# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
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data_sample_4_ae
_database_code_depnum_ccdc_archive 'CCDC 1437363'
_audit_update_record             
;
2015-11-17 deposited with the CCDC.
2016-02-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'5,11,17,23-Tetra-tert-butyl-25,27-di[(hydrazinocarbonyl)methoxy]-26,28-di[(hydroxycarbonyl)methoxy]- 2,8,14,20-tetrathiacalix[4]arene'
_chemical_name_common            ?
_chemical_melting_point          545
_chemical_formula_moiety         'C48 H60 N4 O10 S4, C2 H6 O S'
_chemical_formula_sum            'C50 H66 N4 O11 S5'
_chemical_formula_weight         1059.36

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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                   13.163(5)
_cell_length_b                   29.199(11)
_cell_length_c                   15.137(5)
_cell_angle_alpha                90
_cell_angle_beta                 91.473(5)
_cell_angle_gamma                90
_cell_volume                     5816(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3329
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      17.12

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_F_000             2248
_exptl_transmission_factor_min   0.6670
_exptl_transmission_factor_max   0.7461
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.255
_shelx_estimated_absorpt_T_min   0.939
_shelx_estimated_absorpt_T_max   0.982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_process_details   
;
 G.M. Sheldrick (1998a). SADABS v.2.01, Bruker.
 Siemens Area Detector Absorption Correction Program.
 Bruker AXS. Madison. Wisconsin. USA

 The maximum experimental transmission factor Tmax is equal to the 
 one estimated by SHELX. The minimum experimental transmission factor 
 Tmin is calculated as a product of Tmax and the Tmin-to-Tmax-ratio, 
 evaluated by SADABS.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_number            67104
_diffrn_reflns_av_unetI/netI     0.1996
_diffrn_reflns_av_R_equivalents  0.1259
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.697
_diffrn_reflns_theta_max         30.536
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.873
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.873
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             15532
_reflns_number_gt                4474
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1693P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15532
_refine_ls_number_parameters     797
_refine_ls_number_restraints     447
_refine_ls_R_factor_all          0.2629
_refine_ls_R_factor_gt           0.1075
_refine_ls_wR_factor_ref         0.3323
_refine_ls_wR_factor_gt          0.2694
_refine_ls_goodness_of_fit_ref   0.856
_refine_ls_restrained_S_all      0.875
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.73266(12) 0.22979(5) 0.88180(9) 0.0675(5) Uani 1 1 d . . . . .
C2 C 0.8198(4) 0.18463(17) 0.8735(3) 0.0516(13) Uani 1 1 d . . . . .
C3 C 0.7852(4) 0.14395(19) 0.8349(3) 0.0585(14) Uani 1 1 d . . . . .
H3 H 0.7146 0.1405 0.8223 0.070 Uiso 1 1 calc R U . . .
C4 C 0.8499(4) 0.10869(18) 0.8144(4) 0.0584(14) Uani 1 1 d . . . . .
C5 C 0.9507(5) 0.11368(19) 0.8369(3) 0.0634(15) Uani 1 1 d . . . . .
H5 H 0.9959 0.0893 0.8244 0.076 Uiso 1 1 calc R U . . .
C6 C 0.9905(4) 0.1536(2) 0.8780(3) 0.0553(14) Uani 1 1 d . . . . .
C7 C 0.9253(4) 0.18995(18) 0.8973(3) 0.0534(13) Uani 1 1 d . . . . .
O7 O 0.9543(3) 0.22788(14) 0.9399(2) 0.0651(10) Uani 1 1 d . . . . .
S8 S 1.12255(11) 0.15556(6) 0.88834(10) 0.0743(5) Uani 1 1 d . . . . .
C9 C 1.1560(4) 0.18014(19) 0.9907(3) 0.0528(13) Uani 1 1 d . . . . .
C10 C 1.2332(4) 0.21250(19) 0.9904(4) 0.0588(14) Uani 1 1 d . . . . .
H10 H 1.2585 0.2222 0.9353 0.071 Uiso 1 1 calc R U . . .
C11 C 1.2750(4) 0.23124(17) 1.0673(3) 0.0526(13) Uani 1 1 d . . . . .
C12 C 1.2350(4) 0.21566(18) 1.1472(3) 0.0535(13) Uani 1 1 d . . . . .
H12 H 1.2621 0.2273 1.2014 0.064 Uiso 1 1 calc R U . . .
C13 C 1.1577(4) 0.18412(18) 1.1490(3) 0.0554(14) Uani 1 1 d . . . . .
C14 C 1.1205(4) 0.16410(19) 1.0707(4) 0.0555(13) Uani 1 1 d . . . . .
O14 O 1.0428(3) 0.13187(15) 1.0725(2) 0.0722(11) Uani 1 1 d . . . . .
S15 S 1.12654(11) 0.16585(6) 1.25656(9) 0.0675(5) Uani 1 1 d . . . . .
C16 C 0.9940(4) 0.1578(2) 1.2581(3) 0.0537(13) Uani 1 1 d . . . . .
C17 C 0.9646(4) 0.1156(2) 1.2958(3) 0.0625(15) Uani 1 1 d . . . . .
H17 H 1.0146 0.0931 1.3097 0.075 Uiso 1 1 calc R U . . .
C18 C 0.8627(4) 0.10699(18) 1.3127(4) 0.0587(14) Uani 1 1 d . . . . .
C19 C 0.7931(5) 0.14092(19) 1.2898(3) 0.0628(15) Uani 1 1 d . . . . .
H19 H 0.7230 0.1354 1.2987 0.075 Uiso 1 1 calc R U . . .
C20 C 0.8218(4) 0.18246(17) 1.2546(3) 0.0480(12) Uani 1 1 d . . . . .
C21 C 0.9223(4) 0.18949(18) 1.2399(3) 0.0530(13) Uani 1 1 d . . . . .
O21 O 0.9521(3) 0.23018(14) 1.1990(3) 0.0705(11) Uani 1 1 d . . . . .
S22 S 0.72640(12) 0.22456(5) 1.24603(10) 0.0704(5) Uani 1 1 d . . . . .
C23 C 0.7402(4) 0.25344(19) 1.1449(3) 0.0562(13) Uani 1 1 d . . . . .
C24 C 0.7238(4) 0.30064(17) 1.1464(3) 0.0561(13) Uani 1 1 d . . . . .
H24 H 0.7178 0.3159 1.2014 0.067 Uiso 1 1 calc R U . . .
C25 C 0.7163(4) 0.32536(17) 1.0696(4) 0.0550(13) Uani 1 1 d . . . . .
C26 C 0.7285(4) 0.30249(18) 0.9897(3) 0.0537(13) Uani 1 1 d . . . . .
H26 H 0.7276 0.3193 0.9360 0.064 Uiso 1 1 calc R U . . .
C27 C 0.7419(4) 0.25519(17) 0.9882(3) 0.0485(12) Uani 1 1 d . . . . .
C28 C 0.7493(4) 0.23104(16) 1.0638(3) 0.0471(12) Uani 1 1 d . . . . .
O28 O 0.7702(3) 0.18441(11) 1.0635(2) 0.0550(9) Uani 1 1 d . . . . .
C29 C 0.8091(5) 0.0662(2) 0.7700(5) 0.0875(19) Uani 1 1 d D U . . .
C30 C 0.7149(9) 0.0481(4) 0.8192(10) 0.154(5) Uani 0.771(11) 1 d D U P A 1
H30A H 0.7354 0.0391 0.8794 0.231 Uiso 0.771(11) 1 calc R U P A 1
H30B H 0.6634 0.0722 0.8216 0.231 Uiso 0.771(11) 1 calc R U P A 1
H30C H 0.6867 0.0215 0.7876 0.231 Uiso 0.771(11) 1 calc R U P A 1
C31 C 0.8861(9) 0.0279(3) 0.7705(9) 0.131(4) Uani 0.771(11) 1 d D U P A 1
H31A H 0.9063 0.0205 0.8316 0.196 Uiso 0.771(11) 1 calc R U P A 1
H31B H 0.8561 0.0008 0.7421 0.196 Uiso 0.771(11) 1 calc R U P A 1
H31C H 0.9460 0.0376 0.7381 0.196 Uiso 0.771(11) 1 calc R U P A 1
C32 C 0.7743(12) 0.0796(4) 0.6785(7) 0.143(5) Uani 0.771(11) 1 d D U P A 1
H32A H 0.7471 0.0526 0.6474 0.215 Uiso 0.771(11) 1 calc R U P A 1
H32B H 0.7211 0.1029 0.6819 0.215 Uiso 0.771(11) 1 calc R U P A 1
H32C H 0.8318 0.0919 0.6462 0.215 Uiso 0.771(11) 1 calc R U P A 1
C30' C 0.867(2) 0.0608(10) 0.6808(14) 0.092(8) Uani 0.229(11) 1 d D U P A 2
H30D H 0.8421 0.0334 0.6497 0.138 Uiso 0.229(11) 1 calc R U P A 2
H30E H 0.8541 0.0878 0.6437 0.138 Uiso 0.229(11) 1 calc R U P A 2
H30F H 0.9398 0.0579 0.6935 0.138 Uiso 0.229(11) 1 calc R U P A 2
C31' C 0.6960(12) 0.0673(10) 0.742(2) 0.100(8) Uani 0.229(11) 1 d D U P A 2
H31D H 0.6773 0.0382 0.7136 0.151 Uiso 0.229(11) 1 calc R U P A 2
H31E H 0.6546 0.0721 0.7938 0.151 Uiso 0.229(11) 1 calc R U P A 2
H31F H 0.6841 0.0924 0.6997 0.151 Uiso 0.229(11) 1 calc R U P A 2
C32' C 0.829(3) 0.0217(7) 0.8200(17) 0.107(8) Uani 0.229(11) 1 d D U P A 2
H32D H 0.7994 -0.0039 0.7861 0.161 Uiso 0.229(11) 1 calc R U P A 2
H32E H 0.9020 0.0171 0.8282 0.161 Uiso 0.229(11) 1 calc R U P A 2
H32F H 0.7969 0.0233 0.8778 0.161 Uiso 0.229(11) 1 calc R U P A 2
C33 C 1.3618(4) 0.26586(19) 1.0653(3) 0.0637(14) Uani 1 1 d D U . . .
C34 C 1.3335(10) 0.3046(4) 1.0021(8) 0.102(4) Uani 0.614(14) 1 d D U P B 1
H34A H 1.3161 0.2919 0.9437 0.153 Uiso 0.614(14) 1 calc R U P B 1
H34B H 1.2750 0.3213 1.0246 0.153 Uiso 0.614(14) 1 calc R U P B 1
H34C H 1.3913 0.3256 0.9973 0.153 Uiso 0.614(14) 1 calc R U P B 1
C35 C 1.3883(12) 0.2863(5) 1.1549(6) 0.095(4) Uani 0.614(14) 1 d D U P B 1
H35A H 1.4067 0.2617 1.1964 0.142 Uiso 0.614(14) 1 calc R U P B 1
H35B H 1.4458 0.3073 1.1495 0.142 Uiso 0.614(14) 1 calc R U P B 1
H35C H 1.3296 0.3030 1.1767 0.142 Uiso 0.614(14) 1 calc R U P B 1
C36 C 1.4584(9) 0.2421(5) 1.0328(12) 0.127(6) Uani 0.614(14) 1 d D U P B 1
H36A H 1.4443 0.2284 0.9747 0.190 Uiso 0.614(14) 1 calc R U P B 1
H36B H 1.5131 0.2647 1.0282 0.190 Uiso 0.614(14) 1 calc R U P B 1
H36C H 1.4791 0.2181 1.0748 0.190 Uiso 0.614(14) 1 calc R U P B 1
C34' C 1.4380(14) 0.2645(8) 1.1424(10) 0.092(6) Uani 0.386(14) 1 d D U P B 2
H34D H 1.4899 0.2881 1.1342 0.139 Uiso 0.386(14) 1 calc R U P B 2
H34E H 1.4028 0.2703 1.1976 0.139 Uiso 0.386(14) 1 calc R U P B 2
H34F H 1.4703 0.2343 1.1452 0.139 Uiso 0.386(14) 1 calc R U P B 2
C35' C 1.4213(14) 0.2629(7) 0.9790(9) 0.083(6) Uani 0.386(14) 1 d D U P B 2
H35D H 1.3736 0.2637 0.9283 0.124 Uiso 0.386(14) 1 calc R U P B 2
H35E H 1.4682 0.2888 0.9758 0.124 Uiso 0.386(14) 1 calc R U P B 2
H35F H 1.4599 0.2342 0.9783 0.124 Uiso 0.386(14) 1 calc R U P B 2
C36' C 1.3128(13) 0.3136(5) 1.0673(17) 0.108(7) Uani 0.386(14) 1 d D U P B 2
H36D H 1.2627 0.3163 1.0185 0.161 Uiso 0.386(14) 1 calc R U P B 2
H36E H 1.2790 0.3179 1.1236 0.161 Uiso 0.386(14) 1 calc R U P B 2
H36F H 1.3654 0.3370 1.0609 0.161 Uiso 0.386(14) 1 calc R U P B 2
C37 C 0.8292(5) 0.06180(19) 1.3525(4) 0.0812(17) Uani 1 1 d D U . . .
C38 C 0.7508(10) 0.0396(4) 1.2886(7) 0.114(4) Uani 0.650(9) 1 d D U P C 1
H38A H 0.6959 0.0614 1.2755 0.170 Uiso 0.650(9) 1 calc R U P C 1
H38B H 0.7839 0.0312 1.2337 0.170 Uiso 0.650(9) 1 calc R U P C 1
H38C H 0.7227 0.0121 1.3159 0.170 Uiso 0.650(9) 1 calc R U P C 1
C39 C 0.7718(10) 0.0729(3) 1.4372(7) 0.100(3) Uani 0.650(9) 1 d D U P C 1
H39A H 0.7157 0.0939 1.4231 0.150 Uiso 0.650(9) 1 calc R U P C 1
H39B H 0.7447 0.0446 1.4621 0.150 Uiso 0.650(9) 1 calc R U P C 1
H39C H 0.8185 0.0873 1.4804 0.150 Uiso 0.650(9) 1 calc R U P C 1
C40 C 0.9154(9) 0.0295(4) 1.3747(12) 0.136(5) Uani 0.650(9) 1 d D U P C 1
H40A H 0.8882 0.0012 1.3999 0.205 Uiso 0.650(9) 1 calc R U P C 1
H40B H 0.9519 0.0222 1.3209 0.205 Uiso 0.650(9) 1 calc R U P C 1
H40C H 0.9621 0.0439 1.4178 0.205 Uiso 0.650(9) 1 calc R U P C 1
C38' C 0.9016(15) 0.0490(8) 1.4311(12) 0.105(6) Uani 0.350(9) 1 d D U P C 2
H38D H 0.9721 0.0505 1.4122 0.158 Uiso 0.350(9) 1 calc R U P C 2
H38E H 0.8920 0.0706 1.4798 0.158 Uiso 0.350(9) 1 calc R U P C 2
H38F H 0.8864 0.0179 1.4511 0.158 Uiso 0.350(9) 1 calc R U P C 2
C39' C 0.8497(19) 0.0266(5) 1.2803(10) 0.100(3) Uani 0.350(9) 1 d D U P C 2
H39D H 0.9206 0.0290 1.2627 0.150 Uiso 0.350(9) 1 calc R U P C 2
H39E H 0.8370 -0.0043 1.3030 0.150 Uiso 0.350(9) 1 calc R U P C 2
H39F H 0.8046 0.0324 1.2290 0.150 Uiso 0.350(9) 1 calc R U P C 2
C40' C 0.7209(11) 0.0595(9) 1.3820(17) 0.126(8) Uani 0.350(9) 1 d D U P C 2
H40D H 0.7076 0.0290 1.4064 0.190 Uiso 0.350(9) 1 calc R U P C 2
H40E H 0.7101 0.0828 1.4274 0.190 Uiso 0.350(9) 1 calc R U P C 2
H40F H 0.6748 0.0651 1.3313 0.190 Uiso 0.350(9) 1 calc R U P C 2
C41 C 0.6975(5) 0.37737(18) 1.0711(4) 0.0711(15) Uani 1 1 d D U . . .
C42 C 0.7170(11) 0.4005(4) 0.9837(6) 0.095(4) Uani 0.601(11) 1 d D U P D 1
H42A H 0.7870 0.3943 0.9664 0.142 Uiso 0.601(11) 1 calc R U P D 1
H42B H 0.6696 0.3885 0.9384 0.142 Uiso 0.601(11) 1 calc R U P D 1
H42C H 0.7072 0.4336 0.9897 0.142 Uiso 0.601(11) 1 calc R U P D 1
C43 C 0.5912(8) 0.3856(4) 1.1011(10) 0.101(4) Uani 0.601(11) 1 d D U P D 1
H43A H 0.5816 0.3701 1.1578 0.151 Uiso 0.601(11) 1 calc R U P D 1
H43B H 0.5801 0.4185 1.1083 0.151 Uiso 0.601(11) 1 calc R U P D 1
H43C H 0.5426 0.3735 1.0570 0.151 Uiso 0.601(11) 1 calc R U P D 1
C44 C 0.7736(10) 0.3979(4) 1.1406(8) 0.104(4) Uani 0.601(11) 1 d D U P D 1
H44A H 0.8433 0.3928 1.1215 0.156 Uiso 0.601(11) 1 calc R U P D 1
H44B H 0.7614 0.4309 1.1461 0.156 Uiso 0.601(11) 1 calc R U P D 1
H44C H 0.7641 0.3831 1.1978 0.156 Uiso 0.601(11) 1 calc R U P D 1
C42' C 0.6452(14) 0.3902(5) 1.1553(9) 0.087(5) Uani 0.399(11) 1 d D U P D 2
H42D H 0.5810 0.3734 1.1589 0.130 Uiso 0.399(11) 1 calc R U P D 2
H42E H 0.6892 0.3825 1.2063 0.130 Uiso 0.399(11) 1 calc R U P D 2
H42F H 0.6313 0.4232 1.1553 0.130 Uiso 0.399(11) 1 calc R U P D 2
C43' C 0.7956(11) 0.4014(6) 1.0601(14) 0.112(6) Uani 0.399(11) 1 d D U P D 2
H43D H 0.8258 0.3917 1.0047 0.168 Uiso 0.399(11) 1 calc R U P D 2
H43E H 0.7840 0.4346 1.0588 0.168 Uiso 0.399(11) 1 calc R U P D 2
H43F H 0.8419 0.3938 1.1098 0.168 Uiso 0.399(11) 1 calc R U P D 2
C44' C 0.6216(14) 0.3888(5) 0.9939(10) 0.100(6) Uani 0.399(11) 1 d D U P D 2
H44D H 0.5575 0.3726 1.0027 0.150 Uiso 0.399(11) 1 calc R U P D 2
H44E H 0.6090 0.4219 0.9926 0.150 Uiso 0.399(11) 1 calc R U P D 2
H44F H 0.6506 0.3792 0.9379 0.150 Uiso 0.399(11) 1 calc R U P D 2
C45 C 1.0128(6) 0.2580(2) 0.8952(5) 0.091(2) Uani 1 1 d D U . . .
H45A H 1.0343 0.2420 0.8412 0.109 Uiso 0.564(6) 1 calc R U P E 1
H45B H 1.0751 0.2629 0.9321 0.109 Uiso 0.564(6) 1 calc R U P E 1
H45C H 0.9782 0.2674 0.8393 0.109 Uiso 0.436(6) 1 calc R U P E 2
H45D H 1.0789 0.2439 0.8812 0.109 Uiso 0.436(6) 1 calc R U P E 2
C46 C 0.9781(8) 0.3033(3) 0.8674(7) 0.070(3) Uani 0.564(6) 1 d D U P E 1
O47 O 0.8954(6) 0.3109(3) 0.8454(7) 0.114(3) Uani 0.564(6) 1 d D U P E 1
O48 O 1.0496(6) 0.3345(3) 0.8677(9) 0.101(4) Uani 0.564(6) 1 d D U P E 1
H48 H 1.0571 0.3442 0.8160 0.151 Uiso 0.564(6) 1 calc R U P E 1
C46' C 1.0279(14) 0.2972(5) 0.9529(11) 0.108(5) Uani 0.436(6) 1 d D U P E 2
O47' O 1.069(2) 0.3311(7) 0.9302(14) 0.233(13) Uani 0.436(6) 1 d D U P E 2
O48' O 1.0101(15) 0.2903(6) 1.0378(10) 0.152(6) Uani 0.436(6) 1 d D U P E 2
H48' H 0.9504 0.2807 1.0432 0.228 Uiso 0.436(6) 1 calc R U P E 2
C49 C 1.0713(6) 0.0869(2) 1.1024(6) 0.101(2) Uani 1 1 d . . . . .
H49A H 1.0097 0.0690 1.1152 0.121 Uiso 1 1 calc R U . . .
H49B H 1.1132 0.0893 1.1574 0.121 Uiso 1 1 calc R U . . .
C50 C 1.1296(9) 0.0636(3) 1.0336(9) 0.145(3) Uani 1 1 d D U . . .
O50 O 1.2236(6) 0.0656(3) 1.0396(7) 0.215(4) Uani 1 1 d D U . . .
N50 N 1.0794(7) 0.0407(3) 0.9783(7) 0.177(4) Uani 1 1 d D U . . .
H50 H 1.0128 0.0416 0.9820 0.212 Uiso 1 1 calc R U . . .
N51 N 1.1178(13) 0.0139(5) 0.9118(11) 0.309(7) Uani 1 1 d D U . . .
C52 C 0.9893(7) 0.2660(3) 1.2488(6) 0.117(3) Uani 1 1 d D U . . .
H52A H 1.0504 0.2561 1.2833 0.141 Uiso 0.564(6) 1 calc R U P E 1
H52B H 0.9374 0.2762 1.2908 0.141 Uiso 0.564(6) 1 calc R U P E 1
H52C H 1.0599 0.2668 1.2278 0.141 Uiso 0.436(6) 1 calc R U P E 2
H52D H 0.9953 0.2507 1.3071 0.141 Uiso 0.436(6) 1 calc R U P E 2
C53 C 1.0161(10) 0.3049(4) 1.1879(9) 0.092(4) Uani 0.564(6) 1 d D U P E 1
O54 O 1.0342(9) 0.3407(4) 1.2185(8) 0.120(4) Uani 0.564(6) 1 d D U P E 1
O55 O 1.0040(8) 0.2960(3) 1.1013(8) 0.115(3) Uani 0.564(6) 1 d D U P E 1
H55 H 1.0299 0.2704 1.0901 0.172 Uiso 0.564(6) 1 calc R U P E 1
C53' C 0.9801(14) 0.3128(5) 1.2778(13) 0.142(8) Uani 0.436(6) 1 d D U P E 2
O54' O 1.0314(13) 0.3432(6) 1.299(2) 0.225(12) Uani 0.436(6) 1 d D U P E 2
O55' O 0.8792(11) 0.3160(6) 1.2828(11) 0.149(5) Uani 0.436(6) 1 d D U P E 2
H55' H 0.8519 0.3056 1.2363 0.224 Uiso 0.436(6) 1 calc R U P E 2
C56 C 0.6828(4) 0.15626(19) 1.0605(4) 0.0687(16) Uani 1 1 d . . . . .
H56A H 0.6394 0.1644 1.0085 0.082 Uiso 1 1 calc R U . . .
H56B H 0.6430 0.1610 1.1143 0.082 Uiso 1 1 calc R U . . .
C57 C 0.7145(7) 0.1069(2) 1.0545(5) 0.087(2) Uani 1 1 d D . . . .
O57 O 0.6453(4) 0.07823(18) 1.0496(4) 0.132(2) Uani 1 1 d D . . . .
N57 N 0.8075(5) 0.09789(16) 1.0555(3) 0.0761(15) Uani 1 1 d D . . . .
H57 H 0.8524 0.1197 1.0661 0.091 Uiso 1 1 calc R U . . .
N58 N 0.8398(7) 0.0531(3) 1.0395(8) 0.197(4) Uani 1 1 d D . . . .
S90 S 0.4277(5) 0.07444(17) 0.2249(5) 0.283(3) Uani 1 1 d . U . . .
O90 O 0.3222(12) 0.0789(5) 0.2712(14) 0.348(7) Uani 1 1 d . U . . .
C91 C 0.4135(10) 0.1246(4) 0.1807(14) 0.270(7) Uani 1 1 d . U . . .
H91A H 0.3634 0.1228 0.1318 0.405 Uiso 1 1 calc R U . . .
H91B H 0.3899 0.1462 0.2253 0.405 Uiso 1 1 calc R U . . .
H91C H 0.4787 0.1351 0.1583 0.405 Uiso 1 1 calc R U . . .
C92 C 0.5073(10) 0.0888(4) 0.2954(11) 0.224(6) Uani 1 1 d . U . . .
H92A H 0.5753 0.0868 0.2709 0.337 Uiso 1 1 calc R U . . .
H92B H 0.4942 0.1204 0.3138 0.337 Uiso 1 1 calc R U . . .
H92C H 0.5032 0.0685 0.3466 0.337 Uiso 1 1 calc R U . . .
H51A H 1.0819 -0.0081 0.8950 0.337 Uiso 1 1 d . U . . .
H51C H 1.1104 0.0370 0.8575 0.337 Uiso 1 1 d . U . . .
H58A H 0.9055 0.0534 1.0242 0.337 Uiso 1 1 d . U . . .
H58B H 0.8013 0.0427 0.9901 0.337 Uiso 1 1 d . U . . .


