# Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is © The Royal Society of Chemistry 2003

data_global

_journal_coden_Cambridge         177

loop_
_publ_author_name
'Benjamin G. Davies'
'Andrei S. Batsanov'
'Daniel P.G. Emmerson'
'William P. Hems'
'Judith A.K. Howard'
'Claudia Mugnaini'
'Robert P. Tooze'
'Renaud Villard'

_publ_contact_author_name        'Dr Benjamin G Davies'
_publ_contact_author_address     
;
Dyson Perrins Laboratory, Department of Chemistry
University of Oxford
South Parks Road
Oxford
OX1 3QY
UNITED KINGDOM
;

_publ_contact_author_email       BEN.DAVIS@CHEM.OX.AC.UK

_publ_requested_journal          'Organic & Biomolecular Chemistry'

_publ_section_title              
;
Precise Structure Activity Relationships in
Asymmetric Catalysis using Carbohydrate Scaffolds to allow Ready Fine
Tuning: Dialkylzinc-Aldehyde additions
;
#======================================================================

data_4f
_database_code_CSD               184042

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
methyl 2-N-benzylamino-4,6-O-benzylidene-2-deoxy-α-D-glucopyranoside
;
_chemical_name_common            ?
_chemical_melting_point          '171\% C'
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H25 N O5'
_chemical_formula_weight         371.42
_chemical_absolute_configuration syn
_chemical_optical_rotation       '[\a]^25^~D~ +22 (c 0.70, CHCl~3~)'

_ccdc_disorder                   
'C(9) and H(91) are disordered between positions A (85%) and B (15%)'

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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)

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

_cell_length_a                   6.444(1)
_cell_length_b                   11.612(2)
_cell_length_c                   12.764(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.00(1)
_cell_angle_gamma                90.00
_cell_volume                     945.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    941
_cell_measurement_theta_min      12.0
_cell_measurement_theta_max      25.1

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.67
_exptl_crystal_density_meas      Not_measured
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             396
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 -1.00 0.1100
0.00 0.00 1.00 0.1100
0.00 -1.00 -1.00 0.1600
1.00 0.00 0.00 0.3300
-1.00 0.00 0.00 0.3300
0.00 1.00 -1.00 0.1200

_exptl_special_details           
;The data collection nominally covered full sphere
of reciprocal space, by a combination of 5 sets of ω scans;
each set at different φ and/or 2θ angles and each
scan (10 sec exposure) covering 0.3° in ω. Crystal to
detector distance 4.51 cm. 2347 Friedel equivalents (of which
2221 observed) were merged.
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SMART 1K CCD area detector'
_diffrn_measurement_method       'Ω scans'
_diffrn_detector_area_resol_mean 8
_diffrn_standards_decay_%        0
_diffrn_reflns_number            11594
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0132
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.6
_diffrn_reflns_theta_max         29.0
_reflns_number_total             2625
_reflns_number_gt                2537
_reflns_threshold_expression     I>2σ(I)
_reflns_Friedel_coverage         0.894

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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.
Amino and hydroxy H - refall, methyl group - rigid body with refined U,
other H atoms - riding.
;

_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)+(0.0566P)²+0.1812P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
undeterminable, Friedel pairs merged, all \Df'' set to 0
;
_refine_ls_number_reflns         2625
_refine_ls_number_parameters     259
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.0948
_refine_ls_wR_factor_gt          0.0932
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_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
O1 O 0.87057(19) 0.80757(12) 0.31504(10) 0.0260(3) Uani 1 1 d . . .
O3 O 0.36448(18) 0.58452(12) 0.15243(10) 0.0248(3) Uani 1 1 d . . .
H03 H 0.266(5) 0.623(3) 0.168(2) 0.045(8) Uiso 1 1 d . . .
O4 O 0.62436(17) 0.43659(10) 0.29455(9) 0.0207(2) Uani 1 1 d . . .
O5 O 0.99652(17) 0.65221(10) 0.22502(9) 0.0215(2) Uani 1 1 d . . .
O6 O 0.96514(18) 0.37808(11) 0.36368(10) 0.0257(3) Uani 1 1 d . . .
N N 0.4995(2) 0.82660(14) 0.16797(13) 0.0251(3) Uani 1 1 d . . .
H1N H 0.505(4) 0.855(3) 0.236(2) 0.041(7) Uiso 1 1 d . . .
C1 C 0.8708(2) 0.75448(15) 0.21589(13) 0.0215(3) Uani 1 1 d . . .
H1 H 0.9318 0.8096 0.1683 0.026 Uiso 1 1 d R . .
C2 C 0.6424(2) 0.72822(14) 0.16722(13) 0.0203(3) Uani 1 1 d . . .
H2 H 0.6454 0.7076 0.0914 0.024 Uiso 1 1 d R . .
C3 C 0.5465(2) 0.62464(14) 0.21891(12) 0.0194(3) Uani 1 1 d . . .
H3 H 0.5087 0.6477 0.2893 0.023 Uiso 1 1 d R . .
C4 C 0.7020(2) 0.52625(14) 0.23275(12) 0.0187(3) Uani 1 1 d . . .
H4 H 0.7201 0.4948 0.1617 0.022 Uiso 1 1 d R . .
C5 C 0.9135(2) 0.56650(14) 0.28877(13) 0.0199(3) Uani 1 1 d . . .
H5 H 0.8961 0.6000 0.3592 0.024 Uiso 1 1 d R . .
C6 C 1.0608(3) 0.46352(16) 0.30387(15) 0.0255(3) Uani 1 1 d . . .
H61 H 1.1982 0.4872 0.3425 0.033 Uiso 1 1 d R . .
H62 H 1.0834 0.4317 0.2344 0.033 Uiso 1 1 d R . .
C7 C 0.7671(2) 0.34331(14) 0.30874(13) 0.0207(3) Uani 1 1 d . . .
H7 H 0.7875 0.3122 0.2378 0.025 Uiso 1 1 d R . .
C8 C 1.0745(3) 0.8499(2) 0.35823(18) 0.0354(4) Uani 1 1 d . . .
H81 H 1.1204(14) 0.9066(14) 0.3108(10) 0.048(4) Uiso 1 1 d R . .
H82 H 1.0673(6) 0.8851(14) 0.4264(13) 0.048(4) Uiso 1 1 d R . .
H83 H 1.1731(18) 0.7866(11) 0.3667(12) 0.048(4) Uiso 1 1 d R . .
C9A C 0.5462(4) 0.9212(2) 0.0997(3) 0.0383(6) Uani 0.85 1 d P . .
H91A H 0.6857 0.9541 0.1256 0.050 Uiso 0.85 1 d PR . .
H92 H 0.5499 0.8909 0.0275 0.050 Uiso 1 1 d R . .
C9B C 0.454(3) 0.8968(18) 0.0731(15) 0.048(4) Uiso 0.15 1 d P . .
H91B H 0.3741 0.8359 -0.0029 0.062 Uiso 0.15 1 d PR . .
C11 C 0.3780(3) 1.01418(17) 0.09476(15) 0.0283(4) Uani 1 1 d . . .
C12 C 0.4373(3) 1.1222(2) 0.13300(15) 0.0337(4) Uani 1 1 d . . .
H12 H 0.5799 1.1355 0.1608 0.040 Uiso 1 1 d R . .
C13 C 0.2963(4) 1.21191(19) 0.13156(18) 0.0420(5) Uani 1 1 d . . .
H13 H 0.3408 1.2848 0.1601 0.050 Uiso 1 1 d R . .
C14 C 0.0904(4) 1.1943(2) 0.08911(18) 0.0451(6) Uani 1 1 d . . .
H14 H -0.0075 1.2558 0.0870 0.054 Uiso 1 1 d R . .
C15 C 0.0242(3) 1.0867(3) 0.04857(17) 0.0451(6) Uani 1 1 d . . .
H15 H -0.1176 1.0743 0.0188 0.054 Uiso 1 1 d R . .
C16 C 0.1697(3) 0.9957(2) 0.05250(16) 0.0366(5) Uani 1 1 d . . .
H16 H 0.1264 0.9217 0.0263 0.044 Uiso 1 1 d R . .
C21 C 0.6753(2) 0.25011(15) 0.37060(12) 0.0206(3) Uani 1 1 d . . .
C22 C 0.4871(3) 0.26667(15) 0.41065(14) 0.0242(3) Uani 1 1 d . . .
H22 H 0.4184 0.3392 0.4022 0.029 Uiso 1 1 d R . .
C23 C 0.3982(3) 0.17788(17) 0.46293(15) 0.0291(4) Uani 1 1 d . . .
H23 H 0.2716 0.1908 0.4914 0.035 Uiso 1 1 d R . .
C24 C 0.4944(3) 0.07056(17) 0.47374(15) 0.0316(4) Uani 1 1 d . . .
H24 H 0.4325 0.0096 0.5082 0.038 Uiso 1 1 d R . .
C25 C 0.6832(3) 0.05319(18) 0.43367(17) 0.0347(4) Uani 1 1 d . . .
H25 H 0.7499 -0.0199 0.4409 0.042 Uiso 1 1 d R . .
C26 C 0.7738(3) 0.14230(17) 0.38303(15) 0.0300(4) Uani 1 1 d . . .
H26 H 0.9027 0.1300 0.3565 0.036 Uiso 1 1 d 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
O1 C1 1.408(2) . ?
O1 C8 1.439(2) . ?
O3 C3 1.4270(19) . ?
O4 C7 1.4162(18) . ?
O4 C4 1.4374(19) . ?
O5 C1 1.4330(19) . ?
O5 C5 1.4353(19) . ?
O6 C7 1.4265(19) . ?
O6 C6 1.442(2) . ?
N C9B 1.46(2) . ?
N C9A 1.460(3) . ?
N C2 1.468(2) . ?
C1 C2 1.547(2) . ?
C2 C3 1.542(2) . ?
C3 C4 1.514(2) . ?
C4 C5 1.522(2) . ?
C5 C6 1.522(2) . ?
C7 C21 1.508(2) . ?
C9A C9B 0.70(2) . ?
C9A C11 1.525(3) . ?
C9B C11 1.49(2) . ?
C11 C12 1.380(3) . ?
C11 C16 1.392(3) . ?
C12 C13 1.381(3) . ?
C13 C14 1.377(4) . ?
C14 C15 1.396(4) . ?
C15 C16 1.409(4) . ?
C21 C22 1.393(2) . ?
C21 C26 1.403(2) . ?
C22 C23 1.394(2) . ?
C23 C24 1.390(3) . ?
C24 C25 1.398(3) . ?
C25 C26 1.391(3) . ?

