  
data_03005x 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          '2(C30 H22 N6 S3), C3 H6 O' 
_chemical_formula_sum 
 'C63 H50 N12 O S6' 
_chemical_formula_weight          1183.57 
  
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' 
 'S'  'S'   0.1246   0.1234 
 '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    'P 21/n' 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    7.7157(9) 
_cell_length_b                    19.226(2) 
_cell_length_c                    43.385(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.028(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      6436.0(13) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     3146 
_cell_measurement_theta_min       1.16 
_cell_measurement_theta_max       25.06 
  
_exptl_crystal_description        'plate' 
_exptl_crystal_colour             'metallic green' 
_exptl_crystal_size_max           0.4 
_exptl_crystal_size_mid           0.15 
_exptl_crystal_size_min           0.1 
_exptl_crystal_density_meas       0 
_exptl_crystal_density_diffrn     1.221 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2464 
_exptl_absorpt_coefficient_mu     0.262 
_exptl_absorpt_correction_type    'multi-scans' 
_exptl_absorpt_correction_T_min   0.7720 
_exptl_absorpt_correction_T_max   1.0000 
_exptl_absorpt_process_details    'SADABS, R. Blessing, 1995' 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       173(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'normal-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Siemens SMART Platform CCD' 
_diffrn_measurement_method        'area detector, omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             42659 
_diffrn_reflns_av_R_equivalents   0.0606 
_diffrn_reflns_av_sigmaI/netI     0.0608 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -22 
_diffrn_reflns_limit_k_max        22 
_diffrn_reflns_limit_l_min        -51 
_diffrn_reflns_limit_l_max        50 
_diffrn_reflns_theta_min          1.16 
_diffrn_reflns_theta_max          25.06 
_reflns_number_total              11393 
_reflns_number_gt                 8924 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'SMART, Bruker' 
_computing_cell_refinement        'SAINT, Bruker' 
_computing_data_reduction         'SAINT, Bruker' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXTL, Bruker' 
_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.  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)+(0.0559P)²+51.5091P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     riding 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          11393 
_refine_ls_number_parameters      739 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1638 
_refine_ls_R_factor_gt            0.1419 
_refine_ls_wR_factor_ref          0.3151 
_refine_ls_wR_factor_gt           0.3062 
_refine_ls_goodness_of_fit_ref    1.203 
_refine_ls_restrained_S_all       1.203 
_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 
S5 S -0.2519(3) 0.26558(10) 0.33575(5) 0.0392(5) Uani 1 1 d . . . 
S4 S 0.2059(3) 0.13589(11) 0.34798(5) 0.0424(5) Uani 1 1 d . . . 
S2 S -0.7299(3) -0.28764(10) 0.32885(5) 0.0416(5) Uani 1 1 d . . . 
S6 S -0.7049(3) 0.30634(11) 0.39279(5) 0.0445(5) Uani 1 1 d . . . 
S1 S -0.2731(3) -0.16262(11) 0.34532(5) 0.0442(5) Uani 1 1 d . . . 
S3 S -1.1794(3) -0.34247(12) 0.38333(5) 0.0501(6) Uani 1 1 d . . . 
C20 C -0.8271(10) -0.2383(4) 0.38130(19) 0.0392(18) Uani 1 1 d . . . 
C11 C -0.6656(10) -0.2044(4) 0.37403(18) 0.0378(18) Uani 1 1 d . . . 
C22 C -1.0367(10) -0.3237(4) 0.35387(19) 0.0394(19) Uani 1 1 d . . . 
C21 C -0.8795(10) -0.2842(4) 0.35839(18) 0.0374(18) Uani 1 1 d . . . 
C36 C 0.3285(11) 0.1493(4) 0.3148(2) 0.048(2) Uani 1 1 d . . . 
C10 C -0.5956(11) -0.2270(4) 0.34702(19) 0.0412(19) Uani 1 1 d . . . 
C6 C -0.1556(10) -0.1677(4) 0.3118(2) 0.043(2) Uani 1 1 d . . . 
C56 C -1.0051(10) 0.3858(4) 0.3804(2) 0.044(2) Uani 1 1 d . . . 
C50 C -0.3482(10) 0.2070(4) 0.38674(18) 0.0396(18) Uani 1 1 d . . . 
C51 C -0.3989(10) 0.2554(4) 0.36575(18) 0.0391(18) Uani 1 1 d . . . 
C2 C 0.0498(10) -0.0770(4) 0.3536(2) 0.0392(18) Uani 1 1 d . . . 
C52 C -0.5572(11) 0.2980(4) 0.36287(19) 0.0429(19) Uani 1 1 d . . . 
C32 C 0.5332(10) 0.0533(4) 0.35537(18) 0.0384(18) Uani 1 1 d . . . 
C12 C -0.5869(11) -0.1481(5) 0.3939(2) 0.050(2) Uani 1 1 d . . . 
H12A H -0.6819 -0.1213 0.4036 0.060 Uiso 1 1 calc R . . 
H12B H -0.5215 -0.1158 0.3804 0.060 Uiso 1 1 calc R . . 
C19 C -0.9268(11) -0.2226(5) 0.41035(19) 0.048(2) Uani 1 1 d . . . 
H19A H -1.0522 -0.2223 0.4055 0.057 Uiso 1 1 calc R . . 
H19B H -0.8948 -0.1756 0.4177 0.057 Uiso 1 1 calc R . . 
C4 C 0.1066(12) -0.1004(5) 0.3248(2) 0.051(2) Uani 1 1 d . . . 
C40 C -0.1164(9) 0.2029(4) 0.35159(18) 0.0360(17) Uani 1 1 d . . . 