_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
S1 C2 1.754(5) . ?
S1 C27 1.774(5) . ?
C2 C3 1.394(7) . ?
C2 C7 1.435(7) . ?
C3 C4 1.376(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.369(7) . ?
C4 C29 1.503(8) . ?
C5 C6 1.416(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.400(7) . ?
C6 S8 1.742(5) . ?
C7 O7 1.332(6) . ?
O7 C45 1.361(8) . ?
S8 C9 1.754(5) . ?
C9 C10 1.388(7) . ?
C9 C14 1.390(7) . ?
C10 C11 1.387(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.407(7) . ?
C11 C33 1.526(7) . ?
C12 C13 1.373(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.398(7) . ?
C13 S15 1.771(5) . ?
C14 O14 1.391(6) . ?
O14 C49 1.434(8) . ?
S15 C16 1.761(5) . ?
C16 C21 1.344(7) . ?
C16 C17 1.417(7) . ?
C17 C18 1.395(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.387(7) . ?
C18 C37 1.521(8) . ?
C19 C20 1.382(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.362(7) . ?
C20 S22 1.760(5) . ?
C21 O21 1.401(6) . ?
O21 C52 1.373(9) . ?
S22 C23 1.762(5) . ?
C23 C28 1.398(7) . ?
C23 C24 1.395(7) . ?
C24 C25 1.369(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.394(7) . ?
C25 C41 1.539(7) . ?
C26 C27 1.393(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.346(7) . ?
C28 O28 1.389(5) . ?
O28 C56 1.413(6) . ?
C29 C32 1.500(10) . ?
C29 C31 1.509(10) . ?
C29 C30 1.556(9) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C35 1.514(9) . ?
C33 C34 1.521(9) . ?
C33 C36 1.540(10) . ?
C37 C40 1.508(10) . ?
C37 C39 1.539(9) . ?
C37 C38 1.539(10) . ?
C41 C43 1.501(10) . ?
C41 C42 1.514(9) . ?
C41 C44 1.554(9) . ?
C45 C46 1.457(11) . ?
C46 O47 1.152(10) . ?
C46 O48 1.311(11) . ?
O48 H48 0.8400 . ?
C49 C50 1.476(14) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 O50 1.240(10) . ?
C50 N50 1.248(11) . ?
N50 N51 1.380(12) . ?
N50 H50 0.8800 . ?
N51 H51A 0.833(15) . ?
C52 C53 1.511(12) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C52 H52C 0.9900 . ?
C52 H52D 0.9900 . ?
C53 O54 1.165(12) . ?
C53 O55 1.341(13) . ?
O55 H55 0.8400 . ?
C56 C57 1.505(9) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 O57 1.238(7) . ?
C57 N57 1.251(7) . ?
N57 N58 1.399(8) . ?
N57 H57 0.8800 . ?
N58 H58A 0.901(10) . ?
N58 H58B 0.942(10) . ?
S90 C92 1.536(12) . ?
S90 O90 1.577(17) . ?
S90 C91 1.618(14) . ?

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 S1 C27 110.5(2) . . ?
C3 C2 C7 120.0(5) . . ?
C3 C2 S1 117.6(4) . . ?
C7 C2 S1 122.1(4) . . ?
C4 C3 C2 122.3(5) . . ?
C4 C3 H3 118.8 . . ?
C2 C3 H3 118.8 . . ?
C5 C4 C3 117.7(5) . . ?
C5 C4 C29 122.1(5) . . ?
C3 C4 C29 120.1(5) . . ?
C4 C5 C6 122.8(5) . . ?
C4 C5 H5 118.6 . . ?
C6 C5 H5 118.6 . . ?
C7 C6 C5 119.6(5) . . ?
C7 C6 S8 124.9(4) . . ?
C5 C6 S8 115.0(4) . . ?
O7 C7 C6 124.1(5) . . ?
O7 C7 C2 118.4(5) . . ?
C6 C7 C2 117.4(5) . . ?
C7 O7 C45 117.1(4) . . ?
C6 S8 C9 108.6(2) . . ?
C10 C9 C14 119.7(5) . . ?
C10 C9 S8 116.3(4) . . ?
C14 C9 S8 123.3(5) . . ?
C11 C10 C9 122.7(5) . . ?
C11 C10 H10 118.6 . . ?
C9 C10 H10 118.6 . . ?
C10 C11 C12 116.4(5) . . ?
C10 C11 C33 121.7(5) . . ?
C12 C11 C33 121.9(5) . . ?
C13 C12 C11 121.9(5) . . ?
C13 C12 H12 119.1 . . ?
C11 C12 H12 119.1 . . ?
C12 C13 C14 120.5(5) . . ?
C12 C13 S15 114.2(4) . . ?
C14 C13 S15 124.7(4) . . ?
O14 C14 C9 120.6(5) . . ?
O14 C14 C13 120.6(5) . . ?
C9 C14 C13 118.6(5) . . ?
C14 O14 C49 116.0(5) . . ?
C16 S15 C13 107.7(2) . . ?
C21 C16 C17 118.9(5) . . ?
C21 C16 S15 126.7(4) . . ?
C17 C16 S15 113.7(4) . . ?
C18 C17 C16 120.3(5) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C19 C18 C17 117.2(5) . . ?
C19 C18 C37 121.5(5) . . ?
C17 C18 C37 121.3(5) . . ?
C20 C19 C18 122.5(5) . . ?
C20 C19 H19 118.7 . . ?
C18 C19 H19 118.7 . . ?
C21 C20 C19 118.2(5) . . ?
C21 C20 S22 125.2(4) . . ?
C19 C20 S22 116.1(4) . . ?
C16 C21 C20 122.9(5) . . ?
C16 C21 O21 118.0(5) . . ?
C20 C21 O21 119.0(5) . . ?
C52 O21 C21 120.2(5) . . ?
C20 S22 C23 108.0(2) . . ?
C28 C23 C24 119.5(4) . . ?
C28 C23 S22 123.5(4) . . ?
C24 C23 S22 116.1(4) . . ?
C25 C24 C23 121.0(5) . . ?
C25 C24 H24 119.5 . . ?
C23 C24 H24 119.5 . . ?
C24 C25 C26 118.4(5) . . ?
C24 C25 C41 121.0(5) . . ?
C26 C25 C41 120.5(5) . . ?
C25 C26 C27 120.5(5) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C28 C27 C26 120.8(4) . . ?
C28 C27 S1 123.7(4) . . ?
C26 C27 S1 115.1(4) . . ?
C27 C28 O28 121.4(4) . . ?
C27 C28 C23 119.7(4) . . ?
O28 C28 C23 118.9(4) . . ?
C28 O28 C56 114.2(4) . . ?
C32 C29 C4 107.2(6) . . ?
C32 C29 C31 112.7(7) . . ?
C4 C29 C31 112.1(7) . . ?
C32 C29 C30 107.6(7) . . ?
C4 C29 C30 110.3(6) . . ?
C31 C29 C30 106.8(7) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C35 C33 C34 108.5(7) . . ?
C35 C33 C11 113.5(6) . . ?
C34 C33 C11 109.5(6) . . ?
C11 C33 C36' 106.6(8) . . ?
C35 C33 C36 106.9(7) . . ?
C34 C33 C36 109.0(7) . . ?
C11 C33 C36 109.4(7) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C33 C34' H34D 109.5 . . ?
C33 C34' H34E 109.5 . . ?
H34D C34' H34E 109.5 . . ?
C33 C34' H34F 109.5 . . ?
H34D C34' H34F 109.5 . . ?
H34E C34' H34F 109.5 . . ?
C33 C35' H35D 109.5 . . ?
C33 C35' H35E 109.5 . . ?
H35D C35' H35E 109.5 . . ?
C33 C35' H35F 109.5 . . ?
H35D C35' H35F 109.5 . . ?
H35E C35' H35F 109.5 . . ?
C33 C36' H36D 109.5 . . ?
C33 C36' H36E 109.5 . . ?
H36D C36' H36E 109.5 . . ?
C33 C36' H36F 109.5 . . ?
H36D C36' H36F 109.5 . . ?
H36E C36' H36F 109.5 . . ?
C40' C37 C18 116.3(10) . . ?
C40 C37 C18 114.1(7) . . ?
C40' C37 C39' 111.5(10) . . ?
C18 C37 C39' 104.0(8) . . ?
C40 C37 C39 109.2(7) . . ?
C18 C37 C39 107.5(6) . . ?
C40 C37 C38 111.4(7) . . ?
C18 C37 C38 108.2(6) . . ?
C39 C37 C38 106.1(7) . . ?
C43 C41 C42 112.0(7) . . ?
C43 C41 C25 108.3(6) . . ?
C42 C41 C25 113.3(6) . . ?
C43 C41 C44 108.8(7) . . ?
C42 C41 C44 107.3(7) . . ?
C25 C41 C44 106.9(5) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
O7 C45 C46 123.6(7) . . ?
O47 C46 O48 122.7(10) . . ?
O47 C46 C45 123.1(10) . . ?
O48 C46 C45 114.2(9) . . ?
C46 O48 H48 109.5 . . ?
O14 C49 C50 109.7(7) . . ?
O50 C50 N50 125.8(14) . . ?
O50 C50 C49 117.5(12) . . ?
N50 C50 C49 116.4(11) . . ?
C50 N50 N51 126.6(13) . . ?
C50 N50 H50 116.7 . . ?
N51 N50 H50 116.7 . . ?
N50 N51 H51A 116.4(16) . . ?
N50 N51 H51C 100.1(12) . . ?
H51A N51 H51C 102.3(17) . . ?
O21 C52 C53 108.8(8) . . ?
O54 C53 O55 125.6(11) . . ?
O54 C53 C52 118.6(12) . . ?
O55 C53 C52 115.2(10) . . ?
C53 O55 H55 109.5 . . ?
O28 C56 C57 109.4(5) . . ?
O57 C57 N57 125.3(7) . . ?
O57 C57 C56 116.5(7) . . ?
N57 C57 C56 118.2(6) . . ?
C57 N57 N58 119.7(7) . . ?
C57 N57 H57 120.2 . . ?
N58 N57 H57 120.2 . . ?
N57 N58 H58A 109.4(8) . . ?
N57 N58 H58B 106.2(8) . . ?
C92 S90 O90 105.1(11) . . ?
C92 S90 C91 96.2(8) . . ?
O90 S90 C91 90.9(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
C27 S1 C2 C3 135.1(4) . . . . ?
C27 S1 C2 C7 -50.8(5) . . . . ?
C7 C2 C3 C4 -3.1(8) . . . . ?
S1 C2 C3 C4 171.1(4) . . . . ?
C2 C3 C4 C5 3.0(8) . . . . ?
C2 C3 C4 C29 -177.9(5) . . . . ?
C3 C4 C5 C6 -1.5(8) . . . . ?
C29 C4 C5 C6 179.4(5) . . . . ?
C4 C5 C6 C7 0.2(8) . . . . ?
C4 C5 C6 S8 -172.4(4) . . . . ?
C5 C6 C7 O7 176.4(5) . . . . ?
S8 C6 C7 O7 -11.9(7) . . . . ?
C5 C6 C7 C2 -0.3(7) . . . . ?
S8 C6 C7 C2 171.5(4) . . . . ?
C3 C2 C7 O7 -175.1(5) . . . . ?
S1 C2 C7 O7 10.9(6) . . . . ?
C3 C2 C7 C6 1.7(7) . . . . ?
S1 C2 C7 C6 -172.3(4) . . . . ?
C6 C7 O7 C45 72.0(7) . . . . ?
C2 C7 O7 C45 -111.4(5) . . . . ?
C7 C6 S8 C9 46.4(5) . . . . ?
C5 C6 S8 C9 -141.5(4) . . . . ?
C6 S8 C9 C10 -135.8(4) . . . . ?
C6 S8 C9 C14 54.0(5) . . . . ?
C14 C9 C10 C11 -2.5(8) . . . . ?
S8 C9 C10 C11 -173.0(4) . . . . ?
C9 C10 C11 C12 0.1(8) . . . . ?
C9 C10 C11 C33 178.4(5) . . . . ?
C10 C11 C12 C13 -0.9(7) . . . . ?
C33 C11 C12 C13 -179.2(5) . . . . ?
C11 C12 C13 C14 4.2(8) . . . . ?
C11 C12 C13 S15 174.9(4) . . . . ?
C10 C9 C14 O14 179.7(5) . . . . ?
S8 C9 C14 O14 -10.5(7) . . . . ?
C10 C9 C14 C13 5.5(7) . . . . ?
S8 C9 C14 C13 175.4(4) . . . . ?
C12 C13 C14 O14 179.5(5) . . . . ?
S15 C13 C14 O14 9.7(7) . . . . ?
C12 C13 C14 C9 -6.4(7) . . . . ?
S15 C13 C14 C9 -176.2(4) . . . . ?
C9 C14 O14 C49 110.3(6) . . . . ?
C13 C14 O14 C49 -75.7(7) . . . . ?
C12 C13 S15 C16 143.6(4) . . . . ?
C14 C13 S15 C16 -46.1(5) . . . . ?
C13 S15 C16 C21 -58.5(5) . . . . ?
C13 S15 C16 C17 131.9(4) . . . . ?
C21 C16 C17 C18 0.7(8) . . . . ?
S15 C16 C17 C18 171.2(4) . . . . ?
C16 C17 C18 C19 0.9(8) . . . . ?
C16 C17 C18 C37 179.5(5) . . . . ?
C17 C18 C19 C20 -2.2(8) . . . . ?
C37 C18 C19 C20 179.2(5) . . . . ?
C18 C19 C20 C21 1.8(8) . . . . ?
C18 C19 C20 S22 -170.2(4) . . . . ?
C17 C16 C21 C20 -1.3(8) . . . . ?
S15 C16 C21 C20 -170.4(4) . . . . ?
C17 C16 C21 O21 -177.2(4) . . . . ?
S15 C16 C21 O21 13.6(7) . . . . ?
C19 C20 C21 C16 0.0(7) . . . . ?
S22 C20 C21 C16 171.3(4) . . . . ?
C19 C20 C21 O21 175.9(4) . . . . ?
S22 C20 C21 O21 -12.8(6) . . . . ?
C16 C21 O21 C52 -85.2(7) . . . . ?
C20 C21 O21 C52 98.7(7) . . . . ?
C21 C20 S22 C23 48.5(5) . . . . ?
C19 C20 S22 C23 -140.1(4) . . . . ?
C20 S22 C23 C28 49.9(5) . . . . ?
C20 S22 C23 C24 -140.9(4) . . . . ?
C28 C23 C24 C25 0.2(8) . . . . ?
S22 C23 C24 C25 -169.4(4) . . . . ?
C23 C24 C25 C26 -1.9(8) . . . . ?
C23 C24 C25 C41 179.5(5) . . . . ?
C24 C25 C26 C27 3.7(7) . . . . ?
C41 C25 C26 C27 -177.7(5) . . . . ?
C25 C26 C27 C28 -4.0(7) . . . . ?
C25 C26 C27 S1 168.8(4) . . . . ?
C2 S1 C27 C28 -44.0(5) . . . . ?
C2 S1 C27 C26 143.5(4) . . . . ?
C26 C27 C28 O28 -175.2(4) . . . . ?
S1 C27 C28 O28 12.7(7) . . . . ?
C26 C27 C28 C23 2.2(7) . . . . ?
S1 C27 C28 C23 -169.9(4) . . . . ?
C24 C23 C28 C27 -0.3(8) . . . . ?
S22 C23 C28 C27 168.5(4) . . . . ?
C24 C23 C28 O28 177.1(4) . . . . ?
S22 C23 C28 O28 -14.1(7) . . . . ?
C27 C28 O28 C56 -91.6(6) . . . . ?
C23 C28 O28 C56 91.0(6) . . . . ?
C5 C4 C29 C32 -113.0(8) . . . . ?
C3 C4 C29 C32 67.9(9) . . . . ?
C5 C4 C29 C31 11.3(10) . . . . ?
C3 C4 C29 C31 -167.8(7) . . . . ?
C5 C4 C29 C32' 57.6(16) . . . . ?
C3 C4 C29 C32' -121.6(15) . . . . ?
C5 C4 C29 C31' -175.0(15) . . . . ?
C3 C4 C29 C31' 5.9(16) . . . . ?
C5 C4 C29 C30 130.1(8) . . . . ?
C3 C4 C29 C30 -49.0(9) . . . . ?
C5 C4 C29 C30' -59.0(14) . . . . ?
C3 C4 C29 C30' 121.8(14) . . . . ?
C10 C11 C33 C35 173.3(8) . . . . ?
C12 C11 C33 C35 -8.5(9) . . . . ?
C10 C11 C33 C34' -147.1(10) . . . . ?
C12 C11 C33 C34' 31.1(11) . . . . ?
C10 C11 C33 C34 51.9(9) . . . . ?
C12 C11 C33 C34 -129.9(8) . . . . ?
C10 C11 C33 C36' 94.7(11) . . . . ?
C12 C11 C33 C36' -87.1(11) . . . . ?
C10 C11 C33 C36 -67.5(10) . . . . ?
C12 C11 C33 C36 110.8(9) . . . . ?
C10 C11 C33 C35' -21.9(11) . . . . ?
C12 C11 C33 C35' 156.3(9) . . . . ?
C19 C18 C37 C40' -11.6(14) . . . . ?
C17 C18 C37 C40' 169.9(12) . . . . ?
C19 C18 C37 C40 -178.9(9) . . . . ?
C17 C18 C37 C40 2.6(10) . . . . ?
C19 C18 C37 C39' 111.5(11) . . . . ?
C17 C18 C37 C39' -67.0(11) . . . . ?
C19 C18 C37 C39 -57.7(8) . . . . ?
C17 C18 C37 C39 123.8(7) . . . . ?
C19 C18 C37 C38 56.5(9) . . . . ?
C17 C18 C37 C38 -122.0(8) . . . . ?
C19 C18 C37 C38' -136.0(11) . . . . ?
C17 C18 C37 C38' 45.5(12) . . . . ?
C24 C25 C41 C43' 99.5(10) . . . . ?
C26 C25 C41 C43' -79.1(10) . . . . ?
C24 C25 C41 C43 -69.3(8) . . . . ?
C26 C25 C41 C43 112.2(8) . . . . ?
C24 C25 C41 C42 165.8(7) . . . . ?
C26 C25 C41 C42 -12.7(9) . . . . ?
C24 C25 C41 C42' -24.8(10) . . . . ?
C26 C25 C41 C42' 156.6(9) . . . . ?
C24 C25 C41 C44' -140.1(9) . . . . ?
C26 C25 C41 C44' 41.3(10) . . . . ?
C24 C25 C41 C44 47.8(8) . . . . ?
C26 C25 C41 C44 -130.7(7) . . . . ?
C7 O7 C45 C46' 176.1(9) . . . . ?
C7 O7 C45 C46 112.0(8) . . . . ?
O7 C45 C46 O47 -34.4(15) . . . . ?
O7 C45 C46 O48 147.0(9) . . . . ?
O7 C45 C46' O47' -174(2) . . . . ?
O7 C45 C46' O48' 18.3(19) . . . . ?
C14 O14 C49 C50 -73.2(8) . . . . ?
O14 C49 C50 O50 95.3(10) . . . . ?
O14 C49 C50 N50 -90.0(10) . . . . ?
O50 C50 N50 N51 -2(2) . . . . ?
C49 C50 N50 N51 -175.8(13) . . . . ?
C21 O21 C52 C53' -118.4(18) . . . . ?
C21 O21 C52 C53 179.5(7) . . . . ?
O21 C52 C53 O54 168.5(12) . . . . ?
O21 C52 C53 O55 -3.4(14) . . . . ?
O21 C52 C53' O54' -148(3) . . . . ?
O21 C52 C53' O55' 36(2) . . . . ?
C28 O28 C56 C57 176.4(5) . . . . ?
O28 C56 C57 O57 -178.6(6) . . . . ?
O28 C56 C57 N57 1.8(8) . . . . ?
O57 C57 N57 N58 8.1(12) . . . . ?
C56 C57 N57 N58 -172.4(8) . . . . ?

