# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_ydkr_a
_database_code_depnum_ccdc_archive 'CCDC 2016537'
loop_
_audit_author_name
_audit_author_address
'Takuya Kuwabara'
;Chuo Univesity
Japan
;
_audit_update_record             
;
2020-07-15 deposited with the CCDC.	2020-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C75 H82 O4 S4 Sn'
_chemical_formula_weight         1294.33

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'
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'
Sn Sn -0.6537 1.4246 '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                   12.094(3)
_cell_length_b                   12.497(3)
_cell_length_c                   22.902(6)
_cell_angle_alpha                83.617(10)
_cell_angle_beta                 85.056(11)
_cell_angle_gamma                75.959(9)
_cell_volume                     3330.9(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    8831
_cell_measurement_theta_min      2.4018
_cell_measurement_theta_max      31.1704

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_F_000             1356
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1700
_exptl_crystal_size_mid          0.1500
_exptl_crystal_size_min          0.0500
_exptl_absorpt_coefficient_mu    0.557
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8455
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_device_type  'Rigaku VariMax Saturn'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            26547
_diffrn_reflns_av_unetI/netI     0.1145
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.039
_diffrn_reflns_theta_max         27.438
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             14566
_reflns_number_gt                11317
_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       'RIGAKU CrystalClear'
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Yadokari-XG 2009(Wakita Nemoto et al.)'
_computing_publication_material  'Yadokari-XG 2009(Wakita,Nemoto et al.)'
_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)+(0.0307P)²+18.1878P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14566
_refine_ls_number_parameters     795
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0851
_refine_ls_wR_factor_ref         0.1827
_refine_ls_wR_factor_gt          0.1655
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.098
_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
Sn1 Sn 0.72395(3) 0.48912(3) 0.62342(2) 0.01739(11) Uani 1 1 d . . . . .
O1 O 0.6389(3) 0.4119(3) 0.69146(17) 0.0176(8) Uani 1 1 d . . . . .
O2 O 0.7887(3) 0.5513(3) 0.68984(17) 0.0189(8) Uani 1 1 d . . . . .
C1 C 0.5692(5) 0.3448(4) 0.7040(2) 0.0154(11) Uani 1 1 d . . . . .
C2 C 0.6099(5) 0.2287(5) 0.7140(2) 0.0180(11) Uani 1 1 d . . . . .
C3 C 0.5359(5) 0.1580(5) 0.7286(2) 0.0171(11) Uani 1 1 d . . . . .
H3 H 0.566754 0.082259 0.735138 0.020 Uiso 1 1 calc R U . . .
C4 C 0.4175(5) 0.1970(5) 0.7336(2) 0.0188(11) Uani 1 1 d . . . . .
C5 C 0.3781(5) 0.3121(5) 0.7260(2) 0.0173(11) Uani 1 1 d . . . . .
H5 H 0.299897 0.342065 0.730654 0.021 Uiso 1 1 calc R U . . .
C6 C 0.4500(5) 0.3842(4) 0.7117(2) 0.0156(11) Uani 1 1 d . . . . .
C7 C 0.3338(5) 0.1214(5) 0.7453(3) 0.0213(12) Uani 1 1 d . . . . .
C8 C 0.2577(5) 0.1413(5) 0.6925(3) 0.0282(14) Uani 1 1 d . . . . .
H8 H 0.217013 0.217671 0.688258 0.042 Uiso 1 1 calc R U . . .
H8A H 0.204119 0.095094 0.699225 0.042 Uiso 1 1 calc R U . . .
H8B H 0.304586 0.123603 0.657315 0.042 Uiso 1 1 calc R U . . .
C9 C 0.3952(5) -0.0007(5) 0.7535(3) 0.0315(15) Uani 1 1 d . . . . .
H9 H 0.440643 -0.021250 0.718207 0.047 Uiso 1 1 calc R U . . .
H9A H 0.339977 -0.044987 0.761565 0.047 Uiso 1 1 calc R U . . .
H9B H 0.443684 -0.012813 0.785812 0.047 Uiso 1 1 calc R U . . .
C10 C 0.2569(6) 0.1497(6) 0.8020(3) 0.0359(16) Uani 1 1 d . . . . .
H10 H 0.303079 0.133698 0.835367 0.054 Uiso 1 1 calc R U . . .
H10A H 0.200912 0.105973 0.807205 0.054 Uiso 1 1 calc R U . . .
H10B H 0.219039 0.226893 0.798491 0.054 Uiso 1 1 calc R U . . .
S1 S 0.75536(12) 0.16156(12) 0.69847(7) 0.0196(3) Uani 1 1 d . . . . .
C11 C 0.8951(5) 0.3006(4) 0.7096(2) 0.0171(11) Uani 1 1 d . . . . .
C12 C 0.8328(5) 0.2281(4) 0.7392(2) 0.0178(11) Uani 1 1 d . . . . .
C13 C 0.8381(5) 0.2057(5) 0.8001(3) 0.0195(12) Uani 1 1 d . . . . .
H13 H 0.797050 0.157232 0.819838 0.023 Uiso 1 1 calc R U . . .
C14 C 0.9030(5) 0.2536(5) 0.8322(3) 0.0213(12) Uani 1 1 d . . . . .
C15 C 0.9637(5) 0.3276(5) 0.8016(2) 0.0205(12) Uani 1 1 d . . . . .
H15 H 1.007052 0.361239 0.822134 0.025 Uiso 1 1 calc R U . . .
C16 C 0.9591(5) 0.3510(4) 0.7405(3) 0.0177(11) Uani 1 1 d . . . . .
O3 O 0.8847(3) 0.3304(3) 0.64979(16) 0.0170(8) Uani 1 1 d . . . . .
C17 C 0.9652(5) 0.2583(5) 0.6116(3) 0.0218(12) Uani 1 1 d . . . . .
H17 H 0.963778 0.181605 0.623288 0.026 Uiso 1 1 calc R U . . .
H17A H 1.041980 0.266674 0.615090 0.026 Uiso 1 1 calc R U . . .
C18 C 0.9322(5) 0.2892(5) 0.5490(3) 0.0202(12) Uani 1 1 d . . . . .
C19 C 0.9861(5) 0.3572(5) 0.5110(3) 0.0248(13) Uani 1 1 d . . . . .
H19 H 1.043510 0.384562 0.524211 0.030 Uiso 1 1 calc R U . . .
C20 C 0.9552(6) 0.3847(6) 0.4536(3) 0.0311(15) Uani 1 1 d . . . . .
H20 H 0.992287 0.430175 0.428403 0.037 Uiso 1 1 calc R U . . .
C21 C 0.8698(6) 0.3453(6) 0.4334(3) 0.0349(16) Uani 1 1 d . . . . .
H21 H 0.848407 0.365099 0.394906 0.042 Uiso 1 1 calc R U . . .
C22 C 0.8160(6) 0.2757(6) 0.4710(3) 0.0319(15) Uani 1 1 d . . . . .
H22 H 0.759621 0.247510 0.457395 0.038 Uiso 1 1 calc R U . . .
C23 C 0.8464(5) 0.2480(5) 0.5293(3) 0.0227(13) Uani 1 1 d . . . . .
H23 H 0.809563 0.202457 0.554646 0.027 Uiso 1 1 calc R U . . .
C24 C 0.9066(6) 0.2239(5) 0.8992(3) 0.0275(14) Uani 1 1 d . . . . .
C25 C 0.9841(6) 0.2804(6) 0.9273(3) 0.0368(17) Uani 1 1 d . . . . .
H25 H 1.061342 0.255093 0.911932 0.055 Uiso 1 1 calc R U . . .
H25A H 0.979806 0.262679 0.969141 0.055 Uiso 1 1 calc R U . . .
H25B H 0.959899 0.359216 0.918438 0.055 Uiso 1 1 calc R U . . .
C26 C 0.9522(7) 0.0970(6) 0.9115(3) 0.0380(17) Uani 1 1 d . . . . .
H26 H 1.028150 0.075425 0.893775 0.057 Uiso 1 1 calc R U . . .
H26A H 0.903278 0.059523 0.895104 0.057 Uiso 1 1 calc R U . . .
H26B H 0.953265 0.077486 0.953208 0.057 Uiso 1 1 calc R U . . .
C27 C 0.7854(7) 0.2584(7) 0.9277(3) 0.0448(19) Uani 1 1 d . . . . .
H27 H 0.786386 0.236384 0.969247 0.067 Uiso 1 1 calc R U . . .
H27A H 0.735708 0.223031 0.910465 0.067 Uiso 1 1 calc R U . . .
H27B H 0.758198 0.337353 0.921395 0.067 Uiso 1 1 calc R U . . .
S2 S 1.04488(12) 0.43664(11) 0.70092(6) 0.0187(3) Uani 1 1 d . . . . .
C28 C 0.8535(5) 0.6162(4) 0.7010(2) 0.0151(11) Uani 1 1 d . . . . .
C29 C 0.9712(5) 0.5751(5) 0.7122(2) 0.0175(11) Uani 1 1 d . . . . .
C30 C 1.0391(5) 0.6444(5) 0.7242(3) 0.0218(12) Uani 1 1 d . . . . .
H30 H 1.115478 0.613673 0.731002 0.026 Uiso 1 1 calc R U . . .
C31 C 0.9966(5) 0.7588(5) 0.7264(3) 0.0208(12) Uani 1 1 d . . . . .
C32 C 0.8813(5) 0.7992(5) 0.7184(3) 0.0192(12) Uani 1 1 d . . . . .
H32 H 0.849254 0.874143 0.721428 0.023 Uiso 1 1 calc R U . . .
C33 C 0.8111(5) 0.7316(4) 0.7059(2) 0.0164(11) Uani 1 1 d . . . . .