C54 C -0.7734(12) 0.3655(4) 0.3416(2) 0.056(2) Uani 1 1 d . . . 
H54A H -0.8300 0.3920 0.3261 0.067 Uiso 1 1 calc R . . 
C35 C 0.4968(11) 0.1203(4) 0.3089(2) 0.044(2) Uani 1 1 d . . . 
C9 C -0.4429(10) -0.2091(4) 0.32905(19) 0.0416(19) Uani 1 1 d . . . 
C38 C 0.0796(11) 0.2116(4) 0.3055(2) 0.051(2) Uani 1 1 d . . . 
H38A H 0.0021 0.2395 0.2938 0.061 Uiso 1 1 calc R . . 
C55 C -0.8388(11) 0.3568(4) 0.3699(2) 0.043(2) Uani 1 1 d . . . 
C42 C -0.1021(10) 0.1166(4) 0.39626(18) 0.0404(18) Uani 1 1 d . . . 
H42A H -0.0360 0.0872 0.3817 0.049 Uiso 1 1 calc R . . 
H42B H -0.1954 0.0875 0.4052 0.049 Uiso 1 1 calc R . . 
C39 C 0.0417(10) 0.1876(4) 0.33444(19) 0.0390(18) Uani 1 1 d . . . 
C3 C 0.0966(11) -0.1590(5) 0.2758(2) 0.051(2) Uani 1 1 d . . . 
C25 C -1.3187(11) -0.3842(4) 0.3578(2) 0.049(2) Uani 1 1 d . . . 
C41 C -0.1837(10) 0.1755(4) 0.37858(18) 0.0387(18) Uani 1 1 d . . . 
C5 C 0.0154(12) -0.1393(5) 0.3062(2) 0.054(2) Uani 1 1 d . . . 
C53 C -0.6145(11) 0.3323(4) 0.3368(2) 0.052(2) Uani 1 1 d . . . 
H53A H -0.5532 0.3331 0.3178 0.062 Uiso 1 1 calc R . . 
C57 C -1.0820(11) 0.3796(5) 0.4078(2) 0.051(2) Uani 1 1 d . . . 
C34 C 0.5890(12) 0.0780(4) 0.3267(2) 0.050(2) Uani 1 1 d . . . 
C49 C -0.4465(11) 0.1874(4) 0.41521(19) 0.044(2) Uani 1 1 d . . . 
H49A H -0.4113 0.1400 0.4216 0.053 Uiso 1 1 calc R . . 
H49B H -0.5717 0.1861 0.4103 0.053 Uiso 1 1 calc R . . 
C48 C -0.4177(11) 0.2373(5) 0.4422(2) 0.054(2) Uani 1 1 d . . . 
H48A H -0.4424 0.2854 0.4353 0.064 Uiso 1 1 calc R . . 
H48B H -0.2945 0.2352 0.4486 0.064 Uiso 1 1 calc R . . 
C26 C -1.4786(12) -0.4180(4) 0.3664(2) 0.053(2) Uani 1 1 d . . . 
C33 C 0.5793(12) 0.1397(4) 0.2790(2) 0.050(2) Uani 1 1 d . . . 
C31 C 0.7641(12) 0.0544(4) 0.3161(2) 0.046(2) Uani 1 1 d . . . 
C43 C 0.0193(11) 0.1397(4) 0.4222(2) 0.047(2) Uani 1 1 d . . . 
H43A H 0.1066 0.1722 0.4137 0.057 Uiso 1 1 calc R . . 
H43B H -0.0488 0.1652 0.4379 0.057 Uiso 1 1 calc R . . 
C58 C -1.0942(12) 0.4253(4) 0.3574(2) 0.051(2) Uani 1 1 d . . . 
C23 C -1.0961(11) -0.3499(4) 0.3269(2) 0.053(2) Uani 1 1 d . . . 
H23A H -1.0352 -0.3450 0.3080 0.063 Uiso 1 1 calc R . . 
C37 C 0.2424(12) 0.1914(4) 0.2947(2) 0.054(2) Uani 1 1 d . . . 
H37A H 0.2883 0.2055 0.2754 0.065 Uiso 1 1 calc R . . 
C8 C -0.4053(11) -0.2257(5) 0.2992(2) 0.053(2) Uani 1 1 d . . . 
H8A H -0.4835 -0.2505 0.2863 0.064 Uiso 1 1 calc R . . 
C7 C -0.2462(12) -0.2038(4) 0.2892(2) 0.052(2) Uani 1 1 d . . . 
H7A H -0.2026 -0.2123 0.2691 0.062 Uiso 1 1 calc R . . 
C60 C -1.2515(13) 0.4122(5) 0.4126(2) 0.060(3) Uani 1 1 d . . . 
C44 C 0.1122(13) 0.0794(5) 0.4377(3) 0.065(3) Uani 1 1 d . . . 
H44A H 0.1779 0.0532 0.4220 0.078 Uiso 1 1 calc R . . 
H44B H 0.1966 0.0982 0.4528 0.078 Uiso 1 1 calc R . . 
C18 C -0.8935(12) -0.2753(5) 0.4364(2) 0.056(2) Uani 1 1 d . . . 
H18A H -0.9159 -0.3228 0.4285 0.067 Uiso 1 1 calc R . . 
H18B H -0.7699 -0.2728 0.4425 0.067 Uiso 1 1 calc R . . 
C1 C 0.2780(13) -0.0747(4) 0.3145(2) 0.055(2) Uani 1 1 d . . . 
C24 C -1.2527(13) -0.3843(5) 0.3292(2) 0.059(3) Uani 1 1 d . . . 
H24A H -1.3084 -0.4059 0.3122 0.071 Uiso 1 1 calc R . . 