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 O1 C8 112.25(13) . . ?
C7 O4 C4 110.78(11) . . ?
C1 O5 C5 111.70(12) . . ?
C7 O6 C6 110.73(12) . . ?
C9B N C9A 27.8(8) . . ?
C9B N C2 118.9(8) . . ?
C9A N C2 113.58(14) . . ?
O1 C1 O5 111.17(13) . . ?
O1 C1 C2 109.10(13) . . ?
O5 C1 C2 111.40(13) . . ?
N C2 C3 108.38(12) . . ?
N C2 C1 114.01(14) . . ?
C3 C2 C1 113.43(13) . . ?
O3 C3 C4 107.39(14) . . ?
O3 C3 C2 110.20(13) . . ?
C4 C3 C2 109.93(12) . . ?
O4 C4 C3 109.61(11) . . ?
O4 C4 C5 108.77(12) . . ?
C3 C4 C5 110.97(13) . . ?
O5 C5 C4 109.06(12) . . ?
O5 C5 C6 109.97(13) . . ?
C4 C5 C6 108.67(13) . . ?
O6 C6 C5 107.61(13) . . ?
O4 C7 O6 111.53(13) . . ?
O4 C7 C21 108.72(12) . . ?
O6 C7 C21 109.57(13) . . ?
C9B C9A N 75.8(17) . . ?
C9B C9A C11 73.6(17) . . ?
N C9A C11 110.67(16) . . ?
C9A C9B N 76.4(16) . . ?
C9A C9B C11 79.5(18) . . ?
N C9B C11 113.0(13) . . ?
C12 C11 C16 118.79(19) . . ?
C12 C11 C9B 144.6(8) . . ?
C16 C11 C9B 96.5(8) . . ?
C12 C11 C9A 117.9(2) . . ?
C16 C11 C9A 123.3(2) . . ?
C9B C11 C9A 26.8(8) . . ?
C11 C12 C13 122.10(19) . . ?
C14 C13 C12 119.3(2) . . ?
C13 C14 C15 120.4(2) . . ?
C14 C15 C16 119.35(19) . . ?
C11 C16 C15 120.0(2) . . ?
C22 C21 C26 119.01(16) . . ?
C22 C21 C7 121.18(14) . . ?
C26 C21 C7 119.70(15) . . ?
C21 C22 C23 120.68(16) . . ?
C24 C23 C22 120.22(17) . . ?
C23 C24 C25 119.44(18) . . ?
C26 C25 C24 120.37(18) . . ?
C25 C26 C21 120.25(17) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N H1N O1 0.93(3) 2.49(3) 2.836(2) 102.1(19) .
O3 H03 O5 0.82(3) 2.00(3) 2.7766(17) 156(3) 1_455

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        29.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.038

#==============================================================END

data_4g
_database_code_CSD               184043

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
methyl 2-N,N-dibenzylamino-4,6-O-benzylidene-2-deoxy-α-D-glucopyranoside
;
_chemical_name_common            ?
_chemical_melting_point          '147\% C'
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H31 N O5'
_chemical_formula_weight         461.54
_chemical_absolute_configuration syn
_chemical_optical_rotation       '[\a]^25^~D~ +43.7 (c 1.12, CHCl~3~)'

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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)

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

_cell_length_a                   6.282(1)
_cell_length_b                   19.484(4)
_cell_length_c                   10.205(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.22(1)
_cell_angle_gamma                90.00
_cell_volume                     1249.1(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6129
_cell_measurement_theta_min      4.51
_cell_measurement_theta_max      54.92

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.32
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             492
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   none