_refine_diff_density_max         0.545
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.078


# start Validation Reply Form
_vrf_PUBL008_GLOBAL              
;
PROBLEM: _publ_section_title is missing. Title of paper.
RESPONSE: ...
;
_vrf_PUBL009_GLOBAL              
;
PROBLEM: _publ_author_name is missing. List of author(s) name(s).
RESPONSE: ...
;
_vrf_PUBL010_GLOBAL              
;
PROBLEM: _publ_author_address is missing. Author(s) address(es).
RESPONSE: ...
;
_vrf_PLAT026_I                   
;
PROBLEM: Ratio Observed / Unique Reflections too Low ....         29 %     
RESPONSE: ...
;
_vrf_PLAT413_I                   
;
PROBLEM: Short Inter XH3 .. XHn     H38A   ..  H92A    ..       1.75 Ang.  
RESPONSE: ...
;
_vrf_PLAT414_I                   
;
PROBLEM: Short Intra D-H..H-X       H58B   ..  H32F    ..       1.79 Ang.  
RESPONSE: ...
;
_vrf_PLAT415_I                   
;
PROBLEM: Short Inter D-H..H-X       H48    ..  H92B    ..       1.32 Ang.  
RESPONSE: ...
;
_vrf_PLAT601_I                   
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        347 Ang3  
RESPONSE: ...
;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMSO'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_sample_4_af
_database_code_depnum_ccdc_archive 'CCDC 1437364'
_audit_update_record             
;
2015-11-17 deposited with the CCDC.
2016-02-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'5,11,17,23-Tetra-tert-butyl-25,27-di[(hydrazinocarbonyl)methoxy]-26,28-di[(hydroxycarbonyl)methoxy]- 2,8,14,20-tetrathiacalix[4]arene'
_chemical_name_common            ?
_chemical_melting_point          545
_chemical_formula_moiety         'C48 H60 N4 O10 S4, 2(H4 N2)'
_chemical_formula_sum            'C48 H68 N8 O10 S4'
_chemical_formula_weight         1045.34

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 Tabl.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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   35.723(8)
_cell_length_b                   13.121(3)
_cell_length_c                   25.422(6)
_cell_angle_alpha                90
_cell_angle_beta                 108.104(3)
_cell_angle_gamma                90
_cell_volume                     11326(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2427
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      18.20

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_F_000             4448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    0.226
_shelx_estimated_absorpt_T_min   0.913
_shelx_estimated_absorpt_T_max   0.971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_process_details   
;
 G.M. Sheldrick (1998a). SADABS v.2.01, Bruker.
 Siemens Area Detector Absorption Correction Program.
 Bruker AXS. Madison. Wisconsin. USA

 The maximum experimental transmission factor Tmax is equal to the 
 one estimated by SHELX. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_number            13275
_diffrn_reflns_av_unetI/netI     0.3002
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.376
_diffrn_reflns_theta_max         27.990
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             13275
_reflns_number_gt                3458
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1389P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13275
_refine_ls_number_parameters     650
_refine_ls_number_restraints     121
_refine_ls_R_factor_all          0.2839
_refine_ls_R_factor_gt           0.0952
_refine_ls_wR_factor_ref         0.2684
_refine_ls_wR_factor_gt          0.2080
_refine_ls_goodness_of_fit_ref   0.751
_refine_ls_restrained_S_all      0.763
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.05932(4) 1.08702(12) 0.32098(7) 0.0496(4) Uani 1 1 d . . . . .
C2 C 0.08084(14) 1.1524(4) 0.2774(2) 0.0414(14) Uani 1 1 d . . . . .
C3 C 0.05585(15) 1.2088(4) 0.2349(2) 0.0444(15) Uani 1 1 d . . . . .
H3 H 0.0288 1.1997 0.2265 0.053 Uiso 1 1 calc R U . . .
C4 C 0.06969(15) 1.2784(5) 0.2043(2) 0.0473(15) Uani 1 1 d . U . . .
C5 C 0.10945(16) 1.2794(5) 0.2132(3) 0.0534(17) Uani 1 1 d . . . . .
H5 H 0.1196 1.3202 0.1909 0.064 Uiso 1 1 calc R U . . .
C6 C 0.13526(14) 1.2210(4) 0.2546(2) 0.0432(15) Uani 1 1 d . . . . .
C7 C 0.12109(14) 1.1618(4) 0.2880(2) 0.0352(13) Uani 1 1 d . . . . .
O7 O 0.14697(10) 1.1109(3) 0.33300(16) 0.0479(10) Uani 1 1 d . . . . .
S8 S 0.18621(4) 1.24623(12) 0.26757(7) 0.0519(5) Uani 1 1 d . . . . .
C9 C 0.20866(14) 1.1273(4) 0.2729(3) 0.0463(15) Uani 1 1 d . . . . .
C10 C 0.24142(16) 1.1077(5) 0.3194(2) 0.0528(17) Uani 1 1 d . . . . .
H10 H 0.2484 1.1562 0.3475 0.063 Uiso 1 1 calc R U . . .
C11 C 0.26343(15) 1.0216(5) 0.3256(3) 0.0462(15) Uani 1 1 d . . . . .
C12 C 0.25131(15) 0.9468(5) 0.2859(3) 0.0516(16) Uani 1 1 d . . . . .
H12 H 0.2643 0.8845 0.2912 0.062 Uiso 1 1 calc R U . . .
C13 C 0.21934(15) 0.9635(5) 0.2372(2) 0.0456(15) Uani 1 1 d . . . . .
C14 C 0.19894(14) 1.0536(5) 0.2314(2) 0.0436(15) Uani 1 1 d . . . . .
O14 O 0.16797(10) 1.0703(3) 0.18288(16) 0.0546(11) Uani 1 1 d . . . . .
C16 C 0.16096(15) 0.8344(5) 0.1686(2) 0.0488(16) Uani 1 1 d . . . . .
C17 C 0.14043(16) 0.8340(5) 0.1105(3) 0.0509(16) Uani 1 1 d . . . . .
H17 H 0.1526 0.8582 0.0856 0.061 Uiso 1 1 calc R U . . .
C18 C 0.10192(17) 0.7970(5) 0.0916(2) 0.0555(17) Uani 1 1 d . . . . .
C19 C 0.08460(16) 0.7671(5) 0.1306(2) 0.0486(16) Uani 1 1 d . . . . .
H19 H 0.0584 0.7462 0.1188 0.058 Uiso 1 1 calc R U . . .
C20 C 0.10495(16) 0.7672(4) 0.1873(2) 0.0471(15) Uani 1 1 d . . . . .
C21 C 0.14406(16) 0.7985(5) 0.2045(2) 0.0452(15) Uani 1 1 d . . . . .
O21 O 0.16529(11) 0.7873(4) 0.26120(16) 0.0628(12) Uani 1 1 d . . . . .
S22 S 0.08015(5) 0.71064(13) 0.22987(7) 0.0557(5) Uani 1 1 d . . . . .
C23 C 0.08037(15) 0.7942(5) 0.2843(2) 0.0455(15) Uani 1 1 d . . . . .
C24 C 0.07979(15) 0.7501(5) 0.3330(2) 0.0459(15) Uani 1 1 d . . . . .
H24 H 0.0834 0.6800 0.3368 0.055 Uiso 1 1 calc R U . . .
C25 C 0.07434(15) 0.8028(5) 0.3755(2) 0.0433(15) Uani 1 1 d . . . . .
C26 C 0.07131(14) 0.9057(5) 0.3712(2) 0.0450(15) Uani 1 1 d . . . . .
H26 H 0.0691 0.9438 0.4010 0.054 Uiso 1 1 calc R U . . .
C27 C 0.07144(13) 0.9560(4) 0.3217(2) 0.0401(14) Uani 1 1 d . . . . .
C28 C 0.07526(14) 0.8996(5) 0.2789(2) 0.0401(14) Uani 1 1 d . . . . .
O28 O 0.07553(9) 0.9484(3) 0.23105(14) 0.0422(10) Uani 1 1 d . . . . .
C29 C 0.04180(18) 1.3482(5) 0.1619(3) 0.071(2) Uani 1 1 d . U . . .
C30 C 0.0003(2) 1.3098(7) 0.1428(3) 0.104(3) Uani 1 1 d . U . . .
H30A H -0.0087 1.2988 0.1742 0.156 Uiso 1 1 calc R U . . .
H30B H -0.0163 1.3592 0.1187 0.156 Uiso 1 1 calc R U . . .
H30C H -0.0008 1.2468 0.1232 0.156 Uiso 1 1 calc R U . . .
C31 C 0.0441(3) 1.4521(7) 0.1888(5) 0.165(5) Uani 1 1 d . U . . .
H31A H 0.0359 1.4467 0.2212 0.248 Uiso 1 1 calc R U . . .
H31B H 0.0707 1.4766 0.1989 0.248 Uiso 1 1 calc R U . . .
H31C H 0.0271 1.4987 0.1631 0.248 Uiso 1 1 calc R U . . .
C32 C 0.0550(3) 1.3647(9) 0.1124(4) 0.154(4) Uani 1 1 d . U . . .
H32A H 0.0816 1.3894 0.1239 0.231 Uiso 1 1 calc R U . . .
H32B H 0.0537 1.3015 0.0929 0.231 Uiso 1 1 calc R U . . .
H32C H 0.0381 1.4139 0.0884 0.231 Uiso 1 1 calc R U . . .
C33 C 0.29974(17) 1.0047(6) 0.3759(3) 0.072(2) Uani 1 1 d . U . . .
C34 C 0.3054(2) 1.0922(7) 0.4172(3) 0.107(3) Uani 1 1 d . U . . .
H34A H 0.2827 1.0974 0.4295 0.161 Uiso 1 1 calc R U . . .
H34B H 0.3283 1.0794 0.4484 0.161 Uiso 1 1 calc R U . . .
H34C H 0.3089 1.1548 0.3997 0.161 Uiso 1 1 calc R U . . .
C35 C 0.3350(2) 0.9971(9) 0.3571(4) 0.144(4) Uani 1 1 d . U . . .
H35A H 0.3376 1.0584 0.3379 0.216 Uiso 1 1 calc R U . . .
H35B H 0.3580 0.9882 0.3886 0.216 Uiso 1 1 calc R U . . .
H35C H 0.3322 0.9399 0.3327 0.216 Uiso 1 1 calc R U . . .
C36 C 0.2937(3) 0.9105(7) 0.4066(4) 0.132(4) Uani 1 1 d . U . . .
H36A H 0.2706 0.9190 0.4178 0.198 Uiso 1 1 calc R U . . .
H36B H 0.2904 0.8523 0.3827 0.198 Uiso 1 1 calc R U . . .
H36C H 0.3162 0.9005 0.4387 0.198 Uiso 1 1 calc R U . . .
C37 C 0.0801(2) 0.7867(7) 0.0302(3) 0.079(2) Uani 1 1 d . U . . .
C38 C 0.1044(3) 0.8229(11) -0.0039(3) 0.165(5) Uani 1 1 d . U . . .
H38A H 0.1287 0.7856 0.0057 0.248 Uiso 1 1 calc R U . . .
H38B H 0.0903 0.8124 -0.0424 0.248 Uiso 1 1 calc R U . . .
H38C H 0.1099 0.8942 0.0027 0.248 Uiso 1 1 calc R U . . .
C39 C 0.0714(3) 0.6746(9) 0.0178(4) 0.150(4) Uani 1 1 d . U . . .
H39A H 0.0957 0.6372 0.0274 0.225 Uiso 1 1 calc R U . . .
H39B H 0.0554 0.6496 0.0391 0.225 Uiso 1 1 calc R U . . .
H39C H 0.0577 0.6660 -0.0209 0.225 Uiso 1 1 calc R U . . .
C40 C 0.0426(3) 0.8441(9) 0.0155(3) 0.144(4) Uani 1 1 d . U . . .
H40A H 0.0269 0.8204 0.0377 0.216 Uiso 1 1 calc R U . . .
H40B H 0.0480 0.9154 0.0221 0.216 Uiso 1 1 calc R U . . .
H40C H 0.0284 0.8335 -0.0229 0.216 Uiso 1 1 calc R U . . .
C41 C 0.07133(18) 0.7457(5) 0.4269(3) 0.0578(17) Uani 1 1 d . . . . .
C42 C 0.1120(2) 0.6928(8) 0.4567(4) 0.122(4) Uani 1 1 d . . . . .
H42A H 0.1095 0.6518 0.4868 0.183 Uiso 1 1 calc R U . . .
H42B H 0.1318 0.7439 0.4708 0.183 Uiso 1 1 calc R U . . .
H42C H 0.1193 0.6503 0.4308 0.183 Uiso 1 1 calc R U . . .
C43 C 0.0395(3) 0.6691(7) 0.4103(4) 0.109(3) Uani 1 1 d . . . . .
H43A H 0.0349 0.6416 0.4427 0.164 Uiso 1 1 calc R U . . .
H43B H 0.0471 0.6152 0.3901 0.164 Uiso 1 1 calc R U . . .
H43C H 0.0159 0.7007 0.3872 0.164 Uiso 1 1 calc R U . . .
C44 C 0.0617(3) 0.8165(7) 0.4669(3) 0.101(3) Uani 1 1 d . . . . .
H44A H 0.0367 0.8482 0.4495 0.151 Uiso 1 1 calc R U . . .
H44B H 0.0817 0.8680 0.4782 0.151 Uiso 1 1 calc R U . . .
H44C H 0.0605 0.7788 0.4988 0.151 Uiso 1 1 calc R U . . .
C45 C 0.1563(2) 1.1780(7) 0.3804(3) 0.083(2) Uani 1 1 d . . . . .
H45A H 0.1330 1.1855 0.3920 0.100 Uiso 1 1 calc R U . . .
H45B H 0.1627 1.2447 0.3691 0.100 Uiso 1 1 calc R U . . .
C46 C 0.1898(2) 1.1429(8) 0.4291(3) 0.079(2) Uani 1 1 d D . . . .
O46 O 0.20759(18) 1.0647(6) 0.4289(2) 0.112(2) Uani 1 1 d . . . . .
O47 O 0.19733(17) 1.2048(6) 0.4683(3) 0.125(2) Uani 1 1 d D . . . .
C48 C 0.17556(19) 1.1436(5) 0.1466(3) 0.0621(18) Uani 1 1 d D U . . .
H48A H 0.2013 1.1738 0.1637 0.075 Uiso 1 1 calc R U . . .
H48B H 0.1560 1.1974 0.1401 0.075 Uiso 1 1 calc R U . . .
C49 C 0.1745(2) 1.0971(6) 0.0934(3) 0.0713(19) Uani 1 1 d D U . . .
O49 O 0.1467(7) 1.049(3) 0.0616(10) 0.169(14) Uani 0.453(15) 1 d D U P A 1
N49 N 0.2018(4) 1.1330(16) 0.0742(6) 0.074(4) Uani 0.453(15) 1 d D U P A 1
H49 H 0.2168 1.1809 0.0923 0.089 Uiso 0.453(15) 1 calc R U P A 1
N50 N 0.2080(7) 1.098(2) 0.0259(8) 0.115(6) Uani 0.453(15) 1 d D U P A 1
O49' O 0.1430(4) 1.0551(11) 0.0639(6) 0.079(5) Uani 0.547(15) 1 d D U P A 2
N49' N 0.2062(3) 1.0808(14) 0.0823(6) 0.074(4) Uani 0.547(15) 1 d D U P A 2
H49' H 0.2278 1.1049 0.1042 0.089 Uiso 0.547(15) 1 calc R U P A 2
N50' N 0.2075(5) 1.0252(18) 0.0360(7) 0.115(6) Uani 0.547(15) 1 d D U P A 2
C51 C 0.1820(2) 0.6846(7) 0.2683(3) 0.089(3) Uani 1 1 d . . . . .
H51A H 0.1958 0.6738 0.2414 0.107 Uiso 1 1 calc R U . . .
H51B H 0.1607 0.6354 0.2608 0.107 Uiso 1 1 calc R U . . .
C52 C 0.2102(2) 0.6658(9) 0.3260(4) 0.092(3) Uani 1 1 d D . . . .
O52 O 0.21798(19) 0.5770(6) 0.3386(3) 0.126(2) Uani 1 1 d . . . . .
O53 O 0.22407(19) 0.7399(6) 0.3543(3) 0.124(2) Uani 1 1 d D . . . .
C54 C 0.03645(15) 0.9537(5) 0.1909(2) 0.0493(16) Uani 1 1 d . . . . .
H54A H 0.0188 0.9896 0.2068 0.059 Uiso 1 1 calc R U . . .
H54B H 0.0262 0.8854 0.1812 0.059 Uiso 1 1 calc R U . . .
C55 C 0.03849(17) 1.0070(5) 0.1414(3) 0.0552(18) Uani 1 1 d . . . . .
O55 O 0.00761(12) 1.0195(4) 0.10255(19) 0.0885(17) Uani 1 1 d . . . . .
N55 N 0.07203(15) 1.0424(5) 0.1396(2) 0.0670(16) Uani 1 1 d . . . . .
H55 H 0.0930 1.0280 0.1661 0.080 Uiso 1 1 calc R U . . .
N75 N 0.1851(2) 0.9150(6) 0.3567(3) 0.107(2) Uani 1 1 d D . . . .
N76 N 0.1658(2) 0.8636(7) 0.3895(4) 0.145(3) Uani 1 1 d D . . . .
N56 N 0.07508(18) 1.1027(5) 0.0962(3) 0.094(2) Uani 1 1 d . . . . .
N80 N 0.2301(2) 0.3868(9) 0.4586(4) 0.158(4) Uani 1 1 d . . . . .
N81 N 0.2466(3) 0.3546(11) 0.4175(4) 0.184(5) Uani 1 1 d . . . . .
S15 S 0.21127(4) 0.86886(14) 0.18611(7) 0.0625(5) Uani 1 1 d . . . . .
H56A H 0.0511 1.1092 0.0716 0.094 Uiso 1 1 d . U . . .
H56B H 0.0903 1.0689 0.0791 0.094 Uiso 1 1 d . U . . .
H50A H 0.1849 1.0734 0.0032 0.094 Uiso 0.453(15) 1 d . U P A 1
H50B H 0.2254 1.0477 0.0340 0.094 Uiso 0.453(15) 1 d . U P A 1
H50E H 0.2197 1.0631 0.0168 0.094 Uiso 0.547(15) 1 d . U P A 2
H50F H 0.1820 1.0179 0.0134 0.094 Uiso 0.547(15) 1 d . U P A 2
H75A H 0.1961 0.9707 0.3734 0.094 Uiso 1 1 d . U . . .
H75C H 0.2039 0.8728 0.3522 0.094 Uiso 1 1 d . U . . .
H76A H 0.1635 0.9069 0.4169 0.094 Uiso 1 1 d . U . . .
H76B H 0.1826 0.8121 0.4100 0.094 Uiso 1 1 d . U . . .
H80A H 0.2496 0.3841 0.4917 0.094 Uiso 1 1 d . U . . .
H80B H 0.2126 0.3369 0.4605 0.094 Uiso 1 1 d . U . . .
H81A H 0.2656 0.4025 0.4183 0.094 Uiso 1 1 d . U . . .
H81B H 0.2274 0.3648 0.3847 0.094 Uiso 1 1 d . U . . .
H647 H 0.2106 1.1739 0.4974 0.094 Uiso 1 1 d . U . . .
H653 H 0.2354 0.7192 0.3888 0.094 Uiso 1 1 d . U . . .


_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
S1 C2 1.756(6) . ?
S1 C27 1.771(6) . ?
C2 C7 1.383(7) . ?
C2 C3 1.383(7) . ?
C3 C4 1.387(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.367(7) . ?
C4 C29 1.525(8) . ?
C5 C6 1.394(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.360(7) . ?
C6 S8 1.777(5) . ?
C7 O7 1.397(6) . ?
O7 C45 1.445(8) . ?
S8 C9 1.740(6) . ?
C9 C14 1.393(8) . ?
C9 C10 1.406(7) . ?
C10 C11 1.357(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.377(8) . ?
C11 C33 1.528(7) . ?
C12 C13 1.416(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.373(8) . ?
C13 S15 1.755(6) . ?
C14 O14 1.395(6) . ?
O14 C48 1.415(7) . ?
C16 C21 1.328(8) . ?
C16 C17 1.430(8) . ?
C16 S15 1.771(6) . ?
C17 C18 1.396(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.380(8) . ?
C18 C37 1.517(8) . ?
C19 C20 1.398(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.390(7) . ?
C20 S22 1.761(6) . ?
C21 O21 1.412(6) . ?
O21 C51 1.461(9) . ?
S22 C23 1.764(6) . ?
C23 C24 1.372(8) . ?
C23 C28 1.396(8) . ?
C24 C25 1.347(8) . ?
C24 H24 0.9300 . ?
C25 C26 1.356(8) . ?
C25 C41 1.538(8) . ?
C26 C27 1.422(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.358(7) . ?
C28 O28 1.377(6) . ?
O28 C54 1.453(5) . ?
C29 C32 1.491(11) . ?
C29 C30 1.497(9) . ?
C29 C31 1.515(11) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C35 1.483(10) . ?
C33 C36 1.513(11) . ?
C33 C34 1.526(10) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 C40 1.481(10) . ?
C37 C38 1.483(12) . ?
C37 C39 1.517(12) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 C43 1.478(10) . ?
C41 C44 1.495(9) . ?
C41 C42 1.575(9) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 C46 1.503(10) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 O46 1.209(9) . ?
C46 O47 1.248(8) . ?
O47 H647 0.847(6) . ?
C48 C49 1.473(9) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C49 O49 1.242(13) . ?
C49 O49' 1.267(10) . ?
C49 N49' 1.268(11) . ?
C49 N49 1.309(12) . ?
N49 N50 1.393(14) . ?
N49 H49 0.8600 . ?
N50 H50A 0.90(2) . ?
N50 H50B 0.88(3) . ?
N49' N50' 1.399(12) . ?
N49' H49' 0.8600 . ?
N50' H50E 0.90(2) . ?
N50' H50F 0.920(19) . ?
C51 C52 1.521(11) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 O53 1.219(9) . ?
C52 O52 1.217(10) . ?
O53 H653 0.887(6) . ?
C54 C55 1.461(8) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C55 O55 1.242(6) . ?
C55 N55 1.299(7) . ?
N55 N56 1.388(7) . ?
N55 H55 0.8600 . ?
N75 N76 1.408(7) . ?
N75 H75A 0.875(8) . ?
N75 H75C 0.905(7) . ?
N76 H76A 0.921(9) . ?
N76 H76B 0.946(10) . ?
N56 H56A 0.895(6) . ?
N56 H56B 0.911(7) . ?
N80 N81 1.414(12) . ?
N80 H80A 0.910(7) . ?
N80 H80B 0.919(10) . ?
N81 H81A 0.920(11) . ?
N81 H81B 0.912(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
C2 S1 C27 109.1(3) . . ?
C7 C2 C3 119.0(5) . . ?
C7 C2 S1 123.5(4) . . ?
C3 C2 S1 116.8(4) . . ?
C2 C3 C4 122.3(5) . . ?
C2 C3 H3 118.8 . . ?
C4 C3 H3 118.8 . . ?
C5 C4 C3 116.6(5) . . ?
C5 C4 C29 121.9(6) . . ?
C3 C4 C29 121.5(5) . . ?
C4 C5 C6 121.9(5) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 H5 119.0 . . ?
C7 C6 C5 119.9(5) . . ?
C7 C6 S8 123.3(4) . . ?
C5 C6 S8 115.9(4) . . ?
C6 C7 C2 119.7(5) . . ?
C6 C7 O7 120.3(4) . . ?
C2 C7 O7 120.1(5) . . ?
C7 O7 C45 108.2(4) . . ?
C9 S8 C6 105.6(3) . . ?
C14 C9 C10 117.1(5) . . ?
C14 C9 S8 124.3(4) . . ?
C10 C9 S8 118.2(5) . . ?
C11 C10 C9 123.4(6) . . ?
C11 C10 H10 118.3 . . ?
C9 C10 H10 118.3 . . ?
C10 C11 C12 118.0(5) . . ?
C10 C11 C33 121.9(6) . . ?
C12 C11 C33 120.1(5) . . ?
C11 C12 C13 121.0(5) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C14 C13 C12 118.9(5) . . ?
C14 C13 S15 124.8(4) . . ?
C12 C13 S15 116.1(5) . . ?
C13 C14 O14 118.6(5) . . ?
C13 C14 C9 121.2(5) . . ?
O14 C14 C9 120.2(5) . . ?
C14 O14 C48 115.0(4) . . ?
C21 C16 C17 120.8(5) . . ?
C21 C16 S15 124.1(4) . . ?
C17 C16 S15 114.5(5) . . ?
C18 C17 C16 119.4(6) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C19 C18 C17 117.7(5) . . ?
C19 C18 C37 120.8(6) . . ?
C17 C18 C37 121.4(6) . . ?
C18 C19 C20 122.4(5) . . ?
C18 C19 H19 118.8 . . ?
C20 C19 H19 118.8 . . ?
C21 C20 C19 118.3(6) . . ?
C21 C20 S22 125.4(5) . . ?
C19 C20 S22 115.7(4) . . ?
C16 C21 C20 121.0(5) . . ?
C16 C21 O21 121.6(5) . . ?
C20 C21 O21 117.3(5) . . ?
C21 O21 C51 106.9(5) . . ?
C20 S22 C23 109.8(3) . . ?
C24 C23 C28 118.0(6) . . ?
C24 C23 S22 116.6(5) . . ?
C28 C23 S22 124.7(5) . . ?
C25 C24 C23 123.6(6) . . ?
C25 C24 H24 118.2 . . ?
C23 C24 H24 118.2 . . ?
C24 C25 C26 118.3(6) . . ?
C24 C25 C41 119.8(6) . . ?
C26 C25 C41 121.9(6) . . ?
C25 C26 C27 120.7(6) . . ?
C25 C26 H26 119.6 . . ?
C27 C26 H26 119.6 . . ?
C28 C27 C26 119.0(6) . . ?
C28 C27 S1 127.3(5) . . ?
C26 C27 S1 113.1(5) . . ?
C27 C28 O28 119.0(6) . . ?
C27 C28 C23 120.2(5) . . ?
O28 C28 C23 120.7(5) . . ?
C28 O28 C54 112.0(4) . . ?
C32 C29 C30 108.3(7) . . ?
C32 C29 C31 105.2(8) . . ?
C30 C29 C31 111.0(7) . . ?
C32 C29 C4 112.0(6) . . ?
C30 C29 C4 113.0(6) . . ?
C31 C29 C4 106.9(6) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C35 C33 C36 112.6(8) . . ?
C35 C33 C11 109.0(6) . . ?
C36 C33 C11 109.2(6) . . ?
C35 C33 C34 109.1(7) . . ?
C36 C33 C34 105.6(7) . . ?
C11 C33 C34 111.3(6) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C40 C37 C38 109.7(8) . . ?
C40 C37 C18 110.5(6) . . ?
C38 C37 C18 111.5(6) . . ?
C40 C37 C39 109.2(8) . . ?
C38 C37 C39 107.9(8) . . ?
C18 C37 C39 107.8(7) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C43 C41 C44 107.3(7) . . ?
C43 C41 C25 109.8(6) . . ?
C44 C41 C25 111.6(6) . . ?
C43 C41 C42 110.4(7) . . ?
C44 C41 C42 108.6(7) . . ?
C25 C41 C42 109.1(5) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O7 C45 C46 114.7(6) . . ?
O7 C45 H45A 108.6 . . ?
C46 C45 H45A 108.6 . . ?
O7 C45 H45B 108.6 . . ?
C46 C45 H45B 108.6 . . ?
H45A C45 H45B 107.6 . . ?
O46 C46 O47 124.9(8) . . ?
O46 C46 C45 122.8(8) . . ?
O47 C46 C45 112.3(8) . . ?
C46 O47 H647 108.1(8) . . ?
O14 C48 C49 111.1(6) . . ?
O14 C48 H48A 109.4 . . ?
C49 C48 H48A 109.4 . . ?
O14 C48 H48B 109.4 . . ?
C49 C48 H48B 109.4 . . ?
H48A C48 H48B 108.0 . . ?
O49' C49 N49' 118.9(11) . . ?
O49 C49 N49 118.5(15) . . ?
O49 C49 C48 126.8(14) . . ?
O49' C49 C48 119.3(10) . . ?
N49' C49 C48 120.3(8) . . ?
N49 C49 C48 112.6(10) . . ?
C49 N49 N50 123.4(15) . . ?
C49 N49 H49 118.3 . . ?
N50 N49 H49 118.3 . . ?
N49 N50 H50A 108.4(17) . . ?
N49 N50 H50B 109(2) . . ?
H50A N50 H50B 109(3) . . ?
C49 N49' N50' 122.8(13) . . ?
C49 N49' H49' 118.6 . . ?
N50' N49' H49' 118.6 . . ?
N49' N50' H50E 108.4(15) . . ?
N49' N50' H50F 107.0(14) . . ?
H50E N50' H50F 106(2) . . ?
O21 C51 C52 113.1(7) . . ?
O21 C51 H51A 109.0 . . ?
C52 C51 H51A 109.0 . . ?
O21 C51 H51B 109.0 . . ?
C52 C51 H51B 109.0 . . ?
H51A C51 H51B 107.8 . . ?
O53 C52 O52 126.1(9) . . ?
O53 C52 C51 117.8(9) . . ?
O52 C52 C51 116.0(9) . . ?
C52 O53 H653 108.5(8) . . ?
O28 C54 C55 109.5(4) . . ?
O28 C54 H54A 109.8 . . ?
C55 C54 H54A 109.8 . . ?
O28 C54 H54B 109.8 . . ?
C55 C54 H54B 109.8 . . ?
H54A C54 H54B 108.2 . . ?
O55 C55 N55 121.7(6) . . ?
O55 C55 C54 118.6(6) . . ?
N55 C55 C54 119.7(5) . . ?
C55 N55 N56 122.2(5) . . ?
C55 N55 H55 118.9 . . ?
N56 N55 H55 118.9 . . ?
N76 N75 H75A 109.9(8) . . ?
N76 N75 H75C 107.6(8) . . ?
H75A N75 H75C 109.5(7) . . ?
N75 N76 H76A 109.0(8) . . ?
N75 N76 H76B 109.0(8) . . ?
H76A N76 H76B 102.2(9) . . ?
N55 N56 H56A 108.4(6) . . ?
N55 N56 H56B 107.9(6) . . ?
H56A N56 H56B 107.2(7) . . ?
N81 N80 H80A 107.1(8) . . ?
N81 N80 H80B 105.9(10) . . ?
H80A N80 H80B 105.3(10) . . ?
N80 N81 H81A 104.7(12) . . ?
N80 N81 H81B 105.2(9) . . ?
H81A N81 H81B 105.0(11) . . ?
C13 S15 C16 106.7(3) . . ?