C13 C -0.4670(12) -0.1741(5) 0.4190(2) 0.055(2) Uani 1 1 d . . . 
H13A H -0.3784 -0.2049 0.4097 0.066 Uiso 1 1 calc R . . 
H13B H -0.5346 -0.2019 0.4339 0.066 Uiso 1 1 calc R . . 
C17 C -1.0039(13) -0.2633(6) 0.4646(2) 0.066(3) Uani 1 1 d . . . 
H17A H -0.9863 -0.3024 0.4791 0.079 Uiso 1 1 calc R . . 
H17B H -1.1272 -0.2635 0.4583 0.079 Uiso 1 1 calc R . . 
C14 C -0.3758(14) -0.1145(6) 0.4361(2) 0.074(3) Uani 1 1 d . . . 
H14A H -0.2912 -0.1347 0.4507 0.089 Uiso 1 1 calc R . . 
H14B H -0.3101 -0.0865 0.4209 0.089 Uiso 1 1 calc R . . 
C28 C -1.5737(14) -0.4537(5) 0.3417(3) 0.068(3) Uani 1 1 d . . . 
C30 C -1.7233(13) -0.4515(5) 0.3983(3) 0.076(3) Uani 1 1 d . . . 
C27 C -1.5559(13) -0.4177(5) 0.3935(3) 0.062(3) Uani 1 1 d . . . 
C47 C -0.5328(13) 0.2200(6) 0.4700(2) 0.066(3) Uani 1 1 d . . . 
H47A H -0.6551 0.2174 0.4632 0.080 Uiso 1 1 calc R . . 
H47B H -0.5000 0.1737 0.4781 0.080 Uiso 1 1 calc R . . 
C29 C -1.4852(14) -0.3869(6) 0.4205(3) 0.071(3) Uani 1 1 d . . . 
C59 C -1.0111(12) 0.3435(5) 0.4331(2) 0.053(2) Uani 1 1 d . . . 
C45 C -0.0088(18) 0.0305(7) 0.4541(3) 0.094(4) Uani 1 1 d . . . 
H45A H 0.0580 -0.0076 0.4633 0.141 Uiso 1 1 calc R . . 
H45B H -0.0924 0.0115 0.4393 0.141 Uiso 1 1 calc R . . 
H45C H -0.0708 0.0557 0.4703 0.141 Uiso 1 1 calc R . . 
C16 C -0.9666(17) -0.1959(7) 0.4814(3) 0.089(4) Uani 1 1 d . . . 
H16A H -1.0449 -0.1916 0.4991 0.134 Uiso 1 1 calc R . . 
H16B H -0.9844 -0.1567 0.4674 0.134 Uiso 1 1 calc R . . 
H16C H -0.8463 -0.1960 0.4886 0.134 Uiso 1 1 calc R . . 
C46 C -0.5184(18) 0.2708(8) 0.4945(3) 0.106(5) Uani 1 1 d . . . 
H46A H -0.5944 0.2575 0.5116 0.159 Uiso 1 1 calc R . . 
H46B H -0.5529 0.3166 0.4868 0.159 Uiso 1 1 calc R . . 
H46C H -0.3982 0.2727 0.5018 0.159 Uiso 1 1 calc R . . 
C15 C -0.4944(16) -0.0672(7) 0.4535(3) 0.089(4) Uani 1 1 d . . . 
H15A H -0.4264 -0.0305 0.4635 0.134 Uiso 1 1 calc R . . 
H15B H -0.5569 -0.0939 0.4692 0.134 Uiso 1 1 calc R . . 
H15C H -0.5777 -0.0461 0.4393 0.134 Uiso 1 1 calc R . . 
N1 N 0.4124(11) -0.0551(4) 0.30791(17) 0.056(2) Uani 1 1 d . . . 
N7 N 0.8935(10) 0.0322(4) 0.30915(18) 0.0550(19) Uani 1 1 d . . . 
N2 N 0.0096(12) -0.0588(4) 0.37777(19) 0.066(2) Uani 1 1 d . . . 
N8 N 0.4947(11) 0.0306(4) 0.37885(18) 0.060(2) Uani 1 1 d . . . 
N10 N -1.1690(11) 0.4567(4) 0.3387(2) 0.063(2) Uani 1 1 d . . . 
N9 N 0.6313(12) 0.1556(5) 0.2557(2) 0.074(3) Uani 1 1 d . . . 
N11 N -0.9563(13) 0.3137(5) 0.4539(2) 0.081(3) Uani 1 1 d . . . 
N3 N 0.1505(11) -0.1759(5) 0.2530(2) 0.073(3) Uani 1 1 d . . . 
N4 N -1.6389(13) -0.4793(5) 0.3215(3) 0.098(4) Uani 1 1 d . . . 
N12 N -1.3823(12) 0.4392(5) 0.4157(3) 0.090(3) Uani 1 1 d . . . 
N5 N -1.4294(14) -0.3589(6) 0.4416(2) 0.095(3) Uani 1 1 d . . . 
N6 N -1.8576(13) -0.4756(5) 0.4024(3) 0.099(4) Uani 1 1 d . . . 
O1 O -0.400(2) -0.1418(5) 0.2251(3) 0.157(5) Uani 1 1 d . . . 
C61 C -0.381(2) -0.0787(7) 0.2299(3) 0.093(4) Uani 1 1 d . . . 
C62 C -0.204(2) -0.0478(8) 0.2354(3) 0.117(5) Uani 1 1 d . . . 
H62C H -0.1174 -0.0850 0.2355 0.176 Uiso 1 1 calc R . . 
H62D H -0.2033 -0.0239 0.2554 0.176 Uiso 1 1 calc R . . 
