#------------------------------------------------------------------------------
#$Date: 2019-11-28 19:40:49 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244423 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/07/4350746.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4350746
loop_
_publ_author_name
'Akine, Shigehisa'
'Miyashita, Masato'
'Piao, Shunjin'
'Nabeshima, Tatsuya'
_publ_section_title
;
 Perfect encapsulation of a guanidinium ion in a helical trinickel(ii)
 metallocryptand for efficient regulation of the helix inversion rate
;
_journal_issue                   1
_journal_name_full               'Inorg. Chem. Front.'
_journal_page_first              53
_journal_paper_doi               10.1039/C3QI00067B
_journal_volume                  1
_journal_year                    2014
_chemical_formula_moiety         C124H180N6O26S11
_chemical_formula_sum            'C124 H180 N6 O26 S11'
_chemical_formula_weight         2523.40
_chemical_name_common            C102H108N6O12(Me2SO)11(H2O)3
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   24.1319(10)
_cell_length_b                   24.1319(10)
_cell_length_c                   43.5952(18)
_cell_measurement_reflns_used    39568
_cell_measurement_temperature    120
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.16
_cell_volume                     21986.3(16)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2009)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2009)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  ORTEP-3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayer confocal mirror'
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            39568
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  0.9865
_exptl_absorpt_correction_T_min  0.9143
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             8100
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     999
_refine_ls_number_reflns         8570
_refine_ls_number_restraints     1210
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0962
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0534P)²+145.2930P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2112
_refine_ls_wR_factor_ref         0.2262
_reflns_number_gt                6674
_reflns_number_total             8570
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3qi00067b.txt
_cod_data_source_block           H6L
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4350746
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.39963(19) 0.69206(19) 0.36891(9) 0.0550(10) Uani 1 1 d . . .
C2 C 0.35827(19) 0.62600(19) 0.36902(9) 0.0548(10) Uani 1 1 d . . .
H1 H 0.3755 0.5982 0.3692 0.066 Uiso 1 1 calc R . .
C3 C 0.35317(16) 0.62093(16) 0.21145(7) 0.0396(8) Uani 1 1 d . . .
C4 C 0.39802(16) 0.68608(16) 0.21149(7) 0.0407(8) Uani 1 1 d . . .
H2 H 0.4423 0.6994 0.2115 0.049 Uiso 1 1 calc R . .
C5 C 0.47070(19) 0.71956(19) 0.36950(9) 0.0556(10) Uani 1 1 d . . .
C6 C 0.50150(19) 0.69332(19) 0.35245(9) 0.0538(9) Uani 1 1 d . . .
C7 C 0.56769(19) 0.7199(2) 0.35462(9) 0.0560(10) Uani 1 1 d . . .
C8 C 0.6040(2) 0.7750(2) 0.37269(9) 0.0591(10) Uani 1 1 d . . .
H3 H 0.6491 0.7931 0.3737 0.071 Uiso 1 1 calc R . .
C9 C 0.5755(2) 0.8034(2) 0.38890(10) 0.0590(10) Uani 1 1 d . . .
C10 C 0.5084(2) 0.7738(2) 0.38720(9) 0.0579(10) Uani 1 1 d . . .
H4 H 0.4877 0.7917 0.3987 0.069 Uiso 1 1 calc R . .
O1 O 0.46626(13) 0.64262(14) 0.33402(7) 0.0602(7) Uani 1 1 d . . .
H5 H 0.4906 0.6332 0.3244 0.090 Uiso 1 1 calc R . .
C11 C 0.6126(2) 0.8636(2) 0.40849(11) 0.0705(13) Uani 1 1 d . . .
C12 C 0.5980(3) 0.9152(2) 0.39687(15) 0.0912(17) Uani 1 1 d . . .
H6 H 0.6213 0.9540 0.4094 0.137 Uiso 1 1 calc R . .
H7 H 0.5519 0.8993 0.3985 0.137 Uiso 1 1 calc R . .
H8 H 0.6114 0.9253 0.3754 0.137 Uiso 1 1 calc R . .
C13 C 0.5917(2) 0.8475(3) 0.44199(11) 0.0904(18) Uani 1 1 d . . .
H9 H 0.6150 0.8860 0.4546 0.136 Uiso 1 1 calc R . .
H10 H 0.6011 0.8146 0.4492 0.136 Uiso 1 1 calc R . .
H11 H 0.5457 0.8315 0.4436 0.136 Uiso 1 1 calc R . .
C14 C 0.6847(2) 0.8899(2) 0.40645(12) 0.0775(14) Uani 1 1 d . . .
H12 H 0.7071 0.9284 0.4191 0.116 Uiso 1 1 calc R . .
H13 H 0.6986 0.9005 0.3851 0.116 Uiso 1 1 calc R . .
H14 H 0.6947 0.8575 0.4138 0.116 Uiso 1 1 calc R . .
C15 C 0.60065(19) 0.6921(2) 0.33859(9) 0.0558(10) Uani 1 1 d . A .
H15 H 0.6456 0.7109 0.3409 0.067 Uiso 1 1 calc R . .
N1 N 0.57042(15) 0.64232(16) 0.32118(7) 0.0528(8) Uani 1 1 d . . .
C16 C 0.60292(17) 0.61390(17) 0.30724(9) 0.0498(6) Uani 0.50 1 d PDU A 1
C17 C 0.6582(4) 0.6181(5) 0.3202(3) 0.0626(15) Uani 0.50 1 d PDU A 1
H16 H 0.6736 0.6388 0.3394 0.075 Uiso 0.50 1 calc PR A 1
C18 C 0.6898(4) 0.5924(5) 0.3052(2) 0.0629(15) Uani 0.50 1 d PDU A 1
C19 C 0.6678(5) 0.5618(6) 0.2772(2) 0.0695(15) Uani 0.50 1 d PDU A 1
C20 C 0.6134(5) 0.5571(7) 0.2642(3) 0.0663(18) Uani 0.50 1 d PDU A 1
H17 H 0.5991 0.5376 0.2447 0.080 Uiso 0.50 1 calc PR A 1
C21 C 0.57940(17) 0.58107(17) 0.27987(9) 0.0471(6) Uani 0.50 1 d PDU A 1
O2 O 0.7429(4) 0.5916(6) 0.3165(2) 0.083(2) Uani 0.50 1 d PDU A 1
C22 C 0.7740(6) 0.6333(7) 0.3419(3) 0.099(4) Uani 0.50 1 d PDU A 1
H18 H 0.8104 0.6290 0.3484 0.149 Uiso 0.50 1 calc PR A 1
H19 H 0.7436 0.6219 0.3589 0.149 Uiso 0.50 1 calc PR A 1
H20 H 0.7891 0.6777 0.3357 0.149 Uiso 0.50 1 calc PR A 1
O3 O 0.7049(4) 0.5397(5) 0.2642(2) 0.106(2) Uani 0.50 1 d PDU A 1
C23 C 0.6835(8) 0.5084(9) 0.2349(3) 0.144(5) Uani 0.50 1 d PDU A 1
H21 H 0.7103 0.4904 0.2288 0.215 Uiso 0.50 1 calc PR A 1
H22 H 0.6869 0.5396 0.2195 0.215 Uiso 0.50 1 calc PR A 1
H23 H 0.6389 0.4740 0.2366 0.215 Uiso 0.50 1 calc PR A 1
C24 C 0.60292(17) 0.61390(17) 0.30724(9) 0.0498(6) Uani 0.50 1 d PDU A 2
C25 C 0.6543(4) 0.6126(5) 0.3219(3) 0.0556(14) Uani 0.50 1 d PDU A 2
H24 H 0.6695 0.6341 0.3409 0.067 Uiso 0.50 1 calc PR A 2
C26 C 0.6829(4) 0.5811(5) 0.3094(2) 0.0572(12) Uani 0.50 1 d PDU A 2
C27 C 0.6601(4) 0.5487(5) 0.2818(2) 0.0613(13) Uani 0.50 1 d PDU A 2
C28 C 0.6095(5) 0.5494(5) 0.2672(3) 0.0539(14) Uani 0.50 1 d PDU A 2
H25 H 0.5948 0.5279 0.2481 0.065 Uiso 0.50 1 calc PR A 2
C29 C 0.57940(17) 0.58107(17) 0.27987(9) 0.0471(6) Uani 0.50 1 d PDU A 2
O4 O 0.7340(4) 0.5780(5) 0.3216(3) 0.0777(18) Uani 0.50 1 d PDU A 2
C30 C 0.7575(7) 0.6062(7) 0.3510(3) 0.098(4) Uani 0.50 1 d PDU A 2
H26 H 0.7924 0.5990 0.3572 0.148 Uiso 0.50 1 calc PR A 2
H27 H 0.7228 0.5866 0.3661 0.148 Uiso 0.50 1 calc PR A 2
H28 H 0.7733 0.6523 0.3499 0.148 Uiso 0.50 1 calc PR A 2
O5 O 0.6907(4) 0.5179(4) 0.2706(2) 0.091(2) Uani 0.50 1 d PDU A 2
C31 C 0.6569(7) 0.4710(7) 0.2464(4) 0.123(4) Uani 0.50 1 d PDU A 2
H29 H 0.6826 0.4521 0.2399 0.184 Uiso 0.50 1 calc PR A 2
H30 H 0.6499 0.4923 0.2289 0.184 Uiso 0.50 1 calc PR A 2
H31 H 0.6156 0.4374 0.2542 0.184 Uiso 0.50 1 calc PR A 2
N2 N 0.52525(13) 0.57884(14) 0.26578(7) 0.0443(7) Uani 1 1 d . . .