_exptl_special_details           
;The data collection nominally covered full sphere
of reciprocal space, by a combination of 5 sets of ω scans;
each set at different φ and/or 2θ angles and each
scan (10 s exposure) covering 0.3° in ω. Crystal to
detector distance 4.51 cm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SMART 1K CCD area detector'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 8
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8585
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         27.48
_reflns_number_total             2937
_reflns_number_gt                2810
_reflns_threshold_expression     I>2σ(I)
_reflns_Friedel_coverage         0.50

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 1465 Friedel
equivalents [of which 1372 with I>2σ(I)] were merged. Absolute
configuration (undeterminable from anomalous dispersion)assigned by
reference to unchanging chiral centres in the synthetic procedure.
Hydroxy H atom - refall, methyl group - rigid rotating body with a common
refined U for three H, other H atoms - riding in idealised positions.
;

_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)+(0.0444P)²+0.2061P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
undeterminable, Friedel pairs merged, all \Df'' set to 0
;
_refine_ls_number_reflns         2937
_refine_ls_number_parameters     314
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0311
_refine_ls_wR_factor_ref         0.0785
_refine_ls_wR_factor_gt          0.0773
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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
O1 O -0.18965(19) 0.35579(7) 0.22849(12) 0.0189(3) Uani 1 1 d . . .
O2 O 0.0313(2) 0.49914(7) 0.41543(13) 0.0221(3) Uani 1 1 d . . .
O3 O 0.30808(19) 0.44783(6) 0.29653(12) 0.0177(3) Uani 1 1 d . . .
O4 O 0.4336(2) 0.35775(7) 0.08216(12) 0.0185(2) Uani 1 1 d . . .
H04 H 0.539(4) 0.3680(13) 0.127(2) 0.027(6) Uiso 1 1 d . . .
O5 O -0.0485(2) 0.24800(7) 0.28424(12) 0.0210(3) Uani 1 1 d . . .
N1 N 0.1506(2) 0.24079(7) 0.02715(14) 0.0172(3) Uani 1 1 d . . .
C1 C -0.1059(3) 0.29193(9) 0.18068(16) 0.0174(3) Uani 1 1 d . . .
H1 H -0.2184 0.2688 0.1270 0.021 Uiso 1 1 calc R . .
C2 C 0.0889(3) 0.30463(8) 0.09315(16) 0.0155(3) Uani 1 1 d . . .
H2 H 0.0398 0.3365 0.0224 0.019 Uiso 1 1 calc R . .
C3 C 0.2626(3) 0.34371(9) 0.16967(16) 0.0152(3) Uani 1 1 d . . .
H3 H 0.3142 0.3154 0.2451 0.018 Uiso 1 1 calc R . .
C4 C 0.1593(3) 0.40926(9) 0.21915(16) 0.0163(3) Uani 1 1 d . . .
H4 H 0.1139 0.4376 0.1423 0.020 Uiso 1 1 calc R . .
C5 C -0.0353(3) 0.39361(9) 0.30353(17) 0.0173(3) Uani 1 1 d . . .
H5 H 0.0086 0.3664 0.3822 0.021 Uiso 1 1 calc R . .
C6 C -0.1310(3) 0.46166(10) 0.34642(18) 0.0218(4) Uani 1 1 d . . .
H61 H -0.1799 0.4880 0.2691 0.028 Uiso 1 1 calc R . .
H62 H -0.2545 0.4536 0.4043 0.028 Uiso 1 1 calc R . .
C7 C 0.2131(3) 0.51101(9) 0.33746(17) 0.0199(4) Uani 1 1 d . . .
H7 H 0.1732 0.5390 0.2590 0.024 Uiso 1 1 calc R . .
C8 C -0.2297(3) 0.22097(11) 0.3527(2) 0.0280(4) Uani 1 1 d . . .
H81 H -0.311(2) 0.1918(8) 0.2941(11) 0.042(4) Uiso 1 1 calc R . .
H82 H -0.318(2) 0.2585(6) 0.3826(15) 0.042(4) Uiso 1 1 calc R . .
H83 H -0.1817(8) 0.1943(8) 0.4274(15) 0.042(4) Uiso 1 1 calc R . .
C9 C 0.2248(3) 0.25063(10) -0.10930(17) 0.0208(4) Uani 1 1 d . . .
H91 H 0.2621 0.2054 -0.1470 0.027 Uiso 1 1 calc R . .
H92 H 0.3554 0.2791 -0.1083 0.027 Uiso 1 1 calc R . .
C10 C 0.3056(3) 0.19860(9) 0.09912(17) 0.0189(3) Uani 1 1 d . . .
H101 H 0.2873 0.2063 0.1943 0.025 Uiso 1 1 calc R . .
H102 H 0.4513 0.2133 0.0755 0.025 Uiso 1 1 calc R . .
C20 C 0.0600(3) 0.28471(10) -0.19599(16) 0.0200(4) Uani 1 1 d . . .
C21 C -0.1329(3) 0.25192(11) -0.22369(19) 0.0260(4) Uani 1 1 d . . .
H21 H -0.1601 0.2077 -0.1884 0.031 Uiso 1 1 calc R . .
C22 C -0.2855(3) 0.28351(12) -0.30244(19) 0.0304(4) Uani 1 1 d . . .
H22 H -0.4161 0.2608 -0.3206 0.037 Uiso 1 1 calc R . .
C23 C -0.2474(3) 0.34807(12) -0.35447(19) 0.0295(4) Uani 1 1 d . . .
H23 H -0.3521 0.3696 -0.4079 0.035 Uiso 1 1 calc R . .
C24 C -0.0565(4) 0.38136(11) -0.32868(19) 0.0303(4) Uani 1 1 d . . .
H24 H -0.0301 0.4256 -0.3644 0.036 Uiso 1 1 calc R . .
C25 C 0.0969(3) 0.34947(10) -0.24984(18) 0.0253(4) Uani 1 1 d . . .
H25 H 0.2279 0.3722 -0.2327 0.030 Uiso 1 1 calc R . .
C30 C 0.2813(3) 0.12279(9) 0.07005(17) 0.0188(3) Uani 1 1 d . . .
C31 C 0.0878(3) 0.09002(10) 0.09582(18) 0.0221(4) Uani 1 1 d . . .
H31 H -0.0321 0.1163 0.1221 0.026 Uiso 1 1 calc R . .
C32 C 0.0700(3) 0.01917(10) 0.08323(19) 0.0256(4) Uani 1 1 d . . .
H32 H -0.0614 -0.0028 0.1020 0.031 Uiso 1 1 calc R . .
C33 C 0.2447(3) -0.01971(10) 0.04305(19) 0.0251(4) Uani 1 1 d . . .
H33 H 0.2331 -0.0682 0.0362 0.030 Uiso 1 1 calc R . .
C34 C 0.4353(3) 0.01259(10) 0.01312(19) 0.0261(4) Uani 1 1 d . . .
H34 H 0.5533 -0.0135 -0.0167 0.031 Uiso 1 1 calc R . .
C35 C 0.4531(3) 0.08382(10) 0.02706(18) 0.0214(4) Uani 1 1 d . . .
H35 H 0.5839 0.1058 0.0070 0.026 Uiso 1 1 calc R . .
C40 C 0.3770(3) 0.54872(9) 0.41790(18) 0.0197(3) Uani 1 1 d . . .
C41 C 0.4949(3) 0.60173(10) 0.36298(19) 0.0249(4) Uani 1 1 d . . .
H41 H 0.4654 0.6164 0.2760 0.030 Uiso 1 1 calc R . .
C42 C 0.6568(3) 0.63363(11) 0.4352(2) 0.0281(4) Uani 1 1 d . . .
H42 H 0.7363 0.6701 0.3977 0.034 Uiso 1 1 calc R . .
C43 C 0.7010(3) 0.61161(11) 0.56202(19) 0.0266(4) Uani 1 1 d . . .
H43 H 0.8115 0.6329 0.6111 0.032 Uiso 1 1 calc R . .
C44 C 0.5838(3) 0.55859(11) 0.61713(19) 0.0265(4) Uani 1 1 d . . .
H44 H 0.6147 0.5436 0.7037 0.032 Uiso 1 1 calc R . .
C45 C 0.4212(3) 0.52741(10) 0.54583(18) 0.0234(4) Uani 1 1 d . . .
H45 H 0.3401 0.4916 0.5842 0.028 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
O1 C5 1.437(2) . ?
O1 C1 1.437(2) . ?
O2 C7 1.414(2) . ?
O2 C6 1.436(2) . ?
O3 C7 1.431(2) . ?
O3 C4 1.4337(19) . ?
O4 C3 1.426(2) . ?
O4 H04 0.83(3) . ?
O5 C1 1.406(2) . ?
O5 C8 1.438(2) . ?
N1 C10 1.469(2) . ?
N1 C2 1.468(2) . ?
N1 C9 1.483(2) . ?
C1 C2 1.538(2) . ?
C1 H1 1.0000 . ?
C2 C3 1.540(2) . ?
C2 H2 1.0000 . ?
C3 C4 1.520(2) . ?
C3 H3 1.0000 . ?
C4 C5 1.529(2) . ?
C4 H4 1.0000 . ?
C5 C6 1.521(2) . ?
C5 H5 1.0000 . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
C7 C40 1.506(2) . ?
C7 H7 1.0000 . ?
C8 H81 0.9700 . ?
C8 H82 0.9700 . ?
C8 H83 0.9700 . ?
C9 C20 1.513(2) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
C10 C30 1.514(2) . ?
C10 H101 0.9900 . ?
C10 H102 0.9900 . ?
C20 C25 1.396(3) . ?
C20 C21 1.398(3) . ?
C21 C22 1.392(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.387(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.388(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.399(3) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C30 C35 1.392(3) . ?
C30 C31 1.399(3) . ?
C31 C32 1.391(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.397(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.388(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.400(3) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C40 C41 1.390(3) . ?
C40 C45 1.397(3) . ?
C41 C42 1.399(3) . ?
C41 H41 0.9500 . ?
C42 C43 1.391(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.389(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.391(3) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?

