) . . ?
C32 C29 Si2B 111.2(7) . . ?
C31A C29 Si2B 107.0(10) . . ?
C30B C29 Si2B 112.5(11) . . ?
C31B C29 Si2B 109.7(11) . . ?
C30A C29 Si2B 104.6(12) . . ?
Si2A C29 Si2B 0.9(7) . . ?
C17 O18 Si3 124.9(5) . . ?
O18 Si3 C33 109.8(4) . . ?
O18 Si3 C34 109.4(4) . . ?
C33 Si3 C34 110.3(5) . . ?
O18 Si3 C35 103.9(3) . . ?
C33 Si3 C35 112.5(5) . . ?
C34 Si3 C35 110.6(5) . . ?
C37 C35 C38 110.0(10) . . ?
C37 C35 C36 108.9(8) . . ?
C38 C35 C36 107.7(8) . . ?
C37 C35 Si3 111.2(6) . . ?
C38 C35 Si3 109.6(7) . . ?
C36 C35 Si3 109.3(7) . . ?

_diffrn_measured_fraction_theta_max 0.672
_diffrn_reflns_theta_full        73.03
_diffrn_measured_fraction_theta_full 0.672
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.072

#===END

#========================================================
data_5
_database_code_depnum_ccdc_archive 'CCDC 225962'
#========================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
2',3'-O-bis(tert-butyldimethylsilyl)-adenosine
;
_chemical_name_common            
2',3'-O-bis(tert-butyldimethylsilyl)-adenosine
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H41 N5 O4 Si2'
_chemical_formula_sum            'C22 H41 N5 O4 Si2'
_chemical_formula_weight         495.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   16.428(4)
_cell_length_b                   7.794(6)
_cell_length_c                   23.465(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.988(16)
_cell_angle_gamma                90.00
_cell_volume                     2902(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    24
_cell_measurement_theta_min      11.1
_cell_measurement_theta_max      13.8

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.410
_exptl_crystal_size_min          0.080
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1072.00
_exptl_absorpt_coefficient_mu    0.155
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_T_max  1.000

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_detector       'scintillation counter'
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       ω

_diffrn_standards_number         3
_diffrn_standards_interval_count 150
_diffrn_standards_decay_%        0.01
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
3 0 -4
1 -1 2
2 -1 0

_diffrn_reflns_number            7376
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.57
_diffrn_reflns_theta_max         27.47
_reflns_number_total             7133
_reflns_number_gt                3767
_reflns_threshold_expression     >2sigma(I)

_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_orient_matrix_UB_11      0.06230
_diffrn_orient_matrix_UB_12      0.01535
_diffrn_orient_matrix_UB_13      0.01499
_diffrn_orient_matrix_UB_21      -0.00691
_diffrn_orient_matrix_UB_22      0.02530
_diffrn_orient_matrix_UB_23      0.04027
_diffrn_orient_matrix_UB_31      0.00626
_diffrn_orient_matrix_UB_32      -0.12484
_diffrn_orient_matrix_UB_33      0.01000