C32 C 0.48760(17) 0.52948(17) 0.24954(8) 0.0457(8) Uani 1 1 d . A .
H32 H 0.4945 0.4940 0.2493 0.055 Uiso 1 1 calc R . .
C33 C 0.43536(16) 0.52574(16) 0.23173(8) 0.0426(8) Uani 1 1 d . . .
C34 C 0.42225(16) 0.57621(16) 0.23072(7) 0.0404(8) Uani 1 1 d . A .
C35 C 0.37232(16) 0.57108(16) 0.21214(7) 0.0403(8) Uani 1 1 d . . .
C36 C 0.33721(16) 0.51525(16) 0.19501(8) 0.0424(8) Uani 1 1 d . A .
H33 H 0.3043 0.5123 0.1820 0.051 Uiso 1 1 calc R . .
C37 C 0.34799(18) 0.46339(17) 0.19606(8) 0.0476(9) Uani 1 1 d . . .
C38 C 0.39741(17) 0.46984(17) 0.21464(8) 0.0479(9) Uani 1 1 d . A .
H34 H 0.4060 0.4355 0.2159 0.057 Uiso 1 1 calc R . .
O6 O 0.45622(12) 0.62910(11) 0.24820(5) 0.0466(6) Uani 1 1 d . . .
H35 H 0.4820 0.6243 0.2592 0.070 Uiso 1 1 calc R A .
C39 C 0.3065(2) 0.40334(18) 0.17681(9) 0.0580(10) Uani 1 1 d . A .
C40 C 0.3152(4) 0.3477(2) 0.18726(17) 0.162(4) Uani 1 1 d . . .
H36 H 0.2884 0.3099 0.1747 0.243 Uiso 1 1 calc R A .
H37 H 0.3027 0.3380 0.2088 0.243 Uiso 1 1 calc R . .
H38 H 0.3602 0.3595 0.1850 0.243 Uiso 1 1 calc R . .
C41 C 0.3274(2) 0.4178(2) 0.14391(10) 0.0699(12) Uani 1 1 d . . .
H39 H 0.3014 0.3799 0.1313 0.105 Uiso 1 1 calc R A .
H40 H 0.3725 0.4299 0.1422 0.105 Uiso 1 1 calc R . .
H41 H 0.3219 0.4533 0.1367 0.105 Uiso 1 1 calc R . .
C42 C 0.2361(2) 0.3854(3) 0.17836(14) 0.099(2) Uani 1 1 d . . .
H42 H 0.2104 0.3470 0.1660 0.148 Uiso 1 1 calc R A .
H43 H 0.2315 0.4208 0.1704 0.148 Uiso 1 1 calc R . .
H44 H 0.2215 0.3770 0.1997 0.148 Uiso 1 1 calc R . .
S1 S 0.28629(7) 0.45845(7) 0.30268(4) 0.0675(4) Uani 0.75 1 d PDU B 1
O7 O 0.2940(3) 0.4106(3) 0.28168(17) 0.126(2) Uani 0.75 1 d PDU B 1
C43 C 0.3654(3) 0.5052(4) 0.3160(2) 0.106(3) Uani 0.75 1 d PDU B 1
H45 H 0.3773 0.4782 0.3278 0.158 Uiso 0.75 1 calc PR B 1
H46 H 0.3685 0.5396 0.3291 0.158 Uiso 0.75 1 calc PR B 1
H47 H 0.3944 0.5237 0.2985 0.158 Uiso 0.75 1 calc PR B 1
C44 C 0.2783(4) 0.5119(4) 0.2810(2) 0.126(3) Uani 0.75 1 d PDU B 1
H48 H 0.2350 0.4916 0.2724 0.189 Uiso 0.75 1 calc PR B 1
H49 H 0.3097 0.5267 0.2643 0.189 Uiso 0.75 1 calc PR B 1
H50 H 0.2856 0.5485 0.2937 0.189 Uiso 0.75 1 calc PR B 1
S2 S 0.3457(3) 0.4849(3) 0.29129(15) 0.0533(14) Uani 0.15 1 d PDU C 2
O8 O 0.2918(8) 0.4388(8) 0.2701(4) 0.055(3) Uani 0.15 1 d PDU C 2
C45 C 0.3135(10) 0.5413(8) 0.2904(5) 0.047(3) Uani 0.15 1 d PDU C 2
H51 H 0.3051 0.5480 0.2691 0.071 Uiso 0.15 1 calc PR C 2
H52 H 0.3449 0.5824 0.2994 0.071 Uiso 0.15 1 calc PR C 2
H53 H 0.2736 0.5231 0.3022 0.071 Uiso 0.15 1 calc PR C 2
C46 C 0.3335(12) 0.4689(11) 0.3291(3) 0.050(4) Uani 0.15 1 d PDU C 2
H54 H 0.3667 0.4610 0.3373 0.075 Uiso 0.15 1 calc PR C 2
H55 H 0.2913 0.4309 0.3323 0.075 Uiso 0.15 1 calc PR C 2
H56 H 0.3352 0.5055 0.3398 0.075 Uiso 0.15 1 calc PR C 2
S3 S 0.3172(7) 0.4715(7) 0.2811(4) 0.086(2) Uani 0.10 1 d PDU D 3
O9 O 0.2899(16) 0.4075(10) 0.2968(7) 0.076(3) Uani 0.10 1 d PDU D 3
C47 C 0.358(2) 0.5242(17) 0.3124(9) 0.076(4) Uani 0.10 1 d PDU D 3
H57 H 0.3923 0.5176 0.3195 0.114 Uiso 0.10 1 calc PR D 3
H58 H 0.3272 0.5152 0.3292 0.114 Uiso 0.10 1 calc PR D 3
H59 H 0.3752 0.5686 0.3057 0.114 Uiso 0.10 1 calc PR D 3
C48 C 0.2572(15) 0.4874(18) 0.2752(13) 0.080(5) Uani 0.10 1 d PDU D 3
H60 H 0.2317 0.4631 0.2574 0.119 Uiso 0.10 1 calc PR D 3
H61 H 0.2753 0.5333 0.2713 0.119 Uiso 0.10 1 calc PR D 3
H62 H 0.2297 0.4752 0.2934 0.119 Uiso 0.10 1 calc PR D 3
S4 S 0.4769(2) 0.5624(2) 0.42894(9) 0.1013(9) Uani 0.45 1 d PDU E 1
O10 O 0.4116(4) 0.5537(6) 0.4288(3) 0.120(3) Uani 0.45 1 d PDU E 1
C49 C 0.5270(8) 0.6477(6) 0.4327(4) 0.099(4) Uani 0.45 1 d PDU E 1
H63 H 0.5210 0.6610 0.4531 0.148 Uiso 0.45 1 calc PR E 1