C34 C 1.0773(11) 0.8299(9) 0.7394(5) 0.019(2) Uani 0.777(11) 1 d . . P A 1
C35 C 1.1740(8) 0.8203(8) 0.6892(4) 0.025(2) Uani 0.777(11) 1 d . . P A 1
H35 H 1.140846 0.844050 0.651906 0.038 Uiso 0.777(11) 1 calc R U P A 1
H35A H 1.216585 0.744732 0.689228 0.038 Uiso 0.777(11) 1 calc R U P A 1
H35B H 1.224137 0.866389 0.695428 0.038 Uiso 0.777(11) 1 calc R U P A 1
C36 C 1.1328(7) 0.7892(7) 0.7987(3) 0.027(2) Uani 0.777(11) 1 d . . P A 1
H36 H 1.179263 0.837793 0.806367 0.040 Uiso 0.777(11) 1 calc R U P A 1
H36A H 1.179516 0.715481 0.796742 0.040 Uiso 0.777(11) 1 calc R U P A 1
H36B H 1.074207 0.789035 0.829708 0.040 Uiso 0.777(11) 1 calc R U P A 1
C37 C 1.0143(7) 0.9515(7) 0.7415(4) 0.025(2) Uani 0.777(11) 1 d . . P A 1
H37 H 0.951951 0.957148 0.770832 0.038 Uiso 0.777(11) 1 calc R U P A 1
H37A H 0.985408 0.980500 0.703780 0.038 Uiso 0.777(11) 1 calc R U P A 1
H37B H 1.066023 0.993246 0.751308 0.038 Uiso 0.777(11) 1 calc R U P A 1
C38 C 1.065(6) 0.850(5) 0.725(3) 0.044(8) Uani 0.223(11) 1 d . . P A 2
C39 C 1.030(3) 0.911(3) 0.7758(19) 0.044(8) Uani 0.223(11) 1 d . . P A 2
H39 H 1.037760 0.860046 0.810747 0.066 Uiso 0.223(11) 1 calc R U P A 2
H39A H 0.952120 0.950987 0.773501 0.066 Uiso 0.223(11) 1 calc R U P A 2
H39B H 1.077891 0.961509 0.776969 0.066 Uiso 0.223(11) 1 calc R U P A 2
C40 C 1.050(3) 0.934(2) 0.6669(15) 0.035(9) Uani 0.223(11) 1 d . . P A 2
H40 H 1.097618 0.984805 0.667315 0.052 Uiso 0.223(11) 1 calc R U P A 2
H40A H 0.971277 0.974610 0.665708 0.052 Uiso 0.223(11) 1 calc R U P A 2
H40B H 1.070534 0.893515 0.632860 0.052 Uiso 0.223(11) 1 calc R U P A 2
C41 C 1.192(3) 0.791(3) 0.723(2) 0.045(11) Uani 0.223(11) 1 d . . P A 2
H41 H 1.207594 0.738669 0.756901 0.068 Uiso 0.223(11) 1 calc R U P A 2
H41A H 1.237293 0.844321 0.721985 0.068 Uiso 0.223(11) 1 calc R U P A 2
H41B H 1.211254 0.751988 0.687933 0.068 Uiso 0.223(11) 1 calc R U P A 2
S3 S 0.66971(12) 0.80160(11) 0.68818(6) 0.0190(3) Uani 1 1 d . . . . .
C42 C 0.5266(5) 0.6589(4) 0.7027(2) 0.0154(11) Uani 1 1 d . . . . .
C43 C 0.5820(5) 0.7232(4) 0.7303(2) 0.0165(11) Uani 1 1 d . . . . .
C44 C 0.5606(5) 0.7278(5) 0.7908(3) 0.0215(12) Uani 1 1 d . . . . .
H44 H 0.596146 0.771232 0.809726 0.026 Uiso 1 1 calc R U . . .
C45 C 0.4891(5) 0.6709(5) 0.8236(2) 0.0200(12) Uani 1 1 d . . . . .
C46 C 0.4344(5) 0.6064(5) 0.7942(2) 0.0178(11) Uani 1 1 d . . . . .
H46 H 0.384833 0.567807 0.815329 0.021 Uiso 1 1 calc R U . . .
C47 C 0.4540(5) 0.6004(4) 0.7339(3) 0.0180(11) Uani 1 1 d . . . . .
O4 O 0.5562(3) 0.6438(3) 0.64298(16) 0.0166(8) Uani 1 1 d . . . . .
C48 C 0.4903(5) 0.7254(5) 0.6011(2) 0.0213(12) Uani 1 1 d . . . . .
H48 H 0.489353 0.799683 0.610016 0.026 Uiso 1 1 calc R U . . .
H48A H 0.412191 0.717499 0.602948 0.026 Uiso 1 1 calc R U . . .
C49 C 0.5464(5) 0.7051(5) 0.5411(2) 0.0198(12) Uani 1 1 d . . . . .
C50 C 0.6456(5) 0.7427(5) 0.5229(3) 0.0240(13) Uani 1 1 d . . . . .
H50 H 0.673616 0.783839 0.547017 0.029 Uiso 1 1 calc R U . . .
C51 C 0.7015(5) 0.7181(5) 0.4688(3) 0.0284(14) Uani 1 1 d . . . . .
H51 H 0.767041 0.743224 0.456983 0.034 Uiso 1 1 calc R U . . .
C52 C 0.6617(6) 0.6572(5) 0.4322(3) 0.0284(14) Uani 1 1 d . . . . .
H52 H 0.700360 0.641012 0.396173 0.034 Uiso 1 1 calc R U . . .
C53 C 0.5628(6) 0.6201(5) 0.4497(3) 0.0296(15) Uani 1 1 d . . . . .
H53 H 0.534910 0.579829 0.425000 0.036 Uiso 1 1 calc R U . . .
C54 C 0.5060(5) 0.6432(5) 0.5040(3) 0.0250(13) Uani 1 1 d . . . . .
H54 H 0.440834 0.617455 0.515738 0.030 Uiso 1 1 calc R U . . .
C55 C 0.4709(6) 0.6717(6) 0.8911(3) 0.0344(16) Uani 1 1 d . . . . .
C56 C 0.5468(10) 0.5607(7) 0.9186(4) 0.072(3) Uani 1 1 d . . . . .
H56 H 0.526351 0.551027 0.959956 0.108 Uiso 1 1 calc R U . . .
H56A H 0.625772 0.563243 0.912947 0.108 Uiso 1 1 calc R U . . .
H56B H 0.534928 0.499873 0.899782 0.108 Uiso 1 1 calc R U . . .
C57 C 0.3510(9) 0.6719(13) 0.9121(4) 0.109(6) Uani 1 1 d . . . . .
H57 H 0.343615 0.669791 0.954212 0.163 Uiso 1 1 calc R U . . .
H57A H 0.331131 0.608090 0.900047 0.163 Uiso 1 1 calc R U . . .
H57B H 0.300715 0.737911 0.895428 0.163 Uiso 1 1 calc R U . . .
C58 C 0.5063(8) 0.7673(6) 0.9131(3) 0.045(2) Uani 1 1 d . . . . .
H58 H 0.462129 0.835985 0.895562 0.067 Uiso 1 1 calc R U . . .
H58A H 0.585903 0.762139 0.902704 0.067 Uiso 1 1 calc R U . . .
H58B H 0.493358 0.764566 0.955176 0.067 Uiso 1 1 calc R U . . .
S4 S 0.38006(12) 0.52529(12) 0.69538(6) 0.0183(3) Uani 1 1 d . . . . .
C59 C 0.5661(6) 0.0679(6) 0.5902(3) 0.0366(16) Uani 1 1 d . . . . .
H59 H 0.571107 0.137008 0.603032 0.055 Uiso 1 1 calc R U . . .
H59A H 0.566408 0.014200 0.623605 0.055 Uiso 1 1 calc R U . . .
H59B H 0.496677 0.078258 0.570616 0.055 Uiso 1 1 calc R U . . .
C60 C 0.6676(6) 0.0271(5) 0.5478(3) 0.0251(13) Uani 1 1 d . . . . .
C61 C 0.7748(6) -0.0237(5) 0.5686(3) 0.0318(15) Uani 1 1 d . . . . .
H61 H 0.783538 -0.033708 0.608937 0.038 Uiso 1 1 calc R U . . .
C62 C 0.8677(7) -0.0592(6) 0.5307(4) 0.049(2) Uani 1 1 d . . . . .
H62 H 0.938270 -0.094260 0.545149 0.059 Uiso 1 1 calc R U . . .
C63 C 0.8548(8) -0.0421(6) 0.4704(4) 0.053(2) Uani 1 1 d . . . . .
H63 H 0.917506 -0.062978 0.444129 0.064 Uiso 1 1 calc R U . . .
C64 C 0.7483(8) 0.0061(6) 0.4495(3) 0.047(2) Uani 1 1 d . . . . .
H64 H 0.739666 0.016255 0.409142 0.056 Uiso 1 1 calc R U . . .
C65 C 0.6557(6) 0.0388(5) 0.4874(3) 0.0315(15) Uani 1 1 d . . . . .
H65 H 0.584264 0.069167 0.472796 0.038 Uiso 1 1 calc R U . . .
C66 C 0.7151(8) -0.0654(7) 1.0324(3) 0.048(2) Uani 1 1 d . . . . .
H66 H 0.734072 -0.140455 1.049942 0.072 Uiso 1 1 calc R U . . .
H66A H 0.642039 -0.027811 1.048663 0.072 Uiso 1 1 calc R U . . .
H66B H 0.772148 -0.028151 1.040385 0.072 Uiso 1 1 calc R U . . .
C67 C 0.7107(6) -0.0650(6) 0.9666(3) 0.0376(17) Uani 1 1 d . . . . .
C68 C 0.6322(6) 0.0180(6) 0.9355(3) 0.0348(16) Uani 1 1 d . . . . .
H68 H 0.580310 0.070844 0.955911 0.042 Uiso 1 1 calc R U . . .
C69 C 0.6304(6) 0.0228(6) 0.8747(3) 0.0361(16) Uani 1 1 d . . . . .
H69 H 0.577597 0.078653 0.854857 0.043 Uiso 1 1 calc R U . . .
C70 C 0.7066(6) -0.0548(6) 0.8436(3) 0.0330(15) Uani 1 1 d . . . . .
H70 H 0.706037 -0.051394 0.802876 0.040 Uiso 1 1 calc R U . . .
C71 C 0.7842(6) -0.1385(6) 0.8742(3) 0.0344(16) Uani 1 1 d . . . . .
H71 H 0.834974 -0.192255 0.853919 0.041 Uiso 1 1 calc R U . . .
C72 C 0.7861(6) -0.1417(6) 0.9348(3) 0.0360(16) Uani 1 1 d . . . . .
H72 H 0.839519 -0.197125 0.954563 0.043 Uiso 1 1 calc R U . . .
C73 C 0.4199(9) 0.3031(10) 0.8828(6) 0.092(4) Uani 1 1 d . . . . .