_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    teXsan
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0570P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.13(15)
_refine_ls_number_reflns         7133
_refine_ls_number_parameters     616
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1288
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.1288
_refine_ls_wR_factor_gt          0.1035
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_restrained_S_all      0.988
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N -0.5610(2) 0.4336(5) -0.45155(15) 0.0588(10) Uani 1 1 d . . .
C1 C -0.5947(3) 0.4716(6) -0.40724(19) 0.0607(12) Uani 1 1 d . . .
H1A H -0.6125 0.5845 -0.4063 0.073 Uiso 1 1 calc R . .
N2 N -0.6065(2) 0.3724(4) -0.36437(14) 0.0481(9) Uani 1 1 d . . .
C2 C -0.5815(2) 0.2111(5) -0.37107(17) 0.0382(9) Uani 1 1 d . . .
C3 C -0.5477(2) 0.1529(5) -0.41489(18) 0.0430(10) Uani 1 1 d . . .
C4 C -0.5360(3) 0.2698(6) -0.45647(17) 0.0482(10) Uani 1 1 d . . .
N3 N -0.5016(3) 0.2347(5) -0.50016(18) 0.0671(10) Uani 1 1 d . . .
H3A H -0.4958 0.3144 -0.5241 0.080 Uiso 1 1 calc R . .
H3B H -0.4850 0.1321 -0.5046 0.080 Uiso 1 1 calc R . .
N4 N -0.5290(2) -0.0199(5) -0.40755(15) 0.0545(10) Uani 1 1 d . . .
C5 C -0.5516(3) -0.0603(6) -0.36006(18) 0.0517(11) Uani 1 1 d . . .
H5A H -0.5461 -0.1703 -0.3442 0.062 Uiso 1 1 calc R . .
N5 N -0.58411(19) 0.0737(4) -0.33584(13) 0.0411(7) Uani 1 1 d . . .
C6 C -0.6209(2) 0.0646(6) -0.28566(15) 0.0403(9) Uani 1 1 d . . .
H6A H -0.6196 0.1784 -0.2677 0.048 Uiso 1 1 calc R . .
C7 C -0.7096(2) -0.0047(5) -0.30092(15) 0.0409(9) Uani 1 1 d . . .
H7A H -0.7141 -0.0999 -0.3288 0.049 Uiso 1 1 calc R . .
O1 O -0.76943(15) 0.1207(4) -0.32529(11) 0.0499(7) Uani 1 1 d . . .
C8 C -0.7140(2) -0.0748(5) -0.24091(15) 0.0430(9) Uani 1 1 d . . .
H8 H -0.7593 -0.1590 -0.2444 0.052 Uiso 1 1 calc R . .
O2 O -0.72180(16) 0.0637(4) -0.20424(11) 0.0528(7) Uani 1 1 d . . .
C9 C -0.6273(2) -0.1556(6) -0.21992(16) 0.0462(10) Uani 1 1 d . . .
H9A H -0.6091 -0.1458 -0.1769 0.055 Uiso 1 1 calc R . .
O3 O -0.57231(15) -0.0503(4) -0.24469(11) 0.0488(7) Uani 1 1 d . . .
C10 C -0.6205(3) -0.3395(6) -0.2361(2) 0.0588(12) Uani 1 1 d . . .
H10A H -0.5615 -0.3714 -0.2280 0.071 Uiso 1 1 calc R . .
H10B H -0.6467 -0.4114 -0.2121 0.071 Uiso 1 1 calc R . .
O4 O -0.6598(2) -0.3667(4) -0.29591(14) 0.0730(10) Uani 1 1 d . . .
H4O H -0.6426 -0.4567 -0.3067 0.110 Uiso 1 1 calc R . .
Si1 Si -0.84398(8) 0.08214(18) -0.38606(5) 0.0538(3) Uani 1 1 d . . .
C11 C -0.7949(3) 0.0065(10) -0.4444(2) 0.100(2) Uani 1 1 d . . .
H11A H -0.7532 0.0879 -0.4491 0.149 Uiso 1 1 calc R . .
H11B H -0.8374 -0.0046 -0.4810 0.149 Uiso 1 1 calc R . .
H11C H -0.7686 -0.1028 -0.4334 0.149 Uiso 1 1 calc R . .
C12 C -0.9139(3) -0.0888(8) -0.3713(2) 0.0873(17) Uani 1 1 d . . .
H12A H -0.8813 -0.1897 -0.3575 0.131 Uiso 1 1 calc R . .
H12B H -0.9560 -0.1151 -0.4070 0.131 Uiso 1 1 calc R . .
H12C H -0.9408 -0.0503 -0.3418 0.131 Uiso 1 1 calc R . .
C13 C -0.8997(3) 0.2890(7) -0.4054(2) 0.0708(14) Uani 1 1 d . . .
C14 C -0.8385(4) 0.4275(9) -0.4152(3) 0.111(2) Uani 1 1 d . . .
H14A H -0.8697 0.5278 -0.4318 0.167 Uiso 1 1 calc R . .
H14B H -0.8076 0.3851 -0.4419 0.167 Uiso 1 1 calc R . .
H14C H -0.8000 0.4563 -0.3782 0.167 Uiso 1 1 calc R . .
C15 C -0.9693(4) 0.2682(10) -0.4629(3) 0.127(3) Uani 1 1 d . . .
H15A H -1.0066 0.1772 -0.4585 0.190 Uiso 1 1 calc R . .
H15B H -0.9444 0.2411 -0.4946 0.190 Uiso 1 1 calc R . .
H15C H -1.0006 0.3733 -0.4717 0.190 Uiso 1 1 calc R . .
C16 C -0.9394(4) 0.3460(10) -0.3570(3) 0.129(3) Uani 1 1 d . . .
H16A H -0.9737 0.4455 -0.3699 0.194 Uiso 1 1 calc R . .
H16B H -0.8960 0.3734 -0.3222 0.194 Uiso 1 1 calc R . .
H16C H -0.9738 0.2551 -0.3484 0.194 Uiso 1 1 calc R . .
Si2 Si -0.78225(10) 0.0771(2) -0.15949(6) 0.0728(4) Uani 1 1 d . . .
C17 C -0.8911(4) 0.0161(11) -0.1991(3) 0.138(3) Uani 1 1 d . . .
H17A H -0.9122 0.0950 -0.2309 0.207 Uiso 1 1 calc R . .
H17B H -0.9265 0.0197 -0.1723 0.207 Uiso 1 1 calc R . .
H17C H -0.8911 -0.0979 -0.2146 0.207 Uiso 1 1 calc R . .
C18 C -0.7420(6) -0.0692(10) -0.0963(3) 0.148(3) Uani 1 1 d . . .
H18A H -0.7603 -0.1841 -0.1075 0.222 Uiso 1 1 calc R . .
H18B H -0.7632 -0.0339 -0.0637 0.222 Uiso 1 1 calc R . .
H18C H -0.6815 -0.0654 -0.0849 0.222 Uiso 1 1 calc R . .
C19 C -0.7748(5) 0.3073(8) -0.1367(2) 0.0931(19) Uani 1 1 d . . .
C20 C -0.8070(4) 0.4210(9) -0.1899(3) 0.108(2) Uani 1 1 d . . .
H20A H -0.8651 0.3948 -0.2078 0.162 Uiso 1 1 calc R . .
H20B H -0.7744 0.4015 -0.2178 0.162 Uiso 1 1 calc R . .
H20C H -0.8020 0.5391 -0.1778 0.162 Uiso 1 1 calc R . .
C21 C -0.6840(5) 0.3534(10) -0.1084(3) 0.138(3) Uani 1 1 d . . .
H21A H -0.6797 0.4743 -0.1004 0.207 Uiso 1 1 calc R . .
H21B H -0.6500 0.3241 -0.1347 0.207 Uiso 1 1 calc R . .
H21C H -0.6646 0.2910 -0.0721 0.207 Uiso 1 1 calc R . .
C22 C -0.8293(6) 0.3360(11) -0.0933(3) 0.187(4) Uani 1 1 d . . .
H22A H -0.8399 0.4564 -0.0906 0.280 Uiso 1 1 calc R . .
H22B H -0.8002 0.2932 -0.0551 0.280 Uiso 1 1 calc R . .
H22C H -0.8818 0.2762 -0.1071 0.280 Uiso 1 1 calc R . .
N6 N -0.4361(2) -0.5987(5) -0.04266(17) 0.0655(11) Uani 1 1 d . . .
C23 C -0.4010(3) -0.6439(6) -0.0854(2) 0.0724(15) Uani 1 1 d . . .
H23A H -0.3848 -0.7583 -0.0848 0.087 Uiso 1 1 calc R . .
N7 N -0.3855(2) -0.5519(5) -0.12838(17) 0.0627(11) Uani 1 1 d . . .
C24 C -0.4065(3) -0.3883(6) -0.12359(18) 0.0461(10) Uani 1 1 d . . .
C25 C -0.4406(2) -0.3203(5) -0.08073(17) 0.0435(10) Uani 1 1 d . . .
C26 C -0.4583(3) -0.4346(6) -0.03907(18) 0.0515(11) Uani 1 1 d . . .
N8 N -0.4957(3) -0.3934(5) 0.00192(18) 0.0702(11) Uani 1 1 d . . .
H8A H -0.5053 -0.4707 0.0255 0.084 Uiso 1 1 calc R . .
H8B H -0.5107 -0.2889 0.0053 0.084 Uiso 1 1 calc R . .
N9 N -0.4542(2) -0.1452(5) -0.08927(14) 0.0475(9) Uani 1 1 d . . .
C27 C -0.4279(2) -0.1129(5) -0.13604(16) 0.0444(10) Uani 1 1 d . . .
H27A H -0.4295 -0.0040 -0.1525 0.053 Uiso 1 1 calc R . .
N10 N -0.39778(19) -0.2534(5) -0.15859(13) 0.0454(8) Uani 1 1 d . . .
C28 C -0.3680(2) -0.2578(6) -0.21136(15) 0.0455(10) Uani 1 1 d . . .
H28A H -0.3708 -0.1421 -0.2281 0.055 Uiso 1 1 calc R . .
C29 C -0.2796(2) -0.3271(6) -0.20207(16) 0.0463(10) Uani 1 1 d . . .
H29A H -0.2714 -0.4250 -0.1750 0.056 Uiso 1 1 calc R . .
O5 O -0.21965(16) -0.2023(4) -0.17978(11) 0.0572(8) Uani 1 1 d . . .
C30 C -0.2819(2) -0.3892(7) -0.26438(16) 0.0530(11) Uani 1 1 d . . .
H30A H -0.2395 -0.4782 -0.2637 0.064 Uiso 1 1 calc R . .
O6 O -0.27086(17) -0.2490(5) -0.29842(12) 0.0655(9) Uani 1 1 d . . .
C31 C -0.3714(3) -0.4613(7) -0.2848(2) 0.0652(14) Uani 1 1 d . . .
H31A H -0.3935 -0.4338 -0.3267 0.078 Uiso 1 1 calc R . .
O7 O -0.42036(15) -0.3667(4) -0.25197(11) 0.0580(8) Uani 1 1 d . . .
C32 C -0.3817(3) -0.6491(8) -0.2772(3) 0.0831(17) Uani 1 1 d . . .
H32A H -0.4412 -0.6737 -0.2831 0.100 Uiso 1 1 calc R . .
H32B H -0.3629 -0.7092 -0.3077 0.100 Uiso 1 1 calc R . .
O8 O -0.3378(2) -0.7138(5) -0.22220(16) 0.0801(10) Uani 1 1 d . . .
H8O H -0.3529 -0.6634 -0.1960 0.120 Uiso 1 1 calc R . .
Si3 Si -0.14306(8) -0.21261(19) -0.11909(6) 0.0577(3) Uani 1 1 d . . .