H64 H 0.5154 0.6691 0.4169 0.148 Uiso 0.45 1 calc PR E 1
H65 H 0.5719 0.6594 0.4301 0.148 Uiso 0.45 1 calc PR E 1
C50 C 0.4979(8) 0.5546(8) 0.3918(3) 0.109(4) Uani 0.45 1 d PDU E 1
H66 H 0.4739 0.5096 0.3856 0.164 Uiso 0.45 1 calc PR E 1
H67 H 0.5438 0.5698 0.3909 0.164 Uiso 0.45 1 calc PR E 1
H68 H 0.4877 0.5802 0.3778 0.164 Uiso 0.45 1 calc PR E 1
S5 S 0.4746(3) 0.5919(4) 0.41128(18) 0.148(2) Uani 0.30 1 d PDU F 2
O11 O 0.4342(8) 0.5602(9) 0.4398(4) 0.135(4) Uani 0.30 1 d PDU F 2
C51 C 0.5083(15) 0.5431(14) 0.4011(8) 0.206(9) Uani 0.30 1 d PDU F 2
H69 H 0.4756 0.5040 0.3911 0.309 Uiso 0.30 1 calc PR F 2
H70 H 0.5234 0.5318 0.4196 0.309 Uiso 0.30 1 calc PR F 2
H71 H 0.5442 0.5667 0.3870 0.309 Uiso 0.30 1 calc PR F 2
C52 C 0.5393(11) 0.6549(11) 0.4285(7) 0.117(7) Uani 0.30 1 d PDU F 2
H72 H 0.5275 0.6862 0.4355 0.176 Uiso 0.30 1 calc PR F 2
H73 H 0.5745 0.6753 0.4137 0.176 Uiso 0.30 1 calc PR F 2
H74 H 0.5530 0.6394 0.4461 0.176 Uiso 0.30 1 calc PR F 2
S6 S 0.5183(8) 0.5571(11) 0.4253(5) 0.135(3) Uani 0.10 1 d PDU G 3
O12 O 0.5847(11) 0.571(2) 0.4340(9) 0.127(8) Uani 0.10 1 d PDU G 3
C53 C 0.471(2) 0.482(2) 0.4439(13) 0.158(11) Uani 0.10 1 d PDU G 3
H75 H 0.4692 0.4887 0.4659 0.236 Uiso 0.10 1 calc PR G 3
H76 H 0.4895 0.4546 0.4404 0.236 Uiso 0.10 1 calc PR G 3
H77 H 0.4272 0.4610 0.4355 0.236 Uiso 0.10 1 calc PR G 3
C54 C 0.512(3) 0.535(3) 0.3875(6) 0.125(13) Uani 0.10 1 d PDU G 3
H78 H 0.5387 0.5728 0.3749 0.188 Uiso 0.10 1 calc PR G 3
H79 H 0.4671 0.5162 0.3809 0.188 Uiso 0.10 1 calc PR G 3
H80 H 0.5258 0.5036 0.3850 0.188 Uiso 0.10 1 calc PR G 3
S7 S 0.6047(3) 0.3688(3) 0.30475(17) 0.1356(17) Uani 0.33 1 d PDU H -2
O13 O 0.6538(8) 0.3560(8) 0.2904(4) 0.169(4) Uani 0.33 1 d PDU H -2
C55 C 0.5556(12) 0.2978(8) 0.3256(6) 0.144(7) Uani 0.33 1 d PDU H -2
H81 H 0.5302 0.2629 0.3112 0.216 Uiso 0.33 1 calc PR H -2
H82 H 0.5270 0.3045 0.3390 0.216 Uiso 0.33 1 calc PR H -2
H83 H 0.5825 0.2868 0.3380 0.216 Uiso 0.33 1 calc PR H -2
C56 C 0.6446(10) 0.4210(10) 0.3341(5) 0.134(5) Uani 0.33 1 d PDU H -2
H84 H 0.6748 0.4631 0.3256 0.201 Uiso 0.33 1 calc PR H -2
H85 H 0.6681 0.4050 0.3461 0.201 Uiso 0.33 1 calc PR H -2
H86 H 0.6138 0.4246 0.3474 0.201 Uiso 0.33 1 calc PR H -2
S8 S 0.5526(13) 0.3294(13) 0.2799(7) 0.213(5) Uani 0.10 1 d PDU I -3
O14 O 0.5579(19) 0.341(3) 0.2456(7) 0.198(7) Uani 0.10 1 d PDU I -3
C57 C 0.590(3) 0.4106(19) 0.2931(15) 0.189(10) Uani 0.10 1 d PDU I -3
H87 H 0.6360 0.4313 0.2900 0.283 Uiso 0.10 1 calc PR I -3
H88 H 0.5805 0.4111 0.3149 0.283 Uiso 0.10 1 calc PR I -3
H89 H 0.5727 0.4336 0.2815 0.283 Uiso 0.10 1 calc PR I -3
C58 C 0.4750(17) 0.301(4) 0.2896(15) 0.189(9) Uani 0.10 1 d PDU I -3
H90 H 0.4630 0.3333 0.2851 0.284 Uiso 0.10 1 calc PR I -3
H91 H 0.4693 0.2906 0.3115 0.284 Uiso 0.10 1 calc PR I -3
H92 H 0.4477 0.2621 0.2777 0.284 Uiso 0.10 1 calc PR I -3
S9 S 0.4720(3) 0.4340(3) 0.49447(13) 0.0993(14) Uani 0.30 1 d PDU J -1
O15 O 0.5028(7) 0.3942(6) 0.4942(3) 0.116(3) Uani 0.30 1 d PDU J -1
C59 C 0.5375(9) 0.5151(7) 0.4930(5) 0.119(5) Uani 0.30 1 d PDU J -1
H93 H 0.5609 0.5259 0.5125 0.179 Uiso 0.30 1 calc PR J -1
H94 H 0.5209 0.5442 0.4894 0.179 Uiso 0.30 1 calc PR J -1
H95 H 0.5665 0.5193 0.4762 0.179 Uiso 0.30 1 calc PR J -1
C60 C 0.4392(10) 0.4267(10) 0.4589(4) 0.121(6) Uani 0.30 1 d PDU J -1
H96 H 0.4024 0.3836 0.4565 0.182 Uiso 0.30 1 calc PR J -1
H97 H 0.4712 0.4341 0.4432 0.182 Uiso 0.30 1 calc PR J -1
H98 H 0.4253 0.4583 0.4566 0.182 Uiso 0.30 1 calc PR J -1
S10 S 0.6018(13) 0.4178(14) 0.5080(6) 0.216(3) Uani 0.10 1 d PDU K 5
O16 O 0.5432(18) 0.422(2) 0.5016(10) 0.158(4) Uani 0.10 1 d PDU K 5
C61 C 0.580(3) 0.343(2) 0.4896(12) 0.150(8) Uani 0.10 1 d PDU K 5