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
C5 O1 C1 112.19(12) . . ?
C7 O2 C6 112.38(13) . . ?
C7 O3 C4 109.88(13) . . ?
C3 O4 H04 107.7(17) . . ?
C1 O5 C8 112.77(14) . . ?
C10 N1 C2 114.87(13) . . ?
C10 N1 C9 109.40(14) . . ?
C2 N1 C9 113.95(14) . . ?
O5 C1 O1 111.41(13) . . ?
O5 C1 C2 109.42(13) . . ?
O1 C1 C2 110.55(14) . . ?
O5 C1 H1 108.5 . . ?
O1 C1 H1 108.5 . . ?
C2 C1 H1 108.5 . . ?
N1 C2 C1 110.02(13) . . ?
N1 C2 C3 117.64(13) . . ?
C1 C2 C3 110.40(13) . . ?
N1 C2 H2 106.0 . . ?
C1 C2 H2 106.0 . . ?
C3 C2 H2 106.0 . . ?
O4 C3 C4 111.73(14) . . ?
O4 C3 C2 108.12(13) . . ?
C4 C3 C2 106.36(13) . . ?
O4 C3 H3 110.2 . . ?
C4 C3 H3 110.2 . . ?
C2 C3 H3 110.2 . . ?
O3 C4 C3 110.21(13) . . ?
O3 C4 C5 108.37(13) . . ?
C3 C4 C5 111.27(14) . . ?
O3 C4 H4 109.0 . . ?
C3 C4 H4 109.0 . . ?
C5 C4 H4 109.0 . . ?
O1 C5 C6 109.50(13) . . ?
O1 C5 C4 109.98(13) . . ?
C6 C5 C4 107.83(14) . . ?
O1 C5 H5 109.8 . . ?
C6 C5 H5 109.8 . . ?
C4 C5 H5 109.8 . . ?
O2 C6 C5 107.69(13) . . ?
O2 C6 H61 110.2 . . ?
C5 C6 H61 110.2 . . ?
O2 C6 H62 110.2 . . ?
C5 C6 H62 110.2 . . ?
H61 C6 H62 108.5 . . ?
O2 C7 O3 111.24(14) . . ?
O2 C7 C40 108.98(14) . . ?
O3 C7 C40 107.09(14) . . ?
O2 C7 H7 109.8 . . ?
O3 C7 H7 109.8 . . ?
C40 C7 H7 109.8 . . ?
O5 C8 H81 109.5 . . ?
O5 C8 H82 109.5 . . ?
H81 C8 H82 109.5 . . ?
O5 C8 H83 109.5 . . ?
H81 C8 H83 109.5 . . ?
H82 C8 H83 109.5 . . ?
N1 C9 C20 112.90(14) . . ?
N1 C9 H91 109.0 . . ?
C20 C9 H91 109.0 . . ?
N1 C9 H92 109.0 . . ?
C20 C9 H92 109.0 . . ?
H91 C9 H92 107.8 . . ?
N1 C10 C30 112.46(14) . . ?
N1 C10 H101 109.1 . . ?
C30 C10 H101 109.1 . . ?
N1 C10 H102 109.1 . . ?
C30 C10 H102 109.1 . . ?
H101 C10 H102 107.8 . . ?
C25 C20 C21 118.59(17) . . ?
C25 C20 C9 120.84(17) . . ?
C21 C20 C9 120.57(17) . . ?
C22 C21 C20 120.61(19) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C23 C22 C21 120.18(19) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C24 C23 C22 120.12(19) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 119.63(19) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
C20 C25 C24 120.87(18) . . ?
C20 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C35 C30 C31 119.04(17) . . ?
C35 C30 C10 121.10(17) . . ?
C31 C30 C10 119.69(17) . . ?
C32 C31 C30 120.35(18) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C31 C32 C33 120.16(19) . . ?
C31 C32 H32 119.9 . . ?
C33 C32 H32 119.9 . . ?
C34 C33 C32 119.90(18) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C33 C34 C35 119.72(19) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
C30 C35 C34 120.77(19) . . ?
C30 C35 H35 119.6 . . ?
C34 C35 H35 119.6 . . ?
C41 C40 C45 119.54(17) . . ?
C41 C40 C7 120.47(16) . . ?
C45 C40 C7 119.85(17) . . ?
C40 C41 C42 120.35(18) . . ?
C40 C41 H41 119.8 . . ?
C42 C41 H41 119.8 . . ?
C43 C42 C41 119.66(19) . . ?
C43 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?
C44 C43 C42 120.16(18) . . ?
C44 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
C43 C44 C45 120.15(18) . . ?
C43 C44 H44 119.9 . . ?
C45 C44 H44 119.9 . . ?
C44 C45 C40 120.13(18) . . ?
C44 C45 H45 119.9 . . ?
C40 C45 H45 119.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8 O5 C1 O1 70.91(18) . . . . ?
C8 O5 C1 C2 -166.53(15) . . . . ?
C5 O1 C1 O5 62.60(17) . . . . ?
C5 O1 C1 C2 -59.31(16) . . . . ?
C10 N1 C2 C1 -90.18(16) . . . . ?
C9 N1 C2 C1 142.48(14) . . . . ?
C10 N1 C2 C3 37.4(2) . . . . ?
C9 N1 C2 C3 -89.96(17) . . . . ?
O5 C1 C2 N1 66.57(17) . . . . ?
O1 C1 C2 N1 -170.36(12) . . . . ?
O5 C1 C2 C3 -64.90(18) . . . . ?
O1 C1 C2 C3 58.17(17) . . . . ?
N1 C2 C3 O4 56.06(18) . . . . ?
C1 C2 C3 O4 -176.56(13) . . . . ?
N1 C2 C3 C4 176.20(14) . . . . ?
C1 C2 C3 C4 -56.43(17) . . . . ?
C7 O3 C4 C3 177.21(14) . . . . ?
C7 O3 C4 C5 -60.81(16) . . . . ?
O4 C3 C4 O3 -64.56(17) . . . . ?
C2 C3 C4 O3 177.67(13) . . . . ?
O4 C3 C4 C5 175.19(13) . . . . ?
C2 C3 C4 C5 57.42(16) . . . . ?
C1 O1 C5 C6 177.76(13) . . . . ?
C1 O1 C5 C4 59.45(17) . . . . ?
O3 C4 C5 O1 179.15(13) . . . . ?
C3 C4 C5 O1 -59.53(17) . . . . ?
O3 C4 C5 C6 59.80(16) . . . . ?
C3 C4 C5 C6 -178.87(14) . . . . ?
C7 O2 C6 C5 58.81(18) . . . . ?
O1 C5 C6 O2 -177.25(14) . . . . ?
C4 C5 C6 O2 -57.61(17) . . . . ?
C6 O2 C7 O3 -60.65(18) . . . . ?
C6 O2 C7 C40 -178.49(14) . . . . ?
C4 O3 C7 O2 60.99(17) . . . . ?
C4 O3 C7 C40 179.96(14) . . . . ?
C10 N1 C9 C20 171.64(15) . . . . ?
C2 N1 C9 C20 -58.2(2) . . . . ?
C2 N1 C10 C30 150.49(15) . . . . ?
C9 N1 C10 C30 -79.89(18) . . . . ?
N1 C9 C20 C25 115.50(18) . . . . ?
N1 C9 C20 C21 -64.4(2) . . . . ?
N1 C10 C30 C35 125.85(17) . . . . ?
N1 C10 C30 C31 -58.9(2) . . . . ?
O2 C7 C40 C41 -139.15(17) . . . . ?
O3 C7 C40 C41 100.42(19) . . . . ?
O2 C7 C40 C45 45.2(2) . . . . ?
O3 C7 C40 C45 -75.3(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H04 O1 0.83(3) 2.00(3) 2.7940(18) 159(2) 1_655