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
C27 S1 C2 C7 -65.1(5) . . . . ?
C27 S1 C2 C3 124.3(5) . . . . ?
C7 C2 C3 C4 -3.3(9) . . . . ?
S1 C2 C3 C4 167.7(5) . . . . ?
C2 C3 C4 C5 8.3(9) . . . . ?
C2 C3 C4 C29 -173.1(6) . . . . ?
C3 C4 C5 C6 -6.2(9) . . . . ?
C29 C4 C5 C6 175.2(6) . . . . ?
C4 C5 C6 C7 -0.8(9) . . . . ?
C4 C5 C6 S8 -170.5(5) . . . . ?
C5 C6 C7 C2 6.1(9) . . . . ?
S8 C6 C7 C2 175.0(4) . . . . ?
C5 C6 C7 O7 -173.7(5) . . . . ?
S8 C6 C7 O7 -4.8(8) . . . . ?
C3 C2 C7 C6 -4.0(8) . . . . ?
S1 C2 C7 C6 -174.4(5) . . . . ?
C3 C2 C7 O7 175.8(5) . . . . ?
S1 C2 C7 O7 5.4(8) . . . . ?
C6 C7 O7 C45 88.7(6) . . . . ?
C2 C7 O7 C45 -91.1(6) . . . . ?
C7 C6 S8 C9 55.5(6) . . . . ?
C5 C6 S8 C9 -135.2(5) . . . . ?
C6 S8 C9 C14 58.1(5) . . . . ?
C6 S8 C9 C10 -128.8(5) . . . . ?
C14 C9 C10 C11 -0.2(8) . . . . ?
S8 C9 C10 C11 -173.8(5) . . . . ?
C9 C10 C11 C12 -4.7(9) . . . . ?
C9 C10 C11 C33 177.7(6) . . . . ?
C10 C11 C12 C13 6.6(9) . . . . ?
C33 C11 C12 C13 -175.8(6) . . . . ?
C11 C12 C13 C14 -3.7(9) . . . . ?
C11 C12 C13 S15 171.7(5) . . . . ?
C12 C13 C14 O14 178.8(5) . . . . ?
S15 C13 C14 O14 3.8(8) . . . . ?
C12 C13 C14 C9 -1.3(8) . . . . ?
S15 C13 C14 C9 -176.3(4) . . . . ?
C10 C9 C14 C13 3.2(8) . . . . ?
S8 C9 C14 C13 176.4(4) . . . . ?
C10 C9 C14 O14 -176.9(5) . . . . ?
S8 C9 C14 O14 -3.7(8) . . . . ?
C13 C14 O14 C48 -108.3(6) . . . . ?
C9 C14 O14 C48 71.8(7) . . . . ?
C21 C16 C17 C18 1.1(9) . . . . ?
S15 C16 C17 C18 172.8(5) . . . . ?
C16 C17 C18 C19 3.4(9) . . . . ?
C16 C17 C18 C37 -174.8(6) . . . . ?
C17 C18 C19 C20 -3.8(9) . . . . ?
C37 C18 C19 C20 174.4(6) . . . . ?
C18 C19 C20 C21 -0.1(9) . . . . ?
C18 C19 C20 S22 -171.8(5) . . . . ?
C17 C16 C21 C20 -5.3(9) . . . . ?
S15 C16 C21 C20 -176.2(5) . . . . ?
C17 C16 C21 O21 172.6(5) . . . . ?
S15 C16 C21 O21 1.7(9) . . . . ?
C19 C20 C21 C16 4.8(9) . . . . ?
S22 C20 C21 C16 175.5(5) . . . . ?
C19 C20 C21 O21 -173.1(5) . . . . ?
S22 C20 C21 O21 -2.4(8) . . . . ?
C16 C21 O21 C51 -90.3(7) . . . . ?
C20 C21 O21 C51 87.6(6) . . . . ?
C21 C20 S22 C23 59.8(6) . . . . ?
C19 C20 S22 C23 -129.3(5) . . . . ?
C20 S22 C23 C24 -150.4(4) . . . . ?
C20 S22 C23 C28 39.5(5) . . . . ?
C28 C23 C24 C25 0.4(8) . . . . ?
S22 C23 C24 C25 -170.4(4) . . . . ?
C23 C24 C25 C26 -3.6(8) . . . . ?
C23 C24 C25 C41 175.8(5) . . . . ?
C24 C25 C26 C27 3.8(7) . . . . ?
C41 C25 C26 C27 -175.6(5) . . . . ?
C25 C26 C27 C28 -1.0(7) . . . . ?
C25 C26 C27 S1 170.5(4) . . . . ?
C2 S1 C27 C28 -35.7(5) . . . . ?
C2 S1 C27 C26 153.7(4) . . . . ?
C26 C27 C28 O28 -179.8(4) . . . . ?
S1 C27 C28 O28 10.1(7) . . . . ?
C26 C27 C28 C23 -2.2(7) . . . . ?
S1 C27 C28 C23 -172.4(4) . . . . ?
C24 C23 C28 C27 2.5(7) . . . . ?
S22 C23 C28 C27 172.5(4) . . . . ?
C24 C23 C28 O28 -180.0(4) . . . . ?
S22 C23 C28 O28 -10.0(7) . . . . ?
C27 C28 O28 C54 -92.9(5) . . . . ?
C23 C28 O28 C54 89.5(6) . . . . ?
C5 C4 C29 C32 35.1(10) . . . . ?
C3 C4 C29 C32 -143.4(8) . . . . ?
C5 C4 C29 C30 157.8(7) . . . . ?
C3 C4 C29 C30 -20.7(10) . . . . ?
C5 C4 C29 C31 -79.7(9) . . . . ?
C3 C4 C29 C31 101.8(8) . . . . ?
C10 C11 C33 C35 -117.1(8) . . . . ?
C12 C11 C33 C35 65.3(9) . . . . ?
C10 C11 C33 C36 119.5(8) . . . . ?
C12 C11 C33 C36 -58.1(9) . . . . ?
C10 C11 C33 C34 3.3(9) . . . . ?
C12 C11 C33 C34 -174.3(6) . . . . ?
C19 C18 C37 C40 57.9(11) . . . . ?
C17 C18 C37 C40 -123.9(8) . . . . ?
C19 C18 C37 C38 -179.7(8) . . . . ?
C17 C18 C37 C38 -1.6(11) . . . . ?
C19 C18 C37 C39 -61.4(9) . . . . ?
C17 C18 C37 C39 116.7(8) . . . . ?
C24 C25 C41 C43 -56.0(8) . . . . ?
C26 C25 C41 C43 123.4(7) . . . . ?
C24 C25 C41 C44 -174.8(6) . . . . ?
C26 C25 C41 C44 4.6(8) . . . . ?
C24 C25 C41 C42 65.2(8) . . . . ?
C26 C25 C41 C42 -115.4(7) . . . . ?
C7 O7 C45 C46 -168.6(6) . . . . ?
O7 C45 C46 O46 -0.1(12) . . . . ?
O7 C45 C46 O47 178.1(7) . . . . ?
C14 O14 C48 C49 116.9(6) . . . . ?
O14 C48 C49 O49 56(2) . . . . ?
O14 C48 C49 O49' 60.4(11) . . . . ?
O14 C48 C49 N49' -105.4(12) . . . . ?
O14 C48 C49 N49 -140.6(11) . . . . ?
O49 C49 N49 N50 -18(3) . . . . ?
C48 C49 N49 N50 176.9(17) . . . . ?
O49' C49 N49' N50' 6(2) . . . . ?
C48 C49 N49' N50' 171.4(12) . . . . ?
C21 O21 C51 C52 172.4(6) . . . . ?
O21 C51 C52 O53 -19.0(12) . . . . ?
O21 C51 C52 O52 163.7(8) . . . . ?
C28 O28 C54 C55 179.4(5) . . . . ?
O28 C54 C55 O55 -179.4(6) . . . . ?
O28 C54 C55 N55 -1.4(8) . . . . ?
O55 C55 N55 N56 4.9(11) . . . . ?
C54 C55 N55 N56 -173.1(6) . . . . ?
C14 C13 S15 C16 -56.5(6) . . . . ?
C12 C13 S15 C16 128.4(5) . . . . ?
C21 C16 S15 C13 -58.5(6) . . . . ?
C17 C16 S15 C13 130.1(5) . . . . ?

_refine_diff_density_max         0.562
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.087


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: MeOH/CH2Cl2'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_sample_4b
_database_code_depnum_ccdc_archive 'CCDC 1437365'
_audit_update_record             
;
2015-11-17 deposited with the CCDC.
2016-02-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
25,27-Di[(hydrazinocarbonyl)methoxy]-26,28-di[(hydroxycarbonyl)methoxy]-2,8,14,20-tetrathiacalix[4]arene
_chemical_name_common            ?
_chemical_melting_point          560
_chemical_formula_moiety         'C32 H28 N4 O10 S4,  H4 N2, 4(H2 O)'
_chemical_formula_sum            'C32 H40 N6 O14 S4'
_chemical_formula_weight         860.94

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.3996(8)
_cell_length_b                   16.7027(13)
_cell_length_c                   21.9306(18)
_cell_angle_alpha                90
_cell_angle_beta                 90.2490(10)
_cell_angle_gamma                90
_cell_volume                     3809.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9178
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      28.04

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_F_000             1800
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.439
_exptl_crystal_size_mid          0.387
_exptl_crystal_size_min          0.246
_exptl_absorpt_coefficient_mu    0.325
_shelx_estimated_absorpt_T_min   0.871
_shelx_estimated_absorpt_T_max   0.924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_process_details   
;
 G.M. Sheldrick (1998a). SADABS v.2.01, Bruker.
 Siemens Area Detector Absorption Correction Program.
 Bruker AXS. Madison. Wisconsin. USA
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41221
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.222
_diffrn_reflns_theta_max         28.702
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measured_fraction_theta_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_point_group_measured_fraction_full 0.966
_reflns_number_total             9032
_reflns_number_gt                7845
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0574P)²+4.0746P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9032
_refine_ls_number_parameters     522
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0589
_refine_ls_wR_factor_ref         0.1503
_refine_ls_wR_factor_gt          0.1455
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.204
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C2 C 1.0301(2) 0.87300(15) 0.32445(11) 0.0325(5) Uani 1 1 d . . . . .
C3 C 1.0638(2) 0.94278(16) 0.29374(12) 0.0380(5) Uani 1 1 d . . . . .
H3 H 1.1048 0.9394 0.2562 0.046 Uiso 1 1 calc R U . . .
C4 C 1.0368(3) 1.01738(16) 0.31865(13) 0.0409(6) Uani 1 1 d . . . . .
H4 H 1.0637 1.0637 0.2989 0.049 Uiso 1 1 calc R U . . .
C5 C 0.9698(3) 1.02269(16) 0.37291(13) 0.0394(5) Uani 1 1 d . . . . .
H5 H 0.9488 1.0726 0.3888 0.047 Uiso 1 1 calc R U . . .
C6 C 0.9341(2) 0.95323(15) 0.40365(11) 0.0335(5) Uani 1 1 d . . . . .
C7 C 0.9685(2) 0.87836(15) 0.38134(11) 0.0323(5) Uani 1 1 d . . . . .
C9 C 0.7110(2) 0.91971(15) 0.47789(11) 0.0340(5) Uani 1 1 d . . . . .
C10 C 0.6718(3) 0.89670(18) 0.53633(12) 0.0442(6) Uani 1 1 d . . . . .
H10 H 0.7296 0.8990 0.5688 0.053 Uiso 1 1 calc R U . . .
C11 C 0.5475(3) 0.87067(19) 0.54587(13) 0.0505(7) Uani 1 1 d . . . . .
H11 H 0.5223 0.8549 0.5847 0.061 Uiso 1 1 calc R U . . .
C12 C 0.4606(3) 0.86784(18) 0.49853(14) 0.0470(6) Uani 1 1 d . . . . .
H12 H 0.3767 0.8511 0.5058 0.056 Uiso 1 1 calc R U . . .
C13 C 0.4966(2) 0.88970(15) 0.43983(12) 0.0357(5) Uani 1 1 d . . . . .
C14 C 0.6237(2) 0.91479(14) 0.42917(11) 0.0315(5) Uani 1 1 d . . . . .
C16 C 0.4334(2) 0.86260(16) 0.31493(12) 0.0374(5) Uani 1 1 d . . . . .
C17 C 0.4153(3) 0.9115(2) 0.26438(15) 0.0509(7) Uani 1 1 d . . . . .
H17 H 0.3797 0.9621 0.2694 0.061 Uiso 1 1 calc R U . . .
C18 C 0.4496(3) 0.8858(2) 0.20667(15) 0.0582(8) Uani 1 1 d . . . . .
H18 H 0.4351 0.9184 0.1730 0.070 Uiso 1 1 calc R U . . .
C19 C 0.5054(3) 0.8113(2) 0.19934(14) 0.0537(8) Uani 1 1 d . . . . .
H19 H 0.5285 0.7941 0.1606 0.064 Uiso 1 1 calc R U . . .
C20 C 0.5275(2) 0.76185(17) 0.24933(12) 0.0404(6) Uani 1 1 d . . . . .
C21 C 0.4868(2) 0.78609(16) 0.30771(12) 0.0364(5) Uani 1 1 d . . . . .
C23 C 0.7422(2) 0.66367(15) 0.27670(11) 0.0357(5) Uani 1 1 d . . . . .
C24 C 0.7692(3) 0.59528(16) 0.31094(13) 0.0440(6) Uani 1 1 d . . . . .
H24 H 0.7062 0.5563 0.3156 0.053 Uiso 1 1 calc R U . . .
C25 C 0.8879(3) 0.58459(16) 0.33799(13) 0.0464(6) Uani 1 1 d . . . . .
H25 H 0.9059 0.5377 0.3592 0.056 Uiso 1 1 calc R U . . .
C26 C 0.9800(3) 0.64386(16) 0.33338(12) 0.0420(6) Uani 1 1 d . . . . .
H26 H 1.0591 0.6374 0.3527 0.050 Uiso 1 1 calc R U . . .
C27 C 0.9553(2) 0.71328(14) 0.29998(11) 0.0337(5) Uani 1 1 d . . . . .
C28 C 0.8372(2) 0.72250(14) 0.27026(10) 0.0313(5) Uani 1 1 d . . . . .
C29 C 1.0563(3) 0.78967(19) 0.45225(15) 0.0498(7) Uani 1 1 d . . . . .
H291 H 1.0605 0.8255 0.4870 0.060 Uiso 1 1 calc R U . . .
H292 H 1.1335 0.7977 0.4283 0.060 Uiso 1 1 calc R U . . .
C30 C 1.0533(3) 0.70407(19) 0.47487(13) 0.0475(7) Uani 1 1 d . . . . .
C32 C 0.6451(3) 1.01505(15) 0.35455(12) 0.0370(5) Uani 1 1 d . . . . .
H321 H 0.6838 1.0489 0.3855 0.044 Uiso 1 1 calc R U . . .
H322 H 0.5538 1.0270 0.3529 0.044 Uiso 1 1 calc R U . . .
C33 C 0.7051(2) 1.03297(15) 0.29338(11) 0.0348(5) Uani 1 1 d . . . . .
C35 C 0.3971(3) 0.67935(19) 0.36176(15) 0.0500(7) Uani 1 1 d . . . . .
H35A H 0.3649 0.6665 0.3213 0.060 Uiso 1 1 calc R U . . .
H35B H 0.3274 0.7031 0.3847 0.060 Uiso 1 1 calc R U . . .
C36 C 0.4404(3) 0.6043(2) 0.39273(13) 0.0512(7) Uani 1 1 d . . . . .
C38 C 0.8121(3) 0.7796(2) 0.17190(13) 0.0535(7) Uani 1 1 d . . . . .
H381 H 0.7572 0.8198 0.1532 0.064 Uiso 1 1 calc R U . . .
H382 H 0.7765 0.7274 0.1625 0.064 Uiso 1 1 calc R U . . .
C39 C 0.9459(3) 0.78590(18) 0.14543(13) 0.0467(6) Uani 1 1 d . . . . .
N33 N 0.7455(2) 0.97071(13) 0.25998(10) 0.0371(4) Uani 1 1 d D . . . .
N34 N 0.8084(2) 0.98398(15) 0.20360(10) 0.0443(5) Uani 1 1 d D . . . .
N39 N 0.9904(3) 0.86033(15) 0.14644(12) 0.0533(6) Uani 1 1 d D . . . .
N40 N 1.1178(3) 0.87982(17) 0.12908(17) 0.0719(10) Uani 1 1 d D . . . .
O7 O 0.94513(16) 0.81018(11) 0.41533(8) 0.0368(4) Uani 1 1 d . . . . .
O14 O 0.66286(16) 0.93279(10) 0.37081(7) 0.0336(4) Uani 1 1 d . . . . .
O20 O 0.50144(17) 0.73638(11) 0.35678(9) 0.0404(4) Uani 1 1 d . . . . .
O28 O 0.81362(18) 0.79097(11) 0.23701(8) 0.0388(4) Uani 1 1 d . . . . .
O30 O 0.9507(2) 0.66656(15) 0.47660(11) 0.0630(6) Uani 1 1 d D . . . .
H30 H 0.8935 0.6960 0.4892 0.095 Uiso 1 1 calc DR U . . .
O31 O 1.1583(3) 0.67635(18) 0.49123(14) 0.0768(8) Uani 1 1 d . . . . .
O33 O 0.7132(2) 1.10239(12) 0.27611(9) 0.0491(5) Uani 1 1 d . . . . .
O36 O 0.5489(3) 0.60198(16) 0.41748(13) 0.0737(8) Uani 1 1 d D . . . .
H36 H 0.5688 0.6470 0.4291 0.111 Uiso 1 1 calc DR U . . .
O37 O 0.3644(3) 0.54727(17) 0.39236(13) 0.0828(9) Uani 1 1 d . . . . .
O39 O 1.0039(3) 0.72844(14) 0.12634(14) 0.0696(7) Uani 1 1 d . . . . .
S1 S 1.08438(6) 0.78201(4) 0.29188(3) 0.04086(16) Uani 1 1 d . . . . .
S8 S 0.86336(6) 0.96644(5) 0.47644(3) 0.04415(17) Uani 1 1 d . . . . .
S15 S 0.37069(6) 0.89601(5) 0.38532(3) 0.04464(17) Uani 1 1 d . . . . .
S22 S 0.59151(7) 0.66428(5) 0.23782(4) 0.04942(19) Uani 1 1 d . . . . .
H33 H 0.740(3) 0.9190(12) 0.2719(16) 0.059 Uiso 1 1 d D U . . .
H39 H 0.947(3) 0.9031(16) 0.1635(16) 0.059 Uiso 1 1 d D U . . .
H341 H 0.7492 1.0018 0.1765 0.051(9) Uiso 1 1 d D . . . .
H342 H 0.8714 1.0230 0.2114 0.066(11) Uiso 1 1 d D . . . .
H401 H 1.1252 0.8733 0.0879 0.15(3) Uiso 1 1 d D . . . .
H402 H 1.1729 0.8440 0.1481 0.14(3) Uiso 1 1 d D . . . .
H702 H 0.6949 0.7548 0.4661 0.216 Uiso 1 1 d . U . . .
O80A O 0.6565(7) 0.4782(4) 0.4657(4) 0.158(3) Uani 0.572(4) 1 d D . P A 1
O80B O 0.7648(11) 0.4979(4) 0.4813(5) 0.158(3) Uani 0.428(4) 1 d D . P A 2
H801 H 0.5807 0.4395 0.4807 0.237 Uiso 0.572(4) 1 d D U P A 1
H802 H 0.6805 0.4604 0.4250 0.237 Uiso 0.572(4) 1 d D U P A 1
H804 H 0.7905 0.4446 0.4945 0.237 Uiso 0.428(4) 1 d D U P A 2
H803 H 0.7192 0.4784 0.4438 0.237 Uiso 0.428(4) 1 d D U P A 2
O90A O 1.0864(8) 0.9929(5) 0.0014(3) 0.133(2) Uani 0.572(4) 1 d D . P A 1
O90B O 1.1184(10) 1.0098(6) -0.0551(5) 0.133(2) Uani 0.428(4) 1 d D . P A 2
H901 H 1.0660 0.9388 -0.0042 0.199 Uiso 0.572(4) 1 d D U P A 1
H902 H 1.1611 1.0136 -0.0178 0.199 Uiso 0.572(4) 1 d D U P A 1
H903 H 1.1792 1.0482 -0.0317 0.199 Uiso 0.428(4) 1 d D U P A 2
H904 H 1.0258 1.0201 -0.0515 0.199 Uiso 0.428(4) 1 d D U P A 2
O60 O 0.3903(3) 0.68300(17) 0.55036(13) 0.0738(7) Uani 1 1 d D . . . .
H601 H 0.3327 0.6967 0.5182 0.111 Uiso 1 1 d D U . . .
H602 H 0.3612 0.7233 0.5761 0.111 Uiso 1 1 d D U . . .
O65 O 0.2720(3) 0.79350(16) 0.62393(14) 0.0729(7) Uani 1 1 d D . . . .
H651 H 0.1845 0.7832 0.6241 0.109 Uiso 1 1 d D U . . .
H652 H 0.2718 0.8123 0.6636 0.109 Uiso 1 1 d D U . . .
N70 N 0.7083(3) 0.71290(18) 0.46466(18) 0.0723(9) Uani 1 1 d D . . . .
N71 N 0.6810(4) 0.6877(2) 0.52546(18) 0.0855(10) Uani 1 1 d D . . . .
H701 H 0.6735 0.6912 0.4293 0.128 Uiso 1 1 d D U . . .
H711 H 0.7075 0.6384 0.5310 0.128 Uiso 1 1 d D U . . .
H712 H 0.5944 0.6901 0.5302 0.128 Uiso 1 1 d D U . . .