H62E H -0.1776 -0.0145 0.2190 0.176 Uiso 1 1 calc R . . 
C63 C -0.541(2) -0.0293(9) 0.2300(3) 0.126(6) Uani 1 1 d . . . 
H63F H -0.6464 -0.0564 0.2263 0.189 Uiso 1 1 calc R . . 
H63G H -0.5277 0.0055 0.2136 0.189 Uiso 1 1 calc R . . 
H63H H -0.5490 -0.0059 0.2500 0.189 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 
S5 C40 1.737(7) . ? 
S5 C51 1.738(8) . ? 
S4 C39 1.714(8) . ? 
S4 C36 1.742(9) . ? 
S2 C21 1.727(8) . ? 
S2 C10 1.747(9) . ? 
S6 C55 1.730(9) . ? 
S6 C52 1.735(9) . ? 
S1 C6 1.719(8) . ? 
S1 C9 1.736(9) . ? 
S3 C22 1.726(8) . ? 
S3 C25 1.738(9) . ? 
C20 C21 1.389(11) . ? 
C20 C11 1.441(10) . ? 
C20 C19 1.507(11) . ? 
C11 C10 1.362(11) . ? 
C11 C12 1.510(12) . ? 
C22 C23 1.353(12) . ? 
C22 C21 1.445(10) . ? 
C36 C37 1.363(13) . ? 
C36 C35 1.436(11) . ? 
C10 C9 1.454(11) . ? 
C6 C7 1.388(13) . ? 
C6 C5 1.447(12) . ? 
C56 C57 1.334(12) . ? 
C56 C58 1.428(12) . ? 
C56 C55 1.471(11) . ? 
C50 C51 1.359(11) . ? 
C50 C41 1.450(10) . ? 
C50 C49 1.498(11) . ? 
C51 C52 1.476(11) . ? 
C2 N2 1.149(11) . ? 
C2 C4 1.397(12) . ? 
C52 C53 1.382(12) . ? 
C32 N8 1.148(10) . ? 
C32 C34 1.398(12) . ? 
C12 C13 1.513(12) . ? 
C12 H12A 0.9900 . ? 
C12 H12B 0.9900 . ? 
C19 C18 1.540(12) . ? 
C19 H19A 0.9900 . ? 
C19 H19B 0.9900 . ? 
C4 C5 1.306(13) . ? 
C4 C1 1.481(13) . ? 
C40 C41 1.386(11) . ? 
C40 C39 1.459(10) . ? 
C54 C55 1.341(12) . ? 
C54 C53 1.398(12) . ? 
C54 H54A 0.9500 . ? 
C35 C34 1.329(12) . ? 
C35 C33 1.492(12) . ? 
C9 C8 1.365(12) . ? 
C38 C39 1.370(12) . ? 
C38 C37 1.395(12) . ? 
C38 H38A 0.9500 . ? 
C42 C41 1.506(11) . ? 
C42 C43 1.531(11) . ? 
C42 H42A 0.9900 . ? 
C42 H42B 0.9900 . ? 
C3 N3 1.122(11) . ? 
C3 C5 1.509(13) . ? 
C25 C24 1.342(13) . ? 
C25 C26 1.444(12) . ? 
C53 H53A 0.9500 . ? 
C57 C59 1.409(13) . ? 
C57 C60 1.465(12) . ? 
C34 C31 1.499(13) . ? 
C49 C48 1.530(12) . ? 
C49 H49A 0.9900 . ? 
C49 H49B 0.9900 . ? 
C48 C47 1.536(12) . ? 
C48 H48A 0.9900 . ? 
C48 H48B 0.9900 . ? 
C26 C27 1.319(14) . ? 
C26 C28 1.470(14) . ? 
C33 N9 1.127(11) . ? 
C31 N7 1.127(11) . ? 
C43 C44 1.519(12) . ? 
C43 H43A 0.9900 . ? 
C43 H43B 0.9900 . ? 
C58 N10 1.165(11) . ? 
C23 C24 1.381(13) . ? 
C23 H23A 0.9500 . ? 
C37 H37A 0.9500 . ? 
C8 C7 1.369(12) . ? 
C8 H8A 0.9500 . ? 
C7 H7A 0.9500 . ? 
C60 N12 1.143(12) . ? 
C44 C45 1.503(15) . ? 
C44 H44A 0.9900 . ? 
C44 H44B 0.9900 . ? 
C18 C17 1.508(12) . ? 
C18 H18A 0.9900 . ? 
C18 H18B 0.9900 . ? 
C1 N1 1.140(11) . ? 
C24 H24A 0.9500 . ? 
C13 C14 1.535(14) . ? 
C13 H13A 0.9900 . ? 
C13 H13B 0.9900 . ? 
C17 C16 1.513(16) . ? 
C17 H17A 0.9900 . ? 
C17 H17B 0.9900 . ? 
C14 C15 1.496(15) . ? 
C14 H14A 0.9900 . ? 
C14 H14B 0.9900 . ? 
C28 N4 1.123(14) . ? 
C30 N6 1.149(12) . ? 
C30 C27 1.460(13) . ? 
C27 C29 1.421(16) . ? 
C47 C46 1.449(15) . ? 
C47 H47A 0.9900 . ? 
C47 H47B 0.9900 . ? 
C29 N5 1.146(14) . ? 
C59 N11 1.151(12) . ? 
C45 H45A 0.9800 . ? 
C45 H45B 0.9800 . ? 
C45 H45C 0.9800 . ? 
C16 H16A 0.9800 . ? 
C16 H16B 0.9800 . ? 
C16 H16C 0.9800 . ? 
C46 H46A 0.9800 . ? 