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.037

#=====================================================END

data_5g
_database_code_CSD               184044

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
methyl 2-N,N-dibenzylamino-4,6-O-benzylidene-2-deoxy-β-D-glucopyranoside
;
_chemical_name_common            ?
_chemical_melting_point          '72\% C'
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H31 N O5'
_chemical_formula_weight         461.54
_chemical_absolute_configuration syn
_chemical_optical_rotation       '[\a]^25^~D~ -73.1 (c 1.09, CHCl~3~)'

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)

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

_cell_length_a                   10.073(1)
_cell_length_b                   19.170(1)
_cell_length_c                   13.434(1)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.60(1)
_cell_angle_gamma                90.00
_cell_volume                     2498.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    663
_cell_measurement_theta_min      12.0
_cell_measurement_theta_max      21.1

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'Not measured'
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             984
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   none

_exptl_special_details           
; The data collection nominally covered over a hemisphere
of reciprocal space, by a combination of 4 sets of ω scans;
each set at different φ and/or 2θ angles and each
scan (20 sec exposure) covering 0.3° in ω.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SMART 1K CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 8
_diffrn_standards_decay_%        0
_diffrn_reflns_number            18494
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.57
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5891
_reflns_number_gt                4958
_reflns_threshold_expression     I>2σ(I)
_reflns_Friedel_coverage         0.91

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 5376 Friedel
equivalents [of which 4254 with I>2σ(I)] were merged. Absolute
configuration (undeterminable from anomalous dispersion)assigned by
reference to unchanging chiral centres in the synthetic procedure.
Hydroxy H atom - refall, methyl groups - rigid rotating bodies with a
common refined U for three H, other H atoms - riding in idealised
positions.
;