_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 C3 1.392(4) . ?
C2 C7 1.408(3) . ?
C2 S1 1.773(3) . ?
C3 C4 1.390(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.384(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.393(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.390(4) . ?
C6 S8 1.774(2) . ?
C7 O7 1.383(3) . ?
C9 C10 1.400(3) . ?
C9 C14 1.401(3) . ?
C9 S8 1.767(3) . ?
C10 C11 1.381(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.374(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.391(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.408(3) . ?
C13 S15 1.772(3) . ?
C14 O14 1.378(3) . ?
C16 C17 1.389(4) . ?
C16 C21 1.403(4) . ?
C16 S15 1.769(3) . ?
C17 C18 1.385(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.382(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.391(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.410(4) . ?
C20 S22 1.779(3) . ?
C21 O20 1.367(3) . ?
C23 C24 1.395(4) . ?
C23 C28 1.401(3) . ?
C23 S22 1.781(3) . ?
C24 C25 1.379(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.381(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.395(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.397(3) . ?
C27 S1 1.776(3) . ?
C28 O28 1.378(3) . ?
C29 O7 1.450(3) . ?
C29 C30 1.514(4) . ?
C29 H291 0.9700 . ?
C29 H292 0.9700 . ?
C30 O30 1.238(4) . ?
C30 O31 1.239(4) . ?
C32 O14 1.431(3) . ?
C32 C33 1.512(3) . ?
C32 H321 0.9700 . ?
C32 H322 0.9700 . ?
C33 O33 1.223(3) . ?
C33 N33 1.340(3) . ?
C35 O20 1.448(3) . ?
C35 C36 1.495(5) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 O37 1.237(4) . ?
C36 O36 1.251(4) . ?
C38 O28 1.440(3) . ?
C38 C39 1.514(4) . ?
C38 H381 0.9700 . ?
C38 H382 0.9700 . ?
C39 O39 1.209(4) . ?
C39 N39 1.327(4) . ?
N33 N34 1.419(3) . ?
N33 H33 0.904(18) . ?
N34 H341 0.905(2) . ?
N34 H342 0.938(3) . ?
N39 N40 1.418(4) . ?
N39 H39 0.924(18) . ?
N40 H401 0.913(4) . ?
N40 H402 0.926(4) . ?
O30 H30 0.8200 . ?
O36 H36 0.8200 . ?
O80A H801 1.072(8) . ?
O80A H802 0.975(10) . ?
O80B H804 0.973(6) . ?
O80B H803 1.002(8) . ?
O90A O90A 1.814(17) 3_775 ?
O90A H901 0.935(8) . ?
O90A H902 0.950(9) . ?
O90B H903 1.036(11) . ?
O90B H904 0.981(11) . ?
O60 H601 0.951(3) . ?
O60 H602 0.930(3) . ?
O65 H651 0.926(3) . ?
O65 H652 0.924(3) . ?
N70 N71 1.428(5) . ?
N70 H702 0.715(3) . ?
N70 H701 0.928(4) . ?
N71 H711 0.877(4) . ?
N71 H712 0.908(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
C3 C2 C7 119.5(2) . . ?
C3 C2 S1 116.20(19) . . ?
C7 C2 S1 123.96(19) . . ?
C4 C3 C2 120.6(2) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C5 C4 C3 119.9(2) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 119.9(2) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 120.6(2) . . ?
C7 C6 S8 122.48(19) . . ?
C5 C6 S8 116.4(2) . . ?
O7 C7 C6 120.3(2) . . ?
O7 C7 C2 120.5(2) . . ?
C6 C7 C2 119.2(2) . . ?
C10 C9 C14 119.4(2) . . ?
C10 C9 S8 113.7(2) . . ?
C14 C9 S8 126.17(19) . . ?
C11 C10 C9 120.1(3) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C12 C11 C10 120.6(2) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C13 120.7(3) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C12 C13 C14 119.3(2) . . ?
C12 C13 S15 116.0(2) . . ?
C14 C13 S15 124.20(19) . . ?
O14 C14 C9 120.2(2) . . ?
O14 C14 C13 120.0(2) . . ?
C9 C14 C13 119.8(2) . . ?
C17 C16 C21 119.8(3) . . ?
C17 C16 S15 117.5(2) . . ?
C21 C16 S15 122.3(2) . . ?
C18 C17 C16 120.9(3) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C19 C18 C17 119.7(3) . . ?
C19 C18 H18 120.2 . . ?
C17 C18 H18 120.2 . . ?
C18 C19 C20 120.7(3) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
C19 C20 C21 119.7(3) . . ?
C19 C20 S22 119.5(2) . . ?
C21 C20 S22 120.4(2) . . ?
O20 C21 C16 120.5(2) . . ?
O20 C21 C20 120.5(2) . . ?
C16 C21 C20 119.0(2) . . ?
C24 C23 C28 119.2(2) . . ?
C24 C23 S22 115.9(2) . . ?
C28 C23 S22 124.5(2) . . ?
C25 C24 C23 121.1(2) . . ?
C25 C24 H24 119.5 . . ?
C23 C24 H24 119.5 . . ?
C24 C25 C26 119.7(2) . . ?
C24 C25 H25 120.2 . . ?
C26 C25 H25 120.2 . . ?
C25 C26 C27 120.5(3) . . ?
C25 C26 H26 119.7 . . ?
C27 C26 H26 119.7 . . ?
C26 C27 C28 119.8(2) . . ?
C26 C27 S1 116.9(2) . . ?
C28 C27 S1 123.08(19) . . ?
O28 C28 C27 119.5(2) . . ?
O28 C28 C23 120.8(2) . . ?
C27 C28 C23 119.7(2) . . ?
O7 C29 C30 112.8(2) . . ?
O7 C29 H291 109.0 . . ?
C30 C29 H291 109.0 . . ?
O7 C29 H292 109.0 . . ?
C30 C29 H292 109.0 . . ?
H291 C29 H292 107.8 . . ?
O30 C30 O31 124.1(3) . . ?
O30 C30 C29 120.5(3) . . ?
O31 C30 C29 115.3(3) . . ?
O14 C32 C33 110.9(2) . . ?
O14 C32 H321 109.4 . . ?
C33 C32 H321 109.4 . . ?
O14 C32 H322 109.4 . . ?
C33 C32 H322 109.4 . . ?
H321 C32 H322 108.0 . . ?
O33 C33 N33 123.0(2) . . ?
O33 C33 C32 119.4(2) . . ?
N33 C33 C32 117.6(2) . . ?
O20 C35 C36 111.3(2) . . ?
O20 C35 H35A 109.4 . . ?
C36 C35 H35A 109.4 . . ?
O20 C35 H35B 109.4 . . ?
C36 C35 H35B 109.4 . . ?
H35A C35 H35B 108.0 . . ?
O37 C36 O36 123.7(3) . . ?
O37 C36 C35 116.9(3) . . ?
O36 C36 C35 119.4(3) . . ?
O28 C38 C39 111.4(2) . . ?
O28 C38 H381 109.3 . . ?
C39 C38 H381 109.3 . . ?
O28 C38 H382 109.3 . . ?
C39 C38 H382 109.3 . . ?
H381 C38 H382 108.0 . . ?
O39 C39 N39 125.1(3) . . ?
O39 C39 C38 122.6(3) . . ?
N39 C39 C38 112.3(3) . . ?
C33 N33 N34 120.1(2) . . ?
C33 N33 H33 124(2) . . ?
N34 N33 H33 116(2) . . ?
N33 N34 H341 108.0(2) . . ?
N33 N34 H342 105.8(2) . . ?
H341 N34 H342 111.4(2) . . ?
C39 N39 N40 122.5(3) . . ?
C39 N39 H39 124(2) . . ?
N40 N39 H39 113(2) . . ?
N39 N40 H401 108.7(3) . . ?
N39 N40 H402 107.8(3) . . ?
H401 N40 H402 108.3(3) . . ?
C7 O7 C29 110.72(19) . . ?
C14 O14 C32 113.74(18) . . ?
C21 O20 C35 112.2(2) . . ?
C28 O28 C38 114.6(2) . . ?
C30 O30 H30 109.5 . . ?
C36 O36 H36 109.5 . . ?
C2 S1 C27 105.76(11) . . ?
C9 S8 C6 109.66(11) . . ?
C16 S15 C13 107.22(11) . . ?
C20 S22 C23 105.45(12) . . ?
H801 O80A H802 106.8(6) . . ?
H804 O80B H803 94.3(6) . . ?
O90A O90A H901 84.1(7) 3_775 . ?
O90A O90A H902 138.4(8) 3_775 . ?
H901 O90A H902 118.6(8) . . ?
H903 O90B H904 116.7(10) . . ?
H601 O60 H602 94.1(3) . . ?
H651 O65 H652 93.0(2) . . ?
N71 N70 H702 102.0(4) . . ?
N71 N70 H701 125.9(3) . . ?
H702 N70 H701 110.2(4) . . ?
N70 N71 H711 110.0(4) . . ?
N70 N71 H712 107.2(4) . . ?
H711 N71 H712 109.7(4) . . ?

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
C7 C2 C3 C4 -0.2(4) . . . . ?
S1 C2 C3 C4 -173.7(2) . . . . ?
C2 C3 C4 C5 -3.4(4) . . . . ?
C3 C4 C5 C6 2.5(4) . . . . ?
C4 C5 C6 C7 2.0(4) . . . . ?
C4 C5 C6 S8 173.7(2) . . . . ?
C5 C6 C7 O7 172.9(2) . . . . ?
S8 C6 C7 O7 1.7(3) . . . . ?
C5 C6 C7 C2 -5.6(3) . . . . ?
S8 C6 C7 C2 -176.83(17) . . . . ?
C3 C2 C7 O7 -173.8(2) . . . . ?
S1 C2 C7 O7 -0.9(3) . . . . ?
C3 C2 C7 C6 4.7(3) . . . . ?
S1 C2 C7 C6 177.62(17) . . . . ?
C14 C9 C10 C11 -1.1(4) . . . . ?
S8 C9 C10 C11 170.2(2) . . . . ?
C9 C10 C11 C12 -0.7(5) . . . . ?
C10 C11 C12 C13 1.2(5) . . . . ?
C11 C12 C13 C14 0.1(4) . . . . ?
C11 C12 C13 S15 -172.0(2) . . . . ?
C10 C9 C14 O14 -176.3(2) . . . . ?
S8 C9 C14 O14 13.7(3) . . . . ?
C10 C9 C14 C13 2.4(4) . . . . ?
S8 C9 C14 C13 -167.71(19) . . . . ?
C12 C13 C14 O14 176.7(2) . . . . ?
S15 C13 C14 O14 -11.9(3) . . . . ?
C12 C13 C14 C9 -1.9(4) . . . . ?
S15 C13 C14 C9 169.49(19) . . . . ?
C21 C16 C17 C18 -0.1(4) . . . . ?
S15 C16 C17 C18 -173.2(2) . . . . ?
C16 C17 C18 C19 -1.6(5) . . . . ?
C17 C18 C19 C20 0.0(5) . . . . ?
C18 C19 C20 C21 3.2(4) . . . . ?
C18 C19 C20 S22 176.6(2) . . . . ?
C17 C16 C21 O20 -177.9(2) . . . . ?
S15 C16 C21 O20 -5.2(3) . . . . ?
C17 C16 C21 C20 3.3(4) . . . . ?
S15 C16 C21 C20 176.06(18) . . . . ?
C19 C20 C21 O20 176.5(2) . . . . ?
S22 C20 C21 O20 3.0(3) . . . . ?
C19 C20 C21 C16 -4.8(4) . . . . ?
S22 C20 C21 C16 -178.20(18) . . . . ?
C28 C23 C24 C25 -0.5(4) . . . . ?
S22 C23 C24 C25 173.5(2) . . . . ?
C23 C24 C25 C26 2.7(4) . . . . ?
C24 C25 C26 C27 -2.0(4) . . . . ?
C25 C26 C27 C28 -0.9(4) . . . . ?
C25 C26 C27 S1 -175.1(2) . . . . ?
C26 C27 C28 O28 -179.6(2) . . . . ?
S1 C27 C28 O28 -5.7(3) . . . . ?
C26 C27 C28 C23 3.1(3) . . . . ?
S1 C27 C28 C23 176.97(18) . . . . ?
C24 C23 C28 O28 -179.7(2) . . . . ?
S22 C23 C28 O28 6.9(3) . . . . ?
C24 C23 C28 C27 -2.4(3) . . . . ?
S22 C23 C28 C27 -175.83(18) . . . . ?
O7 C29 C30 O30 -20.1(4) . . . . ?
O7 C29 C30 O31 160.4(3) . . . . ?
O14 C32 C33 O33 -170.7(2) . . . . ?
O14 C32 C33 N33 10.3(3) . . . . ?
O20 C35 C36 O37 -170.7(3) . . . . ?
O20 C35 C36 O36 9.6(4) . . . . ?
O28 C38 C39 O39 108.4(4) . . . . ?
O28 C38 C39 N39 -71.0(3) . . . . ?
O33 C33 N33 N34 4.2(4) . . . . ?
C32 C33 N33 N34 -176.9(2) . . . . ?
O39 C39 N39 N40 -5.1(5) . . . . ?
C38 C39 N39 N40 174.3(3) . . . . ?
C6 C7 O7 C29 -93.1(3) . . . . ?
C2 C7 O7 C29 85.4(3) . . . . ?
C30 C29 O7 C7 -162.2(2) . . . . ?
C9 C14 O14 C32 -91.0(3) . . . . ?
C13 C14 O14 C32 90.4(3) . . . . ?
C33 C32 O14 C14 172.8(2) . . . . ?
C16 C21 O20 C35 97.3(3) . . . . ?
C20 C21 O20 C35 -83.9(3) . . . . ?
C36 C35 O20 C21 152.1(2) . . . . ?
C27 C28 O28 C38 108.3(3) . . . . ?
C23 C28 O28 C38 -74.4(3) . . . . ?
C39 C38 O28 C28 -86.4(3) . . . . ?
C3 C2 S1 C27 -140.05(19) . . . . ?
C7 C2 S1 C27 46.8(2) . . . . ?
C26 C27 S1 C2 -120.6(2) . . . . ?
C28 C27 S1 C2 65.4(2) . . . . ?
C10 C9 S8 C6 154.4(2) . . . . ?
C14 C9 S8 C6 -35.1(3) . . . . ?
C7 C6 S8 C9 -64.7(2) . . . . ?
C5 C6 S8 C9 123.7(2) . . . . ?
C17 C16 S15 C13 -129.1(2) . . . . ?
C21 C16 S15 C13 58.0(2) . . . . ?
C12 C13 S15 C16 -144.3(2) . . . . ?
C14 C13 S15 C16 44.1(2) . . . . ?
C19 C20 S22 C23 117.8(2) . . . . ?
C21 C20 S22 C23 -68.8(2) . . . . ?
C24 C23 S22 C20 136.8(2) . . . . ?
C28 C23 S22 C20 -49.6(2) . . . . ?

_refine_diff_density_max         0.944
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.061


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: MeOH/CH2Cl2'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_sample_5
_database_code_depnum_ccdc_archive 'CCDC 1437366'
_audit_update_record             
;
2015-11-17 deposited with the CCDC.
2016-02-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            
5,11,17,23-Tetra-tert-butyl-25,27-Di[((2-pyridinylmethylidene)hydrazinocarbonyl)-methoxy]-26,28-di[(hydroxycarbonyl)methoxy]-2,8,14,20-tetrathiacalix[4]arene
_chemical_melting_point          471
_chemical_formula_moiety         'C60 H66 N6 O10 S4, (C O H4)'
_chemical_formula_sum            'C61 H70 N6 O11 S4'
_chemical_formula_weight         1191.47

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.783(13)
_cell_length_b                   15.091(14)
_cell_length_c                   17.68(2)
_cell_angle_alpha                71.891(12)
_cell_angle_beta                 85.063(18)
_cell_angle_gamma                69.735(12)
_cell_volume                     3278(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1205
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      16.85

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_F_000             1260
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.109
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.037
_exptl_absorpt_coefficient_mu    0.204
_shelx_estimated_absorpt_T_min   0.978
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_process_details   
;
 G.M. Sheldrick (1998a). SADABS v.2.01, Bruker.
 Siemens Area Detector Absorption Correction Program.
 Bruker AXS. Madison. Wisconsin. USA