H99 H 0.5733 0.3459 0.4677 0.224 Uiso 0.10 1 calc PR K 5
H100 H 0.5408 0.3087 0.4989 0.224 Uiso 0.10 1 calc PR K 5
H101 H 0.6148 0.3332 0.4924 0.224 Uiso 0.10 1 calc PR K 5
C62 C 0.601(4) 0.399(4) 0.5458(7) 0.215(14) Uani 0.10 1 d PDU K 5
H102 H 0.6167 0.4384 0.5582 0.322 Uiso 0.10 1 calc PR K 5
H103 H 0.6288 0.3811 0.5490 0.322 Uiso 0.10 1 calc PR K 5
H104 H 0.5572 0.3683 0.5520 0.322 Uiso 0.10 1 calc PR K 5
S11 S 0.6980(8) 0.4029(7) 0.5424(4) 0.193(3) Uani 0.18 1 d PDU L -1
O17 O 0.6970(11) 0.3428(11) 0.5521(5) 0.157(4) Uani 0.18 1 d PDU L -1
C63 C 0.7343(19) 0.420(2) 0.5053(7) 0.172(9) Uani 0.18 1 d PDU L -1
H105 H 0.7801 0.4353 0.5074 0.258 Uiso 0.18 1 calc PR L -1
H106 H 0.7284 0.4534 0.4955 0.258 Uiso 0.18 1 calc PR L -1
H107 H 0.7143 0.3813 0.4927 0.258 Uiso 0.18 1 calc PR L -1
C64 C 0.6205(12) 0.378(2) 0.5340(11) 0.202(11) Uani 0.18 1 d PDU L -1
H108 H 0.5952 0.3653 0.5529 0.303 Uiso 0.18 1 calc PR L -1
H109 H 0.6040 0.3414 0.5199 0.303 Uiso 0.18 1 calc PR L -1
H110 H 0.6175 0.4130 0.5242 0.303 Uiso 0.18 1 calc PR L -1
S12 S 0.6777(2) 0.5240(3) 0.44369(14) 0.1452(15) Uani 0.45 1 d PDU M 1
O18 O 0.7163(4) 0.5809(3) 0.4248(2) 0.0925(19) Uani 0.45 1 d PDU M 1
C65 C 0.7105(9) 0.5413(11) 0.4796(3) 0.157(5) Uani 0.45 1 d PDU M 1
H111 H 0.7539 0.5478 0.4787 0.235 Uiso 0.45 1 calc PR M 1
H112 H 0.6843 0.5056 0.4934 0.235 Uiso 0.45 1 calc PR M 1
H113 H 0.7120 0.5802 0.4871 0.235 Uiso 0.45 1 calc PR M 1
C66 C 0.6013(6) 0.5094(10) 0.4436(5) 0.180(7) Uani 0.45 1 d PDU M 1
H114 H 0.5846 0.5004 0.4226 0.270 Uiso 0.45 1 calc PR M 1
H115 H 0.6003 0.5470 0.4514 0.270 Uiso 0.45 1 calc PR M 1
H116 H 0.5748 0.4724 0.4566 0.270 Uiso 0.45 1 calc PR M 1
S13 S 0.6740(7) 0.5131(6) 0.4141(3) 0.125(3) Uani 0.15 1 d PDU N 2
O19 O 0.6907(14) 0.5818(7) 0.4202(6) 0.111(7) Uani 0.15 1 d PDU N 2
C67 C 0.6304(13) 0.4889(14) 0.3806(4) 0.093(8) Uani 0.15 1 d PDU N 2
H117 H 0.6571 0.5147 0.3635 0.140 Uiso 0.15 1 calc PR N 2
H118 H 0.5930 0.4945 0.3824 0.140 Uiso 0.15 1 calc PR N 2
H119 H 0.6161 0.4437 0.3769 0.140 Uiso 0.15 1 calc PR N 2
C68 C 0.6351(17) 0.4597(9) 0.4412(4) 0.097(8) Uani 0.15 1 d PDU N 2
H120 H 0.6581 0.4749 0.4606 0.145 Uiso 0.15 1 calc PR N 2
H121 H 0.6320 0.4189 0.4356 0.145 Uiso 0.15 1 calc PR N 2
H122 H 0.5919 0.4537 0.4433 0.145 Uiso 0.15 1 calc PR N 2
S14 S 0.7343(8) 0.5524(9) 0.4794(4) 0.109(3) Uani 0.10 1 d PDU O 3
O20 O 0.7442(19) 0.5628(18) 0.4455(5) 0.121(6) Uani 0.10 1 d PDU O 3
C69 C 0.741(2) 0.4827(19) 0.4862(14) 0.152(8) Uani 0.10 1 d PDU O 3
H123 H 0.7356 0.4729 0.5082 0.228 Uiso 0.10 1 calc PR O 3
H124 H 0.7827 0.4906 0.4794 0.228 Uiso 0.10 1 calc PR O 3
H125 H 0.7070 0.4465 0.4748 0.228 Uiso 0.10 1 calc PR O 3
C70 C 0.6532(11) 0.520(2) 0.4853(9) 0.089(9) Uani 0.10 1 d PDU O 3
H126 H 0.6420 0.5540 0.4826 0.134 Uiso 0.10 1 calc PR O 3
H127 H 0.6423 0.5034 0.5062 0.134 Uiso 0.10 1 calc PR O 3
H128 H 0.6294 0.4860 0.4706 0.134 Uiso 0.10 1 calc PR O 3
S15 S 0.6381(8) 0.5197(8) 0.4138(4) 0.107(2) Uani 0.10 1 d PDU P 4
O21 O 0.6678(14) 0.5660(15) 0.4405(7) 0.097(4) Uani 0.10 1 d PDU P 4
C71 C 0.5613(13) 0.515(2) 0.4118(13) 0.108(3) Uani 0.10 1 d PDU P 4
H129 H 0.5660 0.5532 0.4016 0.163 Uiso 0.10 1 calc PR P 4
H130 H 0.5445 0.5120 0.4325 0.163 Uiso 0.10 1 calc PR P 4
H131 H 0.5316 0.4768 0.4000 0.163 Uiso 0.10 1 calc PR P 4
C72 C 0.620(2) 0.4465(13) 0.4272(13) 0.112(6) Uani 0.10 1 d PDU P 4
H132 H 0.5956 0.4142 0.4115 0.168 Uiso 0.10 1 calc PR P 4
H133 H 0.5934 0.4370 0.4458 0.168 Uiso 0.10 1 calc PR P 4
H134 H 0.6591 0.4462 0.4321 0.168 Uiso 0.10 1 calc PR P 4
O22 O 0.6700(2) 0.6580(3) 0.39639(12) 0.0861(15) Uani 0.67 1 d PD . .