_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)+(0.0278P)²+0.7316P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
undeterminable, Friedel pairs merged, all \Df'' set to 0
;
_refine_ls_number_reflns         5891
_refine_ls_number_parameters     625
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.0918
_refine_ls_wR_factor_gt          0.0839
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_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
O1A O 0.0440(2) 0.00181(10) 0.36636(14) 0.0295(4) Uani 1 1 d . . .
O2A O 0.0145(3) -0.05267(10) 0.61859(15) 0.0393(5) Uani 1 1 d . . .
O3A O -0.00613(19) 0.06924(10) 0.60811(13) 0.0265(4) Uani 1 1 d . . .
O4A O -0.0386(2) 0.19408(11) 0.48024(15) 0.0301(4) Uani 1 1 d . . .
H0A H -0.021(4) 0.227(2) 0.438(3) 0.062(12) Uiso 1 1 d . . .
O5A O 0.0919(2) 0.05114(10) 0.22516(15) 0.0309(4) Uani 1 1 d . . .
N1A N 0.0805(2) 0.19399(12) 0.31426(16) 0.0231(5) Uani 1 1 d . . .
C1A C 0.1058(3) 0.06098(15) 0.3307(2) 0.0266(6) Uani 1 1 d . . .
H1A H 0.2056 0.0639 0.3688 0.035 Uiso 1 1 d R . .
C2A C 0.0320(3) 0.12782(14) 0.34823(19) 0.0223(5) Uani 1 1 d . . .
H2A H -0.0673 0.1225 0.3096 0.029 Uiso 1 1 d R . .
C3A C 0.0385(3) 0.13494(14) 0.4644(2) 0.0239(5) Uani 1 1 d . . .
H3A H 0.1368 0.1407 0.5051 0.031 Uiso 1 1 d R . .
C4A C -0.0190(3) 0.06892(15) 0.4988(2) 0.0251(6) Uani 1 1 d . . .
H4A H -0.1185 0.0641 0.4604 0.033 Uiso 1 1 d R . .
C5A C 0.0607(3) 0.00634(15) 0.4748(2) 0.0291(6) Uani 1 1 d . . .
H5A H 0.1606 0.0120 0.5112 0.038 Uiso 1 1 d R . .
C8A C 0.1751(3) -0.00553(16) 0.2063(2) 0.0373(7) Uani 1 1 d . . .
H8A1 H 0.2721 0.0033 0.2419 0.050(6) Uiso 1 1 d R . .
H8A2 H 0.1645 -0.0097 0.1318 0.050(6) Uiso 1 1 d R . .
H8A3 H 0.1453 -0.0490 0.2321 0.050(6) Uiso 1 1 d R . .
C6A C 0.0074(4) -0.06039(16) 0.5108(2) 0.0409(8) Uani 1 1 d . . .
H6A1 H -0.0890 -0.0688 0.4705 0.053 Uiso 1 1 d R . .
H6A2 H 0.0642 -0.1005 0.5007 0.053 Uiso 1 1 d R . .
C7A C -0.0621(3) 0.00580(16) 0.6350(2) 0.0330(7) Uani 1 1 d . . .
H7A H -0.1590 0.0009 0.5912 0.043 Uiso 1 1 d R . .
C9A C 0.2333(3) 0.19953(14) 0.3425(2) 0.0248(5) Uani 1 1 d . . .
H9A1 H 0.2689 0.1733 0.2916 0.032 Uiso 1 1 d R . .
H9A2 H 0.2716 0.1779 0.4111 0.032 Uiso 1 1 d R . .
C10A C 0.0230(3) 0.20979(15) 0.2036(2) 0.0275(6) Uani 1 1 d . . .
H10A H 0.0488 0.1719 0.1624 0.036 Uiso 1 1 d R . .
H10B H 0.0653 0.2534 0.1872 0.036 Uiso 1 1 d R . .
C20A C 0.2813(3) 0.27430(13) 0.3457(2) 0.0228(5) Uani 1 1 d . . .
C21A C 0.3198(3) 0.30404(15) 0.2621(2) 0.0290(6) Uani 1 1 d . . .
H21A H 0.3154 0.2770 0.2020 0.035 Uiso 1 1 d R . .
C22A C 0.3641(3) 0.37281(16) 0.2672(2) 0.0353(7) Uani 1 1 d . . .
H22A H 0.3883 0.3930 0.2099 0.042 Uiso 1 1 d R . .
C23A C 0.3733(3) 0.41229(15) 0.3552(2) 0.0323(6) Uani 1 1 d . . .
H23A H 0.4039 0.4593 0.3584 0.039 Uiso 1 1 d R . .
C24A C 0.3379(3) 0.38256(15) 0.4386(2) 0.0287(6) Uani 1 1 d . . .
H24A H 0.3457 0.4093 0.4995 0.034 Uiso 1 1 d R . .
C25A C 0.2908(3) 0.31419(15) 0.4340(2) 0.0255(6) Uani 1 1 d . . .
H25A H 0.2653 0.2946 0.4911 0.031 Uiso 1 1 d R . .
C30A C -0.1317(3) 0.21794(14) 0.1709(2) 0.0259(6) Uani 1 1 d . . .
C31A C -0.2134(3) 0.16928(17) 0.1052(2) 0.0335(6) Uani 1 1 d . . .
H31A H -0.1717 0.1293 0.0848 0.040 Uiso 1 1 d R . .
C32A C -0.3555(3) 0.17850(19) 0.0690(2) 0.0417(8) Uani 1 1 d . . .
H32A H -0.4097 0.1453 0.0231 0.050 Uiso 1 1 d R . .
C33A C -0.4167(3) 0.23587(19) 0.0998(3) 0.0467(9) Uani 1 1 d . . .
H33A H -0.5137 0.2420 0.0756 0.056 Uiso 1 1 d R . .
C34A C -0.3370(4) 0.28421(19) 0.1661(3) 0.0480(9) Uani 1 1 d . . .
H34A H -0.3795 0.3237 0.1873 0.058 Uiso 1 1 d R . .
C35A C -0.1943(3) 0.27547(16) 0.2021(2) 0.0357(7) Uani 1 1 d . . .
H35A H -0.1403 0.3087 0.2480 0.043 Uiso 1 1 d R . .
C40A C -0.0635(3) 0.00789(16) 0.7468(2) 0.0341(7) Uani 1 1 d . . .
C41A C -0.1401(3) 0.05965(19) 0.7787(2) 0.0383(7) Uani 1 1 d . . .
H41A H -0.1862 0.0940 0.7308 0.046 Uiso 1 1 d R . .
C42A C -0.1491(3) 0.0615(2) 0.8803(3) 0.0474(9) Uani 1 1 d . . .
H42A H -0.1992 0.0976 0.9023 0.057 Uiso 1 1 d R . .
C43A C -0.0849(5) 0.0106(2) 0.9485(3) 0.0596(12) Uani 1 1 d . . .
H43A H -0.0925 0.0111 1.0174 0.071 Uiso 1 1 d R . .
C44A C -0.0106(6) -0.0409(2) 0.9174(3) 0.0786(16) Uani 1 1 d . . .
H44A H 0.0325 -0.0762 0.9649 0.094 Uiso 1 1 d R . .
C45A C 0.0021(5) -0.04192(19) 0.8166(3) 0.0660(13) Uani 1 1 d . . .
H45A H 0.0549 -0.0772 0.7955 0.079 Uiso 1 1 d R . .
O1B O 0.35721(19) 0.12785(11) 0.87440(14) 0.0281(4) Uani 1 1 d . . .
O2B O 0.4959(2) 0.06761(12) 0.66715(16) 0.0446(6) Uani 1 1 d . . .
O3B O 0.37509(18) 0.17049(10) 0.61321(13) 0.0236(4) Uani 1 1 d . . .
O4B O 0.2323(2) 0.29049(11) 0.66542(16) 0.0335(5) Uani 1 1 d . . .
H0B H 0.178(3) 0.3109(19) 0.682(3) 0.039(10) Uiso 1 1 d . . .
O5B O 0.24933(19) 0.17768(10) 0.98533(13) 0.0272(4) Uani 1 1 d . . .
C8B C 0.2451(3) 0.11543(16) 1.0443(2) 0.0358(7) Uani 1 1 d . . .
H8B1 H 0.1539 0.0938 1.0203 0.056(6) Uiso 1 1 d R . .
H8B2 H 0.2629 0.1275 1.1176 0.056(6) Uiso 1 1 d R . .
H8B3 H 0.3155 0.0826 1.0353 0.056(6) Uiso 1 1 d R . .