H73 H 0.413755 0.262823 0.850371 0.137 Uiso 1 1 calc R U . . .
H73A H 0.445145 0.251900 0.916117 0.137 Uiso 1 1 calc R U . . .
H73B H 0.473952 0.347893 0.871907 0.137 Uiso 1 1 calc R U . . .
C74 C 0.3045(4) 0.3767(4) 0.8986(3) 0.058(3) Uani 1 1 d G . . . .
C75 C 0.2263(5) 0.4402(5) 0.8600(2) 0.0412(18) Uani 1 1 d G . . . .
H75 H 0.239673 0.435136 0.819677 0.049 Uiso 1 1 calc R U . . .
C76 C 0.1280(4) 0.5114(4) 0.8816(3) 0.064(3) Uani 1 1 d G . . . .
H76 H 0.075656 0.553880 0.855777 0.077 Uiso 1 1 calc R U . . .
C77 C 0.1080(6) 0.5190(6) 0.9419(4) 0.099(5) Uani 1 1 d G . . . .
H77 H 0.042261 0.566592 0.956339 0.119 Uiso 1 1 calc R U . . .
C78 C 0.1863(8) 0.4555(7) 0.9805(2) 0.106(6) Uani 1 1 d G . . . .
H78 H 0.172883 0.460560 1.020802 0.127 Uiso 1 1 calc R U . . .
C79 C 0.2845(7) 0.3843(6) 0.9589(3) 0.081(4) Uani 1 1 d G . . . .
H79 H 0.336900 0.341814 0.984703 0.097 Uiso 1 1 calc R 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
Sn1 O1 2.071(4) . ?
Sn1 O2 2.072(4) . ?
Sn1 O3 2.479(4) . ?
Sn1 O4 2.487(4) . ?
O1 C1 1.321(6) . ?
O2 C28 1.314(6) . ?
C1 C6 1.409(7) . ?
C1 C2 1.413(7) . ?
C2 C3 1.401(8) . ?
C2 S1 1.780(6) . ?
C3 C4 1.395(8) . ?
C4 C5 1.398(8) . ?
C4 C7 1.533(8) . ?
C5 C6 1.393(7) . ?
C6 S4 1.774(5) . ?
C7 C9 1.525(8) . ?
C7 C8 1.544(8) . ?
C7 C10 1.552(9) . ?
S1 C12 1.772(6) . ?
C11 O3 1.386(6) . ?
C11 C16 1.389(8) . ?
C11 C12 1.398(8) . ?
C12 C13 1.395(8) . ?
C13 C14 1.394(8) . ?
C14 C15 1.408(8) . ?
C14 C24 1.538(8) . ?
C15 C16 1.400(8) . ?
C16 S2 1.790(6) . ?
O3 C17 1.457(7) . ?
C17 C18 1.505(8) . ?
C18 C19 1.382(8) . ?
C18 C23 1.392(8) . ?
C19 C20 1.381(9) . ?
C20 C21 1.380(9) . ?
C21 C22 1.390(10) . ?
C22 C23 1.398(9) . ?
C24 C25 1.522(9) . ?
C24 C27 1.535(10) . ?
C24 C26 1.550(9) . ?
S2 C29 1.780(6) . ?
C28 C33 1.423(7) . ?
C28 C29 1.427(7) . ?
C29 C30 1.391(8) . ?
C30 C31 1.402(8) . ?
C31 C32 1.384(8) . ?
C31 C34 1.536(15) . ?
C31 C38 1.55(7) . ?
C32 C33 1.400(7) . ?
C33 S3 1.781(6) . ?
C34 C37 1.530(13) . ?
C34 C36 1.546(12) . ?
C34 C35 1.561(16) . ?
C38 C39 1.44(8) . ?
C38 C41 1.54(7) . ?
C38 C40 1.60(6) . ?
S3 C43 1.770(6) . ?
C42 C47 1.380(8) . ?
C42 C43 1.395(7) . ?
C42 O4 1.404(6) . ?
C43 C44 1.391(8) . ?
C44 C45 1.373(8) . ?
C45 C46 1.414(7) . ?
C45 C55 1.544(8) . ?
C46 C47 1.386(8) . ?
C47 S4 1.786(6) . ?
O4 C48 1.454(6) . ?
C48 C49 1.500(8) . ?
C49 C54 1.399(8) . ?
C49 C50 1.406(8) . ?
C50 C51 1.388(9) . ?
C51 C52 1.380(9) . ?
C52 C53 1.396(9) . ?
C53 C54 1.394(8) . ?
C55 C57 1.488(11) . ?
C55 C58 1.512(9) . ?
C55 C56 1.566(11) . ?
C59 C60 1.519(9) . ?
C60 C65 1.391(9) . ?
C60 C61 1.396(9) . ?
C61 C62 1.375(11) . ?
C62 C63 1.390(12) . ?
C63 C64 1.384(12) . ?
C64 C65 1.366(10) . ?
C66 C67 1.513(9) . ?
C67 C72 1.376(10) . ?
C67 C68 1.399(10) . ?
C68 C69 1.388(9) . ?
C69 C70 1.380(10) . ?
C70 C71 1.392(9) . ?
C71 C72 1.387(9) . ?
C73 C74 1.512(11) . ?
C74 C75 1.3900 . ?
C74 C79 1.3900 . ?
C75 C76 1.3900 . ?
C76 C77 1.3900 . ?
C77 C78 1.3900 . ?
C78 C79 1.3900 . ?

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
O1 Sn1 O2 84.91(15) . . ?
O1 Sn1 O3 82.23(14) . . ?
O2 Sn1 O3 79.88(14) . . ?
O1 Sn1 O4 80.08(14) . . ?
O2 Sn1 O4 82.09(14) . . ?
O3 Sn1 O4 155.71(12) . . ?
C1 O1 Sn1 144.1(4) . . ?
C28 O2 Sn1 144.4(4) . . ?
O1 C1 C6 122.4(5) . . ?
O1 C1 C2 122.1(5) . . ?
C6 C1 C2 115.4(5) . . ?
C3 C2 C1 122.0(5) . . ?
C3 C2 S1 115.3(4) . . ?
C1 C2 S1 122.1(4) . . ?
C4 C3 C2 122.4(5) . . ?
C3 C4 C5 115.3(5) . . ?
C3 C4 C7 123.8(5) . . ?
C5 C4 C7 120.9(5) . . ?
C6 C5 C4 123.3(5) . . ?
C5 C6 C1 121.5(5) . . ?
C5 C6 S4 115.3(4) . . ?
C1 C6 S4 122.7(4) . . ?
C9 C7 C4 112.1(5) . . ?
C9 C7 C8 109.5(5) . . ?
C4 C7 C8 108.2(5) . . ?
C9 C7 C10 107.8(5) . . ?
C4 C7 C10 110.2(5) . . ?
C8 C7 C10 108.9(5) . . ?
C12 S1 C2 104.2(3) . . ?
O3 C11 C16 119.5(5) . . ?
O3 C11 C12 119.8(5) . . ?
C16 C11 C12 120.4(5) . . ?
C13 C12 C11 118.8(5) . . ?
C13 C12 S1 121.6(4) . . ?
C11 C12 S1 119.5(4) . . ?
C14 C13 C12 122.1(5) . . ?
C13 C14 C15 118.1(5) . . ?
C13 C14 C24 119.5(5) . . ?
C15 C14 C24 122.4(5) . . ?
C16 C15 C14 120.4(5) . . ?
C11 C16 C15 120.1(5) . . ?
C11 C16 S2 119.3(4) . . ?
C15 C16 S2 120.4(4) . . ?
C11 O3 C17 114.9(4) . . ?
C11 O3 Sn1 115.5(3) . . ?
C17 O3 Sn1 129.4(3) . . ?
O3 C17 C18 108.9(4) . . ?
C19 C18 C23 119.8(6) . . ?
C19 C18 C17 121.0(5) . . ?
C23 C18 C17 119.2(5) . . ?
C20 C19 C18 120.4(6) . . ?
C21 C20 C19 120.6(6) . . ?
C20 C21 C22 119.4(6) . . ?
C21 C22 C23 120.3(6) . . ?
C18 C23 C22 119.5(6) . . ?
C25 C24 C27 108.7(6) . . ?
C25 C24 C14 112.9(5) . . ?
C27 C24 C14 109.1(5) . . ?
C25 C24 C26 107.9(6) . . ?
C27 C24 C26 109.4(6) . . ?
C14 C24 C26 108.9(5) . . ?
C29 S2 C16 105.4(3) . . ?
O2 C28 C33 123.0(5) . . ?
O2 C28 C29 122.4(5) . . ?
C33 C28 C29 114.5(5) . . ?
C30 C29 C28 122.0(5) . . ?
C30 C29 S2 115.6(4) . . ?
C28 C29 S2 121.7(4) . . ?
C29 C30 C31 122.5(5) . . ?
C32 C31 C30 116.3(5) . . ?
C32 C31 C34 124.4(6) . . ?
C30 C31 C34 119.3(6) . . ?
C32 C31 C38 114(2) . . ?
C30 C31 C38 128(2) . . ?
C31 C32 C33 122.5(5) . . ?
C32 C33 C28 122.2(5) . . ?
C32 C33 S3 115.7(4) . . ?
C28 C33 S3 121.7(4) . . ?
C37 C34 C31 111.4(9) . . ?
C37 C34 C36 108.1(9) . . ?
C31 C34 C36 111.7(8) . . ?
C37 C34 C35 109.3(9) . . ?
C31 C34 C35 107.8(8) . . ?
C36 C34 C35 108.4(9) . . ?
C39 C38 C41 113(5) . . ?
C39 C38 C31 110(5) . . ?
C41 C38 C31 107(4) . . ?
C39 C38 C40 109(4) . . ?
C41 C38 C40 105(5) . . ?
C31 C38 C40 113(4) . . ?
C43 S3 C33 104.3(3) . . ?
C47 C42 C43 121.5(5) . . ?
C47 C42 O4 119.6(5) . . ?
C43 C42 O4 118.4(5) . . ?
C44 C43 C42 117.7(5) . . ?
C44 C43 S3 122.1(4) . . ?
C42 C43 S3 120.1(4) . . ?
C45 C44 C43 122.7(5) . . ?
C44 C45 C46 118.2(5) . . ?
C44 C45 C55 122.2(5) . . ?