H135 H 0.686(2) 0.637(2) 0.4037(19) 0.129 Uiso 0.67 1 d PD . .
H136 H 0.699(2) 0.6896(11) 0.3900(15) 0.129 Uiso 0.67 1 d PD . .
O23 O 0.6667 0.3333 0.2252(4) 0.291(9) Uani 1 3 d SD . .
H137 H 0.662(6) 0.339(6) 0.2446(10) 0.436 Uiso 0.33 1 d PD . .
H138 H 0.666(5) 0.298(3) 0.227(3) 0.436 Uiso 0.33 1 d PD . .
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'
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
C2 C1 C2 119.0(4) 2_665 .
C2 C1 C5 120.1(4) 2_665 .
C2 C1 C5 120.8(4) . .
C1 C2 C1 121.0(4) 3_565 .
C1 C2 H1 119.5 3_565 .
C1 C2 H1 119.5 . .
C4 C3 C4 118.7(4) . 3_565
C4 C3 C35 122.1(3) . .
C4 C3 C35 119.2(3) 3_565 .
C3 C4 C3 121.3(4) . 2_665
C3 C4 H2 119.4 . .
C3 C4 H2 119.4 2_665 .
C10 C5 C6 118.1(4) . .
C10 C5 C1 119.4(4) . .
C6 C5 C1 122.5(4) . .
O1 C6 C7 120.9(4) . .
O1 C6 C5 119.2(4) . .
C7 C6 C5 119.9(4) . .
C6 C7 C8 119.9(4) . .
C6 C7 C15 121.4(4) . .
C8 C7 C15 118.7(4) . .
C9 C8 C7 121.7(4) . .
C9 C8 H3 119.2 . .
C7 C8 H3 119.2 . .
C8 C9 C10 116.9(4) . .
C8 C9 C11 123.8(4) . .
C10 C9 C11 119.3(4) . .
C5 C10 C9 123.4(4) . .
C5 C10 H4 118.3 . .
C9 C10 H4 118.3 . .
C6 O1 H5 109.5 . .
C14 C11 C9 111.4(4) . .
C14 C11 C13 108.8(4) . .
C9 C11 C13 109.2(4) . .
C14 C11 C12 108.7(4) . .
C9 C11 C12 108.8(4) . .
C13 C11 C12 109.9(4) . .
C11 C12 H6 109.5 . .
C11 C12 H7 109.5 . .
H6 C12 H7 109.5 . .
C11 C12 H8 109.5 . .
H6 C12 H8 109.5 . .
H7 C12 H8 109.5 . .
C11 C13 H9 109.5 . .
C11 C13 H10 109.5 . .
H9 C13 H10 109.5 . .
C11 C13 H11 109.5 . .
H9 C13 H11 109.5 . .
H10 C13 H11 109.5 . .
C11 C14 H12 109.5 . .
C11 C14 H13 109.5 . .
H12 C14 H13 109.5 . .
C11 C14 H14 109.5 . .
H12 C14 H14 109.5 . .
H13 C14 H14 109.5 . .
N1 C15 C7 121.8(4) . .
N1 C15 H15 119.1 . .
C7 C15 H15 119.1 . .
C15 N1 C16 120.7(3) . .
C21 C16 C17 119.3(6) . .
C21 C16 N1 118.7(3) . .
C17 C16 N1 122.0(6) . .
C18 C17 C16 120.1(10) . .
C18 C17 H16 120.0 . .
C16 C17 H16 120.0 . .
C17 C18 O2 124.7(9) . .
C17 C18 C19 120.7(9) . .
O2 C18 C19 114.6(9) . .
O3 C19 C20 125.3(9) . .
O3 C19 C18 114.8(9) . .
C20 C19 C18 119.9(9) . .
C19 C20 C21 119.9(9) . .
C19 C20 H17 120.1 . .
C21 C20 H17 120.1 . .
C16 C21 C20 120.0(6) . .
C16 C21 N2 120.0(3) . .
C20 C21 N2 119.6(6) . .
C18 O2 C22 115.3(11) . .
O2 C22 H18 109.5 . .
O2 C22 H19 109.5 . .
H18 C22 H19 109.5 . .
O2 C22 H20 109.5 . .
H18 C22 H20 109.5 . .
H19 C22 H20 109.5 . .
C19 O3 C23 115.9(10) . .
O3 C23 H21 109.5 . .
O3 C23 H22 109.5 . .
H21 C23 H22 109.5 . .
O3 C23 H23 109.5 . .
H21 C23 H23 109.5 . .
H22 C23 H23 109.5 . .
C26 C25 H24 119.2 . .
C25 C26 O4 126.1(9) . .
C25 C26 C27 119.4(9) . .
O4 C26 C27 114.5(9) . .
O5 C27 C28 124.0(9) . .
O5 C27 C26 116.5(8) . .
C28 C27 C26 119.5(9) . .
C27 C28 H25 119.2 . .
C26 O4 C30 118.2(10) . .
O4 C30 H26 109.5 . .
O4 C30 H27 109.5 . .
H26 C30 H27 109.5 . .
O4 C30 H28 109.5 . .
H26 C30 H28 109.5 . .
H27 C30 H28 109.5 . .
C27 O5 C31 115.7(9) . .
O5 C31 H29 109.5 . .
O5 C31 H30 109.5 . .
H29 C31 H30 109.5 . .
O5 C31 H31 109.5 . .
H29 C31 H31 109.5 . .
H30 C31 H31 109.5 . .
C32 N2 C21 118.8(3) . .
N2 C32 C33 122.8(3) . .
N2 C32 H32 118.6 . .
C33 C32 H32 118.6 . .
C34 C33 C38 119.6(3) . .
C34 C33 C32 122.1(3) . .
C38 C33 C32 118.3(3) . .
O6 C34 C33 120.4(3) . .
O6 C34 C35 119.7(3) . .
C33 C34 C35 119.8(3) . .
C36 C35 C34 118.2(3) . .
C36 C35 C3 119.0(3) . .
C34 C35 C3 122.6(3) . .
C35 C36 C37 123.4(3) . .
C35 C36 H33 118.3 . .
C37 C36 H33 118.3 . .
C38 C37 C36 116.9(3) . .
C38 C37 C39 123.0(3) . .
C36 C37 C39 120.1(3) . .
C37 C38 C33 121.9(3) . .
C37 C38 H34 119.0 . .
C33 C38 H34 119.0 . .
C34 O6 H35 109.5 . .
C41 C39 C40 108.2(5) . .
C41 C39 C42 107.6(4) . .
C40 C39 C42 111.0(5) . .
C41 C39 C37 108.5(3) . .
C40 C39 C37 110.8(3) . .
C42 C39 C37 110.5(4) . .
C39 C40 H36 109.5 . .
C39 C40 H37 109.5 . .
H36 C40 H37 109.5 . .
C39 C40 H38 109.5 . .
H36 C40 H38 109.5 . .
H37 C40 H38 109.5 . .
C39 C41 H39 109.5 . .
C39 C41 H40 109.5 . .
H39 C41 H40 109.5 . .
C39 C41 H41 109.5 . .
H39 C41 H41 109.5 . .
H40 C41 H41 109.5 . .
C39 C42 H42 109.5 . .
C39 C42 H43 109.5 . .
H42 C42 H43 109.5 . .