C33 C -0.1747(4) -0.3487(8) -0.0641(2) 0.0860(17) Uani 1 1 d . . .
H33A H -0.2261 -0.3054 -0.0572 0.129 Uiso 1 1 calc R . .
H33B H -0.1312 -0.3473 -0.0278 0.129 Uiso 1 1 calc R . .
H33C H -0.1834 -0.4642 -0.0786 0.129 Uiso 1 1 calc R . .
C34 C -0.0483(3) -0.3069(9) -0.1365(3) 0.105(2) Uani 1 1 d . . .
H34A H -0.0574 -0.4272 -0.1445 0.158 Uiso 1 1 calc R . .
H34B H -0.0003 -0.2915 -0.1035 0.158 Uiso 1 1 calc R . .
H34C H -0.0385 -0.2508 -0.1705 0.158 Uiso 1 1 calc R . .
C35 C -0.1262(3) 0.0132(7) -0.0931(2) 0.0759(15) Uani 1 1 d . . .
C36 C -0.2029(4) 0.0828(9) -0.0772(3) 0.110(2) Uani 1 1 d . . .
H36A H -0.2162 0.0114 -0.0475 0.165 Uiso 1 1 calc R . .
H36B H -0.2496 0.0840 -0.1116 0.165 Uiso 1 1 calc R . .
H36C H -0.1918 0.1975 -0.0623 0.165 Uiso 1 1 calc R . .
C37 C -0.0505(4) 0.0231(10) -0.0396(3) 0.143(3) Uani 1 1 d . . .
H37A H -0.0453 0.1376 -0.0241 0.215 Uiso 1 1 calc R . .
H37B H -0.0003 -0.0066 -0.0512 0.215 Uiso 1 1 calc R . .
H37C H -0.0581 -0.0556 -0.0100 0.215 Uiso 1 1 calc R . .
C38 C -0.1093(4) 0.1268(8) -0.1419(3) 0.114(2) Uani 1 1 d . . .
H38A H -0.0607 0.0850 -0.1531 0.171 Uiso 1 1 calc R . .
H38B H -0.0993 0.2425 -0.1278 0.171 Uiso 1 1 calc R . .
H38C H -0.1573 0.1242 -0.1755 0.171 Uiso 1 1 calc R . .
Si4 Si -0.21811(10) -0.2458(3) -0.34837(7) 0.0835(5) Uani 1 1 d . . .
C39 C -0.1095(4) -0.3256(13) -0.3161(4) 0.157(4) Uani 1 1 d . . .
H39A H -0.0754 -0.3023 -0.3428 0.235 Uiso 1 1 calc R . .
H39B H -0.1111 -0.4471 -0.3097 0.235 Uiso 1 1 calc R . .
H39C H -0.0860 -0.2688 -0.2792 0.235 Uiso 1 1 calc R . .
C40 C -0.2723(6) -0.3895(12) -0.4103(3) 0.155(3) Uani 1 1 d . . .
H40A H -0.2624 -0.5070 -0.3982 0.232 Uiso 1 1 calc R . .
H40B H -0.2505 -0.3685 -0.4439 0.232 Uiso 1 1 calc R . .
H40C H -0.3317 -0.3667 -0.4205 0.232 Uiso 1 1 calc R . .
C41 C -0.2199(3) -0.0191(9) -0.3711(2) 0.0881(18) Uani 1 1 d . . .
C42 C -0.3116(4) 0.0405(10) -0.3939(3) 0.108(2) Uani 1 1 d . . .
H42A H -0.3126 0.1569 -0.4075 0.162 Uiso 1 1 calc R . .
H42B H -0.3392 0.0340 -0.3625 0.162 Uiso 1 1 calc R . .
H42C H -0.3403 -0.0320 -0.4258 0.162 Uiso 1 1 calc R . .
C43 C -0.1777(5) 0.0957(12) -0.3184(3) 0.142(3) Uani 1 1 d . . .
H43A H -0.1275 0.0408 -0.2955 0.213 Uiso 1 1 calc R . .
H43B H -0.2159 0.1135 -0.2941 0.213 Uiso 1 1 calc R . .
H43C H -0.1634 0.2042 -0.3325 0.213 Uiso 1 1 calc R . .
C44 C -0.1776(5) 0.0053(12) -0.4209(3) 0.151(3) Uani 1 1 d . . .
H44A H -0.1700 0.1255 -0.4268 0.226 Uiso 1 1 calc R . .
H44B H -0.2123 -0.0436 -0.4565 0.226 Uiso 1 1 calc R . .
H44C H -0.1237 -0.0507 -0.4110 0.226 Uiso 1 1 calc R . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.331(5) . ?
N1 C4 1.355(6) . ?
C1 N2 1.322(5) . ?
N2 C2 1.345(5) . ?
C2 N5 1.360(5) . ?
C2 C3 1.366(5) . ?
C3 N4 1.383(5) . ?
C3 C4 1.384(6) . ?
C4 N3 1.321(5) . ?
N4 C5 1.301(5) . ?
C5 N5 1.362(5) . ?
N5 C6 1.457(4) . ?
C6 O3 1.402(4) . ?
C6 C7 1.508(5) . ?
C7 O1 1.400(4) . ?
C7 C8 1.529(5) . ?
O1 Si1 1.649(3) . ?
C8 O2 1.407(5) . ?
C8 C9 1.518(5) . ?
O2 Si2 1.625(3) . ?
C9 O3 1.449(4) . ?
C9 C10 1.494(7) . ?
C10 O4 1.402(5) . ?
Si1 C12 1.849(6) . ?
Si1 C13 1.852(6) . ?
Si1 C11 1.856(5) . ?
C13 C16 1.515(7) . ?
C13 C14 1.533(8) . ?
C13 C15 1.535(7) . ?
Si2 C18 1.851(7) . ?
Si2 C17 1.852(6) . ?
Si2 C19 1.868(7) . ?
C19 C21 1.510(9) . ?
C19 C20 1.511(8) . ?
C19 C22 1.536(7) . ?
N6 C23 1.327(5) . ?
N6 C26 1.338(6) . ?
C23 N7 1.315(5) . ?
N7 C24 1.334(6) . ?
C24 N10 1.364(5) . ?
C24 C25 1.378(5) . ?
C25 N9 1.389(5) . ?
C25 C26 1.407(6) . ?
C26 N8 1.308(5) . ?
N9 C27 1.304(5) . ?
C27 N10 1.364(5) . ?
N10 C28 1.445(4) . ?
C28 O7 1.394(5) . ?
C28 C29 1.511(5) . ?
C29 O5 1.386(5) . ?
C29 C30 1.531(5) . ?
O5 Si3 1.640(3) . ?
C30 O6 1.393(6) . ?
C30 C31 1.531(6) . ?
O6 Si4 1.628(3) . ?
C31 O7 1.450(5) . ?
C31 C32 1.489(8) . ?
C32 O8 1.401(6) . ?
Si3 C33 1.847(5) . ?
Si3 C35 1.860(6) . ?
Si3 C34 1.860(5) . ?
C35 C36 1.505(7) . ?
C35 C37 1.523(7) . ?
C35 C38 1.529(8) . ?
Si4 C41 1.844(7) . ?
Si4 C39 1.856(6) . ?
Si4 C40 1.867(8) . ?
C41 C44 1.518(7) . ?
C41 C42 1.534(8) . ?
C41 C43 1.539(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C4 118.2(4) . . ?
N2 C1 N1 129.6(4) . . ?
C1 N2 C2 110.4(3) . . ?
N2 C2 N5 127.3(3) . . ?
N2 C2 C3 126.5(4) . . ?
N5 C2 C3 106.2(3) . . ?
C2 C3 N4 110.5(4) . . ?
C2 C3 C4 118.0(4) . . ?
N4 C3 C4 131.5(4) . . ?
N3 C4 N1 117.5(4) . . ?
N3 C4 C3 125.1(4) . . ?
N1 C4 C3 117.4(3) . . ?
C5 N4 C3 103.8(4) . . ?
N4 C5 N5 113.7(4) . . ?
C2 N5 C5 105.8(3) . . ?
C2 N5 C6 127.9(3) . . ?
C5 N5 C6 126.1(3) . . ?
O3 C6 N5 107.7(3) . . ?
O3 C6 C7 106.1(3) . . ?
N5 C6 C7 113.7(3) . . ?
O1 C7 C6 112.4(3) . . ?
O1 C7 C8 115.5(3) . . ?
C6 C7 C8 100.5(3) . . ?
C7 O1 Si1 120.8(3) . . ?
O2 C8 C9 110.3(3) . . ?
O2 C8 C7 108.8(3) . . ?
C9 C8 C7 100.6(3) . . ?
C8 O2 Si2 127.7(3) . . ?
O3 C9 C10 110.2(3) . . ?
O3 C9 C8 105.4(3) . . ?
C10 C9 C8 116.2(4) . . ?
C6 O3 C9 109.5(3) . . ?
O4 C10 C9 110.7(4) . . ?
O1 Si1 C12 109.1(2) . . ?
O1 Si1 C13 105.25(19) . . ?
C12 Si1 C13 112.4(3) . . ?
O1 Si1 C11 109.18(19) . . ?
C12 Si1 C11 108.6(3) . . ?
C13 Si1 C11 112.2(3) . . ?
C16 C13 C14 109.4(5) . . ?
C16 C13 C15 108.8(5) . . ?
C14 C13 C15 108.1(5) . . ?
C16 C13 Si1 110.7(4) . . ?
C14 C13 Si1 110.4(4) . . ?
C15 C13 Si1 109.4(4) . . ?
O2 Si2 C18 109.1(3) . . ?
O2 Si2 C17 109.4(2) . . ?
C18 Si2 C17 110.0(4) . . ?
O2 Si2 C19 103.9(2) . . ?
C18 Si2 C19 112.3(3) . . ?
C17 Si2 C19 112.0(4) . . ?
C21 C19 C20 108.6(6) . . ?
C21 C19 C22 110.7(6) . . ?
C20 C19 C22 108.8(6) . . ?
C21 C19 Si2 109.8(5) . . ?
C20 C19 Si2 110.1(4) . . ?
C22 C19 Si2 108.8(5) . . ?
C23 N6 C26 118.7(4) . . ?
N7 C23 N6 130.0(5) . . ?
C23 N7 C24 110.5(4) . . ?
N7 C24 N10 128.0(4) . . ?
N7 C24 C25 126.3(4) . . ?
N10 C24 C25 105.6(4) . . ?
C24 C25 N9 110.7(4) . . ?
C24 C25 C26 117.4(4) . . ?
N9 C25 C26 131.9(4) . . ?
N8 C26 N6 117.9(4) . . ?
N8 C26 C25 125.1(4) . . ?
N6 C26 C25 116.9(4) . . ?
C27 N9 C25 103.6(3) . . ?
N9 C27 N10 113.8(4) . . ?
C27 N10 C24 106.3(3) . . ?
C27 N10 C28 126.1(3) . . ?
C24 N10 C28 127.5(3) . . ?
O7 C28 N10 108.3(3) . . ?
O7 C28 C29 106.4(3) . . ?
N10 C28 C29 114.3(3) . . ?
O5 C29 C28 111.5(4) . . ?
O5 C29 C30 115.0(3) . . ?
C28 C29 C30 100.9(3) . . ?
C29 O5 Si3 127.1(3) . . ?
O6 C30 C31 111.5(4) . . ?
O6 C30 C29 108.9(4) . . ?
C31 C30 C29 101.5(3) . . ?
C30 O6 Si4 126.7(3) . . ?
O7 C31 C32 109.9(4) . . ?
O7 C31 C30 105.5(3) . . ?
C32 C31 C30 116.9(5) . . ?
C28 O7 C31 110.1(3) . . ?
O8 C32 C31 114.6(4) . . ?
O5 Si3 C33 110.1(2) . . ?
O5 Si3 C35 104.7(2) . . ?
C33 Si3 C35 111.1(3) . . ?
O5 Si3 C34 109.0(2) . . ?
C33 Si3 C34 109.3(3) . . ?
C35 Si3 C34 112.6(3) . . ?
C36 C35 C37 109.6(5) . . ?
C36 C35 C38 107.6(5) . . ?
C37 C35 C38 108.7(5) . . ?
C36 C35 Si3 111.0(4) . . ?
C37 C35 Si3 109.8(5) . . ?
C38 C35 Si3 110.1(4) . . ?
O6 Si4 C41 104.6(2) . . ?
O6 Si4 C39 109.6(3) . . ?
C41 Si4 C39 112.4(4) . . ?
O6 Si4 C40 108.4(3) . . ?
C41 Si4 C40 112.4(4) . . ?
C39 Si4 C40 109.3(4) . . ?
C44 C41 C42 107.3(5) . . ?
C44 C41 C43 110.3(6) . . ?
C42 C41 C43 107.5(6) . . ?
C44 C41 Si4 111.5(5) . . ?
C42 C41 Si4 109.3(5) . . ?
C43 C41 Si4 110.7(5) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.160
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.037