C46 C45 C55 119.6(5) . . ?
C47 C46 C45 120.4(5) . . ?
C42 C47 C46 119.5(5) . . ?
C42 C47 S4 119.3(4) . . ?
C46 C47 S4 121.0(4) . . ?
C42 O4 C48 115.7(4) . . ?
C42 O4 Sn1 115.3(3) . . ?
C48 O4 Sn1 128.8(3) . . ?
O4 C48 C49 107.2(4) . . ?
C54 C49 C50 119.1(6) . . ?
C54 C49 C48 121.1(5) . . ?
C50 C49 C48 119.7(5) . . ?
C51 C50 C49 119.7(6) . . ?
C52 C51 C50 121.3(6) . . ?
C51 C52 C53 119.5(6) . . ?
C54 C53 C52 120.1(6) . . ?
C53 C54 C49 120.4(6) . . ?
C57 C55 C58 110.2(7) . . ?
C57 C55 C45 111.9(6) . . ?
C58 C55 C45 112.4(6) . . ?
C57 C55 C56 106.4(8) . . ?
C58 C55 C56 108.6(6) . . ?
C45 C55 C56 107.0(6) . . ?
C6 S4 C47 104.6(2) . . ?
C65 C60 C61 118.4(6) . . ?
C65 C60 C59 120.7(6) . . ?
C61 C60 C59 120.9(6) . . ?
C62 C61 C60 121.4(7) . . ?
C61 C62 C63 119.1(8) . . ?
C64 C63 C62 119.8(8) . . ?
C65 C64 C63 120.8(8) . . ?
C64 C65 C60 120.4(7) . . ?
C72 C67 C68 117.8(7) . . ?
C72 C67 C66 121.9(7) . . ?
C68 C67 C66 120.2(7) . . ?
C69 C68 C67 121.1(7) . . ?
C70 C69 C68 120.3(7) . . ?
C69 C70 C71 119.0(6) . . ?
C72 C71 C70 120.2(7) . . ?
C67 C72 C71 121.6(7) . . ?
C75 C74 C79 120.0 . . ?
C75 C74 C73 127.1(7) . . ?
C79 C74 C73 112.7(7) . . ?
C74 C75 C76 120.0 . . ?
C75 C76 C77 120.0 . . ?
C78 C77 C76 120.0 . . ?
C77 C78 C79 120.0 . . ?
C78 C79 C74 120.0 . . ?

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
Sn1 O1 C1 C6 -93.5(7) . . . . ?
Sn1 O1 C1 C2 90.2(7) . . . . ?
O1 C1 C2 C3 178.6(5) . . . . ?
C6 C1 C2 C3 2.1(8) . . . . ?
O1 C1 C2 S1 -10.9(8) . . . . ?
C6 C1 C2 S1 172.7(4) . . . . ?
C1 C2 C3 C4 0.7(8) . . . . ?
S1 C2 C3 C4 -170.5(4) . . . . ?
C2 C3 C4 C5 -3.0(8) . . . . ?
C2 C3 C4 C7 175.7(5) . . . . ?
C3 C4 C5 C6 2.8(8) . . . . ?
C7 C4 C5 C6 -176.0(5) . . . . ?
C4 C5 C6 C1 -0.1(9) . . . . ?
C4 C5 C6 S4 172.6(4) . . . . ?
O1 C1 C6 C5 -178.9(5) . . . . ?
C2 C1 C6 C5 -2.4(8) . . . . ?
O1 C1 C6 S4 9.1(8) . . . . ?
C2 C1 C6 S4 -174.5(4) . . . . ?
C3 C4 C7 C9 2.5(8) . . . . ?
C5 C4 C7 C9 -178.8(5) . . . . ?
C3 C4 C7 C8 -118.3(6) . . . . ?
C5 C4 C7 C8 60.3(7) . . . . ?
C3 C4 C7 C10 122.6(6) . . . . ?
C5 C4 C7 C10 -58.7(7) . . . . ?
C3 C2 S1 C12 -133.2(4) . . . . ?
C1 C2 S1 C12 55.6(5) . . . . ?
O3 C11 C12 C13 -175.4(5) . . . . ?
C16 C11 C12 C13 -1.2(8) . . . . ?
O3 C11 C12 S1 7.8(7) . . . . ?
C16 C11 C12 S1 -178.0(4) . . . . ?
C2 S1 C12 C13 75.6(5) . . . . ?
C2 S1 C12 C11 -107.7(5) . . . . ?
C11 C12 C13 C14 0.3(8) . . . . ?
S1 C12 C13 C14 177.0(4) . . . . ?
C12 C13 C14 C15 0.6(9) . . . . ?
C12 C13 C14 C24 -179.0(5) . . . . ?
C13 C14 C15 C16 -0.6(8) . . . . ?
C24 C14 C15 C16 179.1(5) . . . . ?
O3 C11 C16 C15 175.4(5) . . . . ?
C12 C11 C16 C15 1.3(8) . . . . ?
O3 C11 C16 S2 -9.7(7) . . . . ?
C12 C11 C16 S2 176.2(4) . . . . ?
C14 C15 C16 C11 -0.4(8) . . . . ?
C14 C15 C16 S2 -175.2(4) . . . . ?
C16 C11 O3 C17 95.9(6) . . . . ?
C12 C11 O3 C17 -89.9(6) . . . . ?
C16 C11 O3 Sn1 -88.4(5) . . . . ?
C12 C11 O3 Sn1 85.8(5) . . . . ?
C11 O3 C17 C18 171.0(5) . . . . ?
Sn1 O3 C17 C18 -3.9(7) . . . . ?
O3 C17 C18 C19 98.2(6) . . . . ?
O3 C17 C18 C23 -82.0(6) . . . . ?
C23 C18 C19 C20 0.1(9) . . . . ?
C17 C18 C19 C20 179.9(6) . . . . ?
C18 C19 C20 C21 0.3(10) . . . . ?
C19 C20 C21 C22 -1.1(10) . . . . ?
C20 C21 C22 C23 1.5(10) . . . . ?
C19 C18 C23 C22 0.2(9) . . . . ?
C17 C18 C23 C22 -179.5(5) . . . . ?
C21 C22 C23 C18 -1.0(9) . . . . ?
C13 C14 C24 C25 178.2(6) . . . . ?
C15 C14 C24 C25 -1.5(9) . . . . ?
C13 C14 C24 C27 -60.9(7) . . . . ?
C15 C14 C24 C27 119.4(7) . . . . ?
C13 C14 C24 C26 58.4(8) . . . . ?
C15 C14 C24 C26 -121.3(6) . . . . ?
C11 C16 S2 C29 105.8(5) . . . . ?
C15 C16 S2 C29 -79.3(5) . . . . ?
Sn1 O2 C28 C33 88.3(7) . . . . ?
Sn1 O2 C28 C29 -95.1(7) . . . . ?
O2 C28 C29 C30 -179.8(5) . . . . ?
C33 C28 C29 C30 -2.9(8) . . . . ?
O2 C28 C29 S2 9.8(8) . . . . ?
C33 C28 C29 S2 -173.3(4) . . . . ?
C16 S2 C29 C30 136.8(5) . . . . ?
C16 S2 C29 C28 -52.1(5) . . . . ?
C28 C29 C30 C31 0.4(9) . . . . ?
S2 C29 C30 C31 171.3(5) . . . . ?
C29 C30 C31 C32 2.6(9) . . . . ?
C29 C30 C31 C34 -179.4(7) . . . . ?
C29 C30 C31 C38 -165(3) . . . . ?
C30 C31 C32 C33 -3.0(9) . . . . ?
C34 C31 C32 C33 179.2(7) . . . . ?
C38 C31 C32 C33 166(3) . . . . ?
C31 C32 C33 C28 0.4(9) . . . . ?
C31 C32 C33 S3 -172.5(5) . . . . ?
O2 C28 C33 C32 179.4(5) . . . . ?
C29 C28 C33 C32 2.5(8) . . . . ?
O2 C28 C33 S3 -8.1(8) . . . . ?
C29 C28 C33 S3 175.1(4) . . . . ?
C32 C31 C34 C37 -0.7(12) . . . . ?
C30 C31 C34 C37 -178.5(7) . . . . ?
C32 C31 C34 C36 120.3(8) . . . . ?
C30 C31 C34 C36 -57.5(11) . . . . ?
C32 C31 C34 C35 -120.7(8) . . . . ?
C30 C31 C34 C35 61.6(9) . . . . ?
C32 C31 C38 C39 68(4) . . . . ?
C30 C31 C38 C39 -124(3) . . . . ?
C32 C31 C38 C41 -170(3) . . . . ?
C30 C31 C38 C41 -2(6) . . . . ?
C32 C31 C38 C40 -54(5) . . . . ?
C30 C31 C38 C40 113(3) . . . . ?
C32 C33 S3 C43 -133.9(4) . . . . ?
C28 C33 S3 C43 53.1(5) . . . . ?
C47 C42 C43 C44 -0.9(8) . . . . ?
O4 C42 C43 C44 -173.4(5) . . . . ?
C47 C42 C43 S3 -177.3(4) . . . . ?
O4 C42 C43 S3 10.2(7) . . . . ?
C33 S3 C43 C44 74.7(5) . . . . ?
C33 S3 C43 C42 -109.0(5) . . . . ?
C42 C43 C44 C45 0.9(8) . . . . ?
S3 C43 C44 C45 177.3(5) . . . . ?
C43 C44 C45 C46 -0.9(9) . . . . ?
C43 C44 C45 C55 176.7(6) . . . . ?
C44 C45 C46 C47 0.8(8) . . . . ?
C55 C45 C46 C47 -176.9(6) . . . . ?
C43 C42 C47 C46 0.8(8) . . . . ?
O4 C42 C47 C46 173.2(5) . . . . ?
C43 C42 C47 S4 176.9(4) . . . . ?
O4 C42 C47 S4 -10.7(7) . . . . ?
C45 C46 C47 C42 -0.7(8) . . . . ?
C45 C46 C47 S4 -176.7(4) . . . . ?
C47 C42 O4 C48 97.1(6) . . . . ?
C43 C42 O4 C48 -90.2(6) . . . . ?
C47 C42 O4 Sn1 -87.2(5) . . . . ?
C43 C42 O4 Sn1 85.4(5) . . . . ?
C42 O4 C48 C49 171.4(5) . . . . ?