C46 H46B 0.9800 . ? 
C46 H46C 0.9800 . ? 
C15 H15A 0.9800 . ? 
C15 H15B 0.9800 . ? 
C15 H15C 0.9800 . ? 
O1 C61 1.240(15) . ? 
C61 C62 1.505(19) . ? 
C61 C63 1.56(2) . ? 
C62 H62C 0.9800 . ? 
C62 H62D 0.9800 . ? 
C62 H62E 0.9800 . ? 
C63 H63F 0.9800 . ? 
C63 H63G 0.9800 . ? 
C63 H63H 0.9800 . ? 
  
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 
C40 S5 C51 91.1(4) . . ? 
C39 S4 C36 91.9(4) . . ? 
C21 S2 C10 92.1(4) . . ? 
C55 S6 C52 90.9(4) . . ? 
C6 S1 C9 91.4(4) . . ? 
C22 S3 C25 91.1(4) . . ? 
C21 C20 C11 112.5(7) . . ? 
C21 C20 C19 125.2(7) . . ? 
C11 C20 C19 122.3(7) . . ? 
C10 C11 C20 112.7(7) . . ? 
C10 C11 C12 124.1(7) . . ? 
C20 C11 C12 123.1(7) . . ? 
C23 C22 C21 126.6(8) . . ? 
C23 C22 S3 110.3(6) . . ? 
C21 C22 S3 123.0(6) . . ? 
C20 C21 C22 132.5(8) . . ? 
C20 C21 S2 111.2(6) . . ? 
C22 C21 S2 116.1(6) . . ? 
C37 C36 C35 123.8(8) . . ? 
C37 C36 S4 110.6(6) . . ? 
C35 C36 S4 125.6(7) . . ? 
C11 C10 C9 135.0(8) . . ? 
C11 C10 S2 111.5(6) . . ? 
C9 C10 S2 113.4(6) . . ? 
C7 C6 C5 122.0(8) . . ? 
C7 C6 S1 111.1(6) . . ? 
C5 C6 S1 126.9(7) . . ? 
C57 C56 C58 117.0(8) . . ? 
C57 C56 C55 129.0(8) . . ? 
C58 C56 C55 114.0(8) . . ? 
C51 C50 C41 112.0(7) . . ? 
C51 C50 C49 125.3(7) . . ? 
C41 C50 C49 122.7(7) . . ? 
C50 C51 C52 132.4(7) . . ? 
C50 C51 S5 113.0(6) . . ? 
C52 C51 S5 114.5(6) . . ? 
N2 C2 C4 177.1(9) . . ? 
C53 C52 C51 126.7(8) . . ? 
C53 C52 S6 111.0(6) . . ? 
C51 C52 S6 122.1(6) . . ? 
N8 C32 C34 176.3(9) . . ? 
C11 C12 C13 114.8(8) . . ? 
C11 C12 H12A 108.6 . . ? 
C13 C12 H12A 108.6 . . ? 
C11 C12 H12B 108.6 . . ? 
C13 C12 H12B 108.6 . . ? 
H12A C12 H12B 107.6 . . ? 
C20 C19 C18 113.5(7) . . ? 
C20 C19 H19A 108.9 . . ? 
C18 C19 H19A 108.9 . . ? 
C20 C19 H19B 108.9 . . ? 
C18 C19 H19B 108.9 . . ? 
H19A C19 H19B 107.7 . . ? 
C5 C4 C2 124.5(9) . . ? 
C5 C4 C1 119.0(9) . . ? 
C2 C4 C1 116.3(8) . . ? 
C41 C40 C39 131.9(7) . . ? 
C41 C40 S5 111.9(5) . . ? 
C39 C40 S5 116.2(6) . . ? 
C55 C54 C53 114.2(8) . . ? 
C55 C54 H54A 122.9 . . ? 
C53 C54 H54A 122.9 . . ? 
C34 C35 C36 128.0(9) . . ? 
C34 C35 C33 115.6(8) . . ? 
C36 C35 C33 116.4(8) . . ? 
C8 C9 C10 128.8(8) . . ? 
C8 C9 S1 110.2(6) . . ? 
C10 C9 S1 121.0(6) . . ? 
C39 C38 C37 114.0(8) . . ? 
C39 C38 H38A 123.0 . . ? 
C37 C38 H38A 123.0 . . ? 
C54 C55 C56 124.3(8) . . ? 
C54 C55 S6 111.8(6) . . ? 
C56 C55 S6 123.9(7) . . ? 
C41 C42 C43 114.3(7) . . ? 
C41 C42 H42A 108.7 . . ? 
C43 C42 H42A 108.7 . . ? 
C41 C42 H42B 108.7 . . ? 
C43 C42 H42B 108.7 . . ? 
H42A C42 H42B 107.6 . . ? 
C38 C39 C40 125.3(8) . . ? 
C38 C39 S4 110.6(6) . . ? 
C40 C39 S4 124.1(6) . . ? 
N3 C3 C5 176.5(10) . . ? 
C24 C25 C26 124.3(9) . . ? 
C24 C25 S3 110.8(7) . . ? 
C26 C25 S3 124.8(8) . . ? 
C40 C41 C50 112.1(7) . . ? 
C40 C41 C42 124.0(7) . . ? 
C50 C41 C42 123.7(7) . . ? 
C4 C5 C6 127.2(9) . . ? 
C4 C5 C3 117.4(8) . . ? 
C6 C5 C3 115.4(8) . . ? 
C52 C53 C54 112.1(9) . . ? 
C52 C53 H53A 123.9 . . ? 
C54 C53 H53A 123.9 . . ? 
C56 C57 C59 124.4(8) . . ? 