C39 C42 H44 109.5 . .
H42 C42 H44 109.5 . .
H43 C42 H44 109.5 . .
O7 S1 C44 109.8(5) . .
O7 S1 C43 100.2(4) . .
C44 S1 C43 101.4(4) . .
S1 C43 H45 109.5 . .
S1 C43 H46 109.5 . .
H45 C43 H46 109.5 . .
S1 C43 H47 109.5 . .
H45 C43 H47 109.5 . .
H46 C43 H47 109.5 . .
S1 C44 H48 109.5 . .
S1 C44 H49 109.5 . .
H48 C44 H49 109.5 . .
S1 C44 H50 109.5 . .
H48 C44 H50 109.5 . .
H49 C44 H50 109.5 . .
O8 S2 C46 116.0(11) . .
O8 S2 C45 90.3(10) . .
C46 S2 C45 95.6(10) . .
S2 C45 H51 109.5 . .
S2 C45 H52 109.5 . .
H51 C45 H52 109.5 . .
S2 C45 H53 109.5 . .
H51 C45 H53 109.5 . .
H52 C45 H53 109.5 . .
S2 C46 H54 109.5 . .
S2 C46 H55 109.5 . .
H54 C46 H55 109.5 . .
S2 C46 H56 109.5 . .
H54 C46 H56 109.5 . .
H55 C46 H56 109.5 . .
O9 S3 C48 108.5(17) . .
O9 S3 C47 100.7(16) . .
C48 S3 C47 100.2(16) . .
S3 C47 H57 109.5 . .
S3 C47 H58 109.5 . .
H57 C47 H58 109.5 . .
S3 C47 H59 109.5 . .
H57 C47 H59 109.5 . .
H58 C47 H59 109.5 . .
S3 C48 H60 109.5 . .
S3 C48 H61 109.5 . .
H60 C48 H61 109.5 . .
S3 C48 H62 109.5 . .
H60 C48 H62 109.5 . .
H61 C48 H62 109.5 . .
O10 S4 C50 109.1(8) . .
O10 S4 C49 102.8(8) . .
C50 S4 C49 98.2(8) . .
S4 C49 H63 109.5 . .
S4 C49 H64 109.5 . .
H63 C49 H64 109.5 . .
S4 C49 H65 109.5 . .
H63 C49 H65 109.5 . .
H64 C49 H65 109.5 . .
S4 C50 H66 109.5 . .
S4 C50 H67 109.5 . .
H66 C50 H67 109.5 . .
S4 C50 H68 109.5 . .
H66 C50 H68 109.5 . .
H67 C50 H68 109.5 . .
O11 S5 C52 99.0(12) . .
O11 S5 C51 105.0(13) . .
C52 S5 C51 100.4(14) . .
S5 C51 H69 109.5 . .
S5 C51 H70 109.5 . .
H69 C51 H70 109.5 . .
S5 C51 H71 109.5 . .
H69 C51 H71 109.5 . .
H70 C51 H71 109.5 . .
S5 C52 H72 109.5 . .
S5 C52 H73 109.5 . .
H72 C52 H73 109.5 . .
S5 C52 H74 109.5 . .
H72 C52 H74 109.5 . .
H73 C52 H74 109.5 . .
O12 S6 C54 103.6(19) . .
O12 S6 C53 100.9(18) . .
C54 S6 C53 102.0(18) . .
S6 C53 H75 109.5 . .
S6 C53 H76 109.5 . .
H75 C53 H76 109.5 . .
S6 C53 H77 109.5 . .
H75 C53 H77 109.5 . .
H76 C53 H77 109.5 . .
S6 C54 H78 109.5 . .
S6 C54 H79 109.5 . .
H78 C54 H79 109.5 . .
S6 C54 H80 109.5 . .
H78 C54 H80 109.5 . .
H79 C54 H80 109.5 . .
O13 S7 C56 104.4(10) . .
O13 S7 C55 103.2(11) . .
C56 S7 C55 100.7(13) . .
S7 C55 H81 109.5 . .
S7 C55 H82 109.5 . .
H81 C55 H82 109.5 . .
S7 C55 H83 109.5 . .
H81 C55 H83 109.5 . .
H82 C55 H83 109.5 . .
S7 C56 H84 109.5 . .
S7 C56 H85 109.5 . .
H84 C56 H85 109.5 . .
S7 C56 H86 109.5 . .
H84 C56 H86 109.5 . .
H85 C56 H86 109.5 . .
O14 S8 C58 107(2) . .
O14 S8 C57 99.5(19) . .
C58 S8 C57 102.2(19) . .
S8 C57 H87 109.5 . .
S8 C57 H88 109.5 . .
H87 C57 H88 109.5 . .
S8 C57 H89 109.5 . .
H87 C57 H89 109.5 . .
H88 C57 H89 109.5 . .
S8 C58 H90 109.5 . .
S8 C58 H91 109.5 . .
H90 C58 H91 109.5 . .
S8 C58 H92 109.5 . .
H90 C58 H92 109.5 . .
H91 C58 H92 109.5 . .
O15 S9 C60 106.4(10) . .
O15 S9 C59 104.6(10) . .
C60 S9 C59 100.9(10) . .
S9 C59 H93 109.5 . .
S9 C59 H94 109.5 . .
H93 C59 H94 109.5 . .
S9 C59 H95 109.5 . .
H93 C59 H95 109.5 . .
H94 C59 H95 109.5 . .
S9 C60 H96 109.5 . .
S9 C60 H97 109.5 . .
H96 C60 H97 109.5 . .
S9 C60 H98 109.5 . .
H96 C60 H98 109.5 . .
H97 C60 H98 109.5 . .
O16 S10 C62 108(2) . .
O16 S10 C61 100.1(18) . .
C62 S10 C61 102.0(19) . .
S10 C61 H99 109.5 . .
S10 C61 H100 109.5 . .
H99 C61 H100 109.5 . .
S10 C61 H101 109.5 . .
H99 C61 H101 109.5 . .
H100 C61 H101 109.5 . .
S10 C62 H102 109.5 . .
S10 C62 H103 109.5 . .
H102 C62 H103 109.5 . .
S10 C62 H104 109.5 . .
H102 C62 H104 109.5 . .
H103 C62 H104 109.5 . .
O17 S11 C64 103.7(16) . .
O17 S11 C63 104.6(15) . .
C64 S11 C63 102.3(17) . .
S11 C63 H105 109.5 . .
S11 C63 H106 109.5 . .
H105 C63 H106 109.5 . .
S11 C63 H107 109.5 . .
H105 C63 H107 109.5 . .
H106 C63 H107 109.5 . .
S11 C64 H108 109.5 . .
S11 C64 H109 109.5 . .
H108 C64 H109 109.5 . .
S11 C64 H110 109.5 . .
H108 C64 H110 109.5 . .
H109 C64 H110 109.5 . .
O18 S12 C66 108.0(8) . .
O18 S12 C65 106.7(9) . .
C66 S12 C65 112.2(11) . .
S12 C65 H111 109.5 . .
S12 C65 H112 109.5 . .
H111 C65 H112 109.5 . .
S12 C65 H113 109.5 . .
H111 C65 H113 109.5 . .
H112 C65 H113 109.5 . .
S12 C66 H114 109.5 . .
S12 C66 H115 109.5 . .
H114 C66 H115 109.5 . .
S12 C66 H116 109.5 . .
H114 C66 H116 109.5 . .
H115 C66 H116 109.5 . .