#===END

#========================================================
data_6
_database_code_depnum_ccdc_archive 'CCDC 225963'
#========================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
3',5'-O-bis(tert-butyldimethylsiyl)-2'-deoxy-adenosine
;
_chemical_name_common            
3',5'-O-bis(tert-butyldimethylsiyl)-2'-deoxy-adenosine
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H41 N5 O3 Si2'
_chemical_formula_sum            'C22 H41 N5 O3 Si2'
_chemical_formula_weight         479.78
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   p212121

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   7.50000(10)
_cell_length_b                   8.32900(10)
_cell_length_c                   43.3190(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2706.03(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    24965
_cell_measurement_theta_min      4.08
_cell_measurement_theta_max      73.32

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1040
_exptl_absorpt_coefficient_mu    1.480
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.6823
_exptl_absorpt_correction_T_max  0.8609
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54180
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'MacScience DIPLabo'
_diffrn_measurement_method       IP
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24965
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_av_sigmaI/netI    0.0157
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_theta_min         4.08
_diffrn_reflns_theta_max         73.32
_reflns_number_total             4159
_reflns_number_gt                4138
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'MacScience Xpress'
_computing_cell_refinement       'HKL Scalepack'
_computing_data_reduction        'Denzo and HKL Scalepack'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    maXus
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0707P)²+2.0518P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.17(3)
_refine_ls_number_reflns         4159
_refine_ls_number_parameters     300
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.1256
_refine_ls_wR_factor_gt          0.1226
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.7816(4) 0.4518(3) 0.24238(5) 0.0244(5) Uani 1 1 d . . .
C2 C 0.6200(4) 0.4797(4) 0.23033(5) 0.0258(6) Uani 1 1 d . . .
H2 H 0.5776 0.5863 0.2329 0.031 Uiso 1 1 calc R . .
N3 N 0.5095(4) 0.3822(3) 0.21535(5) 0.0243(5) Uani 1 1 d . . .
C4 C 0.5821(4) 0.2345(4) 0.21257(5) 0.0233(6) Uani 1 1 d . . .
C5 C 0.7473(4) 0.1867(4) 0.22366(5) 0.0230(6) Uani 1 1 d . . .
C6 C 0.8501(4) 0.3016(3) 0.23945(5) 0.0215(6) Uani 1 1 d . . .
N6 N 1.0109(4) 0.2712(3) 0.25149(5) 0.0262(6) Uani 1 1 d . . .
H6A H 1.0699 0.3478 0.2611 0.031 Uiso 1 1 calc R . .
H6B H 1.0576 0.1747 0.2498 0.031 Uiso 1 1 calc R . .
N7 N 0.7797(4) 0.0260(3) 0.21688(5) 0.0266(6) Uani 1 1 d . . .
C8 C 0.6345(5) -0.0191(4) 0.20222(6) 0.0279(7) Uani 1 1 d . . .
H8 H 0.6177 -0.1251 0.1947 0.033 Uiso 1 1 calc R . .
N9 N 0.5098(3) 0.0993(3) 0.19870(5) 0.0237(5) Uani 1 1 d . . .
C10 C 0.3372(4) 0.0671(4) 0.18348(5) 0.0239(6) Uani 1 1 d . . .
H10 H 0.2759 -0.0224 0.1946 0.029 Uiso 1 1 calc R . .
C11 C 0.2132(4) 0.2085(4) 0.18186(5) 0.0221(6) Uani 1 1 d . . .
H11A H 0.2277 0.2797 0.2000 0.026 Uiso 1 1 calc R . .
H11B H 0.0872 0.1737 0.1804 0.026 Uiso 1 1 calc R . .
C12 C 0.2740(4) 0.2905(4) 0.15231(5) 0.0211(6) Uani 1 1 d . . .
H12 H 0.3788 0.3611 0.1567 0.025 Uiso 1 1 calc R . .
O13 O 0.1366(3) 0.3812(2) 0.13787(4) 0.0246(4) Uani 1 1 d . . .
C14 C 0.3310(4) 0.1502(3) 0.13188(5) 0.0220(6) Uani 1 1 d . . .
H14 H 0.2290 0.1193 0.1183 0.026 Uiso 1 1 calc R . .
O15 O 0.3693(3) 0.0189(2) 0.15256(4) 0.0264(5) Uani 1 1 d . . .
C16 C 0.4891(5) 0.1899(4) 0.11207(6) 0.0292(7) Uani 1 1 d . . .
H16A H 0.4723 0.2974 0.1028 0.035 Uiso 1 1 calc R . .
H16B H 0.5976 0.1935 0.1251 0.035 Uiso 1 1 calc R . .
O17 O 0.5127(3) 0.0754(3) 0.08836(4) 0.0309(5) Uani 1 1 d . . .
Si18 Si 0.13103(11) 0.58002(10) 0.139763(15) 0.02333(19) Uani 1 1 d . . .
C19 C 0.1970(5) 0.6450(4) 0.17939(7) 0.0367(8) Uani 1 1 d . . .
H19A H 0.1519 0.5676 0.1945 0.055 Uiso 1 1 calc R . .
H19B H 0.1464 0.7512 0.1837 0.055 Uiso 1 1 calc R . .
H19C H 0.3273 0.6503 0.1808 0.055 Uiso 1 1 calc R . .
C20 C 0.2849(5) 0.6624(4) 0.11026(7) 0.0346(8) Uani 1 1 d . . .
H20A H 0.4060 0.6231 0.1142 0.052 Uiso 1 1 calc R . .
H20B H 0.2839 0.7799 0.1113 0.052 Uiso 1 1 calc R . .
H20C H 0.2463 0.6278 0.0897 0.052 Uiso 1 1 calc R . .
C21 C -0.1066(5) 0.6354(4) 0.13129(6) 0.0282(7) Uani 1 1 d . . .
C22 C -0.2279(5) 0.5697(5) 0.15710(7) 0.0392(8) Uani 1 1 d . . .
H22A H -0.1924 0.6166 0.1769 0.059 Uiso 1 1 calc R . .
H22B H -0.2164 0.4526 0.1581 0.059 Uiso 1 1 calc R . .
H22C H -0.3521 0.5982 0.1527 0.059 Uiso 1 1 calc R . .
C23 C -0.1261(6) 0.8176(4) 0.12935(8) 0.0418(9) Uani 1 1 d . . .
H23A H -0.0548 0.8582 0.1121 0.063 Uiso 1 1 calc R . .
H23B H -0.0843 0.8662 0.1486 0.063 Uiso 1 1 calc R . .
H23C H -0.2517 0.8452 0.1261 0.063 Uiso 1 1 calc R . .
C24 C -0.1644(5) 0.5600(5) 0.10055(7) 0.0380(8) Uani 1 1 d . . .
H24A H -0.2883 0.5894 0.0962 0.057 Uiso 1 1 calc R . .
H24B H -0.1544 0.4429 0.1019 0.057 Uiso 1 1 calc R . .
H24C H -0.0873 0.5994 0.0839 0.057 Uiso 1 1 calc R . .
Si25 Si 0.59179(12) 0.11503(10) 0.053676(15) 0.0262(2) Uani 1 1 d . . .
C26 C 0.5205(6) 0.3189(4) 0.04149(7) 0.0443(10) Uani 1 1 d . . .
H26A H 0.3904 0.3272 0.0429 0.066 Uiso 1 1 calc R . .
H26B H 0.5578 0.3378 0.0201 0.066 Uiso 1 1 calc R . .
H26C H 0.5756 0.3992 0.0550 0.066 Uiso 1 1 calc R . .
C27 C 0.8393(5) 0.1030(6) 0.05392(8) 0.0470(9) Uani 1 1 d . . .
H27A H 0.8870 0.1787 0.0692 0.070 Uiso 1 1 calc R . .
H27B H 0.8852 0.1304 0.0334 0.070 Uiso 1 1 calc R . .
H27C H 0.8762 -0.0063 0.0593 0.070 Uiso 1 1 calc R . .
C28 C 0.4915(5) -0.0452(4) 0.02804(6) 0.0300(7) Uani 1 1 d . . .
C29 C 0.5527(6) -0.2106(4) 0.03866(7) 0.0381(9) Uani 1 1 d . . .
H29A H 0.5224 -0.2251 0.0605 0.057 Uiso 1 1 calc R . .
H29B H 0.6821 -0.2198 0.0360 0.057 Uiso 1 1 calc R . .
H29C H 0.4930 -0.2933 0.0263 0.057 Uiso 1 1 calc R . .
C30 C 0.2877(5) -0.0347(5) 0.03064(8) 0.0472(10) Uani 1 1 d . . .
H30A H 0.2332 -0.1182 0.0178 0.071 Uiso 1 1 calc R . .
H30B H 0.2477 0.0711 0.0236 0.071 Uiso 1 1 calc R . .
H30C H 0.2521 -0.0503 0.0522 0.071 Uiso 1 1 calc R . .
C31 C 0.5477(6) -0.0191(5) -0.00563(6) 0.0476(11) Uani 1 1 d . . .
H31A H 0.6781 -0.0172 -0.0070 0.071 Uiso 1 1 calc R . .
H31B H 0.4997 0.0834 -0.0130 0.071 Uiso 1 1 calc R . .
H31C H 0.5012 -0.1067 -0.0184 0.071 Uiso 1 1 calc R . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C2 1.340(4) . ?
N1 C6 1.358(4) . ?
C2 N3 1.329(4) . ?
N3 C4 1.351(4) . ?
C4 N9 1.387(4) . ?
C4 C5 1.387(4) . ?
C5 N7 1.392(4) . ?
C5 C6 1.406(4) . ?
C6 N6 1.338(4) . ?
N7 C8 1.315(4) . ?
C8 N9 1.368(4) . ?
N9 C10 1.477(4) . ?
C10 O15 1.419(3) . ?
C10 C11 1.502(4) . ?
C11 C12 1.521(3) . ?
C12 O13 1.422(3) . ?
C12 C14 1.527(4) . ?
O13 Si18 1.659(2) . ?
C14 O15 1.442(3) . ?
C14 C16 1.501(4) . ?
C16 O17 1.412(3) . ?
O17 Si25 1.6489(19) . ?
Si18 C20 1.854(3) . ?
Si18 C19 1.867(3) . ?
Si18 C21 1.877(3) . ?
C21 C23 1.527(4) . ?
C21 C24 1.535(4) . ?
C21 C22 1.542(4) . ?
Si25 C26 1.856(4) . ?
Si25 C27 1.859(4) . ?
Si25 C28 1.893(3) . ?
C28 C29 1.523(5) . ?
C28 C31 1.534(4) . ?
C28 C30 1.535(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N1 C6 117.7(3) . . ?
N3 C2 N1 130.4(3) . . ?
C2 N3 C4 110.4(3) . . ?
N3 C4 N9 128.4(3) . . ?
N3 C4 C5 126.2(3) . . ?
N9 C4 C5 105.5(3) . . ?
C4 C5 N7 111.0(3) . . ?
C4 C5 C6 117.6(3) . . ?
N7 C5 C6 131.4(3) . . ?
N6 C6 N1 118.6(3) . . ?
N6 C6 C5 123.7(3) . . ?
N1 C6 C5 117.7(3) . . ?
C8 N7 C5 103.4(3) . . ?
N7 C8 N9 114.5(3) . . ?
C8 N9 C4 105.6(2) . . ?
C8 N9 C10 121.2(3) . . ?
C4 N9 C10 133.1(3) . . ?
O15 C10 N9 108.9(2) . . ?
O15 C10 C11 106.4(2) . . ?
N9 C10 C11 114.9(2) . . ?
C10 C11 C12 101.9(2) . . ?
O13 C12 C11 113.0(2) . . ?
O13 C12 C14 110.8(2) . . ?
C11 C12 C14 103.2(2) . . ?
C12 O13 Si18 121.79(17) . . ?
O15 C14 C16 111.4(2) . . ?
O15 C14 C12 106.02(19) . . ?
C16 C14 C12 112.6(2) . . ?
C10 O15 C14 109.8(2) . . ?
O17 C16 C14 111.5(3) . . ?
C16 O17 Si25 124.9(2) . . ?
O13 Si18 C20 108.65(14) . . ?
O13 Si18 C19 109.17(13) . . ?
C20 Si18 C19 111.20(17) . . ?
O13 Si18 C21 105.05(13) . . ?
C20 Si18 C21 111.43(15) . . ?
C19 Si18 C21 111.12(15) . . ?
C23 C21 C24 109.4(3) . . ?
C23 C21 C22 109.6(3) . . ?
C24 C21 C22 108.5(3) . . ?
C23 C21 Si18 110.2(3) . . ?
C24 C21 Si18 109.7(2) . . ?
C22 C21 Si18 109.4(2) . . ?
O17 Si25 C26 109.79(14) . . ?
O17 Si25 C27 110.08(15) . . ?
C26 Si25 C27 109.8(2) . . ?
O17 Si25 C28 104.51(13) . . ?
C26 Si25 C28 111.33(16) . . ?
C27 Si25 C28 111.25(17) . . ?
C29 C28 C31 109.5(3) . . ?
C29 C28 C30 109.2(3) . . ?
C31 C28 C30 109.6(3) . . ?
C29 C28 Si25 109.9(2) . . ?
C31 C28 Si25 110.4(2) . . ?
C30 C28 Si25 108.2(2) . . ?

_diffrn_measured_fraction_theta_max 0.832
_diffrn_reflns_theta_full        73.32
_diffrn_measured_fraction_theta_full 0.832
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.076

#===END

#========================================================
data_2b
_database_code_depnum_ccdc_archive 'CCDC 225964'
#========================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
2',3'-O-bis(triisopropylsilyl)-guanosine
;
_chemical_name_common            2',3'-O-bis(triisopropylsilyl)-guanosine
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H53 N5 O5 Si2'
_chemical_formula_sum            'C28 H53 N5 O5 Si2'
_chemical_formula_weight         595.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   p1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'

_cell_length_a                   7.9550(2)
_cell_length_b                   12.3980(4)
_cell_length_c                   18.0350(4)
_cell_angle_alpha                98.980(2)
_cell_angle_beta                 99.526(2)
_cell_angle_gamma                101.012(2)
_cell_volume                     1689.22(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    16949
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      73.37