 The maximum experimental transmission factor Tmax is equal to the 
 one estimated by SHELX. The minimum experimental transmission factor 
 Tmin is calculated as a product of Tmax and the Tmin-to-Tmax-ratio, 
 evaluated by SADABS.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_reflns_number            39008
_diffrn_reflns_av_unetI/netI     0.4454
_diffrn_reflns_av_R_equivalents  0.2261
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.575
_diffrn_reflns_theta_max         30.027
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             16924
_reflns_number_gt                3408
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16924
_refine_ls_number_parameters     752
_refine_ls_number_restraints     690
_refine_ls_R_factor_all          0.3498
_refine_ls_R_factor_gt           0.1530
_refine_ls_wR_factor_ref         0.4690
_refine_ls_wR_factor_gt          0.4178
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_restrained_S_all      0.891
_refine_ls_shift/su_max          0.003
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.5754(2) 0.6034(2) 0.38576(17) 0.0656(8) Uani 1 1 d . U . . .
C2 C 0.5355(7) 0.5504(7) 0.3250(6) 0.050(2) Uani 1 1 d . U . . .
C3 C 0.4711(7) 0.4929(6) 0.3623(6) 0.048(2) Uani 1 1 d . U . . .
H3 H 0.4610 0.4793 0.4168 0.057 Uiso 1 1 calc R U . . .
C4 C 0.4223(7) 0.4563(7) 0.3166(6) 0.053(2) Uani 1 1 d . U . . .
C5 C 0.4406(7) 0.4779(7) 0.2373(5) 0.051(2) Uani 1 1 d . U . . .
H5 H 0.4097 0.4541 0.2069 0.061 Uiso 1 1 calc R U . . .
C6 C 0.5026(7) 0.5331(7) 0.1989(5) 0.046(2) Uani 1 1 d . U . . .
C7 C 0.5494(7) 0.5709(7) 0.2420(6) 0.053(2) Uani 1 1 d . U . . .
O7 O 0.6108(5) 0.6278(5) 0.2089(4) 0.0563(17) Uani 1 1 d . U . . .
S8 S 0.4974(2) 0.5719(3) 0.09435(16) 0.0727(9) Uani 1 1 d . U . . .
C9 C 0.6201(7) 0.5815(8) 0.0606(6) 0.055(2) Uani 1 1 d . U . . .
C10 C 0.6213(8) 0.6751(8) 0.0111(5) 0.059(2) Uani 1 1 d . U . . .
H10 H 0.5606 0.7295 0.0002 0.070 Uiso 1 1 calc R U . . .
C11 C 0.7146(8) 0.6849(8) -0.0213(6) 0.058(2) Uani 1 1 d . U . . .
C12 C 0.8054(8) 0.6003(8) 0.0030(6) 0.064(3) Uani 1 1 d . U . . .
H12 H 0.8693 0.6078 -0.0113 0.077 Uiso 1 1 calc R U . . .
C13 C 0.8035(7) 0.5097(7) 0.0456(6) 0.054(2) Uani 1 1 d . U . . .
C14 C 0.7092(7) 0.4976(8) 0.0768(5) 0.052(2) Uani 1 1 d . U . . .
O14 O 0.7036(5) 0.4065(5) 0.1199(4) 0.0597(17) Uani 1 1 d . U . . .
S15 S 0.9167(2) 0.4088(2) 0.05726(16) 0.0651(8) Uani 1 1 d . U . . .
C16 C 0.9285(8) 0.3447(7) 0.1587(6) 0.060(2) Uani 1 1 d . U . . .
C17 C 0.9373(7) 0.2418(7) 0.1811(7) 0.061(2) Uani 1 1 d . U . . .
H17 H 0.9300 0.2148 0.1422 0.073 Uiso 1 1 calc R U . . .
C19 C 0.9644(7) 0.2288(8) 0.3148(7) 0.066(3) Uani 1 1 d . U . . .
H19 H 0.9757 0.1905 0.3679 0.079 Uiso 1 1 calc R U . . .
C20 C 0.9568(7) 0.3258(7) 0.2964(6) 0.052(2) Uani 1 1 d . U . . .
C21 C 0.9400(7) 0.3826(7) 0.2171(6) 0.051(2) Uani 1 1 d . U . . .
O21 O 0.9386(5) 0.4815(4) 0.1949(4) 0.0624(18) Uani 1 1 d . U . . .
S22 S 0.9825(2) 0.3673(2) 0.37219(18) 0.0740(9) Uani 1 1 d . U . . .
C23 C 0.8887(7) 0.4800(7) 0.3646(5) 0.050(2) Uani 1 1 d . U . . .
C24 C 0.9153(8) 0.5607(7) 0.3610(5) 0.055(2) Uani 1 1 d . U . . .
H24 H 0.9851 0.5541 0.3561 0.066 Uiso 1 1 calc R U . . .
C26 C 0.7434(8) 0.6627(8) 0.3668(5) 0.055(2) Uani 1 1 d . U . . .
H26 H 0.6945 0.7233 0.3669 0.066 Uiso 1 1 calc R U . . .
C27 C 0.7096(8) 0.5858(8) 0.3693(6) 0.060(2) Uani 1 1 d . U . . .
C28 C 0.7817(8) 0.4929(7) 0.3698(5) 0.049(2) Uani 1 1 d . U . . .
O28 O 0.7472(5) 0.4167(5) 0.3678(4) 0.0605(18) Uani 1 1 d . U . . .
C29 C 0.3540(8) 0.3948(8) 0.3580(6) 0.060(2) Uani 1 1 d . U . . .
C30 C 0.4038(8) 0.3132(9) 0.4252(7) 0.080(3) Uani 1 1 d . U . . .
H30A H 0.4296 0.3367 0.4612 0.119 Uiso 1 1 calc R U . . .
H30B H 0.3550 0.2822 0.4519 0.119 Uiso 1 1 calc R U . . .
H30C H 0.4603 0.2661 0.4076 0.119 Uiso 1 1 calc R U . . .
C31 C 0.3119(10) 0.3610(10) 0.2993(8) 0.098(4) Uani 1 1 d . U . . .
H31A H 0.2790 0.4172 0.2549 0.147 Uiso 1 1 calc R U . . .
H31B H 0.3677 0.3142 0.2808 0.147 Uiso 1 1 calc R U . . .
H31C H 0.2625 0.3303 0.3251 0.147 Uiso 1 1 calc R U . . .
C32 C 0.2535(9) 0.4748(9) 0.3869(8) 0.098(4) Uani 1 1 d . U . . .
H32A H 0.2206 0.5292 0.3414 0.146 Uiso 1 1 calc R U . . .
H32B H 0.2051 0.4425 0.4123 0.146 Uiso 1 1 calc R U . . .
H32C H 0.2764 0.4989 0.4238 0.146 Uiso 1 1 calc R U . . .
C33 C 0.7171(9) 0.7834(8) -0.0772(6) 0.072(3) Uani 1 1 d . U . . .
C34 C 0.8045(10) 0.8110(9) -0.0519(8) 0.093(4) Uani 1 1 d . U . . .
H34A H 0.8694 0.7590 -0.0504 0.140 Uiso 1 1 calc R U . . .
H34B H 0.8076 0.8715 -0.0895 0.140 Uiso 1 1 calc R U . . .
H34C H 0.7910 0.8198 0.0000 0.140 Uiso 1 1 calc R U . . .
C35 C 0.6185(10) 0.8669(9) -0.0785(7) 0.090(3) Uani 1 1 d . U . . .
H35A H 0.6241 0.9272 -0.1147 0.135 Uiso 1 1 calc R U . . .
H35B H 0.5624 0.8533 -0.0957 0.135 Uiso 1 1 calc R U . . .
H35C H 0.6056 0.8738 -0.0261 0.135 Uiso 1 1 calc R U . . .
C36 C 0.7375(13) 0.7774(11) -0.1620(7) 0.125(5) Uani 1 1 d . U . . .
H36A H 0.8006 0.7242 -0.1626 0.187 Uiso 1 1 calc R U . . .
H36B H 0.6812 0.7656 -0.1808 0.187 Uiso 1 1 calc R U . . .
H36C H 0.7434 0.8387 -0.1960 0.187 Uiso 1 1 calc R U . . .
C18 C 0.9562(7) 0.1830(8) 0.2586(7) 0.067(3) Uani 1 1 d D U . . .
C37 C 0.9671(8) 0.0728(8) 0.2824(6) 0.085(3) Uani 1 1 d D U . . .
C38 C 0.8710(15) 0.0620(15) 0.3247(16) 0.096(5) Uani 0.543(10) 1 d D U P A 1
H38A H 0.8755 -0.0062 0.3403 0.143 Uiso 0.543(10) 1 calc R U P A 1
H38B H 0.8640 0.0837 0.3712 0.143 Uiso 0.543(10) 1 calc R U P A 1
H38C H 0.8119 0.1017 0.2898 0.143 Uiso 0.543(10) 1 calc R U P A 1
C39 C 1.0591(17) 0.0132(14) 0.3420(15) 0.105(5) Uani 0.543(10) 1 d D U P A 1
H39A H 1.1219 0.0188 0.3163 0.158 Uiso 0.543(10) 1 calc R U P A 1
H39B H 1.0486 0.0388 0.3865 0.158 Uiso 0.543(10) 1 calc R U P A 1
H39C H 1.0640 -0.0552 0.3603 0.158 Uiso 0.543(10) 1 calc R U P A 1
C40 C 0.982(2) 0.0308(16) 0.2116(12) 0.112(5) Uani 0.543(10) 1 d D U P A 1
H40A H 1.0439 0.0376 0.1844 0.168 Uiso 0.543(10) 1 calc R U P A 1
H40B H 0.9889 -0.0379 0.2307 0.168 Uiso 0.543(10) 1 calc R U P A 1
H40C H 0.9238 0.0666 0.1756 0.168 Uiso 0.543(10) 1 calc R U P A 1
C38' C 1.0605(18) 0.0203(16) 0.2415(17) 0.096(5) Uani 0.457(10) 1 d D U P A 2
H38D H 1.0685 -0.0487 0.2556 0.143 Uiso 0.457(10) 1 calc R U P A 2
H38E H 1.0508 0.0491 0.1849 0.143 Uiso 0.457(10) 1 calc R U P A 2
H38F H 1.1213 0.0272 0.2581 0.143 Uiso 0.457(10) 1 calc R U P A 2
C39' C 0.8710(18) 0.0677(18) 0.248(2) 0.105(5) Uani 0.457(10) 1 d D U P A 2
H39D H 0.8103 0.1004 0.2731 0.158 Uiso 0.457(10) 1 calc R U P A 2
H39E H 0.8656 0.0998 0.1919 0.158 Uiso 0.457(10) 1 calc R U P A 2
H39F H 0.8770 -0.0004 0.2586 0.158 Uiso 0.457(10) 1 calc R U P A 2
C40' C 0.975(3) 0.0169(18) 0.3721(11) 0.112(5) Uani 0.457(10) 1 d D U P A 2
H40D H 0.9158 0.0501 0.3980 0.168 Uiso 0.457(10) 1 calc R U P A 2
H40E H 0.9771 -0.0496 0.3797 0.168 Uiso 0.457(10) 1 calc R U P A 2
H40F H 1.0368 0.0153 0.3944 0.168 Uiso 0.457(10) 1 calc R U P A 2
C25 C 0.8447(8) 0.6533(8) 0.3641(5) 0.057(2) Uani 1 1 d . U . . .
C41 C 0.8808(10) 0.7361(9) 0.3633(8) 0.084(3) Uani 1 1 d . U . . .
C42 C 0.9902(12) 0.7185(13) 0.3593(13) 0.160(6) Uani 1 1 d . U . B 1
H42A H 1.0181 0.6900 0.3172 0.241 Uiso 1 1 calc R U . B 1
H42B H 1.0024 0.7800 0.3490 0.241 Uiso 1 1 calc R U . B 1
H42C H 1.0231 0.6737 0.4090 0.241 Uiso 1 1 calc R U . B 1
C43 C 0.8340(12) 0.7803(11) 0.4276(10) 0.128(5) Uani 1 1 d . U . C 1
H43A H 0.7611 0.7912 0.4288 0.192 Uiso 1 1 calc R U . C 1
H43B H 0.8657 0.7360 0.4779 0.192 Uiso 1 1 calc R U . C 1
H43C H 0.8451 0.8423 0.4179 0.192 Uiso 1 1 calc R U . C 1
C44 C 0.8315(14) 0.8227(12) 0.2904(10) 0.149(6) Uani 1 1 d . U . D 1
H44A H 0.7580 0.8373 0.2905 0.223 Uiso 1 1 calc R U . D 1
H44B H 0.8466 0.8798 0.2916 0.223 Uiso 1 1 calc R U . D 1
H44C H 0.8590 0.8056 0.2431 0.223 Uiso 1 1 calc R U . D 1
C45 C 0.5575(9) 0.7294(8) 0.1863(6) 0.069(3) Uani 1 1 d . U . . .
H45A H 0.5187 0.7472 0.2310 0.083 Uiso 1 1 calc R U . . .
H45B H 0.5087 0.7465 0.1434 0.083 Uiso 1 1 calc R U . . .
C46 C 0.6317(12) 0.7877(11) 0.1590(7) 0.077(3) Uani 1 1 d . U . . .
O46 O 0.7211(8) 0.7487(7) 0.1557(5) 0.101(3) Uani 1 1 d . U . . .
O47 O 0.5813(8) 0.8846(7) 0.1374(5) 0.110(3) Uani 1 1 d . U . . .
H47 H 0.5192 0.8949 0.1438 0.165 Uiso 1 1 calc R U . . .
C48 C 0.6926(10) 0.3560(8) 0.0634(6) 0.072(3) Uani 1 1 d . U . . .
H48A H 0.7573 0.3373 0.0363 0.086 Uiso 1 1 calc R U . . .
H48B H 0.6398 0.4018 0.0236 0.086 Uiso 1 1 calc R U . . .
C49 C 0.6645(9) 0.2665(9) 0.1027(7) 0.075(3) Uani 1 1 d . U . . .
O49 O 0.6576(8) 0.2164(6) 0.0658(5) 0.110(3) Uani 1 1 d . U . . .
N49 N 0.6454(7) 0.2478(6) 0.1832(5) 0.073(3) Uani 1 1 d . U . . .
H49 H 0.6543 0.2829 0.2104 0.087 Uiso 1 1 calc R U . . .
N50 N 0.6109(7) 0.1682(6) 0.2170(5) 0.073(2) Uani 1 1 d . U . . .
C50 C 0.6047(8) 0.1384(7) 0.2931(6) 0.062(3) Uani 1 1 d . U . . .
H50 H 0.6208 0.1688 0.3262 0.075 Uiso 1 1 calc R U . . .
C51 C 0.5698(8) 0.0519(8) 0.3237(7) 0.065(3) Uani 1 1 d . U . . .
C52 C 0.5343(9) 0.0137(8) 0.2760(7) 0.076(3) Uani 1 1 d . U . . .
H52 H 0.5300 0.0426 0.2211 0.091 Uiso 1 1 calc R U . . .
C53 C 0.5044(9) -0.0692(8) 0.3103(7) 0.075(3) Uani 1 1 d . U . . .
H53 H 0.4789 -0.0960 0.2789 0.090 Uiso 1 1 calc R U . . .
C54 C 0.5134(8) -0.1097(8) 0.3902(6) 0.065(3) Uani 1 1 d . U . . .
H54 H 0.4923 -0.1638 0.4151 0.078 Uiso 1 1 calc R U . . .
C55 C 0.5547(9) -0.0692(8) 0.4342(7) 0.075(3) Uani 1 1 d . U . . .
H55 H 0.5630 -0.1000 0.4888 0.090 Uiso 1 1 calc R U . . .
N56 N 0.5834(7) 0.0102(6) 0.4045(5) 0.071(2) Uani 1 1 d . U . . .
C57 C 1.0374(8) 0.4880(8) 0.1821(7) 0.072(3) Uani 1 1 d . U . . .
H57A H 1.0701 0.4572 0.1415 0.086 Uiso 1 1 calc R U . . .
H57B H 1.0788 0.4518 0.2308 0.086 Uiso 1 1 calc R U . . .
C58 C 1.0350(14) 0.5931(11) 0.1566(9) 0.107(5) Uani 1 1 d . U . . .
O58 O 1.1098(9) 0.6136(8) 0.1450(6) 0.138(4) Uani 1 1 d . U . . .
O59 O 0.9437(8) 0.6628(7) 0.1422(6) 0.116(3) Uani 1 1 d . U . . .
H59 H 0.8985 0.6374 0.1498 0.174 Uiso 1 1 calc R U . . .
C60 C 0.7389(9) 0.3592(8) 0.4456(6) 0.072(3) Uani 1 1 d . U . . .
H60A H 0.6837 0.3975 0.4725 0.086 Uiso 1 1 calc R U . . .
H60B H 0.8031 0.3378 0.4754 0.086 Uiso 1 1 calc R U . . .
C61 C 0.7152(8) 0.2694(8) 0.4402(7) 0.063(3) Uani 1 1 d . U . . .
O61 O 0.7040(6) 0.2536(5) 0.3805(5) 0.082(2) Uani 1 1 d . U . . .
N61 N 0.7074(7) 0.2066(7) 0.5121(5) 0.079(3) Uani 1 1 d . U . . .
H61 H 0.6983 0.1522 0.5145 0.095 Uiso 1 1 calc R U . . .
N62 N 0.7137(6) 0.2272(6) 0.5810(6) 0.065(2) Uani 1 1 d . U . . .
C62 C 0.7096(8) 0.1622(8) 0.6444(7) 0.069(3) Uani 1 1 d . U . . .
H62 H 0.7027 0.1038 0.6422 0.083 Uiso 1 1 calc R U . . .
C63 C 0.7155(8) 0.1765(8) 0.7236(7) 0.071(3) Uani 1 1 d . U . . .
C64 C 0.7378(8) 0.2571(8) 0.7312(7) 0.075(3) Uani 1 1 d . U . . .
H64 H 0.7485 0.3046 0.6863 0.090 Uiso 1 1 calc R U . . .
C65 C 0.7436(10) 0.2650(10) 0.8058(8) 0.090(4) Uani 1 1 d . U . . .
H65 H 0.7605 0.3163 0.8132 0.108 Uiso 1 1 calc R U . . .
C66 C 0.7232(10) 0.1931(10) 0.8698(8) 0.093(4) Uani 1 1 d . U . . .
H66 H 0.7251 0.1960 0.9214 0.111 Uiso 1 1 calc R U . . .
C67 C 0.7015(9) 0.1224(9) 0.8569(8) 0.084(3) Uani 1 1 d . U . . .
H67 H 0.6880 0.0763 0.9015 0.101 Uiso 1 1 calc R U . . .
N68 N 0.6963(8) 0.1077(7) 0.7860(6) 0.084(3) Uani 1 1 d . U . . .
C82 C 0.2684(16) 0.0784(11) 0.4205(10) 0.157(8) Uani 1 1 d . U . . .
H82A H 0.2325 0.1310 0.4429 0.236 Uiso 1 1 calc R U . . .
H82B H 0.2271 0.0818 0.3780 0.236 Uiso 1 1 calc R U . . .
H82C H 0.3333 0.0850 0.4002 0.236 Uiso 1 1 calc R U . . .
O82 O 0.2861(7) -0.0107(6) 0.4780(5) 0.107(3) Uani 1 1 d . U . . .
H82 H 0.3184 -0.0116 0.5284 0.161 Uiso 1 1 d . U . . .


_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
S1 C2 1.743(9) . ?
S1 C27 1.786(10) . ?
C2 C7 1.412(13) . ?
C2 C3 1.432(12) . ?
C3 C4 1.429(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.359(12) . ?
C4 C29 1.531(12) . ?
C5 C6 1.388(12) . ?
C5 H5 0.9300 . ?
C6 C7 1.391(12) . ?
C6 S8 1.756(9) . ?
C7 O7 1.378(10) . ?
O7 C45 1.392(11) . ?
S8 C9 1.782(10) . ?
C9 C14 1.396(13) . ?
C9 C10 1.417(13) . ?
C10 C11 1.398(13) . ?
C10 H10 0.9300 . ?
C11 C12 1.424(14) . ?
C11 C33 1.518(14) . ?
C12 C13 1.348(12) . ?
C12 H12 0.9300 . ?
C13 C14 1.416(12) . ?
C13 S15 1.736(10) . ?
C14 O14 1.375(11) . ?
O14 C48 1.476(11) . ?
S15 C16 1.744(11) . ?
C16 C21 1.369(13) . ?
C16 C17 1.442(13) . ?
C17 C18 1.371(14) . ?
C17 H17 0.9300 . ?
C19 C20 1.365(13) . ?
C19 C18 1.407(14) . ?
C19 H19 0.9300 . ?
C20 C21 1.387(13) . ?
C20 S22 1.753(10) . ?
C21 O21 1.415(11) . ?
O21 C57 1.394(11) . ?
S22 C23 1.717(10) . ?
C23 C24 1.372(12) . ?
C23 C28 1.418(12) . ?
C24 C25 1.414(13) . ?
C24 H24 0.9300 . ?
C26 C25 1.353(12) . ?
C26 C27 1.379(12) . ?
C26 H26 0.9300 . ?
C27 C28 1.409(13) . ?
C28 O28 1.399(10) . ?
O28 C60 1.400(11) . ?
C29 C30 1.430(14) . ?
C29 C31 1.521(15) . ?
C29 C32 1.655(15) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C35 1.495(15) . ?
C33 C34 1.543(15) . ?
C33 C36 1.526(15) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C18 C37 1.539(15) . ?
C37 C38 1.498(15) . ?
C37 C38' 1.515(15) . ?
C37 C40 1.538(16) . ?
C37 C39' 1.537(16) . ?
C37 C40' 1.540(16) . ?
C37 C39 1.542(15) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C38' H38D 0.9600 . ?
C38' H38E 0.9600 . ?
C38' H38F 0.9600 . ?
C39' H39D 0.9600 . ?
C39' H39E 0.9600 . ?
C39' H39F 0.9600 . ?
C40' H40D 0.9600 . ?
C40' H40E 0.9600 . ?
C40' H40F 0.9600 . ?
C25 C41 1.493(13) . ?
C41 C42 1.436(17) . ?
C41 C43 1.483(17) . ?
C41 C44 1.523(19) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 C46 1.526(15) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 O46 1.173(14) . ?
C46 O47 1.327(15) . ?
O47 H47 0.8200 . ?
C48 C49 1.479(14) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C49 O49 1.172(12) . ?
C49 N49 1.382(13) . ?
N49 N50 1.388(11) . ?
N49 H49 0.8600 . ?
N50 C50 1.285(12) . ?
C50 C51 1.476(14) . ?
C50 H50 0.9300 . ?
C51 N56 1.370(13) . ?
C51 C52 1.360(14) . ?
C52 C53 1.395(14) . ?
C52 H52 0.9300 . ?
C53 C54 1.350(14) . ?
C53 H53 0.9300 . ?
C54 C55 1.383(14) . ?
C54 H54 0.9300 . ?
C55 N56 1.330(12) . ?
C55 H55 0.9300 . ?
C57 C58 1.497(16) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C58 O58 1.161(15) . ?
C58 O59 1.315(17) . ?
O59 H59 0.8200 . ?
C60 C61 1.531(14) . ?
C60 H60A 0.9700 . ?
C60 H60B 0.9700 . ?
C61 O61 1.184(11) . ?
C61 N61 1.350(13) . ?
N61 N62 1.364(11) . ?
N61 H61 0.8600 . ?
N62 C62 1.252(12) . ?
C62 C63 1.494(15) . ?
C62 H62 0.9300 . ?
C63 N68 1.339(13) . ?
C63 C64 1.400(14) . ?
C64 C65 1.372(16) . ?
C64 H64 0.9300 . ?
C65 C66 1.389(16) . ?
C65 H65 0.9300 . ?
C66 C67 1.289(15) . ?
C66 H66 0.9300 . ?
C67 N68 1.350(14) . ?
C67 H67 0.9300 . ?
C82 O82 1.367(16) . ?
C82 H82A 0.9600 . ?
C82 H82B 0.9600 . ?
C82 H82C 0.9600 . ?
O82 H82 1.024(8) . ?