N1B N 0.0975(2) 0.27547(12) 0.82300(16) 0.0237(5) Uani 1 1 d . . .
C1B C 0.2350(3) 0.16339(14) 0.88102(19) 0.0238(5) Uani 1 1 d . . .
H1B H 0.1520 0.1336 0.8524 0.031 Uiso 1 1 d R . .
C2B C 0.2208(2) 0.23340(14) 0.82335(19) 0.0209(5) Uani 1 1 d . . .
H2B H 0.3026 0.2621 0.8591 0.027 Uiso 1 1 d R . .
C3B C 0.2289(3) 0.22363(14) 0.7112(2) 0.0236(5) Uani 1 1 d . . .
H3B H 0.1468 0.1968 0.6709 0.031 Uiso 1 1 d R . .
C4B C 0.3584(3) 0.18376(14) 0.71456(19) 0.0228(5) Uani 1 1 d . . .
H4B H 0.4392 0.2114 0.7548 0.030 Uiso 1 1 d R . .
C5B C 0.3554(3) 0.11463(15) 0.7696(2) 0.0292(6) Uani 1 1 d . . .
H5B H 0.2705 0.0879 0.7345 0.038 Uiso 1 1 d R . .
C6B C 0.4828(4) 0.0726(2) 0.7707(2) 0.0490(10) Uani 1 1 d . . .
H6B1 H 0.5653 0.0952 0.8162 0.064 Uiso 1 1 d R . .
H6B2 H 0.4745 0.0252 0.7978 0.064 Uiso 1 1 d R . .
C7B C 0.5016(3) 0.13397(16) 0.6238(2) 0.0306(6) Uani 1 1 d . . .
H7B H 0.5785 0.1613 0.6700 0.040 Uiso 1 1 d R . .
C9B C 0.1195(3) 0.32333(14) 0.9122(2) 0.0256(6) Uani 1 1 d . . .
H9B1 H 0.1544 0.2967 0.9771 0.033 Uiso 1 1 d R . .
H9B2 H 0.0304 0.3447 0.9133 0.033 Uiso 1 1 d R . .
C10B C -0.0281(3) 0.23258(15) 0.8105(2) 0.0285(6) Uani 1 1 d . . .
H10C H -0.0236 0.2084 0.8765 0.037 Uiso 1 1 d R . .
H10D H -0.0305 0.1965 0.7574 0.037 Uiso 1 1 d R . .
C20B C 0.2206(3) 0.38006(13) 0.9063(2) 0.0231(5) Uani 1 1 d . . .
C21B C 0.3467(3) 0.38630(16) 0.9794(2) 0.0310(6) Uani 1 1 d . . .
H21B H 0.3707 0.3538 1.0348 0.037 Uiso 1 1 d R . .
C22B C 0.4389(3) 0.43894(18) 0.9730(3) 0.0399(8) Uani 1 1 d . . .
H22B H 0.5246 0.4428 1.0240 0.048 Uiso 1 1 d R . .
C23B C 0.4046(3) 0.48630(17) 0.8916(3) 0.0423(8) Uani 1 1 d . . .
H23B H 0.4672 0.5223 0.8866 0.051 Uiso 1 1 d R . .
C24B C 0.2794(3) 0.48073(16) 0.8178(2) 0.0353(7) Uani 1 1 d . . .
H24B H 0.2561 0.5132 0.7624 0.042 Uiso 1 1 d R . .
C25B C 0.1881(3) 0.42805(14) 0.8248(2) 0.0262(6) Uani 1 1 d . . .
H25B H 0.1024 0.4245 0.7737 0.031 Uiso 1 1 d R . .
C30B C -0.1592(3) 0.27505(15) 0.7797(2) 0.0309(6) Uani 1 1 d . . .
C31B C -0.2395(3) 0.28561(16) 0.8483(3) 0.0400(7) Uani 1 1 d . . .
H31B H -0.2099 0.2672 0.9163 0.048 Uiso 1 1 d R . .
C32B C -0.3623(3) 0.32288(18) 0.8184(3) 0.0482(9) Uani 1 1 d . . .
H32B H -0.4151 0.3305 0.8663 0.058 Uiso 1 1 d R . .
C33B C -0.4073(4) 0.34872(18) 0.7191(3) 0.0521(10) Uani 1 1 d . . .
H33B H -0.4924 0.3731 0.6982 0.063 Uiso 1 1 d R . .
C34B C -0.3295(4) 0.33925(18) 0.6496(3) 0.0470(9) Uani 1 1 d . . .
H34B H -0.3603 0.3577 0.5816 0.056 Uiso 1 1 d R . .
C35B C -0.2041(3) 0.30243(16) 0.6799(3) 0.0378(7) Uani 1 1 d . . .
H35B H -0.1503 0.2963 0.6324 0.045 Uiso 1 1 d R . .
C40B C 0.5288(3) 0.12604(16) 0.5187(2) 0.0272(6) Uani 1 1 d . . .
C41B C 0.5771(3) 0.18322(16) 0.4766(2) 0.0330(6) Uani 1 1 d . . .
H41B H 0.5913 0.2260 0.5136 0.040 Uiso 1 1 d R . .
C42B C 0.6048(3) 0.17902(18) 0.3813(2) 0.0381(7) Uani 1 1 d . . .
H42B H 0.6375 0.2188 0.3529 0.046 Uiso 1 1 d R . .
C43B C 0.5850(3) 0.11668(17) 0.3279(2) 0.0367(7) Uani 1 1 d . . .
H43B H 0.6041 0.1136 0.2625 0.044 Uiso 1 1 d R . .
C44B C 0.5367(3) 0.05873(17) 0.3692(2) 0.0366(7) Uani 1 1 d . . .
H44B H 0.5235 0.0159 0.3323 0.044 Uiso 1 1 d R . .
C45B C 0.5078(3) 0.06314(16) 0.4647(2) 0.0315(6) Uani 1 1 d . . .
H45B H 0.4739 0.0236 0.4929 0.038 Uiso 1 1 d 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
O1A C5A 1.424(3) . ?
O1A C1A 1.437(3) . ?
O2A C7A 1.411(4) . ?
O2A C6A 1.438(3) . ?
O3A C7A 1.427(3) . ?
O3A C4A 1.440(3) . ?
O4A C3A 1.422(3) . ?
O5A C1A 1.399(3) . ?
O5A C8A 1.436(3) . ?
N1A C10A 1.474(3) . ?
N1A C2A 1.475(3) . ?
N1A C9A 1.486(3) . ?
C1A C2A 1.531(4) . ?
C2A C3A 1.550(3) . ?
C3A C4A 1.515(4) . ?
C4A C5A 1.525(4) . ?
C5A C6A 1.516(4) . ?
C7A C40A 1.506(4) . ?
C9A C20A 1.509(4) . ?
C10A C30A 1.508(4) . ?
C20A C25A 1.393(4) . ?
C20A C21A 1.403(4) . ?
C21A C22A 1.388(4) . ?
C22A C23A 1.386(4) . ?
C23A C24A 1.387(4) . ?
C24A C25A 1.389(4) . ?
C30A C35A 1.391(4) . ?
C30A C31A 1.391(4) . ?
C31A C32A 1.393(4) . ?
C32A C33A 1.378(5) . ?
C33A C34A 1.383(5) . ?
C34A C35A 1.398(4) . ?
C40A C45A 1.376(5) . ?
C40A C41A 1.394(5) . ?
C41A C42A 1.392(4) . ?
C42A C43A 1.375(6) . ?
C43A C44A 1.370(6) . ?
C44A C45A 1.395(5) . ?
O1B C5B 1.426(3) . ?
O1B C1B 1.431(3) . ?
O2B C7B 1.407(4) . ?
O2B C6B 1.435(3) . ?
O3B C7B 1.427(3) . ?
O3B C4B 1.439(3) . ?
O4B C3B 1.426(3) . ?
O5B C1B 1.397(3) . ?
O5B C8B 1.439(3) . ?
N1B C9B 1.478(3) . ?
N1B C10B 1.480(3) . ?
N1B C2B 1.480(3) . ?
C1B C2B 1.537(4) . ?
C2B C3B 1.542(3) . ?
C3B C4B 1.502(3) . ?
C4B C5B 1.522(4) . ?
C5B C6B 1.512(4) . ?
C7B C40B 1.518(4) . ?
C9B C20B 1.506(4) . ?
C10B C30B 1.511(4) . ?
C20B C21B 1.387(4) . ?
C20B C25B 1.400(4) . ?
C21B C22B 1.390(4) . ?
C22B C23B 1.391(5) . ?
C23B C24B 1.383(4) . ?
C24B C25B 1.386(4) . ?
C30B C31B 1.395(4) . ?
C30B C35B 1.396(4) . ?
C31B C32B 1.391(5) . ?
C32B C33B 1.381(5) . ?
C33B C34B 1.383(6) . ?
C34B C35B 1.407(4) . ?
C40B C41B 1.380(4) . ?
C40B C45B 1.393(4) . ?
C41B C42B 1.384(4) . ?
C42B C43B 1.381(5) . ?
C43B C44B 1.387(5) . ?
C44B C45B 1.393(4) . ?