O19 S13 C68 117.5(13) . .
O19 S13 C67 107.6(12) . .
C68 S13 C67 109.2(12) . .
S13 C67 H117 109.5 . .
S13 C67 H118 109.5 . .
H117 C67 H118 109.5 . .
S13 C67 H119 109.5 . .
H117 C67 H119 109.5 . .
H118 C67 H119 109.5 . .
S13 C68 H120 109.5 . .
S13 C68 H121 109.5 . .
H120 C68 H121 109.5 . .
S13 C68 H122 109.5 . .
H120 C68 H122 109.5 . .
H121 C68 H122 109.5 . .
O20 S14 C70 105.9(18) . .
O20 S14 C69 103.9(19) . .
C70 S14 C69 99.6(16) . .
S14 C69 H123 109.5 . .
S14 C69 H124 109.5 . .
H123 C69 H124 109.5 . .
S14 C69 H125 109.5 . .
H123 C69 H125 109.5 . .
H124 C69 H125 109.5 . .
S14 C70 H126 109.5 . .
S14 C70 H127 109.5 . .
H126 C70 H127 109.5 . .
S14 C70 H128 109.5 . .
H126 C70 H128 109.5 . .
H127 C70 H128 109.5 . .
O21 S15 C72 106.6(19) . .
O21 S15 C71 100.3(17) . .
C72 S15 C71 102.9(17) . .
S15 C71 H129 109.5 . .
S15 C71 H130 109.5 . .
H129 C71 H130 109.5 . .
S15 C71 H131 109.5 . .
H129 C71 H131 109.5 . .
H130 C71 H131 109.5 . .
S15 C72 H132 109.5 . .
S15 C72 H133 109.5 . .
H132 C72 H133 109.5 . .
S15 C72 H134 109.5 . .
H132 C72 H134 109.5 . .
H133 C72 H134 109.5 . .
H135 O22 H136 105(3) . .
H137 O23 H138 98(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.387(5) 2_665
C1 C2 1.395(5) .
C1 C5 1.498(6) .
C2 C1 1.387(6) 3_565
C2 H1 0.9500 .
C3 C4 1.393(5) .
C3 C4 1.400(5) 3_565
C3 C35 1.489(5) .
C4 C3 1.400(5) 2_665
C4 H2 0.9500 .
C5 C10 1.395(6) .
C5 C6 1.406(6) .
C6 O1 1.351(5) .
C6 C7 1.395(6) .
C7 C8 1.411(6) .
C7 C15 1.451(6) .
C8 C9 1.382(6) .
C8 H3 0.9500 .
C9 C10 1.408(6) .
C9 C11 1.531(6) .
C10 H4 0.9500 .
O1 H5 0.8400 .
C11 C14 1.527(6) .
C11 C13 1.531(7) .
C11 C12 1.540(8) .
C12 H6 0.9800 .
C12 H7 0.9800 .
C12 H8 0.9800 .
C13 H9 0.9800 .
C13 H10 0.9800 .
C13 H11 0.9800 .
C14 H12 0.9800 .
C14 H13 0.9800 .
C14 H14 0.9800 .
C15 N1 1.294(5) .
C15 H15 0.9500 .
N1 C16 1.411(5) .
C16 C21 1.387(5) .
C16 C17 1.404(10) .
C17 C18 1.367(11) .
C17 H16 0.9500 .
C18 O2 1.381(10) .
C18 C19 1.387(11) .
C19 O3 1.371(11) .
C19 C20 1.381(11) .
C20 C21 1.395(11) .
C20 H17 0.9500 .
C21 N2 1.420(5) .
O2 C22 1.431(12) .
C22 H18 0.9800 .
C22 H19 0.9800 .
C22 H20 0.9800 .
O3 C23 1.442(13) .
C23 H21 0.9800 .
C23 H22 0.9800 .
C23 H23 0.9800 .
C25 C26 1.367(11) .
C25 H24 0.9500 .
C26 O4 1.380(10) .
C26 C27 1.389(11) .
C27 O5 1.372(10) .
C27 C28 1.387(11) .
C28 H25 0.9500 .
O4 C30 1.428(12) .
C30 H26 0.9800 .
C30 H27 0.9800 .
C30 H28 0.9800 .
O5 C31 1.461(12) .
C31 H29 0.9800 .
C31 H30 0.9800 .
C31 H31 0.9800 .
N2 C32 1.290(4) .
C32 C33 1.444(5) .
C32 H32 0.9500 .
C33 C34 1.404(5) .
C33 C38 1.406(5) .
C34 O6 1.355(4) .
C34 C35 1.405(5) .
C35 C36 1.396(5) .
C36 C37 1.401(5) .
C36 H33 0.9500 .
C37 C38 1.384(5) .
C37 C39 1.535(5) .
C38 H34 0.9500 .
O6 H35 0.8400 .
C39 C41 1.503(6) .
C39 C40 1.529(7) .
C39 C42 1.530(7) .
C40 H36 0.9800 .
C40 H37 0.9800 .
C40 H38 0.9800 .
C41 H39 0.9800 .
C41 H40 0.9800 .
C41 H41 0.9800 .
C42 H42 0.9800 .
C42 H43 0.9800 .
C42 H44 0.9800 .
S1 O7 1.555(5) .
S1 C44 1.687(7) .
S1 C43 1.760(6) .
C43 H45 0.9800 .
C43 H46 0.9800 .
C43 H47 0.9800 .
C44 H48 0.9800 .
C44 H49 0.9800 .
C44 H50 0.9800 .
S2 O8 1.529(13) .
S2 C46 1.687(14) .
S2 C45 1.876(15) .
C45 H51 0.9800 .
C45 H52 0.9800 .
C45 H53 0.9800 .
C46 H54 0.9800 .
C46 H55 0.9800 .
C46 H56 0.9800 .
S3 O9 1.506(16) .
S3 C48 1.695(17) .
S3 C47 1.787(17) .
C47 H57 0.9800 .
C47 H58 0.9800 .
C47 H59 0.9800 .
C48 H60 0.9800 .
C48 H61 0.9800 .
C48 H62 0.9800 .
S4 O10 1.481(10) .
S4 C50 1.735(12) .
S4 C49 1.799(12) .
C49 H63 0.9800 .
C49 H64 0.9800 .
C49 H65 0.9800 .
C50 H66 0.9800 .
C50 H67 0.9800 .
C50 H68 0.9800 .
S5 O11 1.530(13) .
S5 C52 1.715(15) .
S5 C51 1.788(17) .
C51 H69 0.9800 .
C51 H70 0.9800 .
C51 H71 0.9800 .
C52 H72 0.9800 .
C52 H73 0.9800 .
C52 H74 0.9800 .
S6 O12 1.509(16) .
S6 C54 1.716(17) .
S6 C53 1.783(18) .
C53 H75 0.9800 .
C53 H76 0.9800 .
C53 H77 0.9800 .
C54 H78 0.9800 .
C54 H79 0.9800 .
C54 H80 0.9800 .
S7 O13 1.503(11) .
S7 C56 1.714(15) .
S7 C55 1.769(15) .
C55 H81 0.9800 .
C55 H82 0.9800 .
C55 H83 0.9800 .
C56 H84 0.9800 .
C56 H85 0.9800 .
C56 H86 0.9800 .
S8 O14 1.514(17) .
S8 C58 1.694(18) .
S8 C57 1.793(18) .
C57 H87 0.9800 .
C57 H88 0.9800 .
C57 H89 0.9800 .