Sn1 O4 C48 C49 -3.6(6) . . . . ?
O4 C48 C49 C54 97.6(6) . . . . ?
O4 C48 C49 C50 -78.4(6) . . . . ?
C54 C49 C50 C51 0.0(9) . . . . ?
C48 C49 C50 C51 176.1(5) . . . . ?
C49 C50 C51 C52 0.0(9) . . . . ?
C50 C51 C52 C53 0.4(10) . . . . ?
C51 C52 C53 C54 -0.9(10) . . . . ?
C52 C53 C54 C49 0.9(9) . . . . ?
C50 C49 C54 C53 -0.5(9) . . . . ?
C48 C49 C54 C53 -176.5(5) . . . . ?
C44 C45 C55 C57 143.5(8) . . . . ?
C46 C45 C55 C57 -39.0(10) . . . . ?
C44 C45 C55 C58 18.8(9) . . . . ?
C46 C45 C55 C58 -163.6(6) . . . . ?
C44 C45 C55 C56 -100.3(8) . . . . ?
C46 C45 C55 C56 77.3(8) . . . . ?
C5 C6 S4 C47 135.7(4) . . . . ?
C1 C6 S4 C47 -51.8(5) . . . . ?
C42 C47 S4 C6 106.6(5) . . . . ?
C46 C47 S4 C6 -77.4(5) . . . . ?
C65 C60 C61 C62 1.5(9) . . . . ?
C59 C60 C61 C62 -178.8(6) . . . . ?
C60 C61 C62 C63 1.3(10) . . . . ?
C61 C62 C63 C64 -2.6(11) . . . . ?
C62 C63 C64 C65 1.1(11) . . . . ?
C63 C64 C65 C60 1.8(10) . . . . ?
C61 C60 C65 C64 -3.1(9) . . . . ?
C59 C60 C65 C64 177.3(6) . . . . ?
C72 C67 C68 C69 0.0(11) . . . . ?
C66 C67 C68 C69 176.9(7) . . . . ?
C67 C68 C69 C70 0.1(11) . . . . ?
C68 C69 C70 C71 0.6(10) . . . . ?
C69 C70 C71 C72 -1.3(10) . . . . ?
C68 C67 C72 C71 -0.7(11) . . . . ?
C66 C67 C72 C71 -177.6(7) . . . . ?
C70 C71 C72 C67 1.4(11) . . . . ?
C79 C74 C75 C76 0.0 . . . . ?
C73 C74 C75 C76 -174.2(8) . . . . ?
C74 C75 C76 C77 0.0 . . . . ?
C75 C76 C77 C78 0.0 . . . . ?
C76 C77 C78 C79 0.0 . . . . ?
C77 C78 C79 C74 0.0 . . . . ?
C75 C74 C79 C78 0.0 . . . . ?
C73 C74 C79 C78 175.0(7) . . . . ?

_refine_diff_density_max         1.297
_refine_diff_density_min         -1.222
_refine_diff_density_rms         0.136

####################################################################### 
# 
# 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_5-Pb_Thia_TIPS
_database_code_depnum_ccdc_archive 'CCDC 2021968'
loop_
_audit_author_name
_audit_author_address
'Takuya Kuwabara'
;Chuo Univesity
Japan
;
_audit_update_record             
;
2020-08-06 deposited with the CCDC.	2020-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C131 H208 O8 Pb2 S8 Si4'
_chemical_formula_weight         2694.18

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'
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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                   13.4391(8)
_cell_length_b                   13.7334(7)
_cell_length_c                   20.3149(10)
_cell_angle_alpha                71.319(3)
_cell_angle_beta                 77.604(3)
_cell_angle_gamma                77.966(3)
_cell_volume                     3429.3(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    13540
_cell_measurement_theta_min      2.5358
_cell_measurement_theta_max      31.1603

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_F_000             1406
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    2.659
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8718
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_device_type  'Rigaku VariMax Saturn'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            25173
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.011
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             13148
_reflns_number_gt                11126
_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       'RIGAKU CrystalClear'
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0285P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0117(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         13148
_refine_ls_number_parameters     742
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0271
_refine_ls_wR_factor_ref         0.0683
_refine_ls_wR_factor_gt          0.0674
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_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
Pb1 Pb 0.41259(2) 0.51249(2) 0.31380(2) 0.01206(5) Uani 1 1 d . . . . .
O1 O 0.49052(15) 0.37700(15) 0.38301(10) 0.0136(4) Uani 1 1 d . . . . .
O2 O 0.39593(15) 0.42116(15) 0.24714(10) 0.0124(4) Uani 1 1 d . . . . .
C1 C 0.5864(2) 0.3303(2) 0.38399(15) 0.0115(6) Uani 1 1 d . . . . .
C2 C 0.6079(2) 0.2340(2) 0.43561(15) 0.0121(6) Uani 1 1 d . . . . .
C3 C 0.7085(2) 0.1851(2) 0.43994(15) 0.0130(6) Uani 1 1 d . . . . .
H3 H 0.719854 0.120850 0.473187 0.016 Uiso 1 1 calc R U . . .
C4 C 0.7936(2) 0.2283(2) 0.39646(15) 0.0128(6) Uani 1 1 d . . . . .
C5 C 0.7729(2) 0.3215(2) 0.34465(15) 0.0131(6) Uani 1 1 d . . . . .
H5 H 0.827591 0.352157 0.314320 0.016 Uiso 1 1 calc R U . . .
C6 C 0.6721(2) 0.3701(2) 0.33708(15) 0.0117(6) Uani 1 1 d . . . . .
C7 C 0.9033(2) 0.1712(2) 0.40547(16) 0.0168(7) Uani 1 1 d . . . . .
C8 C 0.9204(3) 0.0709(3) 0.38392(19) 0.0280(8) Uani 1 1 d . . . . .
H8 H 0.990131 0.037145 0.386821 0.042 Uiso 1 1 calc R U . . .
H8A H 0.907920 0.087428 0.336488 0.042 Uiso 1 1 calc R U . . .
H8B H 0.873862 0.025330 0.414978 0.042 Uiso 1 1 calc R U . . .
C9 C 0.9169(3) 0.1448(3) 0.48276(17) 0.0235(8) Uani 1 1 d . . . . .
H9 H 0.905584 0.207737 0.496115 0.035 Uiso 1 1 calc R U . . .
H9A H 0.985484 0.109512 0.488321 0.035 Uiso 1 1 calc R U . . .
H9B H 0.867970 0.100633 0.512149 0.035 Uiso 1 1 calc R U . . .
C10 C 0.9859(2) 0.2378(3) 0.36056(19) 0.0302(9) Uani 1 1 d . . . . .
H10 H 0.980848 0.253808 0.311687 0.045 Uiso 1 1 calc R U . . .
H10A H 1.052936 0.200095 0.368634 0.045 Uiso 1 1 calc R U . . .
H10B H 0.975545 0.301183 0.373275 0.045 Uiso 1 1 calc R U . . .
S1 S 0.50670(5) 0.17884(6) 0.50068(4) 0.01242(15) Uani 1 1 d . . . . .
C11 C 0.3329(2) 0.2678(2) 0.43864(14) 0.0102(6) Uani 1 1 d . . . . .
C12 C 0.4151(2) 0.1857(2) 0.44693(14) 0.0112(6) Uani 1 1 d . . . . .
C13 C 0.4348(2) 0.1187(2) 0.40543(15) 0.0132(6) Uani 1 1 d . . . . .
H13 H 0.487417 0.062424 0.413492 0.016 Uiso 1 1 calc R U . . .
C14 C 0.3782(2) 0.1332(2) 0.35181(14) 0.0119(6) Uani 1 1 d . . . . .
C15 C 0.3022(2) 0.2206(2) 0.33989(14) 0.0119(6) Uani 1 1 d . . . . .
H15 H 0.264788 0.233898 0.303585 0.014 Uiso 1 1 calc R U . . .
C16 C 0.2816(2) 0.2878(2) 0.38112(15) 0.0110(6) Uani 1 1 d . . . . .
C17 C 0.4009(2) 0.0590(2) 0.30674(16) 0.0166(6) Uani 1 1 d . . . . .
C18 C 0.3376(3) -0.0308(3) 0.34280(18) 0.0276(8) Uani 1 1 d . . . . .
H18 H 0.265683 -0.003083 0.349899 0.041 Uiso 1 1 calc R U . . .
H18A H 0.358581 -0.069225 0.387443 0.041 Uiso 1 1 calc R U . . .
H18B H 0.349058 -0.076120 0.313546 0.041 Uiso 1 1 calc R U . . .
C19 C 0.5162(3) 0.0134(3) 0.29893(18) 0.0267(8) Uani 1 1 d . . . . .
H19 H 0.532479 -0.030781 0.343763 0.040 Uiso 1 1 calc R U . . .
H19A H 0.556703 0.068988 0.282311 0.040 Uiso 1 1 calc R U . . .
H19B H 0.531400 -0.026365 0.265842 0.040 Uiso 1 1 calc R U . . .
C20 C 0.3734(3) 0.1137(3) 0.23316(17) 0.0317(9) Uani 1 1 d . . . . .
H20 H 0.408264 0.173256 0.211797 0.048 Uiso 1 1 calc R U . . .
H20A H 0.300301 0.135656 0.236616 0.048 Uiso 1 1 calc R U . . .
H20B H 0.394428 0.066592 0.204849 0.048 Uiso 1 1 calc R U . . .
O3 O 0.31011(15) 0.33725(15) 0.47611(10) 0.0121(4) Uani 1 1 d . . . . .
Si1 Si 0.24904(6) 0.34322(6) 0.55570(4) 0.01176(17) Uani 1 1 d . . . . .
C21 C 0.2363(3) 0.2229(3) 0.70022(16) 0.0257(8) Uani 1 1 d . . . . .
H21 H 0.260740 0.159307 0.733298 0.039 Uiso 1 1 calc R U . . .
H21A H 0.162324 0.234194 0.707978 0.039 Uiso 1 1 calc R U . . .
H21B H 0.260740 0.279800 0.706432 0.039 Uiso 1 1 calc R U . . .
C22 C 0.2767(2) 0.2157(2) 0.62466(15) 0.0166(7) Uani 1 1 d . . . . .
H22 H 0.351879 0.199276 0.620690 0.020 Uiso 1 1 calc R U . . .