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
C5A O1A C1A 110.6(2) . . ?
C7A O2A C6A 111.0(2) . . ?
C7A O3A C4A 108.76(19) . . ?
C1A O5A C8A 112.1(2) . . ?
C10A N1A C2A 114.5(2) . . ?
C10A N1A C9A 110.0(2) . . ?
C2A N1A C9A 112.9(2) . . ?
O5A C1A O1A 107.3(2) . . ?
O5A C1A C2A 110.4(2) . . ?
O1A C1A C2A 109.7(2) . . ?
N1A C2A C1A 117.2(2) . . ?
N1A C2A C3A 107.9(2) . . ?
C1A C2A C3A 109.7(2) . . ?
O4A C3A C4A 110.6(2) . . ?
O4A C3A C2A 110.1(2) . . ?
C4A C3A C2A 108.5(2) . . ?
O3A C4A C3A 111.7(2) . . ?
O3A C4A C5A 108.1(2) . . ?
C3A C4A C5A 109.1(2) . . ?
O1A C5A C6A 108.7(2) . . ?
O1A C5A C4A 109.9(2) . . ?
C6A C5A C4A 110.2(2) . . ?
O2A C6A C5A 107.9(2) . . ?
O2A C7A O3A 111.6(2) . . ?
O2A C7A C40A 109.2(3) . . ?
O3A C7A C40A 109.9(2) . . ?
N1A C9A C20A 112.1(2) . . ?
N1A C10A C30A 114.2(2) . . ?
C25A C20A C21A 119.2(2) . . ?
C25A C20A C9A 119.6(2) . . ?
C21A C20A C9A 121.2(2) . . ?
C22A C21A C20A 120.1(3) . . ?
C23A C22A C21A 120.5(3) . . ?
C22A C23A C24A 119.5(3) . . ?
C23A C24A C25A 120.7(3) . . ?
C24A C25A C20A 120.0(2) . . ?
C35A C30A C31A 118.9(3) . . ?
C35A C30A C10A 120.7(3) . . ?
C31A C30A C10A 120.3(3) . . ?
C30A C31A C32A 120.9(3) . . ?
C33A C32A C31A 119.8(3) . . ?
C32A C33A C34A 119.9(3) . . ?
C33A C34A C35A 120.5(3) . . ?
C30A C35A C34A 119.9(3) . . ?
C45A C40A C41A 119.2(3) . . ?
C45A C40A C7A 122.0(3) . . ?
C41A C40A C7A 118.7(3) . . ?
C42A C41A C40A 120.4(3) . . ?
C43A C42A C41A 119.5(4) . . ?
C44A C43A C42A 120.4(3) . . ?
C43A C44A C45A 120.4(4) . . ?
C40A C45A C44A 120.0(4) . . ?
C5B O1B C1B 111.31(19) . . ?
C7B O2B C6B 111.5(2) . . ?
C7B O3B C4B 108.70(18) . . ?
C1B O5B C8B 112.3(2) . . ?
C9B N1B C10B 111.9(2) . . ?
C9B N1B C2B 113.2(2) . . ?
C10B N1B C2B 112.9(2) . . ?
O5B C1B O1B 107.3(2) . . ?
O5B C1B C2B 107.8(2) . . ?
O1B C1B C2B 110.4(2) . . ?
N1B C2B C1B 116.2(2) . . ?
N1B C2B C3B 109.1(2) . . ?
C1B C2B C3B 111.4(2) . . ?
O4B C3B C4B 110.4(2) . . ?
O4B C3B C2B 109.0(2) . . ?
C4B C3B C2B 107.8(2) . . ?
O3B C4B C3B 112.5(2) . . ?
O3B C4B C5B 109.2(2) . . ?
C3B C4B C5B 109.1(2) . . ?
O1B C5B C6B 107.5(2) . . ?
O1B C5B C4B 109.2(2) . . ?
C6B C5B C4B 110.0(2) . . ?
O2B C6B C5B 109.0(2) . . ?
O2B C7B O3B 110.5(2) . . ?
O2B C7B C40B 109.4(2) . . ?
O3B C7B C40B 109.6(2) . . ?
N1B C9B C20B 111.2(2) . . ?
N1B C10B C30B 112.9(2) . . ?
C21B C20B C25B 118.3(3) . . ?
C21B C20B C9B 121.9(2) . . ?
C25B C20B C9B 119.8(2) . . ?
C20B C21B C22B 121.2(3) . . ?
C21B C22B C23B 119.6(3) . . ?
C24B C23B C22B 119.9(3) . . ?
C23B C24B C25B 120.1(3) . . ?
C24B C25B C20B 120.8(3) . . ?
C31B C30B C35B 118.9(3) . . ?
C31B C30B C10B 121.1(3) . . ?
C35B C30B C10B 120.0(3) . . ?
C32B C31B C30B 120.8(3) . . ?
C33B C32B C31B 119.9(3) . . ?
C32B C33B C34B 120.4(3) . . ?
C33B C34B C35B 119.8(3) . . ?
C30B C35B C34B 120.1(3) . . ?
C41B C40B C45B 119.7(3) . . ?
C41B C40B C7B 118.2(3) . . ?
C45B C40B C7B 122.0(3) . . ?
C40B C41B C42B 120.9(3) . . ?
C43B C42B C41B 119.6(3) . . ?
C42B C43B C44B 120.2(3) . . ?
C43B C44B C45B 120.2(3) . . ?
C44B C45B C40B 119.4(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4A H0A N1A 0.89(4) 2.26(4) 2.802(3) 118(3) .
O4B H0B N1B 0.75(3) 2.35(3) 2.820(3) 122(3) .

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.041

#================================================END