C58 H90 0.9800 .
C58 H91 0.9800 .
C58 H92 0.9800 .
S9 O15 1.481(12) .
S9 C60 1.710(13) .
S9 C59 1.800(13) .
C59 H93 0.9800 .
C59 H94 0.9800 .
C59 H95 0.9800 .
C60 H96 0.9800 .
C60 H97 0.9800 .
C60 H98 0.9800 .
S10 O16 1.490(17) .
S10 C62 1.707(18) .
S10 C61 1.801(18) .
C61 H99 0.9800 .
C61 H100 0.9800 .
C61 H101 0.9800 .
C62 H102 0.9800 .
C62 H103 0.9800 .
C62 H104 0.9800 .
S11 O17 1.501(16) .
S11 C64 1.694(17) .
S11 C63 1.784(17) .
C63 H105 0.9800 .
C63 H106 0.9800 .
C63 H107 0.9800 .
C64 H108 0.9800 .
C64 H109 0.9800 .
C64 H110 0.9800 .
S12 O18 1.467(9) .
S12 C66 1.695(13) .
S12 C65 1.707(14) .
C65 H111 0.9800 .
C65 H112 0.9800 .
C65 H113 0.9800 .
C66 H114 0.9800 .
C66 H115 0.9800 .
C66 H116 0.9800 .
S13 O19 1.522(12) .
S13 C68 1.651(12) .
S13 C67 1.722(12) .
C67 H117 0.9800 .
C67 H118 0.9800 .
C67 H119 0.9800 .
C68 H120 0.9800 .
C68 H121 0.9800 .
C68 H122 0.9800 .
S14 O20 1.495(16) .
S14 C70 1.727(17) .
S14 C69 1.787(17) .
C69 H123 0.9800 .
C69 H124 0.9800 .
C69 H125 0.9800 .
C70 H126 0.9800 .
C70 H127 0.9800 .
C70 H128 0.9800 .
S15 O21 1.520(16) .
S15 C72 1.692(17) .
S15 C71 1.800(17) .
C71 H129 0.9800 .
C71 H130 0.9800 .
C71 H131 0.9800 .
C72 H132 0.9800 .
C72 H133 0.9800 .
C72 H134 0.9800 .
O22 H135 0.843(17) .
O22 H136 0.79(2) .
O23 H137 0.871(19) .
O23 H138 0.85(2) .
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_4
C2 C1 C2 C1 0.6(8) 2_665 3_565
C5 C1 C2 C1 179.1(3) . 3_565
C4 C3 C4 C3 -0.2(6) 3_565 2_665
C35 C3 C4 C3 -178.7(2) . 2_665
C2 C1 C5 C10 37.9(6) 2_665 .
C2 C1 C5 C10 -140.5(4) . .
C2 C1 C5 C6 -141.1(4) 2_665 .
C2 C1 C5 C6 40.4(6) . .
C10 C5 C6 O1 -176.9(4) . .
C1 C5 C6 O1 2.2(6) . .
C10 C5 C6 C7 2.8(6) . .
C1 C5 C6 C7 -178.1(4) . .
O1 C6 C7 C8 176.5(4) . .
C5 C6 C7 C8 -3.3(6) . .
O1 C6 C7 C15 -3.5(6) . .
C5 C6 C7 C15 176.8(4) . .
C6 C7 C8 C9 1.0(6) . .
C15 C7 C8 C9 -179.1(4) . .
C7 C8 C9 C10 1.6(6) . .
C7 C8 C9 C11 -179.2(4) . .
C6 C5 C10 C9 -0.1(6) . .
C1 C5 C10 C9 -179.2(4) . .
C8 C9 C10 C5 -2.1(6) . .
C11 C9 C10 C5 178.7(4) . .
C8 C9 C11 C14 2.8(7) . .
C10 C9 C11 C14 -177.9(4) . .
C8 C9 C11 C13 -117.4(5) . .
C10 C9 C11 C13 61.8(6) . .
C8 C9 C11 C12 122.7(5) . .
C10 C9 C11 C12 -58.1(5) . .
C6 C7 C15 N1 1.3(6) . .
C8 C7 C15 N1 -178.6(4) . .
C7 C15 N1 C16 -176.3(4) . .
C15 N1 C16 C21 -152.6(4) . .
C15 N1 C16 C17 27.2(7) . .
C21 C16 C17 C18 2.8(11) . .
N1 C16 C17 C18 -177.0(7) . .
C16 C17 C18 O2 -177.2(10) . .
C16 C17 C18 C19 -0.2(13) . .
C17 C18 C19 O3 178.3(10) . .
O2 C18 C19 O3 -4.4(15) . .
C17 C18 C19 C20 0.0(17) . .
O2 C18 C19 C20 177.2(11) . .
O3 C19 C20 C21 179.5(11) . .
C18 C19 C20 C21 -2.3(19) . .
C17 C16 C21 C20 -5.2(10) . .
N1 C16 C21 C20 174.6(8) . .
C17 C16 C21 N2 -177.2(6) . .
N1 C16 C21 N2 2.6(5) . .
C19 C20 C21 C16 5.0(16) . .
C19 C20 C21 N2 177.0(9) . .
C17 C18 O2 C22 -14.9(16) . .
C19 C18 O2 C22 168.0(11) . .
C20 C19 O3 C23 -1(2) . .
C18 C19 O3 C23 -179.3(13) . .
C25 C26 C27 O5 -179.7(9) . .
O4 C26 C27 O5 0.4(14) . .
C25 C26 C27 C28 0.9(15) . .
O4 C26 C27 C28 -178.9(10) . .
C25 C26 O4 C30 4.6(16) . .
C27 C26 O4 C30 -175.6(11) . .
C28 C27 O5 C31 -15.9(17) . .
C26 C27 O5 C31 164.8(11) . .
C16 C21 N2 C32 -150.0(3) . .
C20 C21 N2 C32 38.0(8) . .
C21 N2 C32 C33 -173.3(3) . .
N2 C32 C33 C34 0.5(5) . .
N2 C32 C33 C38 179.6(3) . .
C38 C33 C34 O6 176.7(3) . .
C32 C33 C34 O6 -4.2(5) . .
C38 C33 C34 C35 -1.4(5) . .
C32 C33 C34 C35 177.6(3) . .
O6 C34 C35 C36 -178.4(3) . .
C33 C34 C35 C36 -0.3(5) . .
O6 C34 C35 C3 -2.0(5) . .
C33 C34 C35 C3 176.1(3) . .
C4 C3 C35 C36 -142.3(3) . .
C4 C3 C35 C36 39.3(4) 3_565 .
C4 C3 C35 C34 41.4(5) . .
C4 C3 C35 C34 -137.1(3) 3_565 .
C34 C35 C36 C37 1.9(5) . .
C3 C35 C36 C37 -174.6(3) . .
C35 C36 C37 C38 -1.7(5) . .
C35 C36 C37 C39 179.1(3) . .
C36 C37 C38 C33 -0.1(5) . .
C39 C37 C38 C33 179.1(3) . .
C34 C33 C38 C37 1.6(5) . .
C32 C33 C38 C37 -177.5(3) . .
C38 C37 C39 C41 -103.8(4) . .
C36 C37 C39 C41 75.3(5) . .
C38 C37 C39 C40 14.8(6) . .
C36 C37 C39 C40 -166.1(5) . .
C38 C37 C39 C42 138.4(4) . .
C36 C37 C39 C42 -42.5(5) . .