C23 C 0.2409(3) 0.1227(2) 0.61536(18) 0.0250(8) Uani 1 1 d . . . . .
H23 H 0.166980 0.130961 0.624415 0.037 Uiso 1 1 calc R U . . .
H23A H 0.268244 0.059820 0.647773 0.037 Uiso 1 1 calc R U . . .
H23B H 0.265069 0.119043 0.568052 0.037 Uiso 1 1 calc R U . . .
C24 C 0.4203(2) 0.4140(2) 0.57596(17) 0.0219(7) Uani 1 1 d . . . . .
H24 H 0.447762 0.470908 0.579611 0.033 Uiso 1 1 calc R U . . .
H24A H 0.456407 0.394605 0.534752 0.033 Uiso 1 1 calc R U . . .
H24B H 0.428719 0.355790 0.616965 0.033 Uiso 1 1 calc R U . . .
C25 C 0.3054(2) 0.4470(2) 0.57047(15) 0.0168(7) Uani 1 1 d . . . . .
H25 H 0.269391 0.458177 0.615426 0.020 Uiso 1 1 calc R U . . .
C26 C 0.2887(3) 0.5515(2) 0.51250(17) 0.0246(8) Uani 1 1 d . . . . .
H26 H 0.321642 0.542408 0.467553 0.037 Uiso 1 1 calc R U . . .
H26A H 0.317860 0.602783 0.521970 0.037 Uiso 1 1 calc R U . . .
H26B H 0.216198 0.574091 0.511988 0.037 Uiso 1 1 calc R U . . .
C27 C 0.0458(3) 0.4261(3) 0.61010(18) 0.0308(9) Uani 1 1 d . . . . .
H27 H 0.040905 0.367072 0.651081 0.046 Uiso 1 1 calc R U . . .
H27A H -0.022086 0.457792 0.599918 0.046 Uiso 1 1 calc R U . . .
H27B H 0.078659 0.475650 0.618653 0.046 Uiso 1 1 calc R U . . .
C28 C 0.1096(2) 0.3908(2) 0.54705(16) 0.0169(7) Uani 1 1 d . . . . .
H28 H 0.108916 0.453322 0.506635 0.020 Uiso 1 1 calc R U . . .
C29 C 0.0546(2) 0.3166(3) 0.52971(17) 0.0220(7) Uani 1 1 d . . . . .
H29 H -0.011531 0.351968 0.517805 0.033 Uiso 1 1 calc R U . . .
H29A H 0.045634 0.257050 0.569912 0.033 Uiso 1 1 calc R U . . .
H29B H 0.095383 0.294542 0.490603 0.033 Uiso 1 1 calc R U . . .
S2 S 0.20675(6) 0.41340(5) 0.35640(4) 0.01237(15) Uani 1 1 d . . . . .
C30 C 0.3090(2) 0.4432(2) 0.22016(15) 0.0119(6) Uani 1 1 d . . . . .
C31 C 0.2125(2) 0.4369(2) 0.26432(15) 0.0120(6) Uani 1 1 d . . . . .
C32 C 0.1209(2) 0.4578(2) 0.23823(15) 0.0135(6) Uani 1 1 d . . . . .
H32 H 0.059172 0.452537 0.269423 0.016 Uiso 1 1 calc R U . . .
C33 C 0.1193(2) 0.4865(2) 0.16575(16) 0.0145(6) Uani 1 1 d . . . . .
C34 C 0.2142(2) 0.4928(2) 0.12208(15) 0.0134(6) Uani 1 1 d . . . . .
H34 H 0.215526 0.511316 0.073705 0.016 Uiso 1 1 calc R U . . .
C35 C 0.3077(2) 0.4726(2) 0.14706(15) 0.0112(6) Uani 1 1 d . . . . .
C36 C 0.0174(2) 0.5072(3) 0.13806(16) 0.0220(7) Uani 1 1 d . . . . .
C37 C -0.0701(3) 0.5598(4) 0.18351(19) 0.0433(11) Uani 1 1 d . . . . .
H37 H -0.051759 0.622942 0.184932 0.065 Uiso 1 1 calc R U . . .
H37A H -0.081002 0.513795 0.230417 0.065 Uiso 1 1 calc R U . . .
H37B H -0.132223 0.575543 0.163564 0.065 Uiso 1 1 calc R U . . .
C38 C -0.0104(3) 0.4045(3) 0.1390(2) 0.0426(11) Uani 1 1 d . . . . .
H38 H -0.020816 0.360693 0.186653 0.064 Uiso 1 1 calc R U . . .
H38A H 0.044650 0.370379 0.111634 0.064 Uiso 1 1 calc R U . . .
H38B H -0.072473 0.417731 0.119389 0.064 Uiso 1 1 calc R U . . .
C39 C 0.0249(2) 0.5784(3) 0.06177(16) 0.0254(8) Uani 1 1 d . . . . .
H39 H 0.073028 0.543457 0.031274 0.038 Uiso 1 1 calc R U . . .
H39A H 0.048041 0.641397 0.059071 0.038 Uiso 1 1 calc R U . . .
H39B H -0.041623 0.594850 0.047409 0.038 Uiso 1 1 calc R U . . .
S3 S 0.41569(5) 0.49857(6) 0.07842(4) 0.01213(15) Uani 1 1 d . . . . .
C40 C 0.5593(2) 0.4925(2) 0.15884(15) 0.0104(6) Uani 1 1 d . . . . .
C41 C 0.5279(2) 0.4442(2) 0.11799(14) 0.0114(6) Uani 1 1 d . . . . .
C42 C 0.5845(2) 0.3496(2) 0.10991(14) 0.0124(6) Uani 1 1 d . . . . .
H42 H 0.565480 0.319307 0.080485 0.015 Uiso 1 1 calc R U . . .
C43 C 0.6683(2) 0.2994(2) 0.14446(15) 0.0122(6) Uani 1 1 d . . . . .
C44 C 0.6891(2) 0.3432(2) 0.19203(15) 0.0121(6) Uani 1 1 d . . . . .
H44 H 0.740868 0.308966 0.218830 0.015 Uiso 1 1 calc R U . A .
C45 C 0.6336(2) 0.4377(2) 0.20037(14) 0.0110(6) Uani 1 1 d . . . A -1
C46 C 0.7365(2) 0.2026(2) 0.12866(16) 0.0153(6) Uani 1 1 d . . . . .
C47 C 0.6740(3) 0.1330(2) 0.11379(17) 0.0214(7) Uani 1 1 d . . . . .
H47 H 0.718480 0.071500 0.106698 0.032 Uiso 1 1 calc R U . . .
H47A H 0.643708 0.170000 0.072272 0.032 Uiso 1 1 calc R U . . .
H47B H 0.620452 0.113697 0.153077 0.032 Uiso 1 1 calc R U . . .
C48 C 0.7935(3) 0.1376(3) 0.19027(19) 0.0307(9) Uani 1 1 d . . . . .
H48 H 0.842885 0.175597 0.194705 0.046 Uiso 1 1 calc R U . . .
H48A H 0.828476 0.073326 0.181554 0.046 Uiso 1 1 calc R U . . .
H48B H 0.744843 0.123127 0.233030 0.046 Uiso 1 1 calc R U . . .
C49 C 0.8150(3) 0.2398(3) 0.06308(19) 0.0322(9) Uani 1 1 d . . . . .
H49 H 0.854322 0.284243 0.071440 0.048 Uiso 1 1 calc R U . . .
H49A H 0.779527 0.277595 0.024009 0.048 Uiso 1 1 calc R U . . .
H49B H 0.860353 0.180826 0.052584 0.048 Uiso 1 1 calc R U . . .
O4 O 0.50916(15) 0.58749(14) 0.16639(10) 0.0119(4) Uani 1 1 d . . . . .
Si2 Si 0.52593(6) 0.70556(6) 0.10815(4) 0.01262(17) Uani 1 1 d . . . . .
C50 C 0.3832(3) 0.8913(2) 0.05999(19) 0.0292(8) Uani 1 1 d . . . . .
H50 H 0.386098 0.918062 0.097652 0.044 Uiso 1 1 calc R U . . .
H50A H 0.318414 0.918879 0.043454 0.044 Uiso 1 1 calc R U . . .
H50B H 0.438400 0.911292 0.022131 0.044 Uiso 1 1 calc R U . . .
C51 C 0.3941(2) 0.7717(2) 0.08682(16) 0.0184(7) Uani 1 1 d . . . . .
H51 H 0.384124 0.749037 0.047921 0.022 Uiso 1 1 calc R U . . .
C52 C 0.3059(2) 0.7390(3) 0.14678(18) 0.0239(7) Uani 1 1 d . . . . .
H52 H 0.241248 0.773246 0.131778 0.036 Uiso 1 1 calc R U . . .
H52A H 0.313060 0.758018 0.186875 0.036 Uiso 1 1 calc R U . . .
H52B H 0.308198 0.665015 0.159317 0.036 Uiso 1 1 calc R U . . .
C53 C 0.7287(2) 0.6447(3) 0.03983(17) 0.0237(7) Uani 1 1 d . . . . .
H53 H 0.754134 0.695305 0.052730 0.035 Uiso 1 1 calc R U . . .
H53A H 0.770116 0.633889 -0.002755 0.035 Uiso 1 1 calc R U . . .
H53B H 0.732076 0.580349 0.076856 0.035 Uiso 1 1 calc R U . . .
C54 C 0.6166(2) 0.6842(2) 0.02811(15) 0.0165(7) Uani 1 1 d . . . . .
H54 H 0.593830 0.628620 0.017129 0.020 Uiso 1 1 calc R U . . .
C55 C 0.6125(3) 0.7787(3) -0.03844(16) 0.0258(8) Uani 1 1 d . . . . .
H55 H 0.658273 0.760805 -0.077499 0.039 Uiso 1 1 calc R U . . .
H55A H 0.633115 0.836162 -0.030254 0.039 Uiso 1 1 calc R U . . .
H55B H 0.543418 0.797953 -0.048855 0.039 Uiso 1 1 calc R U . . .
C56 C 0.5115(3) 0.7818(3) 0.22569(17) 0.0256(8) Uani 1 1 d . . . . .
H56 H 0.452645 0.832835 0.213347 0.038 Uiso 1 1 calc R U . . .
H56A H 0.547816 0.804298 0.252693 0.038 Uiso 1 1 calc R U . . .
H56B H 0.489128 0.716640 0.253123 0.038 Uiso 1 1 calc R U . . .