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             648
_exptl_absorpt_coefficient_mu    1.288
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.5394
_exptl_absorpt_correction_T_max  0.8667
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'MacScience DIPLabo'
_diffrn_measurement_method       IP
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16949
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.53
_diffrn_reflns_theta_max         73.37
_reflns_number_total             7067
_reflns_number_gt                6934
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'MacScience Xpress'
_computing_cell_refinement       Scalepack
_computing_data_reduction        'Denzo and Scalepack'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    maXus
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1808P)²+2.2429P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.17(5)
_refine_ls_number_reflns         7067
_refine_ls_number_parameters     896
_refine_ls_number_restraints     248
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0857
_refine_ls_wR_factor_ref         0.2496
_refine_ls_wR_factor_gt          0.2408
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O -0.4990(6) 0.4904(4) -0.8237(3) 0.0415(11) Uani 1 1 d . . .
O4 O -0.8364(7) 0.0013(4) -0.7573(3) 0.0372(10) Uani 1 1 d . C .
O5 O -1.1224(6) 0.0996(4) -0.7181(3) 0.0357(10) Uani 1 1 d . . .
H170 H -1.0475 0.1377 -0.7370 0.043 Uiso 1 1 calc R . .
O6 O 0.0122(6) -0.4349(4) 0.1426(3) 0.0398(11) Uani 1 1 d . . .
O7 O -0.1750(7) -0.0999(4) -0.1245(3) 0.0417(11) Uani 1 1 d . D .
O8 O -0.1300(7) 0.1255(4) -0.0882(3) 0.0410(11) Uani 1 1 d . . .
O9 O -0.0673(6) 0.0514(4) 0.0689(2) 0.0335(9) Uani 1 1 d . E .
O10 O -0.4509(6) -0.0234(4) 0.0587(3) 0.0405(11) Uani 1 1 d . . .
H171 H -0.3842 -0.0673 0.0660 0.049 Uiso 1 1 calc R . .
N1 N -0.7748(7) 0.4165(4) -0.8118(3) 0.0316(11) Uani 1 1 d . . .
H1 H -0.8082 0.4735 -0.8287 0.038 Uiso 1 1 calc R . .
N2 N -1.0645(7) 0.3565(5) -0.8057(3) 0.0375(12) Uani 1 1 d . . .
H2 H -1.1504 0.3096 -0.7947 0.045 Uiso 1 1 calc R . .
H3 H -1.0852 0.4150 -0.8247 0.045 Uiso 1 1 calc R . .
N3 N -0.8669(7) 0.2519(4) -0.7650(3) 0.0287(10) Uani 1 1 d . . .
N4 N -0.4063(7) 0.2843(5) -0.7630(3) 0.0380(12) Uani 1 1 d . . .
N5 N -0.6213(7) 0.1645(4) -0.7325(3) 0.0331(11) Uani 1 1 d . . .
N6 N -0.2312(7) -0.3635(4) 0.1289(3) 0.0293(10) Uani 1 1 d . . .
H4 H -0.2841 -0.4187 0.1480 0.035 Uiso 1 1 calc R . .
N7 N -0.4900(7) -0.3039(5) 0.1224(3) 0.0387(13) Uani 1 1 d . . .
H5 H -0.5573 -0.2576 0.1113 0.046 Uiso 1 1 calc R . .
H6 H -0.5292 -0.3614 0.1427 0.046 Uiso 1 1 calc R . .
N8 N -0.2643(7) -0.2016(4) 0.0779(3) 0.0273(10) Uani 1 1 d . . .
N9 N 0.1767(7) -0.2343(5) 0.0748(3) 0.0361(12) Uani 1 1 d . . .
N10 N 0.0017(7) -0.1210(4) 0.0387(3) 0.0326(11) Uani 1 1 d . . .
C1 C -0.9023(8) 0.3390(5) -0.7935(3) 0.0296(12) Uani 1 1 d . . .
C2 C -0.6981(8) 0.2469(5) -0.7595(3) 0.0286(12) Uani 1 1 d . . .
C3 C -0.5622(8) 0.3197(5) -0.7766(4) 0.0324(13) Uani 1 1 d . . .
C4 C -0.5990(8) 0.4144(5) -0.8062(4) 0.0317(13) Uani 1 1 d . . .
C5 C -0.4480(9) 0.1933(6) -0.7358(4) 0.0390(15) Uani 1 1 d . . .
H7 H -0.3658 0.1510 -0.7199 0.047 Uiso 1 1 calc R . .
C6 C -0.6955(9) 0.0688(6) -0.7034(4) 0.0380(15) Uani 1 1 d . C .
H8 H -0.6043 0.0244 -0.6937 0.046 Uiso 1 1 calc R . .
C7 C -0.7642(8) 0.0954(6) -0.6292(4) 0.0366(14) Uani 1 1 d D . .
H9 H -0.8245 0.1592 -0.6276 0.044 Uiso 1 1 calc R A 1
C8 C -0.8877(9) -0.0185(6) -0.6339(4) 0.0406(15) Uani 1 1 d D C .
H10 H -0.9781 -0.0133 -0.6018 0.049 Uiso 1 1 calc R B 3
C9 C -0.9657(10) -0.0507(6) -0.7193(4) 0.0405(15) Uani 1 1 d . . .
H11 H -0.9857 -0.1338 -0.7353 0.049 Uiso 1 1 calc R C .
C10 C -1.1341(9) -0.0158(6) -0.7445(4) 0.0402(15) Uani 1 1 d . C .
H12 H -1.1657 -0.0327 -0.8012 0.048 Uiso 1 1 calc R . .
H13 H -1.2285 -0.0602 -0.7250 0.048 Uiso 1 1 calc R . .
C29 C -0.3263(8) -0.2868(5) 0.1083(3) 0.0295(12) Uani 1 1 d . . .
C30 C -0.0970(8) -0.1992(5) 0.0695(3) 0.0301(12) Uani 1 1 d . . .
C31 C 0.0107(8) -0.2692(5) 0.0905(3) 0.0286(12) Uani 1 1 d . . .
C32 C -0.0573(8) -0.3610(5) 0.1221(3) 0.0296(12) Uani 1 1 d . . .
C33 C 0.1644(8) -0.1471(6) 0.0437(4) 0.0353(13) Uani 1 1 d . . .
H14 H 0.2581 -0.1054 0.0263 0.042 Uiso 1 1 calc R . .
C34 C -0.0399(8) -0.0263(5) 0.0077(3) 0.0311(13) Uani 1 1 d . E .
H15 H 0.0610 0.0096 -0.0131 0.037 Uiso 1 1 calc R . .
C35 C -0.2054(9) -0.0518(5) -0.0534(3) 0.0340(14) Uani 1 1 d . . .
H16 H -0.3011 -0.1034 -0.0384 0.041 Uiso 1 1 calc R E .
C36 C -0.2434(8) 0.0662(6) -0.0478(4) 0.0379(15) Uani 1 1 d . E .
H17 H -0.3688 0.0629 -0.0694 0.045 Uiso 1 1 calc R . .
C37 C -0.1985(8) 0.1095(5) 0.0383(4) 0.0342(13) Uani 1 1 d . . .
H18 H -0.1456 0.1917 0.0487 0.041 Uiso 1 1 calc R E .
C38 C -0.3516(9) 0.0893(6) 0.0794(4) 0.0388(14) Uani 1 1 d . E .
H19 H -0.3062 0.1076 0.1354 0.047 Uiso 1 1 calc R . .
H20 H -0.4294 0.1403 0.0669 0.047 Uiso 1 1 calc R . .
O2 O -0.6242(12) 0.1110(8) -0.5682(4) 0.035(2) Uani 0.557(9) 1 d PD C 1
Si1 Si -0.5365(6) 0.2269(5) -0.5064(2) 0.0446(12) Uani 0.557(9) 1 d PD C 1
C11 C -0.6622(17) 0.2388(13) -0.4281(7) 0.064(4) Uani 0.557(9) 1 d PD C 1
H23 H -0.6470 0.1746 -0.4022 0.077 Uiso 0.557(9) 1 calc PR C 1
C12 C -0.8593(19) 0.222(2) -0.4546(12) 0.108(10) Uani 0.557(9) 1 d PD C 1
H24 H -0.9152 0.2229 -0.4100 0.162 Uiso 0.557(9) 1 calc PR C 1
H25 H -0.9051 0.1496 -0.4898 0.162 Uiso 0.557(9) 1 calc PR C 1
H26 H -0.8843 0.2822 -0.4809 0.162 Uiso 0.557(9) 1 calc PR C 1
C13 C -0.587(2) 0.3416(14) -0.3666(8) 0.068(5) Uani 0.557(9) 1 d PD C 1
H27 H -0.5812 0.4086 -0.3896 0.101 Uiso 0.557(9) 1 calc PR C 1
H28 H -0.4685 0.3389 -0.3419 0.101 Uiso 0.557(9) 1 calc PR C 1
H29 H -0.6606 0.3445 -0.3284 0.101 Uiso 0.557(9) 1 calc PR C 1
C14 C -0.508(2) 0.3499(9) -0.5541(7) 0.066(6) Uani 0.557(9) 1 d PD C 1
H30 H -0.4732 0.3244 -0.6037 0.079 Uiso 0.557(9) 1 calc PR C 1
C15 C -0.670(2) 0.3954(12) -0.5743(9) 0.068(5) Uani 0.557(9) 1 d PD C 1
H31 H -0.7086 0.4221 -0.5273 0.102 Uiso 0.557(9) 1 calc PR C 1
H32 H -0.7633 0.3359 -0.6076 0.102 Uiso 0.557(9) 1 calc PR C 1
H33 H -0.6430 0.4576 -0.6010 0.102 Uiso 0.557(9) 1 calc PR C 1
C16 C -0.354(3) 0.4460(14) -0.5068(11) 0.082(7) Uani 0.557(9) 1 d PD C 1
H34 H -0.3557 0.5142 -0.5278 0.123 Uiso 0.557(9) 1 calc PR C 1
H35 H -0.2427 0.4241 -0.5097 0.123 Uiso 0.557(9) 1 calc PR C 1
H36 H -0.3663 0.4601 -0.4532 0.123 Uiso 0.557(9) 1 calc PR C 1
C17 C -0.3118(15) 0.2029(12) -0.4677(7) 0.057(4) Uani 0.557(9) 1 d PD C 1
H37 H -0.2371 0.2754 -0.4371 0.068 Uiso 0.557(9) 1 calc PR C 1