C56 C57 C60 119.1(9) . . ? 
C59 C57 C60 116.4(8) . . ? 
C35 C34 C32 124.1(9) . . ? 
C35 C34 C31 119.2(8) . . ? 
C32 C34 C31 116.7(8) . . ? 
C50 C49 C48 113.6(7) . . ? 
C50 C49 H49A 108.8 . . ? 
C48 C49 H49A 108.8 . . ? 
C50 C49 H49B 108.8 . . ? 
C48 C49 H49B 108.8 . . ? 
H49A C49 H49B 107.7 . . ? 
C49 C48 C47 112.5(8) . . ? 
C49 C48 H48A 109.1 . . ? 
C47 C48 H48A 109.1 . . ? 
C49 C48 H48B 109.1 . . ? 
C47 C48 H48B 109.1 . . ? 
H48A C48 H48B 107.8 . . ? 
C27 C26 C25 128.0(9) . . ? 
C27 C26 C28 115.3(9) . . ? 
C25 C26 C28 116.6(9) . . ? 
N9 C33 C35 175.5(11) . . ? 
N7 C31 C34 175.0(10) . . ? 
C44 C43 C42 113.1(7) . . ? 
C44 C43 H43A 109.0 . . ? 
C42 C43 H43A 109.0 . . ? 
C44 C43 H43B 109.0 . . ? 
C42 C43 H43B 109.0 . . ? 
H43A C43 H43B 107.8 . . ? 
N10 C58 C56 178.9(10) . . ? 
C22 C23 C24 114.3(9) . . ? 
C22 C23 H23A 122.9 . . ? 
C24 C23 H23A 122.9 . . ? 
C36 C37 C38 112.9(8) . . ? 
C36 C37 H37A 123.5 . . ? 
C38 C37 H37A 123.5 . . ? 
C9 C8 C7 114.8(9) . . ? 
C9 C8 H8A 122.6 . . ? 
C7 C8 H8A 122.6 . . ? 
C8 C7 C6 112.5(8) . . ? 
C8 C7 H7A 123.7 . . ? 
C6 C7 H7A 123.7 . . ? 
N12 C60 C57 177.7(12) . . ? 
C45 C44 C43 113.1(9) . . ? 
C45 C44 H44A 109.0 . . ? 
C43 C44 H44A 109.0 . . ? 
C45 C44 H44B 109.0 . . ? 
C43 C44 H44B 109.0 . . ? 
H44A C44 H44B 107.8 . . ? 
C17 C18 C19 113.6(8) . . ? 
C17 C18 H18A 108.8 . . ? 
C19 C18 H18A 108.8 . . ? 
C17 C18 H18B 108.8 . . ? 
C19 C18 H18B 108.8 . . ? 
H18A C18 H18B 107.7 . . ? 
N1 C1 C4 176.9(11) . . ? 
C25 C24 C23 113.5(9) . . ? 
C25 C24 H24A 123.3 . . ? 
C23 C24 H24A 123.3 . . ? 
C12 C13 C14 112.4(8) . . ? 
C12 C13 H13A 109.1 . . ? 
C14 C13 H13A 109.1 . . ? 
C12 C13 H13B 109.1 . . ? 
C14 C13 H13B 109.1 . . ? 
H13A C13 H13B 107.9 . . ? 
C18 C17 C16 114.5(9) . . ? 
C18 C17 H17A 108.6 . . ? 
C16 C17 H17A 108.6 . . ? 
C18 C17 H17B 108.6 . . ? 
C16 C17 H17B 108.6 . . ? 
H17A C17 H17B 107.6 . . ? 
C15 C14 C13 114.7(9) . . ? 
C15 C14 H14A 108.6 . . ? 
C13 C14 H14A 108.6 . . ? 
C15 C14 H14B 108.6 . . ? 
C13 C14 H14B 108.6 . . ? 
H14A C14 H14B 107.6 . . ? 
N4 C28 C26 175.6(13) . . ? 
N6 C30 C27 177.3(12) . . ? 
C26 C27 C29 124.2(9) . . ? 
C26 C27 C30 121.7(10) . . ? 
C29 C27 C30 114.1(10) . . ? 
C46 C47 C48 112.7(10) . . ? 
C46 C47 H47A 109.0 . . ? 
C48 C47 H47A 109.0 . . ? 
C46 C47 H47B 109.0 . . ? 
C48 C47 H47B 109.0 . . ? 
H47A C47 H47B 107.8 . . ? 
N5 C29 C27 176.6(13) . . ? 
N11 C59 C57 178.7(11) . . ? 
C44 C45 H45A 109.5 . . ? 
C44 C45 H45B 109.5 . . ? 
H45A C45 H45B 109.5 . . ? 
C44 C45 H45C 109.5 . . ? 
H45A C45 H45C 109.5 . . ? 
H45B C45 H45C 109.5 . . ? 
C17 C16 H16A 109.5 . . ? 
C17 C16 H16B 109.5 . . ? 
H16A C16 H16B 109.5 . . ? 
C17 C16 H16C 109.5 . . ? 
H16A C16 H16C 109.5 . . ? 
H16B C16 H16C 109.5 . . ? 
C47 C46 H46A 109.5 . . ? 
C47 C46 H46B 109.5 . . ? 
H46A C46 H46B 109.5 . . ? 
C47 C46 H46C 109.5 . . ? 
H46A C46 H46C 109.5 . . ? 
H46B C46 H46C 109.5 . . ? 
C14 C15 H15A 109.5 . . ? 
C14 C15 H15B 109.5 . . ? 
H15A C15 H15B 109.5 . . ? 
C14 C15 H15C 109.5 . . ? 