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 S1 C27 107.8(5) . . ?
C7 C2 C3 118.9(8) . . ?
C7 C2 S1 125.4(7) . . ?
C3 C2 S1 115.1(7) . . ?
C4 C3 C2 120.7(8) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C5 C4 C3 117.0(8) . . ?
C5 C4 C29 123.4(9) . . ?
C3 C4 C29 119.6(8) . . ?
C4 C5 C6 124.1(9) . . ?
C4 C5 H5 117.9 . . ?
C6 C5 H5 117.9 . . ?
C7 C6 C5 119.8(8) . . ?
C7 C6 S8 122.1(7) . . ?
C5 C6 S8 116.9(7) . . ?
C2 C7 O7 116.6(8) . . ?
C2 C7 C6 119.5(8) . . ?
O7 C7 C6 124.0(8) . . ?
C45 O7 C7 114.0(7) . . ?
C6 S8 C9 107.7(4) . . ?
C14 C9 C10 121.9(9) . . ?
C14 C9 S8 120.7(8) . . ?
C10 C9 S8 117.2(8) . . ?
C11 C10 C9 119.4(10) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 117.0(9) . . ?
C10 C11 C33 120.4(10) . . ?
C12 C11 C33 122.6(9) . . ?
C13 C12 C11 123.3(9) . . ?
C13 C12 H12 118.4 . . ?
C11 C12 H12 118.4 . . ?
C12 C13 C14 120.0(10) . . ?
C12 C13 S15 118.8(8) . . ?
C14 C13 S15 121.2(8) . . ?
O14 C14 C9 120.3(8) . . ?
O14 C14 C13 121.8(9) . . ?
C9 C14 C13 117.8(9) . . ?
C14 O14 C48 108.2(7) . . ?
C13 S15 C16 105.7(5) . . ?
C21 C16 C17 118.2(10) . . ?
C21 C16 S15 124.5(8) . . ?
C17 C16 S15 117.0(8) . . ?
C18 C17 C16 121.3(10) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C20 C19 C18 124.2(11) . . ?
C20 C19 H19 117.9 . . ?
C18 C19 H19 117.9 . . ?
C19 C20 C21 117.8(10) . . ?
C19 C20 S22 118.0(8) . . ?
C21 C20 S22 123.9(8) . . ?
C16 C21 C20 122.0(9) . . ?
C16 C21 O21 118.5(9) . . ?
C20 C21 O21 119.4(9) . . ?
C57 O21 C21 112.3(7) . . ?
C23 S22 C20 107.1(5) . . ?
C24 C23 C28 116.5(9) . . ?
C24 C23 S22 120.5(7) . . ?
C28 C23 S22 122.8(7) . . ?
C23 C24 C25 124.9(9) . . ?
C23 C24 H24 117.6 . . ?
C25 C24 H24 117.6 . . ?
C25 C26 C27 122.6(10) . . ?
C25 C26 H26 118.7 . . ?
C27 C26 H26 118.7 . . ?
C28 C27 C26 120.0(9) . . ?
C28 C27 S1 121.6(7) . . ?
C26 C27 S1 117.8(8) . . ?
C27 C28 O28 120.0(8) . . ?
C27 C28 C23 119.6(8) . . ?
O28 C28 C23 120.1(9) . . ?
C28 O28 C60 109.5(7) . . ?
C30 C29 C31 111.3(10) . . ?
C30 C29 C4 113.5(9) . . ?
C31 C29 C4 111.2(9) . . ?
C30 C29 C32 110.1(9) . . ?
C31 C29 C32 106.4(9) . . ?
C4 C29 C32 103.9(8) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C35 C33 C11 112.8(9) . . ?
C35 C33 C34 107.1(10) . . ?
C11 C33 C34 110.5(9) . . ?
C35 C33 C36 108.1(10) . . ?
C11 C33 C36 110.4(9) . . ?
C34 C33 C36 107.8(10) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C17 C18 C19 116.5(10) . . ?
C17 C18 C37 121.3(10) . . ?
C19 C18 C37 122.1(9) . . ?
C38 C37 C18 107.5(10) . . ?
C38' C37 C18 108.3(11) . . ?
C38 C37 C40 109.3(13) . . ?
C18 C37 C40 113.9(11) . . ?
C38' C37 C39' 107.5(15) . . ?
C18 C37 C39' 106.8(11) . . ?
C38' C37 C40' 109.4(15) . . ?
C18 C37 C40' 116.9(12) . . ?
C39' C37 C40' 107.6(15) . . ?
C38 C37 C39 107.7(13) . . ?
C18 C37 C39 108.4(10) . . ?
C40 C37 C39 109.7(14) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C37 C38' H38D 109.5 . . ?
C37 C38' H38E 109.5 . . ?
H38D C38' H38E 109.5 . . ?
C37 C38' H38F 109.5 . . ?
H38D C38' H38F 109.5 . . ?
H38E C38' H38F 109.5 . . ?
C37 C39' H39D 109.5 . . ?
C37 C39' H39E 109.5 . . ?
H39D C39' H39E 109.5 . . ?
C37 C39' H39F 109.5 . . ?
H39D C39' H39F 109.5 . . ?
H39E C39' H39F 109.5 . . ?
C37 C40' H40D 109.5 . . ?
C37 C40' H40E 109.5 . . ?
H40D C40' H40E 109.5 . . ?
C37 C40' H40F 109.5 . . ?
H40D C40' H40F 109.5 . . ?
H40E C40' H40F 109.5 . . ?
C26 C25 C24 116.4(9) . . ?
C26 C25 C41 122.2(10) . . ?
C24 C25 C41 121.4(10) . . ?
C42 C41 C43 111.5(12) . . ?
C42 C41 C25 117.6(11) . . ?
C43 C41 C25 111.8(10) . . ?
C42 C41 C44 106.5(13) . . ?
C43 C41 C44 100.4(13) . . ?
C25 C41 C44 107.5(11) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O7 C45 C46 111.2(10) . . ?
O7 C45 H45A 109.4 . . ?
C46 C45 H45A 109.4 . . ?
O7 C45 H45B 109.4 . . ?
C46 C45 H45B 109.4 . . ?
H45A C45 H45B 108.0 . . ?
O46 C46 O47 126.3(13) . . ?
O46 C46 C45 122.2(13) . . ?
O47 C46 C45 111.4(12) . . ?
C46 O47 H47 109.5 . . ?
O14 C48 C49 112.8(8) . . ?
O14 C48 H48A 109.0 . . ?
C49 C48 H48A 109.0 . . ?
O14 C48 H48B 109.0 . . ?
C49 C48 H48B 109.0 . . ?
H48A C48 H48B 107.8 . . ?
O49 C49 N49 123.1(11) . . ?
O49 C49 C48 120.4(11) . . ?
N49 C49 C48 116.5(10) . . ?
N50 N49 C49 115.2(9) . . ?
N50 N49 H49 122.4 . . ?
C49 N49 H49 122.4 . . ?
C50 N50 N49 118.4(9) . . ?
N50 C50 C51 114.6(10) . . ?
N50 C50 H50 122.7 . . ?
C51 C50 H50 122.7 . . ?
N56 C51 C52 123.5(10) . . ?
N56 C51 C50 113.0(10) . . ?
C52 C51 C50 123.4(10) . . ?
C51 C52 C53 119.3(11) . . ?
C51 C52 H52 120.3 . . ?
C53 C52 H52 120.3 . . ?
C54 C53 C52 118.3(11) . . ?
C54 C53 H53 120.8 . . ?
C52 C53 H53 120.8 . . ?
C55 C54 C53 118.8(11) . . ?
C55 C54 H54 120.6 . . ?
C53 C54 H54 120.6 . . ?
C54 C55 N56 125.2(10) . . ?
C54 C55 H55 117.4 . . ?
N56 C55 H55 117.4 . . ?
C51 N56 C55 114.7(9) . . ?
O21 C57 C58 112.0(11) . . ?
O21 C57 H57A 109.2 . . ?
C58 C57 H57A 109.2 . . ?
O21 C57 H57B 109.2 . . ?
C58 C57 H57B 109.2 . . ?
H57A C57 H57B 107.9 . . ?
O58 C58 O59 120.3(15) . . ?
O58 C58 C57 122.3(16) . . ?
O59 C58 C57 117.2(13) . . ?
C58 O59 H59 109.5 . . ?
O28 C60 C61 107.4(8) . . ?
O28 C60 H60A 110.2 . . ?
C61 C60 H60A 110.2 . . ?
O28 C60 H60B 110.2 . . ?
C61 C60 H60B 110.2 . . ?
H60A C60 H60B 108.5 . . ?
O61 C61 N61 121.3(10) . . ?
O61 C61 C60 125.6(10) . . ?
N61 C61 C60 113.1(10) . . ?
C61 N61 N62 121.7(9) . . ?
C61 N61 H61 119.2 . . ?
N62 N61 H61 119.2 . . ?
C62 N62 N61 116.4(9) . . ?
N62 C62 C63 121.2(10) . . ?
N62 C62 H62 119.4 . . ?
C63 C62 H62 119.4 . . ?
N68 C63 C64 122.8(11) . . ?
N68 C63 C62 115.1(10) . . ?
C64 C63 C62 122.0(11) . . ?
C65 C64 C63 119.0(12) . . ?
C65 C64 H64 120.5 . . ?
C63 C64 H64 120.5 . . ?
C64 C65 C66 117.3(12) . . ?
C64 C65 H65 121.4 . . ?
C66 C65 H65 121.4 . . ?
C67 C66 C65 119.3(13) . . ?
C67 C66 H66 120.3 . . ?
C65 C66 H66 120.3 . . ?
C66 C67 N68 127.4(13) . . ?
C66 C67 H67 116.3 . . ?
N68 C67 H67 116.3 . . ?
C63 N68 C67 114.1(10) . . ?
O82 C82 H82A 109.5 . . ?
O82 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
O82 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C82 O82 H82 111.1(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
C27 S1 C2 C7 -53.0(10) . . . . ?
C27 S1 C2 C3 136.3(7) . . . . ?
C7 C2 C3 C4 0.4(13) . . . . ?
S1 C2 C3 C4 171.8(7) . . . . ?
C2 C3 C4 C5 0.6(13) . . . . ?
C2 C3 C4 C29 179.8(8) . . . . ?
C3 C4 C5 C6 -0.4(14) . . . . ?
C29 C4 C5 C6 -179.7(9) . . . . ?
C4 C5 C6 C7 -0.7(15) . . . . ?
C4 C5 C6 S8 -168.6(8) . . . . ?
C3 C2 C7 O7 179.0(8) . . . . ?
S1 C2 C7 O7 8.6(13) . . . . ?
C3 C2 C7 C6 -1.5(13) . . . . ?
S1 C2 C7 C6 -172.0(7) . . . . ?
C5 C6 C7 C2 1.6(14) . . . . ?
S8 C6 C7 C2 168.9(7) . . . . ?
C5 C6 C7 O7 -178.9(8) . . . . ?
S8 C6 C7 O7 -11.7(13) . . . . ?
C2 C7 O7 C45 -87.6(10) . . . . ?
C6 C7 O7 C45 93.0(11) . . . . ?
C7 C6 S8 C9 41.8(9) . . . . ?
C5 C6 S8 C9 -150.6(8) . . . . ?
C6 S8 C9 C14 64.2(9) . . . . ?
C6 S8 C9 C10 -121.4(8) . . . . ?
C14 C9 C10 C11 -1.5(14) . . . . ?
S8 C9 C10 C11 -175.8(7) . . . . ?
C9 C10 C11 C12 -4.8(13) . . . . ?
C9 C10 C11 C33 177.5(9) . . . . ?
C10 C11 C12 C13 9.6(15) . . . . ?
C33 C11 C12 C13 -172.7(10) . . . . ?
C11 C12 C13 C14 -7.8(15) . . . . ?
C11 C12 C13 S15 169.3(8) . . . . ?
C10 C9 C14 O14 -174.8(8) . . . . ?
S8 C9 C14 O14 -0.7(12) . . . . ?
C10 C9 C14 C13 3.5(13) . . . . ?
S8 C9 C14 C13 177.6(7) . . . . ?
C12 C13 C14 O14 179.3(8) . . . . ?
S15 C13 C14 O14 2.3(12) . . . . ?
C12 C13 C14 C9 1.0(14) . . . . ?
S15 C13 C14 C9 -176.0(7) . . . . ?
C9 C14 O14 C48 94.2(10) . . . . ?
C13 C14 O14 C48 -84.0(10) . . . . ?
C12 C13 S15 C16 131.4(8) . . . . ?
C14 C13 S15 C16 -51.6(9) . . . . ?
C13 S15 C16 C21 -62.9(9) . . . . ?
C13 S15 C16 C17 123.8(8) . . . . ?
C21 C16 C17 C18 0.3(14) . . . . ?
S15 C16 C17 C18 174.0(8) . . . . ?
C18 C19 C20 C21 0.0(14) . . . . ?
C18 C19 C20 S22 -173.4(8) . . . . ?
C17 C16 C21 C20 -1.8(14) . . . . ?
S15 C16 C21 C20 -175.0(7) . . . . ?
C17 C16 C21 O21 175.7(8) . . . . ?
S15 C16 C21 O21 2.4(13) . . . . ?
C19 C20 C21 C16 1.6(13) . . . . ?
S22 C20 C21 C16 174.6(7) . . . . ?
C19 C20 C21 O21 -175.8(8) . . . . ?
S22 C20 C21 O21 -2.8(12) . . . . ?
C16 C21 O21 C57 -92.8(10) . . . . ?
C20 C21 O21 C57 84.7(10) . . . . ?
C19 C20 S22 C23 -136.4(8) . . . . ?
C21 C20 S22 C23 50.7(9) . . . . ?
C20 S22 C23 C24 -127.8(8) . . . . ?
C20 S22 C23 C28 58.7(9) . . . . ?
C28 C23 C24 C25 1.7(14) . . . . ?
S22 C23 C24 C25 -172.2(8) . . . . ?
C25 C26 C27 C28 0.5(15) . . . . ?
C25 C26 C27 S1 172.1(7) . . . . ?
C2 S1 C27 C28 -48.2(9) . . . . ?
C2 S1 C27 C26 140.4(8) . . . . ?
C26 C27 C28 O28 -176.4(8) . . . . ?
S1 C27 C28 O28 12.4(12) . . . . ?
C26 C27 C28 C23 -2.3(14) . . . . ?
S1 C27 C28 C23 -173.6(7) . . . . ?
C24 C23 C28 C27 1.3(13) . . . . ?
S22 C23 C28 C27 174.9(7) . . . . ?
C24 C23 C28 O28 175.3(8) . . . . ?
S22 C23 C28 O28 -11.1(12) . . . . ?
C27 C28 O28 C60 -92.0(10) . . . . ?
C23 C28 O28 C60 94.0(10) . . . . ?
C5 C4 C29 C30 127.1(11) . . . . ?
C3 C4 C29 C30 -52.1(13) . . . . ?
C5 C4 C29 C31 0.7(14) . . . . ?
C3 C4 C29 C31 -178.5(9) . . . . ?
C5 C4 C29 C32 -113.4(11) . . . . ?
C3 C4 C29 C32 67.4(11) . . . . ?
C10 C11 C33 C35 11.7(14) . . . . ?
C12 C11 C33 C35 -165.9(10) . . . . ?
C10 C11 C33 C34 131.5(10) . . . . ?
C12 C11 C33 C34 -46.1(13) . . . . ?
C10 C11 C33 C36 -109.3(12) . . . . ?
C12 C11 C33 C36 73.1(14) . . . . ?
C16 C17 C18 C19 1.2(14) . . . . ?
C16 C17 C18 C37 -179.2(9) . . . . ?
C20 C19 C18 C17 -1.4(14) . . . . ?
C20 C19 C18 C37 179.0(9) . . . . ?
C17 C18 C37 C38 -106.7(14) . . . . ?
C19 C18 C37 C38 72.9(15) . . . . ?
C17 C18 C37 C38' 63.2(16) . . . . ?
C19 C18 C37 C38' -117.2(15) . . . . ?
C17 C18 C37 C40 14.6(16) . . . . ?
C19 C18 C37 C40 -165.8(15) . . . . ?
C17 C18 C37 C39' -52.2(17) . . . . ?
C19 C18 C37 C39' 127.3(16) . . . . ?
C17 C18 C37 C40' -172.7(16) . . . . ?
C19 C18 C37 C40' 6.8(18) . . . . ?
C17 C18 C37 C39 137.1(14) . . . . ?
C19 C18 C37 C39 -43.3(16) . . . . ?
C27 C26 C25 C24 2.3(14) . . . . ?
C27 C26 C25 C41 -178.5(10) . . . . ?
C23 C24 C25 C26 -3.5(14) . . . . ?
C23 C24 C25 C41 177.3(10) . . . . ?
C26 C25 C41 C42 -179.2(13) . . . . ?
C24 C25 C41 C42 0.0(18) . . . . ?
C26 C25 C41 C43 50.0(16) . . . . ?
C24 C25 C41 C43 -130.8(12) . . . . ?
C26 C25 C41 C44 -59.2(15) . . . . ?
C24 C25 C41 C44 120.0(13) . . . . ?
C7 O7 C45 C46 173.6(8) . . . . ?
O7 C45 C46 O46 2.5(15) . . . . ?
O7 C45 C46 O47 -180.0(9) . . . . ?
C14 O14 C48 C49 -168.2(9) . . . . ?
O14 C48 C49 O49 -176.6(11) . . . . ?
O14 C48 C49 N49 4.7(15) . . . . ?
O49 C49 N49 N50 -3.8(17) . . . . ?
C48 C49 N49 N50 174.8(9) . . . . ?
C49 N49 N50 C50 170.9(10) . . . . ?
N49 N50 C50 C51 -178.5(8) . . . . ?
N50 C50 C51 N56 167.9(9) . . . . ?
N50 C50 C51 C52 -8.0(15) . . . . ?
N56 C51 C52 C53 3.6(17) . . . . ?
C50 C51 C52 C53 179.1(10) . . . . ?
C51 C52 C53 C54 -1.0(16) . . . . ?
C52 C53 C54 C55 -1.9(16) . . . . ?
C53 C54 C55 N56 2.7(18) . . . . ?
C52 C51 N56 C55 -2.9(15) . . . . ?
C50 C51 N56 C55 -178.8(9) . . . . ?
C54 C55 N56 C51 -0.3(16) . . . . ?
C21 O21 C57 C58 178.5(10) . . . . ?
O21 C57 C58 O58 177.9(14) . . . . ?
O21 C57 C58 O59 -6.6(17) . . . . ?
C28 O28 C60 C61 -172.5(8) . . . . ?
O28 C60 C61 O61 -1.5(15) . . . . ?
O28 C60 C61 N61 178.7(9) . . . . ?
O61 C61 N61 N62 -175.8(10) . . . . ?
C60 C61 N61 N62 4.0(14) . . . . ?
C61 N61 N62 C62 -177.3(10) . . . . ?
N61 N62 C62 C63 -179.9(9) . . . . ?
N62 C62 C63 N68 171.5(10) . . . . ?
N62 C62 C63 C64 -7.6(16) . . . . ?
N68 C63 C64 C65 2.1(17) . . . . ?
C62 C63 C64 C65 -179.0(10) . . . . ?
C63 C64 C65 C66 -2.1(17) . . . . ?
C64 C65 C66 C67 1.0(19) . . . . ?
C65 C66 C67 N68 0(2) . . . . ?
C64 C63 N68 C67 -0.7(16) . . . . ?
C62 C63 N68 C67 -179.7(10) . . . . ?
C66 C67 N68 C63 -0.6(19) . . . . ?

_refine_diff_density_max         0.692
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.113

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 245 90 ' '
2 0.295 0.472 0.102 12 2 ' '
3 0.705 0.528 0.898 12 3 ' '
_platon_squeeze_details          
;
;

# start Validation Reply Form

_vrf_RFACR01_shelx               
;
PROBLEM: The value of the weighted R factor is > 0.45
RESPONSE: Only a small crystal could be obtained. It was hard to get
a strong diffraction pattern on such sample.
;

_vrf_PLAT026_shelx               
;
PROBLEM: Ratio Observed / Unique Reflections too Low ....         20 %     
RESPONSE: Only a small crystal could be obtained. It was hard to get
a strong diffraction pattern on such sample.
;

_vrf_PLAT084_shelx               
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.47 Report
RESPONSE: Only a small crystal could be obtained. It was hard to get
a strong diffraction pattern on such sample.
;

_vrf_RFACG01_shelx               
;
PROBLEM: The value of the R factor is > 0.15
            R factor given   0.153
RESPONSE: Only a small crystal could be obtained. It was hard to get
a strong diffraction pattern on such sample.
;

_vrf_PLAT420_shelx               
;
PROBLEM: D-H Without Acceptor        O47    -   H47    ..     Please Check 
RESPONSE: O47-H47 probably forms H-bond with solvent molecules,
which were excluded from the model by SQUEEZE.
;

_vrf_PLAT930_shelx               
;
PROBLEM: Check Twin Law ( 0 0  1)[ 0-1  3] Estimated BASF       0.40     
RESPONSE: A refinement with twinning matrix 
(-1.00  0.00  0.00  
 0.00  -1.00  0.00  
 0.06  -0.75  1.00)
gave BASF 0.01372, which is quite small.
;

# end Validation Reply Form
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: MeOH/CH2Cl2'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_sample_7
_database_code_depnum_ccdc_archive 'CCDC 1437367'
_audit_update_record             
;
2015-11-17 deposited with the CCDC.
2016-02-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'25,27-Di[(hydrazinocarbonyl)methoxy]-26,28-di[(ethoxycarbonyl)methoxy]-2,8,14,20-tetrathiacalix[4]arene '
_chemical_name_common            ?
_chemical_melting_point          442-444
_chemical_formula_moiety         'C36 H36 N4 O10 S4'
_chemical_formula_sum            'C36 H36 N4 O10 S4'
_chemical_formula_weight         812.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   9.9936(9)
_cell_length_b                   18.4615(15)
_cell_length_c                   20.6801(17)
_cell_angle_alpha                90
_cell_angle_beta                 94.046(5)
_cell_angle_gamma                90
_cell_volume                     3805.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5782
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      28.86

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.312
_shelx_estimated_absorpt_T_min   0.878
_shelx_estimated_absorpt_T_max   0.975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.916
_exptl_absorpt_correction_T_max  0.975

_exptl_absorpt_process_details   
;
G.M. Sheldrick (1998a). SADABS v.2.01, Bruker.
Siemens Area Detector Absorption Correction Program.
Bruker AXS. Madison. Wisconsin. USA
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            47387
_diffrn_reflns_av_unetI/netI     0.0729
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.974
_diffrn_reflns_theta_max         28.498
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9433
_reflns_number_gt                4234
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0878P)²+0.2624P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9433
_refine_ls_number_parameters     618
_refine_ls_number_restraints     354
_refine_ls_R_factor_all          0.1632
_refine_ls_R_factor_gt           0.0606
_refine_ls_wR_factor_ref         0.1905
_refine_ls_wR_factor_gt          0.1482
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.003
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.12129(8) 0.23683(5) 0.30675(4) 0.0633(3) Uani 1 1 d . . . . .
C2 C 0.2601(3) 0.18920(17) 0.27972(13) 0.0540(7) Uani 1 1 d . . . . .
C3 C 0.2692(4) 0.1174(2) 0.29705(15) 0.0735(10) Uani 1 1 d . . . . .
H3 H 0.2011 0.0963 0.3191 0.088 Uiso 1 1 calc R U . . .
C4 C 0.3771(5) 0.0767(2) 0.28232(19) 0.0932(13) Uani 1 1 d . . . . .
H4 H 0.3842 0.0287 0.2959 0.112 Uiso 1 1 calc R U . . .
C5 C 0.4737(4) 0.1061(3) 0.24791(19) 0.0918(13) Uani 1 1 d . . . . .
H5 H 0.5441 0.0772 0.2360 0.110 Uiso 1 1 calc R U . . .
C6 C 0.4699(3) 0.1784(2) 0.23011(15) 0.0703(10) Uani 1 1 d . . . . .
C7 C 0.3636(3) 0.22152(18) 0.24776(13) 0.0542(8) Uani 1 1 d . . . . .
S8 S 0.61095(9) 0.21588(8) 0.19413(5) 0.1045(4) Uani 1 1 d . . . . .
C9 C 0.5489(3) 0.2690(2) 0.12794(17) 0.0752(10) Uani 1 1 d . . . . .
C10 C 0.5820(4) 0.3426(3) 0.1287(2) 0.0993(14) Uani 1 1 d . . . . .
H10 H 0.6237 0.3633 0.1658 0.119 Uiso 1 1 calc R U . . .
C11 C 0.5528(5) 0.3844(3) 0.0742(3) 0.1098(15) Uani 1 1 d . . . . .
H11 H 0.5804 0.4325 0.0739 0.132 Uiso 1 1 calc R U . . .
C12 C 0.4853(4) 0.3565(3) 0.0218(2) 0.0890(12) Uani 1 1 d . . . . .
H12 H 0.4634 0.3860 -0.0138 0.107 Uiso 1 1 calc R U . . .
C13 C 0.4475(3) 0.2846(2) 0.01993(16) 0.0696(9) Uani 1 1 d . . . . .
S15 S 0.36133(11) 0.25309(6) -0.05191(4) 0.0873(3) Uani 1 1 d . . . . .
C16 C 0.2139(3) 0.2132(2) -0.02553(14) 0.0663(9) Uani 1 1 d . . . . .
C17 C 0.1791(4) 0.1444(2) -0.04595(16) 0.0831(11) Uani 1 1 d . . . . .
H17 H 0.2390 0.1174 -0.0686 0.100 Uiso 1 1 calc R U . . .
C18 C 0.0586(4) 0.1151(2) -0.03357(17) 0.0856(11) Uani 1 1 d . . . . .
H18 H 0.0358 0.0690 -0.0489 0.103 Uiso 1 1 calc R U . . .
C19 C -0.0295(4) 0.1530(2) 0.00137(16) 0.0714(9) Uani 1 1 d . . . . .
H19 H -0.1110 0.1324 0.0104 0.086 Uiso 1 1 calc R U . . .
C20 C 0.0028(3) 0.22254(18) 0.02335(14) 0.0584(8) Uani 1 1 d . . . . .
C21 C 0.1235(3) 0.25297(18) 0.00904(13) 0.0556(8) Uani 1 1 d . . . . .
S22 S -0.12262(8) 0.27311(5) 0.05963(4) 0.0702(3) Uani 1 1 d . . . . .
C23 C -0.0513(3) 0.30706(16) 0.13406(14) 0.0525(7) Uani 1 1 d . . . . .
C24 C -0.0868(3) 0.37674(18) 0.15130(18) 0.0674(9) Uani 1 1 d . . . . .
H24 H -0.1325 0.4064 0.1208 0.081 Uiso 1 1 calc R U . . .
C25 C -0.0554(3) 0.40253(19) 0.21272(19) 0.0725(10) Uani 1 1 d . . . . .
H25 H -0.0810 0.4491 0.2236 0.087 Uiso 1 1 calc R U . . .
C26 C 0.0129(3) 0.36037(18) 0.25779(17) 0.0643(9) Uani 1 1 d . . . . .
H26 H 0.0329 0.3780 0.2995 0.077 Uiso 1 1 calc R U . . .
C27 C 0.0527(3) 0.29146(16) 0.24177(14) 0.0519(7) Uani 1 1 d . . . . .
C28 C 0.0226(3) 0.26497(15) 0.17950(14) 0.0475(7) Uani 1 1 d . . . . .
C14 C 0.4831(3) 0.2405(2) 0.07244(17) 0.0675(9) Uani 1 1 d D U . . .
O14A O 0.470(2) 0.1680(6) 0.0719(12) 0.078(4) Uani 0.427(16) 1 d D U P A 1
C34A C 0.5465(18) 0.1301(7) 0.0249(6) 0.097(4) Uani 0.427(16) 1 d D U P A 1
H340 H 0.6032 0.1645 0.0042 0.116 Uiso 0.427(16) 1 calc R U P A 1
H341 H 0.4853 0.1089 -0.0084 0.116 Uiso 0.427(16) 1 calc R U P A 1
C35A C 0.6303(15) 0.0728(8) 0.0559(6) 0.069(4) Uani 0.427(16) 1 d D U P A 1
O35A O 0.6901(15) 0.0336(8) 0.0225(5) 0.138(5) Uani 0.427(16) 1 d D U P A 1
N35A N 0.641(2) 0.0680(10) 0.1181(5) 0.111(5) Uani 0.427(16) 1 d D U P A 1
H350 H 0.611(9) 0.105(3) 0.142(2) 0.133 Uiso 0.427(16) 1 d D U P A 1
N36A N 0.7192(16) 0.0170(8) 0.1587(7) 0.094(4) Uani 0.427(16) 1 d D U P A 1
H360 H 0.738(8) -0.021(3) 0.125(2) 0.141 Uiso 0.427(16) 1 d D U P A 1
H361 H 0.807(5) 0.045(3) 0.166(4) 0.141 Uiso 0.427(16) 1 d D U P A 1
O14B O 0.4363(16) 0.1686(4) 0.0733(9) 0.081(3) Uani 0.573(16) 1 d D U P A 2
C34B C 0.4896(15) 0.1194(6) 0.0265(5) 0.115(4) Uani 0.573(16) 1 d D U P A 2
H342 H 0.4169 0.0891 0.0085 0.138 Uiso 0.573(16) 1 calc R U P A 2
H343 H 0.5213 0.1478 -0.0088 0.138 Uiso 0.573(16) 1 calc R U P A 2
C35B C 0.5974(14) 0.0731(6) 0.0517(5) 0.088(3) Uani 0.573(16) 1 d D U P A 2
O35B O 0.7063(10) 0.0713(9) 0.0293(7) 0.194(6) Uani 0.573(16) 1 d D U P A 2
N35B N 0.5767(10) 0.0339(6) 0.1024(5) 0.099(3) Uani 0.573(16) 1 d D U P A 2
H351 H 0.491(4) 0.023(3) 0.111(2) 0.119 Uiso 0.573(16) 1 d D U P A 2
N36B N 0.6752(14) -0.0092(7) 0.1382(7) 0.117(4) Uani 0.573(16) 1 d D U P A 2
H362 H 0.755(4) -0.004(4) 0.110(3) 0.176 Uiso 0.573(16) 1 d D U P A 2
H363 H 0.638(5) -0.0597(17) 0.128(4) 0.176 Uiso 0.573(16) 1 d D U P A 2
O7 O 0.35922(19) 0.29241(12) 0.22812(10) 0.0607(5) Uani 1 1 d D . . . .
C29 C 0.3704(3) 0.34729(19) 0.27741(18) 0.0734(10) Uani 1 1 d D . . . .
H290 H 0.3197 0.3324 0.3134 0.088 Uiso 1 1 calc R U . . .
H291 H 0.3311 0.3919 0.2600 0.088 Uiso 1 1 calc R U . . .
C30 C 0.5109(4) 0.3613(2) 0.3015(2) 0.0846(11) Uani 1 1 d D . . . .
O30 O 0.5732(4) 0.41535(19) 0.2878(2) 0.1575(16) Uani 1 1 d D . . . .
O31 O 0.5685(2) 0.30665(15) 0.33166(13) 0.0851(7) Uani 1 1 d D . . . .
C32 C 0.7071(4) 0.3122(3) 0.3555(2) 0.1037(14) Uani 1 1 d D . . . .
H320 H 0.7165 0.3465 0.3910 0.124 Uiso 1 1 calc R U . . .
H321 H 0.7611 0.3290 0.3212 0.124 Uiso 1 1 calc R U . . .
C33 C 0.7514(4) 0.2408(3) 0.3774(2) 0.1269(19) Uani 1 1 d D . . . .
H330 H 0.6979 0.2249 0.4115 0.190 Uiso 1 1 calc R U . . .
H331 H 0.8439 0.2430 0.3934 0.190 Uiso 1 1 calc R U . . .
H332 H 0.7417 0.2073 0.3419 0.190 Uiso 1 1 calc R U . . .
O21 O 0.1569(2) 0.32153(12) 0.03076(10) 0.0632(6) Uani 1 1 d D . . . .
C37 C 0.1149(4) 0.3766(2) -0.0138(2) 0.0973(12) Uani 1 1 d D U . . .
H370 H 0.0178 0.3771 -0.0205 0.117 Uiso 1 1 calc R U . B 1
H371 H 0.1521 0.3683 -0.0552 0.117 Uiso 1 1 calc R U . B 1
C38A C 0.1647(18) 0.4471(6) 0.0149(8) 0.110(4) Uani 0.53(2) 1 d D U P C 1
O38A O 0.178(2) 0.5011(7) -0.0141(10) 0.198(7) Uani 0.53(2) 1 d D U P C 1
O39A O 0.1958(19) 0.4465(7) 0.0782(7) 0.115(4) Uani 0.53(2) 1 d D U P C 1
C40A C 0.240(3) 0.5186(9) 0.1016(10) 0.162(7) Uani 0.53(2) 1 d D U P C 1
H400 H 0.3353 0.5176 0.1133 0.194 Uiso 0.53(2) 1 calc R U P C 1
H401 H 0.2236 0.5535 0.0668 0.194 Uiso 0.53(2) 1 calc R U P C 1
C41A C 0.170(2) 0.5418(9) 0.1572(7) 0.157(6) Uani 0.53(2) 1 d D U P C 1
H410 H 0.1878 0.5083 0.1922 0.235 Uiso 0.53(2) 1 calc R U P C 1
H411 H 0.0752 0.5433 0.1457 0.235 Uiso 0.53(2) 1 calc R U P C 1
H412 H 0.2006 0.5892 0.1704 0.235 Uiso 0.53(2) 1 calc R U P C 1
C38B C 0.1668(19) 0.4482(6) -0.0026(7) 0.094(4) Uani 0.47(2) 1 d D U P C 2
O38B O 0.180(2) 0.4909(8) -0.0438(8) 0.142(5) Uani 0.47(2) 1 d D U P C 2
O39B O 0.189(2) 0.4599(7) 0.0582(7) 0.112(4) Uani 0.47(2) 1 d D U P C 2
C40B C 0.240(4) 0.5294(11) 0.0806(9) 0.178(8) Uani 0.47(2) 1 d D U P C 2
H402 H 0.1749 0.5677 0.0719 0.213 Uiso 0.47(2) 1 calc R U P C 2
H403 H 0.3230 0.5418 0.0613 0.213 Uiso 0.47(2) 1 calc R U P C 2
C41B C 0.263(3) 0.5145(11) 0.1514(9) 0.163(9) Uani 0.47(2) 1 d D U P C 2
H413 H 0.3271 0.4760 0.1581 0.245 Uiso 0.47(2) 1 calc R U P C 2
H414 H 0.1800 0.5006 0.1684 0.245 Uiso 0.47(2) 1 calc R U P C 2
H415 H 0.2969 0.5573 0.1732 0.245 Uiso 0.47(2) 1 calc R U P C 2
O28 O 0.07315(18) 0.19909(10) 0.16184(9) 0.0531(5) Uani 1 1 d . . . . .
C42 C -0.0080(3) 0.13755(16) 0.17050(17) 0.0665(9) Uani 1 1 d . . . . .
H420 H -0.0921 0.1421 0.1444 0.080 Uiso 1 1 calc R U . . .
H421 H -0.0278 0.1334 0.2156 0.080 Uiso 1 1 calc R U . . .
C43 C 0.0673(4) 0.07081(19) 0.15013(15) 0.0674(9) Uani 1 1 d D . . . .
O43 O 0.0129(3) 0.01244(15) 0.15328(14) 0.1079(10) Uani 1 1 d . . . . .
N43 N 0.1875(3) 0.08084(16) 0.13032(15) 0.0757(8) Uani 1 1 d D . . . .
H430 H 0.221(3) 0.1266(17) 0.1298(17) 0.091 Uiso 1 1 d D U . . .
N44 N 0.2714(4) 0.02322(19) 0.11299(19) 0.1076(12) Uani 1 1 d D . . . .
H440 H 0.229(4) 0.008(2) 0.0690(16) 0.161 Uiso 1 1 d D U . . .
H441 H 0.245(4) -0.0165(16) 0.144(2) 0.161 Uiso 1 1 d D U . . .