C57 C 0.5833(3) 0.7682(2) 0.15842(16) 0.0180(7) Uani 1 1 d . . . . .
H57 H 0.643903 0.719323 0.173946 0.022 Uiso 1 1 calc R U . . .
C58 C 0.6224(3) 0.8711(3) 0.11559(18) 0.0297(8) Uani 1 1 d . . . . .
H58 H 0.658826 0.891787 0.143471 0.044 Uiso 1 1 calc R U . . .
H58A H 0.564882 0.923815 0.102696 0.044 Uiso 1 1 calc R U . . .
H58B H 0.667835 0.862095 0.073835 0.044 Uiso 1 1 calc R U . . .
C59 C 0.1851(4) 0.7509(4) 0.3382(2) 0.0578(13) Uani 1 1 d . . . . .
H59 H 0.162621 0.683977 0.355913 0.087 Uiso 1 1 calc R U . . .
H59A H 0.183622 0.777403 0.376814 0.087 Uiso 1 1 calc R U . . .
H59B H 0.254089 0.744214 0.312980 0.087 Uiso 1 1 calc R U . . .
C60 C 0.1164(4) 0.8225(5) 0.2909(3) 0.085(2) Uani 1 1 d . . . . .
H60 H 0.049182 0.833676 0.318875 0.102 Uiso 1 1 calc R U . . .
H60A H 0.108647 0.787602 0.258026 0.102 Uiso 1 1 calc R U . . .
C61 C 0.1449(3) 0.9262(3) 0.2492(2) 0.0454(11) Uani 1 1 d . . . . .
H61 H 0.149601 0.962175 0.282137 0.055 Uiso 1 1 calc R U . . .
H61A H 0.213462 0.914946 0.222855 0.055 Uiso 1 1 calc R U . . .
C62 C 0.0798(4) 0.9954(4) 0.2002(3) 0.092(2) Uani 1 1 d . . . . .
H62 H 0.010942 1.006421 0.226294 0.110 Uiso 1 1 calc R U . . .
H62A H 0.075663 0.960071 0.166740 0.110 Uiso 1 1 calc R U . . .
C63 C 0.1095(4) 1.0999(4) 0.1594(3) 0.0745(17) Uani 1 1 d . . . . .
H63 H 0.066502 1.133403 0.123900 0.112 Uiso 1 1 calc R U . . .
H63A H 0.180305 1.091593 0.137433 0.112 Uiso 1 1 calc R U . . .
H63B H 0.100925 1.141786 0.190650 0.112 Uiso 1 1 calc R U . . .
C64 C -0.0849(16) 0.8485(14) 0.1160(7) 0.076(5) Uani 0.5 1 d . . P B -1
H64 H -0.018178 0.810410 0.124754 0.113 Uiso 0.5 1 calc R U P B -1
H65 H -0.132690 0.800676 0.125730 0.113 Uiso 0.5 1 calc R U P B -1
H66 H -0.108193 0.893251 0.145865 0.113 Uiso 0.5 1 calc R U P B -1
C65 C -0.0779(12) 0.9123(11) 0.0408(8) 0.051(3) Uani 0.5 1 d . . P B -1
H67 H -0.144286 0.954030 0.032728 0.061 Uiso 0.5 1 calc R U P B -1
H68 H -0.060576 0.866787 0.010802 0.061 Uiso 0.5 1 calc R U P B -1
C66 C 0.0045(10) 0.9843(8) 0.0216(5) 0.043(4) Uani 0.5 1 d . . P B -1
H69 H -0.011295 1.027330 0.053226 0.052 Uiso 0.5 1 calc R U P B -1
H70 H 0.071186 0.942174 0.027958 0.052 Uiso 0.5 1 calc R U P B -1
C67 C 0.0099(16) 1.0534(13) -0.0535(8) 0.084(7) Uani 0.5 1 d . . P B -1
H71 H -0.056489 1.095442 -0.061101 0.101 Uiso 0.5 1 calc R U P B -1
H72 H 0.029360 1.011675 -0.086102 0.101 Uiso 0.5 1 calc R U P B -1
C68 C 0.097(2) 1.1276(19) -0.0656(15) 0.145(15) Uani 0.5 1 d . . P B -1
H73 H 0.078686 1.165194 -0.031130 0.218 Uiso 0.5 1 calc R U P B -1
H74 H 0.099608 1.175779 -0.111882 0.218 Uiso 0.5 1 calc R U P B -1
H75 H 0.162783 1.085255 -0.060721 0.218 Uiso 0.5 1 calc R U P B -1
S4 S 0.64929(5) 0.48746(5) 0.26865(4) 0.01116(15) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O1 2.1632(18) . ?
Pb1 O2 2.1891(19) . ?
Pb1 S4 3.0938(7) . ?
O1 C1 1.315(3) . ?
O2 C30 1.333(3) . ?
C1 C6 1.411(4) . ?
C1 C2 1.420(4) . ?
C2 C3 1.385(4) . ?
C2 S1 1.786(3) . ?
C3 C4 1.398(4) . ?
C4 C5 1.391(4) . ?
C4 C7 1.537(4) . ?
C5 C6 1.397(4) . ?
C6 S4 1.780(3) . ?
C7 C8 1.534(4) . ?
C7 C10 1.535(4) . ?
C7 C9 1.537(4) . ?
S1 C12 1.783(3) . ?
C11 O3 1.351(3) . ?
C11 C12 1.400(4) . ?
C11 C16 1.406(4) . ?
C12 C13 1.388(4) . ?
C13 C14 1.400(4) . ?
C14 C15 1.396(4) . ?
C14 C17 1.523(4) . ?
C15 C16 1.386(4) . ?
C16 S2 1.783(3) . ?
C17 C20 1.529(4) . ?
C17 C18 1.540(4) . ?
C17 C19 1.541(4) . ?
O3 Si1 1.668(2) . ?
Si1 C25 1.875(3) . ?
Si1 C28 1.877(3) . ?
Si1 C22 1.884(3) . ?
C21 C22 1.542(4) . ?
C22 C23 1.532(4) . ?
C24 C25 1.534(4) . ?
C25 C26 1.547(4) . ?
C27 C28 1.538(4) . ?
C28 C29 1.537(4) . ?
S2 C31 1.781(3) . ?
C30 C31 1.412(4) . ?
C30 C35 1.412(4) . ?
C31 C32 1.383(4) . ?
C32 C33 1.401(4) . ?
C33 C34 1.390(4) . ?
C33 C36 1.529(4) . ?
C34 C35 1.397(4) . ?
C35 S3 1.791(3) . ?
C36 C38 1.526(5) . ?
C36 C37 1.538(5) . ?
C36 C39 1.540(4) . ?
S3 C41 1.773(3) . ?
C40 O4 1.377(3) . ?
C40 C45 1.385(4) . ?
C40 C41 1.388(4) . ?
C41 C42 1.401(4) . ?
C42 C43 1.394(4) . ?
C43 C44 1.390(4) . ?
C43 C46 1.533(4) . ?
C44 C45 1.397(4) . ?
C45 S4 1.796(3) . ?
C46 C49 1.528(4) . ?
C46 C47 1.529(4) . ?
C46 C48 1.537(4) . ?
O4 Si2 1.700(2) . ?
Si2 C54 1.876(3) . ?
Si2 C57 1.885(3) . ?
Si2 C51 1.887(3) . ?
C50 C51 1.541(4) . ?
C51 C52 1.530(4) . ?
C53 C54 1.534(4) . ?
C54 C55 1.548(4) . ?
C56 C57 1.535(4) . ?
C57 C58 1.535(4) . ?
C59 C60 1.463(6) . ?
C60 C61 1.486(6) . ?
C61 C62 1.442(5) . ?
C62 C63 1.498(7) . ?
C64 C65 1.49(2) . ?
C65 C66 1.54(2) . ?
C66 C67 1.513(17) . ?
C67 C68 1.63(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
O1 Pb1 O2 91.47(7) . . ?
O1 Pb1 S4 67.90(5) . . ?
O2 Pb1 S4 91.84(5) . . ?
C1 O1 Pb1 135.33(17) . . ?
C30 O2 Pb1 117.99(17) . . ?
O1 C1 C6 124.4(2) . . ?
O1 C1 C2 119.4(3) . . ?
C6 C1 C2 116.2(2) . . ?
C3 C2 C1 120.7(3) . . ?
C3 C2 S1 118.6(2) . . ?
C1 C2 S1 120.4(2) . . ?
C2 C3 C4 122.8(3) . . ?
C5 C4 C3 116.7(3) . . ?
C5 C4 C7 123.2(3) . . ?
C3 C4 C7 120.1(2) . . ?
C4 C5 C6 121.6(3) . . ?
C5 C6 C1 121.7(2) . . ?
C5 C6 S4 120.1(2) . . ?
C1 C6 S4 118.2(2) . . ?
C8 C7 C10 108.7(3) . . ?
C8 C7 C9 109.8(3) . . ?
C10 C7 C9 107.4(3) . . ?
C8 C7 C4 109.3(3) . . ?
C10 C7 C4 112.1(2) . . ?
C9 C7 C4 109.5(2) . . ?
C12 S1 C2 100.89(13) . . ?
O3 C11 C12 123.7(2) . . ?
O3 C11 C16 118.2(2) . . ?
C12 C11 C16 117.4(3) . . ?
C13 C12 C11 120.2(3) . . ?
C13 C12 S1 119.2(2) . . ?
C11 C12 S1 119.8(2) . . ?
C12 C13 C14 122.2(3) . . ?
C15 C14 C13 117.1(3) . . ?
C15 C14 C17 121.4(2) . . ?
C13 C14 C17 121.5(3) . . ?
C16 C15 C14 121.2(3) . . ?
C15 C16 C11 121.2(3) . . ?
C15 C16 S2 122.3(2) . . ?
C11 C16 S2 115.6(2) . . ?
C14 C17 C20 111.6(2) . . ?
C14 C17 C18 109.1(3) . . ?
C20 C17 C18 109.0(3) . . ?
C14 C17 C19 110.1(2) . . ?
C20 C17 C19 108.3(3) . . ?
C18 C17 C19 108.7(3) . . ?
C11 O3 Si1 137.67(18) . . ?
O3 Si1 C25 103.05(12) . . ?
O3 Si1 C28 106.27(12) . . ?