H15A C15 H15C 109.5 . . ? 
H15B C15 H15C 109.5 . . ? 
O1 C61 C62 121.2(17) . . ? 
O1 C61 C63 120.3(15) . . ? 
C62 C61 C63 118.4(12) . . ? 
C61 C62 H62C 109.5 . . ? 
C61 C62 H62D 109.5 . . ? 
H62C C62 H62D 109.5 . . ? 
C61 C62 H62E 109.5 . . ? 
H62C C62 H62E 109.5 . . ? 
H62D C62 H62E 109.5 . . ? 
C61 C63 H63F 109.5 . . ? 
C61 C63 H63G 109.5 . . ? 
H63F C63 H63G 109.5 . . ? 
C61 C63 H63H 109.5 . . ? 
H63F C63 H63H 109.5 . . ? 
H63G C63 H63H 109.5 . . ? 
  
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 
C21 C20 C11 C10 -2.8(10) . . . . ? 
C19 C20 C11 C10 178.8(7) . . . . ? 
C21 C20 C11 C12 175.2(7) . . . . ? 
C19 C20 C11 C12 -3.1(12) . . . . ? 
C25 S3 C22 C23 -1.1(6) . . . . ? 
C25 S3 C22 C21 177.7(7) . . . . ? 
C11 C20 C21 C22 -172.8(8) . . . . ? 
C19 C20 C21 C22 5.5(14) . . . . ? 
C11 C20 C21 S2 1.7(8) . . . . ? 
C19 C20 C21 S2 180.0(6) . . . . ? 
C23 C22 C21 C20 158.3(9) . . . . ? 
S3 C22 C21 C20 -20.2(12) . . . . ? 
C23 C22 C21 S2 -15.9(11) . . . . ? 
S3 C22 C21 S2 165.6(4) . . . . ? 
C10 S2 C21 C20 -0.2(6) . . . . ? 
C10 S2 C21 C22 175.3(6) . . . . ? 
C39 S4 C36 C37 -0.4(7) . . . . ? 
C39 S4 C36 C35 179.8(8) . . . . ? 
C20 C11 C10 C9 177.5(8) . . . . ? 
C12 C11 C10 C9 -0.5(14) . . . . ? 
C20 C11 C10 S2 2.6(9) . . . . ? 
C12 C11 C10 S2 -175.4(6) . . . . ? 
C21 S2 C10 C11 -1.4(6) . . . . ? 
C21 S2 C10 C9 -177.5(6) . . . . ? 
C9 S1 C6 C7 0.2(6) . . . . ? 
C9 S1 C6 C5 -179.7(7) . . . . ? 
C41 C50 C51 C52 176.2(8) . . . . ? 
C49 C50 C51 C52 -4.0(14) . . . . ? 
C41 C50 C51 S5 -0.5(9) . . . . ? 
C49 C50 C51 S5 179.3(6) . . . . ? 
C40 S5 C51 C50 0.0(6) . . . . ? 
C40 S5 C51 C52 -177.3(6) . . . . ? 
C50 C51 C52 C53 -162.2(9) . . . . ? 
S5 C51 C52 C53 14.5(11) . . . . ? 
C50 C51 C52 S6 13.5(13) . . . . ? 
S5 C51 C52 S6 -169.8(4) . . . . ? 
C55 S6 C52 C53 -1.0(7) . . . . ? 
C55 S6 C52 C51 -177.3(7) . . . . ? 
C10 C11 C12 C13 -92.7(10) . . . . ? 
C20 C11 C12 C13 89.5(9) . . . . ? 
C21 C20 C19 C18 84.4(10) . . . . ? 
C11 C20 C19 C18 -97.5(9) . . . . ? 
N2 C2 C4 C5 131(18) . . . . ? 
N2 C2 C4 C1 -53(19) . . . . ? 
C51 S5 C40 C41 0.5(6) . . . . ? 
C51 S5 C40 C39 179.2(6) . . . . ? 
C37 C36 C35 C34 -178.7(9) . . . . ? 
S4 C36 C35 C34 1.0(13) . . . . ? 
C37 C36 C35 C33 1.2(12) . . . . ? 
S4 C36 C35 C33 -179.1(6) . . . . ? 
C11 C10 C9 C8 -165.1(9) . . . . ? 
S2 C10 C9 C8 9.7(11) . . . . ? 
C11 C10 C9 S1 17.0(13) . . . . ? 
S2 C10 C9 S1 -168.2(4) . . . . ? 
C6 S1 C9 C8 -0.7(7) . . . . ? 
C6 S1 C9 C10 177.6(6) . . . . ? 
C53 C54 C55 C56 -179.1(8) . . . . ? 
C53 C54 C55 S6 0.2(10) . . . . ? 
C57 C56 C55 C54 179.2(9) . . . . ? 
C58 C56 C55 C54 -0.2(12) . . . . ? 
C57 C56 C55 S6 0.0(13) . . . . ? 
C58 C56 C55 S6 -179.4(6) . . . . ? 
C52 S6 C55 C54 0.5(7) . . . . ? 
C52 S6 C55 C56 179.7(7) . . . . ? 
C37 C38 C39 C40 177.7(8) . . . . ? 
C37 C38 C39 S4 -2.7(10) . . . . ? 
C41 C40 C39 C38 169.6(9) . . . . ? 
S5 C40 C39 C38 -8.8(11) . . . . ? 
C41 C40 C39 S4 -9.9(13) . . . . ? 
S5 C40 C39 S4 171.7(4) . . . . ? 
C36 S4 C39 C38 1.8(7) . . . . ? 
C36 S4 C39 C40 -178.7(7) . . . . ? 