_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
S1 C2 1.766(3) . ?
S1 C27 1.779(3) . ?
C2 C3 1.374(4) . ?
C2 C7 1.399(4) . ?
C3 C4 1.367(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.353(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.383(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.397(4) . ?
C6 S8 1.780(4) . ?
C7 O7 1.370(4) . ?
S8 C9 1.761(4) . ?
C9 C14 1.385(5) . ?
C9 C10 1.398(6) . ?
C10 C11 1.380(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.339(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.381(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.383(5) . ?
C13 S15 1.762(4) . ?
S15 C16 1.767(3) . ?
C16 C17 1.376(5) . ?
C16 C21 1.400(4) . ?
C17 C18 1.362(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.370(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.391(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.381(4) . ?
C20 S22 1.772(3) . ?
C21 O21 1.376(4) . ?
S22 C23 1.765(3) . ?
C23 C24 1.388(4) . ?
C23 C28 1.390(4) . ?
C24 C25 1.372(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.360(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.380(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.390(4) . ?
C28 O28 1.376(3) . ?
C14 O14A 1.346(11) . ?
C14 O14B 1.409(9) . ?
O14A C34A 1.457(11) . ?
C34A C35A 1.469(11) . ?
C34A H340 0.9700 . ?
C34A H341 0.9700 . ?
C35A O35A 1.190(11) . ?
C35A N35A 1.285(11) . ?
N35A N36A 1.454(11) . ?
N35A H350 0.92(3) . ?
N36A H360 1.02(3) . ?
N36A H361 1.02(3) . ?
O14B C34B 1.456(10) . ?
C34B C35B 1.444(10) . ?
C34B H342 0.9700 . ?
C34B H343 0.9700 . ?
C35B O35B 1.212(11) . ?
C35B N35B 1.303(10) . ?
N35B N36B 1.431(9) . ?
N35B H351 0.91(3) . ?
O7 C29 1.436(4) . ?
C29 C30 1.478(5) . ?
C29 H290 0.9700 . ?
C29 H291 0.9700 . ?
C30 O30 1.220(4) . ?
C30 O31 1.300(4) . ?
O31 C32 1.441(4) . ?
C32 C33 1.455(6) . ?
C32 H320 0.9700 . ?
C32 H321 0.9700 . ?
C33 H330 0.9600 . ?
C33 H331 0.9600 . ?
C33 H332 0.9600 . ?
O21 C37 1.416(4) . ?
C37 C38B 1.434(10) . ?
C37 C38A 1.501(11) . ?
C37 H370 0.9700 . ?
C37 H371 0.9700 . ?
C38A O38A 1.176(11) . ?
C38A O39A 1.323(11) . ?
O39A C40A 1.473(11) . ?
C40A C41A 1.450(15) . ?
C40A H400 0.9700 . ?
C40A H401 0.9700 . ?
C41A H410 0.9600 . ?
C41A H411 0.9600 . ?
C41A H412 0.9600 . ?
C38B O38B 1.177(10) . ?
C38B O39B 1.281(11) . ?
O39B C40B 1.443(12) . ?
C40B C41B 1.491(16) . ?
C40B H402 0.9700 . ?
C40B H403 0.9700 . ?
C41B H413 0.9600 . ?
C41B H414 0.9600 . ?
C41B H415 0.9600 . ?
O28 C42 1.415(3) . ?
C42 C43 1.519(5) . ?
C42 H420 0.9700 . ?
C42 H421 0.9700 . ?
C43 O43 1.211(4) . ?
C43 N43 1.309(5) . ?
N43 N44 1.416(4) . ?
N43 H430 0.91(3) . ?
N44 H440 1.02(3) . ?
N44 H441 1.02(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
C2 S1 C27 108.22(13) . . ?
C3 C2 C7 119.8(3) . . ?
C3 C2 S1 115.9(3) . . ?
C7 C2 S1 124.1(2) . . ?
C4 C3 C2 120.8(4) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C5 C4 C3 119.9(4) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 121.4(3) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C6 C7 119.2(3) . . ?
C5 C6 S8 118.6(3) . . ?
C7 C6 S8 121.8(3) . . ?
O7 C7 C6 118.4(3) . . ?
O7 C7 C2 122.6(3) . . ?
C6 C7 C2 118.7(3) . . ?
C9 S8 C6 107.19(15) . . ?
C14 C9 C10 118.4(4) . . ?
C14 C9 S8 123.6(3) . . ?
C10 C9 S8 117.5(3) . . ?
C11 C10 C9 119.9(4) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C12 C11 C10 120.7(4) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 121.0(4) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C14 119.2(4) . . ?
C12 C13 S15 117.2(3) . . ?
C14 C13 S15 123.5(3) . . ?
C13 S15 C16 104.21(14) . . ?
C17 C16 C21 118.9(3) . . ?
C17 C16 S15 119.2(3) . . ?
C21 C16 S15 121.4(3) . . ?
C18 C17 C16 121.2(4) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C17 C18 C19 120.3(4) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C18 C19 C20 120.1(3) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C21 C20 C19 119.4(3) . . ?
C21 C20 S22 122.1(3) . . ?
C19 C20 S22 118.0(3) . . ?
O21 C21 C20 120.0(3) . . ?
O21 C21 C16 119.9(3) . . ?
C20 C21 C16 120.1(3) . . ?
C23 S22 C20 107.59(13) . . ?
C24 C23 C28 118.5(3) . . ?
C24 C23 S22 117.3(2) . . ?
C28 C23 S22 123.6(2) . . ?
C25 C24 C23 120.9(3) . . ?
C25 C24 H24 119.5 . . ?
C23 C24 H24 119.5 . . ?
C26 C25 C24 120.4(3) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C27 120.1(3) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C26 C27 C28 119.9(3) . . ?
C26 C27 S1 116.3(2) . . ?
C28 C27 S1 123.2(2) . . ?
O28 C28 C27 119.8(3) . . ?
O28 C28 C23 120.1(3) . . ?
C27 C28 C23 119.9(3) . . ?
O14A C14 C13 124.0(12) . . ?
O14A C14 C9 115.1(12) . . ?
C13 C14 C9 120.6(4) . . ?
C13 C14 O14B 119.8(9) . . ?
C9 C14 O14B 119.0(9) . . ?
C14 O14A C34A 115.3(12) . . ?
O14A C34A C35A 111.3(10) . . ?
O14A C34A H340 109.4 . . ?
C35A C34A H340 109.4 . . ?
O14A C34A H341 109.4 . . ?
C35A C34A H341 109.4 . . ?
H340 C34A H341 108.0 . . ?
O35A C35A N35A 122.2(10) . . ?
O35A C35A C34A 118.5(9) . . ?
N35A C35A C34A 119.3(9) . . ?
C35A N35A N36A 128.5(9) . . ?
C35A N35A H350 119(3) . . ?
N36A N35A H350 111(3) . . ?
N35A N36A H360 100(2) . . ?
N35A N36A H361 100(2) . . ?
H360 N36A H361 104(4) . . ?
C14 O14B C34B 116.3(9) . . ?
C35B C34B O14B 115.4(9) . . ?
C35B C34B H342 108.4 . . ?
O14B C34B H342 108.4 . . ?
C35B C34B H343 108.4 . . ?
O14B C34B H343 108.4 . . ?
H342 C34B H343 107.5 . . ?
O35B C35B N35B 119.3(9) . . ?
O35B C35B C34B 123.1(10) . . ?
N35B C35B C34B 117.5(9) . . ?
C35B N35B N36B 125.6(8) . . ?
C35B N35B H351 119(3) . . ?
N36B N35B H351 114(3) . . ?
C7 O7 C29 117.7(2) . . ?
O7 C29 C30 112.8(3) . . ?
O7 C29 H290 109.0 . . ?
C30 C29 H290 109.0 . . ?
O7 C29 H291 109.0 . . ?
C30 C29 H291 109.0 . . ?
H290 C29 H291 107.8 . . ?
O30 C30 O31 122.0(4) . . ?
O30 C30 C29 123.6(4) . . ?
O31 C30 C29 113.8(3) . . ?
C30 O31 C32 119.4(3) . . ?
O31 C32 C33 107.8(4) . . ?
O31 C32 H320 110.1 . . ?
C33 C32 H320 110.1 . . ?
O31 C32 H321 110.1 . . ?
C33 C32 H321 110.1 . . ?
H320 C32 H321 108.5 . . ?
C32 C33 H330 109.5 . . ?
C32 C33 H331 109.5 . . ?
H330 C33 H331 109.5 . . ?
C32 C33 H332 109.5 . . ?
H330 C33 H332 109.5 . . ?
H331 C33 H332 109.5 . . ?
C21 O21 C37 113.2(3) . . ?
O21 C37 C38B 118.0(6) . . ?
O21 C37 C38A 106.9(7) . . ?
O21 C37 H370 110.4 . . ?
C38A C37 H370 110.4 . . ?
O21 C37 H371 110.4 . . ?
C38A C37 H371 110.4 . . ?
H370 C37 H371 108.6 . . ?
O38A C38A O39A 119.0(11) . . ?
O38A C38A C37 125.4(12) . . ?
O39A C38A C37 115.6(9) . . ?
C38A O39A C40A 111.1(10) . . ?
C41A C40A O39A 112.3(13) . . ?
C41A C40A H400 109.2 . . ?
O39A C40A H400 109.2 . . ?
C41A C40A H401 109.1 . . ?
O39A C40A H401 109.2 . . ?
H400 C40A H401 107.9 . . ?
C40A C41A H410 109.5 . . ?
C40A C41A H411 109.5 . . ?
H410 C41A H411 109.5 . . ?
C40A C41A H412 109.5 . . ?
H410 C41A H412 109.5 . . ?
H411 C41A H412 109.5 . . ?
O38B C38B O39B 125.3(11) . . ?
O38B C38B C37 124.1(12) . . ?
O39B C38B C37 110.6(10) . . ?
C38B O39B C40B 119.9(11) . . ?
O39B C40B C41B 100.2(13) . . ?
O39B C40B H402 111.7 . . ?
C41B C40B H402 111.7 . . ?
O39B C40B H403 111.7 . . ?
C41B C40B H403 111.7 . . ?
H402 C40B H403 109.5 . . ?
C40B C41B H413 109.5 . . ?
C40B C41B H414 109.5 . . ?
H413 C41B H414 109.5 . . ?
C40B C41B H415 109.5 . . ?
H413 C41B H415 109.5 . . ?
H414 C41B H415 109.5 . . ?
C28 O28 C42 116.8(2) . . ?
O28 C42 C43 108.5(3) . . ?
O28 C42 H420 110.0 . . ?
C43 C42 H420 110.0 . . ?
O28 C42 H421 110.0 . . ?
C43 C42 H421 110.0 . . ?
H420 C42 H421 108.4 . . ?
O43 C43 N43 124.6(4) . . ?
O43 C43 C42 118.3(4) . . ?
N43 C43 C42 117.1(3) . . ?
C43 N43 N44 123.1(3) . . ?
C43 N43 H430 119(2) . . ?
N44 N43 H430 118(2) . . ?
N43 N44 H440 102.5(19) . . ?
N43 N44 H441 101.4(19) . . ?
H440 N44 H441 104(4) . . ?

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
C27 S1 C2 C3 -136.7(2) . . . . ?
C27 S1 C2 C7 49.1(3) . . . . ?
C7 C2 C3 C4 -1.3(5) . . . . ?
S1 C2 C3 C4 -175.7(3) . . . . ?
C2 C3 C4 C5 -2.8(6) . . . . ?
C3 C4 C5 C6 3.7(6) . . . . ?
C4 C5 C6 C7 -0.4(6) . . . . ?
C4 C5 C6 S8 172.0(3) . . . . ?
C5 C6 C7 O7 -178.1(3) . . . . ?
S8 C6 C7 O7 9.7(4) . . . . ?
C5 C6 C7 C2 -3.6(4) . . . . ?
S8 C6 C7 C2 -175.8(2) . . . . ?
C3 C2 C7 O7 178.7(3) . . . . ?
S1 C2 C7 O7 -7.3(4) . . . . ?
C3 C2 C7 C6 4.5(4) . . . . ?
S1 C2 C7 C6 178.5(2) . . . . ?
C5 C6 S8 C9 136.0(3) . . . . ?
C7 C6 S8 C9 -51.7(3) . . . . ?
C6 S8 C9 C14 -67.2(3) . . . . ?
C6 S8 C9 C10 120.6(3) . . . . ?
C14 C9 C10 C11 -2.0(5) . . . . ?
S8 C9 C10 C11 170.7(3) . . . . ?
C9 C10 C11 C12 4.3(6) . . . . ?
C10 C11 C12 C13 -2.5(6) . . . . ?
C11 C12 C13 C14 -1.6(5) . . . . ?
C11 C12 C13 S15 -179.0(3) . . . . ?
C12 C13 S15 C16 -126.4(3) . . . . ?
C14 C13 S15 C16 56.3(3) . . . . ?
C13 S15 C16 C17 -129.8(3) . . . . ?
C13 S15 C16 C21 58.1(3) . . . . ?
C21 C16 C17 C18 0.6(5) . . . . ?
S15 C16 C17 C18 -171.7(3) . . . . ?
C16 C17 C18 C19 -1.9(6) . . . . ?
C17 C18 C19 C20 1.3(5) . . . . ?
C18 C19 C20 C21 0.7(5) . . . . ?
C18 C19 C20 S22 172.5(3) . . . . ?
C19 C20 C21 O21 -179.7(3) . . . . ?
S22 C20 C21 O21 8.8(4) . . . . ?
C19 C20 C21 C16 -2.0(4) . . . . ?
S22 C20 C21 C16 -173.5(2) . . . . ?
C17 C16 C21 O21 179.1(3) . . . . ?
S15 C16 C21 O21 -8.8(4) . . . . ?
C17 C16 C21 C20 1.4(4) . . . . ?
S15 C16 C21 C20 173.5(2) . . . . ?
C21 C20 S22 C23 -58.4(3) . . . . ?
C19 C20 S22 C23 130.0(2) . . . . ?
C20 S22 C23 C24 141.2(2) . . . . ?
C20 S22 C23 C28 -47.8(3) . . . . ?
C28 C23 C24 C25 -3.0(4) . . . . ?
S22 C23 C24 C25 168.4(2) . . . . ?
C23 C24 C25 C26 0.9(5) . . . . ?
C24 C25 C26 C27 0.8(5) . . . . ?
C25 C26 C27 C28 -0.2(4) . . . . ?
C25 C26 C27 S1 -171.9(2) . . . . ?
C2 S1 C27 C26 -139.0(2) . . . . ?
C2 S1 C27 C28 49.6(3) . . . . ?
C26 C27 C28 O28 173.8(2) . . . . ?
S1 C27 C28 O28 -15.0(4) . . . . ?
C26 C27 C28 C23 -2.1(4) . . . . ?
S1 C27 C28 C23 169.1(2) . . . . ?
C24 C23 C28 O28 -172.3(2) . . . . ?
S22 C23 C28 O28 16.8(4) . . . . ?
C24 C23 C28 C27 3.6(4) . . . . ?
S22 C23 C28 C27 -167.3(2) . . . . ?
C12 C13 C14 O14A -169.3(8) . . . . ?
S15 C13 C14 O14A 7.9(9) . . . . ?
C12 C13 C14 C9 3.9(5) . . . . ?
S15 C13 C14 C9 -178.9(2) . . . . ?
C12 C13 C14 O14B 175.0(6) . . . . ?
S15 C13 C14 O14B -7.8(7) . . . . ?
C10 C9 C14 O14A 171.7(7) . . . . ?
S8 C9 C14 O14A -0.5(8) . . . . ?
C10 C9 C14 C13 -2.1(4) . . . . ?
S8 C9 C14 C13 -174.2(2) . . . . ?
C10 C9 C14 O14B -173.3(6) . . . . ?
S8 C9 C14 O14B 14.6(7) . . . . ?
C13 C14 O14A C34A 61(2) . . . . ?
C9 C14 O14A C34A -112.4(16) . . . . ?
C14 O14A C34A C35A 126.9(18) . . . . ?
O14A C34A C35A O35A 174.1(19) . . . . ?
O14A C34A C35A N35A -8(2) . . . . ?
O35A C35A N35A N36A -1(2) . . . . ?
C34A C35A N35A N36A -178.7(14) . . . . ?
C13 C14 O14B C34B 68.2(13) . . . . ?
C9 C14 O14B C34B -120.6(11) . . . . ?
C14 O14B C34B C35B 99.5(16) . . . . ?
O14B C34B C35B O35B -123.4(16) . . . . ?
O14B C34B C35B N35B 53.8(18) . . . . ?
O35B C35B N35B N36B 4.2(18) . . . . ?
C34B C35B N35B N36B -173.0(10) . . . . ?
C6 C7 O7 C29 -116.2(3) . . . . ?
C2 C7 O7 C29 69.5(3) . . . . ?
C7 O7 C29 C30 81.4(4) . . . . ?
O7 C29 C30 O30 106.1(5) . . . . ?
O7 C29 C30 O31 -65.2(4) . . . . ?
O30 C30 O31 C32 6.2(6) . . . . ?
C29 C30 O31 C32 177.7(3) . . . . ?
C30 O31 C32 C33 -171.0(4) . . . . ?
C20 C21 O21 C37 -90.8(4) . . . . ?
C16 C21 O21 C37 91.5(3) . . . . ?
C21 O21 C37 C38B -167.8(10) . . . . ?
C21 O21 C37 C38A -177.0(8) . . . . ?
O21 C37 C38A O38A 160.2(15) . . . . ?
O21 C37 C38A O39A -19.5(13) . . . . ?
O38A C38A O39A C40A 2(2) . . . . ?
C37 C38A O39A C40A -178.3(17) . . . . ?
C38A O39A C40A C41A 130(2) . . . . ?
O21 C37 C38B O38B 152.0(13) . . . . ?
O21 C37 C38B O39B -31.2(14) . . . . ?
O38B C38B O39B C40B -2(3) . . . . ?
C37 C38B O39B C40B -179(2) . . . . ?
C38B O39B C40B C41B -174(2) . . . . ?
C27 C28 O28 C42 92.2(3) . . . . ?
C23 C28 O28 C42 -91.9(3) . . . . ?
C28 O28 C42 C43 -178.4(2) . . . . ?
O28 C42 C43 O43 -179.0(3) . . . . ?
O28 C42 C43 N43 1.0(4) . . . . ?
O43 C43 N43 N44 -3.2(6) . . . . ?
C42 C43 N43 N44 176.8(3) . . . . ?

_refine_diff_density_max         0.622
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.047


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane'