C18 C -0.326(3) 0.1173(16) -0.4154(9) 0.082(6) Uani 0.557(9) 1 d PD C 1
H38 H -0.4194 0.0519 -0.4406 0.122 Uiso 0.557(9) 1 calc PR C 1
H39 H -0.3523 0.1511 -0.3671 0.122 Uiso 0.557(9) 1 calc PR C 1
H40 H -0.2147 0.0939 -0.4050 0.122 Uiso 0.557(9) 1 calc PR C 1
C19 C -0.225(2) 0.164(2) -0.5335(10) 0.089(7) Uani 0.557(9) 1 d PD C 1
H41 H -0.1101 0.1517 -0.5127 0.133 Uiso 0.557(9) 1 calc PR C 1
H42 H -0.2116 0.2213 -0.5652 0.133 Uiso 0.557(9) 1 calc PR C 1
H43 H -0.2985 0.0938 -0.5650 0.133 Uiso 0.557(9) 1 calc PR C 1
O2B O -0.6357(18) 0.1501(10) -0.5583(7) 0.040(4) Uiso 0.443(9) 1 d PD C 2
Si1B Si -0.5718(9) 0.2775(6) -0.5037(3) 0.0545(18) Uani 0.443(9) 1 d PD C 2
C17B C -0.439(4) 0.253(3) -0.4144(14) 0.163(19) Uiso 0.443(9) 1 d PD C 2
H44 H -0.3610 0.2058 -0.4346 0.196 Uiso 0.443(9) 1 calc PR C 2
C18B C -0.545(8) 0.177(5) -0.372(3) 0.25(4) Uiso 0.443(9) 1 d PD C 2
H45 H -0.6673 0.1824 -0.3826 0.382 Uiso 0.443(9) 1 calc PR C 2
H46 H -0.4979 0.1997 -0.3165 0.382 Uiso 0.443(9) 1 calc PR C 2
H47 H -0.5374 0.0990 -0.3887 0.382 Uiso 0.443(9) 1 calc PR C 2
C19B C -0.312(7) 0.353(4) -0.365(3) 0.22(3) Uiso 0.443(9) 1 d PD C 2
H48 H -0.2405 0.3300 -0.3234 0.326 Uiso 0.443(9) 1 calc PR C 2
H49 H -0.3764 0.4062 -0.3434 0.326 Uiso 0.443(9) 1 calc PR C 2
H50 H -0.2363 0.3893 -0.3960 0.326 Uiso 0.443(9) 1 calc PR C 2
C11B C -0.765(2) 0.3332(15) -0.4938(9) 0.068(6) Uani 0.443(9) 1 d PD C 2
H51 H -0.8575 0.2670 -0.4919 0.082 Uiso 0.443(9) 1 calc PR C 2
C12B C -0.844(3) 0.3824(17) -0.5589(12) 0.074(7) Uani 0.443(9) 1 d PD C 2
H52 H -0.9571 0.3972 -0.5509 0.111 Uiso 0.443(9) 1 calc PR C 2
H53 H -0.8611 0.3294 -0.6073 0.111 Uiso 0.443(9) 1 calc PR C 2
H54 H -0.7653 0.4526 -0.5608 0.111 Uiso 0.443(9) 1 calc PR C 2
C13B C -0.741(4) 0.414(3) -0.4153(14) 0.112(12) Uani 0.443(9) 1 d PD C 2
H55 H -0.6446 0.4788 -0.4113 0.167 Uiso 0.443(9) 1 calc PR C 2
H56 H -0.7128 0.3746 -0.3735 0.167 Uiso 0.443(9) 1 calc PR C 2
H57 H -0.8486 0.4399 -0.4118 0.167 Uiso 0.443(9) 1 calc PR C 2
C14B C -0.424(3) 0.3620(19) -0.5563(17) 0.094(12) Uiso 0.443(9) 1 d PD C 2
H58 H -0.4891 0.3489 -0.6105 0.112 Uiso 0.443(9) 1 calc PR C 2
C15B C -0.253(4) 0.321(3) -0.559(2) 0.113(11) Uiso 0.443(9) 1 d PD C 2
H59 H -0.1944 0.3531 -0.5968 0.169 Uiso 0.443(9) 1 calc PR C 2
H60 H -0.2803 0.2386 -0.5737 0.169 Uiso 0.443(9) 1 calc PR C 2
H61 H -0.1753 0.3437 -0.5084 0.169 Uiso 0.443(9) 1 calc PR C 2
C16B C -0.380(4) 0.4883(19) -0.5268(18) 0.087(8) Uiso 0.443(9) 1 d PD C 2
H62 H -0.3650 0.5038 -0.4708 0.130 Uiso 0.443(9) 1 calc PR C 2
H63 H -0.4755 0.5204 -0.5491 0.130 Uiso 0.443(9) 1 calc PR C 2
H64 H -0.2717 0.5219 -0.5414 0.130 Uiso 0.443(9) 1 calc PR C 2
O3 O -0.7940(19) -0.1059(9) -0.6201(7) 0.035(3) Uani 0.563(10) 1 d PD C 3
Si2 Si -0.8367(8) -0.2248(4) -0.5915(3) 0.0524(14) Uani 0.563(10) 1 d PD C 3
C20 C -0.876(4) -0.1966(18) -0.4907(9) 0.100(10) Uiso 0.563(10) 1 d PD C 3
H65 H -1.0062 -0.2119 -0.4975 0.120 Uiso 0.563(10) 1 calc PR C 3
C21 C -0.823(6) -0.285(3) -0.4452(18) 0.173(18) Uiso 0.563(10) 1 d PD C 3
H66 H -0.7129 -0.3008 -0.4562 0.260 Uiso 0.563(10) 1 calc PR C 3
H67 H -0.9148 -0.3540 -0.4603 0.260 Uiso 0.563(10) 1 calc PR C 3
H68 H -0.8088 -0.2561 -0.3902 0.260 Uiso 0.563(10) 1 calc PR C 3
C22 C -0.816(4) -0.0798(17) -0.4462(12) 0.098(7) Uiso 0.563(10) 1 d PD C 3
H69 H -0.8124 -0.0803 -0.3916 0.148 Uiso 0.563(10) 1 calc PR C 3
H70 H -0.8979 -0.0348 -0.4639 0.148 Uiso 0.563(10) 1 calc PR C 3
H71 H -0.6994 -0.0475 -0.4537 0.148 Uiso 0.563(10) 1 calc PR C 3
C23 C -0.633(2) -0.2782(14) -0.5956(10) 0.095(9) Uani 0.563(10) 1 d PD C 3
H72 H -0.6448 -0.3493 -0.5752 0.114 Uiso 0.563(10) 1 calc PR C 3
C24 C -0.474(3) -0.193(2) -0.5466(15) 0.120(12) Uani 0.563(10) 1 d PD C 3
H73 H -0.3674 -0.2108 -0.5614 0.180 Uiso 0.563(10) 1 calc PR C 3
H74 H -0.4696 -0.1966 -0.4924 0.180 Uiso 0.563(10) 1 calc PR C 3
H75 H -0.4816 -0.1178 -0.5546 0.180 Uiso 0.563(10) 1 calc PR C 3
C25 C -0.610(3) -0.303(2) -0.6795(12) 0.122(13) Uani 0.563(10) 1 d PD C 3
H76 H -0.6151 -0.2370 -0.7023 0.183 Uiso 0.563(10) 1 calc PR C 3
H77 H -0.7040 -0.3662 -0.7087 0.183 Uiso 0.563(10) 1 calc PR C 3
H78 H -0.4968 -0.3228 -0.6807 0.183 Uiso 0.563(10) 1 calc PR C 3
C26 C -1.033(3) -0.3248(17) -0.6553(17) 0.071(9) Uani 0.563(10) 1 d PD C 3
H79 H -1.0131 -0.3241 -0.7085 0.085 Uiso 0.563(10) 1 calc PR C 3
C27 C -1.048(3) -0.4492(15) -0.6460(13) 0.084(6) Uiso 0.563(10) 1 d PD C 3
H80 H -1.0567 -0.4551 -0.5931 0.125 Uiso 0.563(10) 1 calc PR C 3
H81 H -0.9446 -0.4744 -0.6580 0.125 Uiso 0.563(10) 1 calc PR C 3
H82 H -1.1531 -0.4963 -0.6811 0.125 Uiso 0.563(10) 1 calc PR C 3
C28 C -1.210(2) -0.2949(15) -0.6556(11) 0.071(5) Uani 0.563(10) 1 d PD C 3
H83 H -1.2630 -0.3255 -0.6157 0.106 Uiso 0.563(10) 1 calc PR C 3
H84 H -1.2872 -0.3268 -0.7058 0.106 Uiso 0.563(10) 1 calc PR C 3
H85 H -1.1950 -0.2133 -0.6456 0.106 Uiso 0.563(10) 1 calc PR C 3
O3B O -0.767(2) -0.0725(12) -0.5969(9) 0.041(5) Uani 0.437(10) 1 d PD C 4
Si2B Si -0.7729(7) -0.1786(5) -0.5543(4) 0.0430(17) Uani 0.437(10) 1 d PD C 4
C20B C -0.940(2) -0.1875(14) -0.4918(8) 0.051(5) Uani 0.437(10) 1 d PD C 4
H86 H -1.0565 -0.2067 -0.5277 0.061 Uiso 0.437(10) 1 calc PR C 4
C21B C -0.935(3) -0.2881(18) -0.4509(12) 0.071(7) Uani 0.437(10) 1 d PD C 4
H87 H -0.8243 -0.3112 -0.4524 0.106 Uiso 0.437(10) 1 calc PR C 4
H88 H -1.0326 -0.3507 -0.4769 0.106 Uiso 0.437(10) 1 calc PR C 4
H89 H -0.9449 -0.2660 -0.3975 0.106 Uiso 0.437(10) 1 calc PR C 4
C22B C -0.938(5) -0.083(2) -0.4386(17) 0.109(11) Uiso 0.437(10) 1 d PD C 4
H90 H -1.0318 -0.0966 -0.4099 0.163 Uiso 0.437(10) 1 calc PR C 4
H91 H -0.9556 -0.0243 -0.4679 0.163 Uiso 0.437(10) 1 calc PR C 4
H92 H -0.8249 -0.0585 -0.4027 0.163 Uiso 0.437(10) 1 calc PR C 4
C23B C -0.5458(19) -0.1592(14) -0.4979(10) 0.058(5) Uani 0.437(10) 1 d PD C 4
H93 H -0.5414 -0.1178 -0.4451 0.070 Uiso 0.437(10) 1 calc PR C 4
C24B C -0.492(3) -0.2689(16) -0.4902(12) 0.062(5) Uani 0.437(10) 1 d PD C 4
H94 H -0.5236 -0.3194 -0.5404 0.093 Uiso 0.437(10) 1 calc PR C 4
H95 H -0.5528 -0.3038 -0.4540 0.093 Uiso 0.437(10) 1 calc PR C 4
H96 H -0.3655 -0.2542 -0.4714 0.093 Uiso 0.437(10) 1 calc PR C 4
C25B C -0.409(2) -0.0867(18) -0.5335(13) 0.066(6) Uani 0.437(10) 1 d PD C 4
H97 H -0.3282 -0.0295 -0.4929 0.099 Uiso 0.437(10) 1 calc PR C 4
H98 H -0.4695 -0.0503 -0.5709 0.099 Uiso 0.437(10) 1 calc PR C 4
H99 H -0.3428 -0.1348 -0.5592 0.099 Uiso 0.437(10) 1 calc PR C 4
C26B C -0.827(3) -0.3109(13) -0.6310(11) 0.080(8) Uani 0.437(10) 1 d PD C 4
H100 H -0.7954 -0.3721 -0.6051 0.096 Uiso 0.437(10) 1 calc PR C 4