C22 S3 C25 C24 1.7(7) . . . . ? 
C22 S3 C25 C26 178.2(7) . . . . ? 
C39 C40 C41 C50 -179.3(8) . . . . ? 
S5 C40 C41 C50 -0.8(9) . . . . ? 
C39 C40 C41 C42 -3.2(14) . . . . ? 
S5 C40 C41 C42 175.3(6) . . . . ? 
C51 C50 C41 C40 0.8(10) . . . . ? 
C49 C50 C41 C40 -178.9(7) . . . . ? 
C51 C50 C41 C42 -175.3(7) . . . . ? 
C49 C50 C41 C42 5.0(12) . . . . ? 
C43 C42 C41 C40 93.9(9) . . . . ? 
C43 C42 C41 C50 -90.4(9) . . . . ? 
C2 C4 C5 C6 -2.4(15) . . . . ? 
C1 C4 C5 C6 -178.1(8) . . . . ? 
C2 C4 C5 C3 179.2(8) . . . . ? 
C1 C4 C5 C3 3.5(13) . . . . ? 
C7 C6 C5 C4 174.6(9) . . . . ? 
S1 C6 C5 C4 -5.5(14) . . . . ? 
C7 C6 C5 C3 -7.0(12) . . . . ? 
S1 C6 C5 C3 172.9(6) . . . . ? 
N3 C3 C5 C4 168(18) . . . . ? 
N3 C3 C5 C6 -10(18) . . . . ? 
C51 C52 C53 C54 177.4(8) . . . . ? 
S6 C52 C53 C54 1.3(10) . . . . ? 
C55 C54 C53 C52 -1.0(12) . . . . ? 
C58 C56 C57 C59 -179.0(9) . . . . ? 
C55 C56 C57 C59 1.6(15) . . . . ? 
C58 C56 C57 C60 0.9(13) . . . . ? 
C55 C56 C57 C60 -178.5(8) . . . . ? 
C36 C35 C34 C32 0.7(14) . . . . ? 
C33 C35 C34 C32 -179.2(8) . . . . ? 
C36 C35 C34 C31 -179.4(8) . . . . ? 
C33 C35 C34 C31 0.7(11) . . . . ? 
N8 C32 C34 C35 168(14) . . . . ? 
N8 C32 C34 C31 -12(15) . . . . ? 
C51 C50 C49 C48 -81.9(10) . . . . ? 
C41 C50 C49 C48 97.9(9) . . . . ? 
C50 C49 C48 C47 174.6(8) . . . . ? 
C24 C25 C26 C27 -176.7(10) . . . . ? 
S3 C25 C26 C27 7.3(13) . . . . ? 
C24 C25 C26 C28 -0.7(13) . . . . ? 
S3 C25 C26 C28 -176.7(6) . . . . ? 
C34 C35 C33 N9 161(12) . . . . ? 
C36 C35 C33 N9 -19(13) . . . . ? 
C35 C34 C31 N7 -146(11) . . . . ? 
C32 C34 C31 N7 34(11) . . . . ? 
C41 C42 C43 C44 -174.7(7) . . . . ? 
C57 C56 C58 N10 -70(53) . . . . ? 
C55 C56 C58 N10 109(53) . . . . ? 
C21 C22 C23 C24 -178.5(8) . . . . ? 
S3 C22 C23 C24 0.2(10) . . . . ? 
C35 C36 C37 C38 178.7(8) . . . . ? 
S4 C36 C37 C38 -1.0(10) . . . . ? 
C39 C38 C37 C36 2.4(12) . . . . ? 
C10 C9 C8 C7 -177.0(8) . . . . ? 
S1 C9 C8 C7 1.1(10) . . . . ? 
C9 C8 C7 C6 -1.0(12) . . . . ? 
C5 C6 C7 C8 -179.7(8) . . . . ? 
S1 C6 C7 C8 0.4(10) . . . . ? 
C56 C57 C60 N12 -30(36) . . . . ? 
C59 C57 C60 N12 150(35) . . . . ? 
C42 C43 C44 C45 -64.2(12) . . . . ? 
C20 C19 C18 C17 -175.3(8) . . . . ? 
C5 C4 C1 N1 -147(18) . . . . ? 
C2 C4 C1 N1 37(19) . . . . ? 
C26 C25 C24 C23 -178.5(8) . . . . ? 
S3 C25 C24 C23 -1.9(10) . . . . ? 
C22 C23 C24 C25 1.1(12) . . . . ? 
C11 C12 C13 C14 173.8(8) . . . . ? 
C19 C18 C17 C16 -65.8(11) . . . . ? 
C12 C13 C14 C15 63.8(12) . . . . ? 
C27 C26 C28 N4 170(15) . . . . ? 
C25 C26 C28 N4 -7(16) . . . . ? 
C25 C26 C27 C29 -4.9(16) . . . . ? 
C28 C26 C27 C29 179.1(9) . . . . ? 
C25 C26 C27 C30 176.7(9) . . . . ? 
C28 C26 C27 C30 0.6(14) . . . . ? 
N6 C30 C27 C26 -119(33) . . . . ? 
N6 C30 C27 C29 62(34) . . . . ? 
C49 C48 C47 C46 -174.4(9) . . . . ? 
C26 C27 C29 N5 69(21) . . . . ? 
C30 C27 C29 N5 -112(21) . . . . ? 
C56 C57 C59 N11 -149(52) . . . . ? 
C60 C57 C59 N11 31(53) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.998 
_diffrn_reflns_theta_full              25.06 
_diffrn_measured_fraction_theta_full   0.998 
_refine_diff_density_max    1.091 
_refine_diff_density_min   -0.620 
_refine_diff_density_rms    0.106 