C27B C -0.713(4) -0.299(2) -0.6929(14) 0.098(11) Uani 0.437(10) 1 d PD C 4
H101 H -0.7186 -0.3732 -0.7226 0.147 Uiso 0.437(10) 1 calc PR C 4
H102 H -0.5920 -0.2636 -0.6680 0.147 Uiso 0.437(10) 1 calc PR C 4
H103 H -0.7584 -0.2525 -0.7273 0.147 Uiso 0.437(10) 1 calc PR C 4
C28B C -1.022(3) -0.348(3) -0.667(2) 0.069(11) Uani 0.437(10) 1 d PD C 4
H104 H -1.0471 -0.3106 -0.7106 0.103 Uiso 0.437(10) 1 calc PR C 4
H105 H -1.0901 -0.3265 -0.6288 0.103 Uiso 0.437(10) 1 calc PR C 4
H106 H -1.0533 -0.4289 -0.6849 0.103 Uiso 0.437(10) 1 calc PR C 4
Si3 Si -0.3045(4) -0.2033(2) -0.19054(13) 0.0678(8) Uani 1 1 d D . .
C39 C -0.1451(19) -0.2972(12) -0.2191(8) 0.060(4) Uani 0.527(10) 1 d PD D 5
H107 H -0.0501 -0.2452 -0.2343 0.072 Uiso 0.527(10) 1 calc PR D 5
C40 C -0.216(3) -0.3910(16) -0.2898(10) 0.084(7) Uani 0.527(10) 1 d PD D 5
H108 H -0.1186 -0.4159 -0.3086 0.127 Uiso 0.527(10) 1 calc PR D 5
H109 H -0.2846 -0.3631 -0.3300 0.127 Uiso 0.527(10) 1 calc PR D 5
H110 H -0.2911 -0.4541 -0.2760 0.127 Uiso 0.527(10) 1 calc PR D 5
C41 C -0.050(3) -0.3431(15) -0.1545(11) 0.071(5) Uani 0.527(10) 1 d PD D 5
H111 H -0.1326 -0.4022 -0.1406 0.106 Uiso 0.527(10) 1 calc PR D 5
H112 H -0.0012 -0.2825 -0.1099 0.106 Uiso 0.527(10) 1 calc PR D 5
H113 H 0.0446 -0.3739 -0.1717 0.106 Uiso 0.527(10) 1 calc PR D 5
C42 C -0.374(2) -0.1497(13) -0.2783(7) 0.063(5) Uani 0.527(10) 1 d PD D 5
H114 H -0.4509 -0.2126 -0.3183 0.076 Uiso 0.527(10) 1 calc PR D 5
C43 C -0.219(3) -0.095(2) -0.3107(11) 0.087(7) Uani 0.527(10) 1 d PD D 5
H115 H -0.2620 -0.0584 -0.3522 0.130 Uiso 0.527(10) 1 calc PR D 5
H116 H -0.1603 -0.1525 -0.3308 0.130 Uiso 0.527(10) 1 calc PR D 5
H117 H -0.1363 -0.0391 -0.2700 0.130 Uiso 0.527(10) 1 calc PR D 5
C44 C -0.478(6) -0.062(4) -0.257(3) 0.16(2) Uiso 0.527(10) 1 d PD D 5
H118 H -0.4035 -0.0011 -0.2166 0.243 Uiso 0.527(10) 1 calc PR D 5
H119 H -0.5797 -0.0966 -0.2380 0.243 Uiso 0.527(10) 1 calc PR D 5
H120 H -0.5171 -0.0315 -0.3020 0.243 Uiso 0.527(10) 1 calc PR D 5
C45 C -0.487(2) -0.2887(15) -0.1615(10) 0.080(7) Uani 0.527(10) 1 d PD D 5
H121 H -0.5436 -0.2341 -0.1338 0.096 Uiso 0.527(10) 1 calc PR D 5
C46 C -0.437(3) -0.3601(17) -0.1056(11) 0.086(7) Uani 0.527(10) 1 d PD D 5
H122 H -0.5326 -0.3797 -0.0789 0.130 Uiso 0.527(10) 1 calc PR D 5
H123 H -0.3314 -0.3187 -0.0683 0.130 Uiso 0.527(10) 1 calc PR D 5
H124 H -0.4136 -0.4286 -0.1331 0.130 Uiso 0.527(10) 1 calc PR D 5
C47 C -0.628(3) -0.358(2) -0.2282(14) 0.112(9) Uiso 0.527(10) 1 d PD D 5
H125 H -0.6459 -0.4371 -0.2245 0.167 Uiso 0.527(10) 1 calc PR D 5
H126 H -0.5922 -0.3479 -0.2766 0.167 Uiso 0.527(10) 1 calc PR D 5
H127 H -0.7375 -0.3330 -0.2265 0.167 Uiso 0.527(10) 1 calc PR D 5
C39B C -0.213(2) -0.2106(18) -0.2726(9) 0.072(6) Uiso 0.473(10) 1 d PD D 6
H128 H -0.2080 -0.1366 -0.2886 0.087 Uiso 0.473(10) 1 calc PR D 6
C40B C -0.025(3) -0.220(3) -0.2499(17) 0.106(9) Uiso 0.473(10) 1 d PD D 6
H129 H -0.0226 -0.2973 -0.2451 0.158 Uiso 0.473(10) 1 calc PR D 6
H130 H 0.0288 -0.1697 -0.2007 0.158 Uiso 0.473(10) 1 calc PR D 6
H131 H 0.0393 -0.1992 -0.2892 0.158 Uiso 0.473(10) 1 calc PR D 6
C41B C -0.322(4) -0.298(3) -0.3401(15) 0.119(11) Uiso 0.473(10) 1 d PD D 6
H132 H -0.3046 -0.2743 -0.3880 0.179 Uiso 0.473(10) 1 calc PR D 6
H133 H -0.4461 -0.3079 -0.3373 0.179 Uiso 0.473(10) 1 calc PR D 6
H134 H -0.2873 -0.3698 -0.3387 0.179 Uiso 0.473(10) 1 calc PR D 6
C42B C -0.521(2) -0.1541(17) -0.2178(12) 0.074(6) Uiso 0.473(10) 1 d PD D 6
H135 H -0.5952 -0.2138 -0.2609 0.089 Uiso 0.473(10) 1 calc PR D 6
C43B C -0.492(3) -0.0497(19) -0.2507(14) 0.058(6) Uiso 0.473(10) 1 d PD D 6
H136 H -0.3787 -0.0010 -0.2242 0.087 Uiso 0.473(10) 1 calc PR D 6
H137 H -0.5852 -0.0102 -0.2441 0.087 Uiso 0.473(10) 1 calc PR D 6
H138 H -0.4912 -0.0699 -0.3054 0.087 Uiso 0.473(10) 1 calc PR D 6
C44B C -0.636(3) -0.141(2) -0.1579(14) 0.093(8) Uiso 0.473(10) 1 d PD D 6
H139 H -0.5625 -0.1008 -0.1086 0.140 Uiso 0.473(10) 1 calc PR D 6
H140 H -0.6955 -0.2154 -0.1523 0.140 Uiso 0.473(10) 1 calc PR D 6
H141 H -0.7230 -0.0991 -0.1745 0.140 Uiso 0.473(10) 1 calc PR D 6
C45B C -0.372(3) -0.3165(15) -0.1419(12) 0.074(6) Uiso 0.473(10) 1 d PD D 6
H142 H -0.4172 -0.2854 -0.0966 0.089 Uiso 0.473(10) 1 calc PR D 6
C46B C -0.218(3) -0.364(2) -0.1133(16) 0.092(8) Uiso 0.473(10) 1 d PD D 6
H143 H -0.2426 -0.4017 -0.0713 0.138 Uiso 0.473(10) 1 calc PR D 6
H144 H -0.1141 -0.3027 -0.0949 0.138 Uiso 0.473(10) 1 calc PR D 6
H145 H -0.1983 -0.4172 -0.1552 0.138 Uiso 0.473(10) 1 calc PR D 6
C47B C -0.513(3) -0.4113(19) -0.1911(16) 0.093(8) Uiso 0.473(10) 1 d PD D 6
H146 H -0.4963 -0.4206 -0.2442 0.140 Uiso 0.473(10) 1 calc PR D 6
H147 H -0.6275 -0.3943 -0.1889 0.140 Uiso 0.473(10) 1 calc PR D 6
H148 H -0.5065 -0.4806 -0.1722 0.140 Uiso 0.473(10) 1 calc PR D 6
Si4 Si -0.0625(2) 0.25470(15) -0.09892(11) 0.0368(4) Uani 1 1 d D E 6
C48 C -0.2375(11) 0.3376(7) -0.1008(4) 0.052(2) Uani 1 1 d D E 6
H149 H -0.1885 0.4089 -0.1167 0.063 Uiso 1 1 calc R E 6
C49 C -0.2866(13) 0.3720(8) -0.0226(5) 0.063(2) Uani 1 1 d D E 6
H150 H -0.3771 0.4154 -0.0287 0.094 Uiso 1 1 calc R E 6
H151 H -0.1828 0.4177 0.0139 0.094 Uiso 1 1 calc R E 6
H152 H -0.3309 0.3046 -0.0033 0.094 Uiso 1 1 calc R E 6
C50 C -0.4004(14) 0.2809(10) -0.1608(6) 0.078(3) Uani 1 1 d D E 6
H153 H -0.4797 0.2305 -0.1386 0.116 Uiso 1 1 calc R E 6
H154 H -0.3679 0.2377 -0.2044 0.116 Uiso 1 1 calc R E 6
H155 H -0.4590 0.3377 -0.1783 0.116 Uiso 1 1 calc R E 6
C51 C -0.008(2) 0.2304(9) -0.1975(6) 0.081(4) Uani 1 1 d . E 6
H156 H -0.1227 0.1890 -0.2307 0.097 Uiso 1 1 calc R E 6
C52 C 0.036(2) 0.3352(10) -0.2321(7) 0.101(5) Uani 1 1 d . E 6
H157 H 0.1449 0.3844 -0.2015 0.151 Uiso 1 1 calc R E 6
H158 H -0.0590 0.3750 -0.2322 0.151 Uiso 1 1 calc R E 6
H159 H 0.0509 0.3130 -0.2848 0.151 Uiso 1 1 calc R E 6
C53 C 0.103(3) 0.1526(14) -0.2092(8) 0.117(6) Uani 1 1 d . E 6
H160 H 0.0898 0.1243 -0.2642 0.175 Uiso 1 1 calc R E 6
H161 H 0.0707 0.0898 -0.1836 0.175 Uiso 1 1 calc R E 6
H162 H 0.2256 0.1908 -0.1877 0.175 Uiso 1 1 calc R E 6
C54 C 0.1213(11) 0.3284(7) -0.0159(5) 0.0525(19) Uani 1 1 d D E 6
H163 H 0.0668 0.3431 0.0298 0.063 Uiso 1 1 calc R E 6
C55 C 0.2163(13) 0.4430(7) -0.0271(7) 0.070(3) Uani 1 1 d D E 6
H164 H 0.3068 0.4789 0.0185 0.105 Uiso 1 1 calc R E 6
H165 H 0.1322 0.4905 -0.0351 0.105 Uiso 1 1 calc R E 6
H166 H 0.2706 0.4328 -0.0720 0.105 Uiso 1 1 calc R E 6
C56 C 0.2545(11) 0.2575(7) 0.0047(5) 0.056(2) Uani 1 1 d D E 6
H167 H 0.3095 0.2395 -0.0391 0.085 Uiso 1 1 calc R E 6
H168 H 0.1946 0.1879 0.0172 0.085 Uiso 1 1 calc R E 6
H169 H 0.3443 0.2996 0.0490 0.085 Uiso 1 1 calc R E 6


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C4 1.229(8) . ?
O4 C6 1.389(9) . ?
O4 C9 1.436(8) . ?
O5 C10 1.416(8) . ?
O6 C32 1.231(7) . ?
O7 C35 1.405(8) . ?
O7 Si3 1.654(5) . ?
O8 C36 1.421(8) . ?
O8 Si4 1.641(5) . ?
O9 C34 1.421(8) . ?
O9 C37 1.461(7) . ?
O10 C38 1.426(8) . ?
N1 C1 1.377(8) . ?
N1 C4 1.391(8) . ?
N2 C1 1.337(8) . ?
N3 C1 1.323(7) . ?
N3 C2 1.344(8) . ?
N4 C5 1.307(9) . ?
N4 C3 1.390(8) . ?
N5 C5 1.370(8) . ?
N5 C2 1.396(7) . ?
N5 C6 1.435(8) . ?
N6 C29 1.382(7) . ?
N6 C32 1.404(8) . ?
N7 C29 1.352(8) . ?
N8 C29 1.315(8) . ?
N8 C30 1.360(8) . ?
N9 C33 1.305(8) . ?
N9 C31 1.398(8) . ?
N10 C30 1.372(8) . ?
N10 C33 1.385(8) . ?
N10 C34 1.446(7) . ?
C2 C3 1.379(9) . ?
C3 C4 1.423(8) . ?
C6 C7 1.540(9) . ?
C7 O2 1.390(9) . ?
C7 O2B 1.473(12) . ?
C7 C8 1.539(10) . ?
C8 O3B 1.408(14) . ?
C8 O3 1.457(12) . ?
C8 C9 1.520(10) . ?
C9 C10 1.506(9) . ?
C30 C31 1.382(8) . ?
C31 C32 1.408(8) . ?
C34 C35 1.517(8) . ?
C35 C36 1.541(9) . ?
C36 C37 1.519(10) . ?
C37 C38 1.528(10) . ?
O2 Si1 1.629(8) . ?
Si1 C14 1.860(11) . ?
Si1 C11 1.864(11) . ?
Si1 C17 1.904(11) . ?
C11 C13 1.504(13) . ?
C11 C12 1.525(13) . ?
C14 C15 1.518(14) . ?
C14 C16 1.557(14) . ?
C17 C19 1.528(15) . ?
C17 C18 1.527(14) . ?
O2B Si1B 1.663(11) . ?
Si1B C11B 1.828(15) . ?
Si1B C17B 1.877(16) . ?
Si1B C14B 1.892(17) . ?
C17B C19B 1.495(19) . ?
C17B C18B 1.528(19) . ?
C11B C12B 1.505(18) . ?
C11B C13B 1.562(18) . ?
C14B C16B 1.53(2) . ?
C14B C15B 1.55(2) . ?
O3 Si2 1.632(10) . ?
Si2 C23 1.869(14) . ?
Si2 C26 1.876(17) . ?
Si2 C20 1.886(14) . ?
C20 C22 1.488(17) . ?
C20 C21 1.546(17) . ?
C23 C24 1.527(18) . ?
C23 C25 1.545(19) . ?
C26 C28 1.52(2) . ?
C26 C27 1.56(2) . ?
O3B Si2B 1.621(11) . ?
Si2B C23B 1.872(14) . ?
Si2B C20B 1.880(13) . ?
Si2B C26B 1.901(15) . ?
C20B C22B 1.484(17) . ?
C20B C21B 1.548(15) . ?
C23B C24B 1.520(17) . ?
C23B C25B 1.565(19) . ?
C26B C28B 1.53(2) . ?
C26B C27B 1.55(2) . ?
Si3 C39B 1.754(15) . ?
Si3 C45B 1.811(15) . ?
Si3 C45 1.826(13) . ?
Si3 C42 1.852(12) . ?
Si3 C42B 1.952(15) . ?
Si3 C39 1.955(14) . ?
C39 C41 1.526(16) . ?
C39 C40 1.531(15) . ?
C42 C44 1.532(19) . ?
C42 C43 1.536(17) . ?
C45 C46 1.496(18) . ?
C45 C47 1.520(17) . ?
C39B C40B 1.510(14) . ?
C39B C41B 1.517(15) . ?
C42B C43B 1.500(18) . ?
C42B C44B 1.532(18) . ?
C45B C46B 1.501(18) . ?
C45B C47B 1.507(18) . ?
Si4 C48 1.881(8) . ?
Si4 C54 1.885(8) . ?
Si4 C51 1.891(9) . ?
C48 C50 1.514(11) . ?
C48 C49 1.544(11) . ?
C51 C53 1.445(16) . ?
C51 C52 1.534(12) . ?
C54 C56 1.537(10) . ?
C54 C55 1.537(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 O4 C9 109.8(5) . . ?
C35 O7 Si3 128.5(4) . . ?
C36 O8 Si4 138.6(5) . . ?
C34 O9 C37 108.7(4) . . ?
C1 N1 C4 126.9(5) . . ?
C1 N3 C2 112.5(5) . . ?
C5 N4 C3 103.8(6) . . ?
C5 N5 C2 106.2(5) . . ?
C5 N5 C6 123.4(5) . . ?
C2 N5 C6 130.4(5) . . ?
C29 N6 C32 125.6(5) . . ?
C29 N8 C30 111.7(5) . . ?
C33 N9 C31 103.8(5) . . ?
C30 N10 C33 106.1(5) . . ?
C30 N10 C34 131.0(5) . . ?
C33 N10 C34 122.9(6) . . ?
N3 C1 N2 121.4(6) . . ?
N3 C1 N1 122.1(6) . . ?
N2 C1 N1 116.5(5) . . ?
N3 C2 C3 129.5(5) . . ?
N3 C2 N5 126.0(6) . . ?
C3 C2 N5 104.5(5) . . ?
C2 C3 N4 111.7(5) . . ?
C2 C3 C4 118.3(6) . . ?
N4 C3 C4 130.0(6) . . ?
O1 C4 N1 119.9(5) . . ?
O1 C4 C3 129.3(6) . . ?
N1 C4 C3 110.7(5) . . ?
N4 C5 N5 113.8(6) . . ?
O4 C6 N5 110.1(5) . . ?
O4 C6 C7 106.2(5) . . ?
N5 C6 C7 115.3(6) . . ?
O2 C7 O2B 20.6(5) . . ?
O2 C7 C6 107.2(6) . . ?
O2B C7 C6 118.0(8) . . ?
O2 C7 C8 108.7(6) . . ?
O2B C7 C8 120.6(7) . . ?
C6 C7 C8 99.2(6) . . ?
O3B C8 O3 21.0(8) . . ?
O3B C8 C9 123.1(9) . . ?
O3 C8 C9 103.4(7) . . ?
O3B C8 C7 99.0(8) . . ?
O3 C8 C7 112.7(8) . . ?
C9 C8 C7 101.3(5) . . ?
O4 C9 C10 108.6(5) . . ?
O4 C9 C8 106.5(6) . . ?
C10 C9 C8 115.8(6) . . ?
O5 C10 C9 112.6(5) . . ?
N8 C29 N7 121.3(6) . . ?
N8 C29 N6 123.5(6) . . ?
N7 C29 N6 115.2(5) . . ?
N8 C30 N10 125.2(5) . . ?
N8 C30 C31 129.2(6) . . ?
N10 C30 C31 105.6(5) . . ?
C30 C31 N9 110.9(5) . . ?
C30 C31 C32 118.7(6) . . ?
N9 C31 C32 130.4(5) . . ?
O6 C32 N6 119.0(6) . . ?
O6 C32 C31 129.8(6) . . ?
N6 C32 C31 111.2(5) . . ?
N9 C33 N10 113.5(6) . . ?
O9 C34 N10 107.5(5) . . ?
O9 C34 C35 105.7(5) . . ?
N10 C34 C35 115.6(5) . . ?
O7 C35 C34 110.5(6) . . ?
O7 C35 C36 115.9(5) . . ?
C34 C35 C36 99.8(5) . . ?
O8 C36 C37 113.6(6) . . ?
O8 C36 C35 106.5(5) . . ?
C37 C36 C35 101.7(5) . . ?
O9 C37 C36 106.0(5) . . ?
O9 C37 C38 108.6(5) . . ?
C36 C37 C38 115.2(5) . . ?
O10 C38 C37 112.7(6) . . ?
C7 O2 Si1 126.2(7) . . ?
O2 Si1 C14 111.5(5) . . ?
O2 Si1 C11 109.7(6) . . ?
C14 Si1 C11 114.7(7) . . ?
O2 Si1 C17 101.7(6) . . ?
C14 Si1 C17 108.6(7) . . ?
C11 Si1 C17 109.9(6) . . ?
C13 C11 C12 112.2(12) . . ?
C13 C11 Si1 113.4(10) . . ?
C12 C11 Si1 115.3(11) . . ?
C15 C14 C16 110.0(12) . . ?
C15 C14 Si1 115.6(11) . . ?
C16 C14 Si1 111.3(9) . . ?
C19 C17 C18 110.3(13) . . ?
C19 C17 Si1 110.5(9) . . ?
C18 C17 Si1 110.6(10) . . ?
C7 O2B Si1B 136.6(9) . . ?
O2B Si1B C11B 108.6(7) . . ?
O2B Si1B C17B 102.8(12) . . ?
C11B Si1B C17B 117.3(13) . . ?
O2B Si1B C14B 105.2(10) . . ?
C11B Si1B C14B 112.1(10) . . ?
C17B Si1B C14B 109.8(13) . . ?
C19B C17B C18B 115(2) . . ?
C19B C17B Si1B 116(2) . . ?
C18B C17B Si1B 113(2) . . ?
C12B C11B C13B 111.0(17) . . ?
C12B C11B Si1B 117.4(13) . . ?
C13B C11B Si1B 112.3(13) . . ?
C16B C14B C15B 109.4(19) . . ?
C16B C14B Si1B 115.1(18) . . ?
C15B C14B Si1B 112.2(17) . . ?
C8 O3 Si2 135.9(11) . . ?
O3 Si2 C23 103.2(8) . . ?
O3 Si2 C26 112.1(10) . . ?
C23 Si2 C26 111.4(9) . . ?
O3 Si2 C20 108.6(8) . . ?
C23 Si2 C20 111.9(10) . . ?
C26 Si2 C20 109.5(11) . . ?
C22 C20 C21 113.4(18) . . ?
C22 C20 Si2 118.0(15) . . ?
C21 C20 Si2 111.5(17) . . ?
C24 C23 C25 110.0(17) . . ?
C24 C23 Si2 110.7(12) . . ?
C25 C23 Si2 109.9(11) . . ?
C28 C26 C27 109.2(16) . . ?
C28 C26 Si2 117.6(15) . . ?
C27 C26 Si2 114.1(15) . . ?
C8 O3B Si2B 137.7(13) . . ?
O3B Si2B C23B 105.3(8) . . ?
O3B Si2B C20B 112.2(9) . . ?
C23B Si2B C20B 112.1(8) . . ?
O3B Si2B C26B 108.0(9) . . ?
C23B Si2B C26B 109.6(8) . . ?
C20B Si2B C26B 109.5(8) . . ?
C22B C20B C21B 112.7(15) . . ?
C22B C20B Si2B 116.4(15) . . ?
C21B C20B Si2B 109.8(12) . . ?
C24B C23B C25B 109.0(15) . . ?
C24B C23B Si2B 113.4(12) . . ?
C25B C23B Si2B 111.2(10) . . ?
C28B C26B C27B 111.5(19) . . ?
C28B C26B Si2B 112.6(18) . . ?
C27B C26B Si2B 111.5(12) . . ?
O7 Si3 C39B 107.4(7) . . ?
O7 Si3 C45B 106.6(7) . . ?
C39B Si3 C45B 127.3(10) . . ?
O7 Si3 C45 117.1(6) . . ?
C39B Si3 C45 135.2(9) . . ?
C45B Si3 C45 34.0(9) . . ?
O7 Si3 C42 109.6(5) . . ?
C39B Si3 C42 52.7(8) . . ?
C45B Si3 C42 141.0(8) . . ?
C45 Si3 C42 112.8(8) . . ?
O7 Si3 C42B 105.6(7) . . ?
C39B Si3 C42B 105.8(8) . . ?
C45B Si3 C42B 102.2(8) . . ?
C45 Si3 C42B 68.3(9) . . ?
C42 Si3 C42B 54.1(8) . . ?
O7 Si3 C39 102.9(5) . . ?
C39B Si3 C39 52.7(8) . . ?
C45B Si3 C39 81.2(8) . . ?
C45 Si3 C39 109.0(8) . . ?
C42 Si3 C39 104.2(7) . . ?
C42B Si3 C39 148.8(8) . . ?
C41 C39 C40 109.5(14) . . ?
C41 C39 Si3 116.1(11) . . ?
C40 C39 Si3 116.6(12) . . ?
C44 C42 C43 109(2) . . ?
C44 C42 Si3 107.1(18) . . ?
C43 C42 Si3 113.0(11) . . ?
C46 C45 C47 110.3(16) . . ?
C46 C45 Si3 115.4(13) . . ?
C47 C45 Si3 113.9(14) . . ?
C40B C39B C41B 115.2(17) . . ?
C40B C39B Si3 108.2(15) . . ?
C41B C39B Si3 113.6(16) . . ?
C43B C42B C44B 109.6(17) . . ?
C43B C42B Si3 111.5(14) . . ?
C44B C42B Si3 118.8(15) . . ?
C46B C45B C47B 108.1(17) . . ?
C46B C45B Si3 110.4(15) . . ?
C47B C45B Si3 113.8(15) . . ?
O8 Si4 C48 113.4(3) . . ?
O8 Si4 C54 108.6(3) . . ?
C48 Si4 C54 107.6(4) . . ?
O8 Si4 C51 101.1(4) . . ?
C48 Si4 C51 108.7(5) . . ?
C54 Si4 C51 117.5(5) . . ?
C50 C48 C49 110.2(8) . . ?
C50 C48 Si4 112.7(6) . . ?
C49 C48 Si4 114.9(5) . . ?
C53 C51 C52 114.3(11) . . ?
C53 C51 Si4 115.6(8) . . ?
C52 C51 Si4 115.8(8) . . ?
C56 C54 C55 109.9(7) . . ?
C56 C54 Si4 113.6(5) . . ?
C55 C54 Si4 112.9(6) . . ?

_diffrn_measured_fraction_theta_max 0.837
_diffrn_reflns_theta_full        73.37
_diffrn_measured_fraction_theta_full 0.837
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.097

#===END