C25 Si1 C28 109.25(14) . . ?
O3 Si1 C22 111.16(12) . . ?
C25 Si1 C22 110.53(14) . . ?
C28 Si1 C22 115.75(14) . . ?
C23 C22 C21 109.6(3) . . ?
C23 C22 Si1 115.5(2) . . ?
C21 C22 Si1 112.7(2) . . ?
C24 C25 C26 110.2(3) . . ?
C24 C25 Si1 111.8(2) . . ?
C26 C25 Si1 111.8(2) . . ?
C29 C28 C27 110.2(3) . . ?
C29 C28 Si1 115.3(2) . . ?
C27 C28 Si1 113.5(2) . . ?
C31 S2 C16 102.54(13) . . ?
O2 C30 C31 120.9(3) . . ?
O2 C30 C35 122.7(3) . . ?
C31 C30 C35 116.4(3) . . ?
C32 C31 C30 122.5(3) . . ?
C32 C31 S2 118.4(2) . . ?
C30 C31 S2 118.9(2) . . ?
C31 C32 C33 121.3(3) . . ?
C34 C33 C32 116.4(3) . . ?
C34 C33 C36 123.1(3) . . ?
C32 C33 C36 120.5(3) . . ?
C33 C34 C35 123.4(3) . . ?
C34 C35 C30 120.0(3) . . ?
C34 C35 S3 113.3(2) . . ?
C30 C35 S3 126.4(2) . . ?
C38 C36 C33 109.4(3) . . ?
C38 C36 C37 109.0(3) . . ?
C33 C36 C37 111.1(3) . . ?
C38 C36 C39 107.9(3) . . ?
C33 C36 C39 111.5(3) . . ?
C37 C36 C39 107.8(3) . . ?
C41 S3 C35 106.70(13) . . ?
O4 C40 C45 118.9(3) . . ?
O4 C40 C41 121.7(3) . . ?
C45 C40 C41 118.9(3) . . ?
C40 C41 C42 119.1(3) . . ?
C40 C41 S3 120.9(2) . . ?
C42 C41 S3 120.0(2) . . ?
C43 C42 C41 122.2(3) . . ?
C44 C43 C42 116.9(3) . . ?
C44 C43 C46 121.7(3) . . ?
C42 C43 C46 121.3(3) . . ?
C43 C44 C45 121.3(3) . . ?
C40 C45 C44 120.4(3) . . ?
C40 C45 S4 117.9(2) . . ?
C44 C45 S4 121.6(2) . . ?
C49 C46 C47 108.5(3) . . ?
C49 C46 C43 107.4(2) . . ?
C47 C46 C43 111.9(2) . . ?
C49 C46 C48 109.4(3) . . ?
C47 C46 C48 108.3(3) . . ?
C43 C46 C48 111.3(3) . . ?
C40 O4 Si2 126.11(18) . . ?
O4 Si2 C54 108.25(12) . . ?
O4 Si2 C57 102.97(12) . . ?
C54 Si2 C57 112.43(14) . . ?
O4 Si2 C51 106.12(12) . . ?
C54 Si2 C51 111.70(14) . . ?
C57 Si2 C51 114.59(15) . . ?
C52 C51 C50 109.9(3) . . ?
C52 C51 Si2 113.9(2) . . ?
C50 C51 Si2 114.1(2) . . ?
C53 C54 C55 109.7(3) . . ?
C53 C54 Si2 114.1(2) . . ?
C55 C54 Si2 114.4(2) . . ?
C56 C57 C58 109.7(3) . . ?
C56 C57 Si2 112.8(2) . . ?
C58 C57 Si2 115.5(2) . . ?
C59 C60 C61 118.9(4) . . ?
C62 C61 C60 119.2(4) . . ?
C61 C62 C63 118.1(5) . . ?
C64 C65 C66 111.1(11) . . ?
C67 C66 C65 112.2(10) . . ?
C66 C67 C68 106.8(17) . . ?
C6 S4 C45 100.95(13) . . ?
C6 S4 Pb1 93.89(10) . . ?
C45 S4 Pb1 88.43(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
Pb1 O1 C1 C6 7.4(4) . . . . ?
Pb1 O1 C1 C2 -173.44(19) . . . . ?
O1 C1 C2 C3 -177.2(3) . . . . ?
C6 C1 C2 C3 2.0(4) . . . . ?
O1 C1 C2 S1 -2.3(4) . . . . ?
C6 C1 C2 S1 176.9(2) . . . . ?
C1 C2 C3 C4 2.4(4) . . . . ?
S1 C2 C3 C4 -172.6(2) . . . . ?
C2 C3 C4 C5 -3.8(4) . . . . ?
C2 C3 C4 C7 178.4(3) . . . . ?
C3 C4 C5 C6 0.8(4) . . . . ?
C7 C4 C5 C6 178.6(3) . . . . ?
C4 C5 C6 C1 3.6(4) . . . . ?
C4 C5 C6 S4 -178.4(2) . . . . ?
O1 C1 C6 C5 174.2(3) . . . . ?
C2 C1 C6 C5 -4.9(4) . . . . ?
O1 C1 C6 S4 -3.8(4) . . . . ?
C2 C1 C6 S4 177.1(2) . . . . ?
C5 C4 C7 C8 -110.1(3) . . . . ?
C3 C4 C7 C8 67.6(4) . . . . ?
C5 C4 C7 C10 10.5(4) . . . . ?
C3 C4 C7 C10 -171.8(3) . . . . ?
C5 C4 C7 C9 129.7(3) . . . . ?
C3 C4 C7 C9 -52.6(4) . . . . ?
C3 C2 S1 C12 -134.9(2) . . . . ?
C1 C2 S1 C12 50.1(3) . . . . ?
O3 C11 C12 C13 -178.7(2) . . . . ?
C16 C11 C12 C13 -8.6(4) . . . . ?
O3 C11 C12 S1 -8.6(4) . . . . ?
C16 C11 C12 S1 161.5(2) . . . . ?
C2 S1 C12 C13 72.2(2) . . . . ?
C2 S1 C12 C11 -98.1(2) . . . . ?
C11 C12 C13 C14 3.5(4) . . . . ?
S1 C12 C13 C14 -166.7(2) . . . . ?
C12 C13 C14 C15 2.1(4) . . . . ?
C12 C13 C14 C17 180.0(3) . . . . ?
C13 C14 C15 C16 -2.3(4) . . . . ?
C17 C14 C15 C16 179.8(3) . . . . ?
C14 C15 C16 C11 -3.1(4) . . . . ?
C14 C15 C16 S2 166.0(2) . . . . ?
O3 C11 C16 C15 179.2(3) . . . . ?
C12 C11 C16 C15 8.5(4) . . . . ?
O3 C11 C16 S2 9.4(3) . . . . ?
C12 C11 C16 S2 -161.3(2) . . . . ?
C15 C14 C17 C20 26.7(4) . . . . ?
C13 C14 C17 C20 -151.0(3) . . . . ?
C15 C14 C17 C18 -93.7(3) . . . . ?
C13 C14 C17 C18 88.5(3) . . . . ?
C15 C14 C17 C19 147.0(3) . . . . ?
C13 C14 C17 C19 -30.8(4) . . . . ?
C12 C11 O3 Si1 -80.5(4) . . . . ?
C16 C11 O3 Si1 109.4(3) . . . . ?
C11 O3 Si1 C25 157.4(3) . . . . ?
C11 O3 Si1 C28 -87.7(3) . . . . ?
C11 O3 Si1 C22 39.0(3) . . . . ?
O3 Si1 C22 C23 -62.2(3) . . . . ?
C25 Si1 C22 C23 -176.0(2) . . . . ?
C28 Si1 C22 C23 59.2(3) . . . . ?
O3 Si1 C22 C21 170.7(2) . . . . ?
C25 Si1 C22 C21 56.9(3) . . . . ?
C28 Si1 C22 C21 -67.9(3) . . . . ?
O3 Si1 C25 C24 -65.8(2) . . . . ?
C28 Si1 C25 C24 -178.4(2) . . . . ?
C22 Si1 C25 C24 53.1(2) . . . . ?
O3 Si1 C25 C26 58.3(2) . . . . ?
C28 Si1 C25 C26 -54.4(3) . . . . ?
C22 Si1 C25 C26 177.1(2) . . . . ?
O3 Si1 C28 C29 65.5(2) . . . . ?
C25 Si1 C28 C29 176.1(2) . . . . ?
C22 Si1 C28 C29 -58.4(3) . . . . ?
O3 Si1 C28 C27 -166.1(2) . . . . ?
C25 Si1 C28 C27 -55.6(3) . . . . ?
C22 Si1 C28 C27 70.0(3) . . . . ?
C15 C16 S2 C31 -19.2(3) . . . . ?
C11 C16 S2 C31 150.4(2) . . . . ?
Pb1 O2 C30 C31 -59.0(3) . . . . ?
Pb1 O2 C30 C35 121.8(2) . . . . ?
O2 C30 C31 C32 -179.0(3) . . . . ?
C35 C30 C31 C32 0.3(4) . . . . ?
O2 C30 C31 S2 7.1(4) . . . . ?
C35 C30 C31 S2 -173.6(2) . . . . ?
C16 S2 C31 C32 122.9(2) . . . . ?
C16 S2 C31 C30 -63.0(3) . . . . ?
C30 C31 C32 C33 0.0(4) . . . . ?
S2 C31 C32 C33 173.9(2) . . . . ?
C31 C32 C33 C34 0.1(4) . . . . ?
C31 C32 C33 C36 178.8(3) . . . . ?
C32 C33 C34 C35 -0.4(4) . . . . ?
C36 C33 C34 C35 -179.1(3) . . . . ?
C33 C34 C35 C30 0.6(4) . . . . ?
C33 C34 C35 S3 -174.5(2) . . . . ?
O2 C30 C35 C34 178.7(3) . . . . ?
C31 C30 C35 C34 -0.6(4) . . . . ?
O2 C30 C35 S3 -6.8(4) . . . . ?
C31 C30 C35 S3 173.9(2) . . . . ?
C34 C33 C36 C38 94.5(4) . . . . ?
C32 C33 C36 C38 -84.1(4) . . . . ?
C34 C33 C36 C37 -145.1(3) . . . . ?
C32 C33 C36 C37 36.3(4) . . . . ?
C34 C33 C36 C39 -24.8(4) . . . . ?
C32 C33 C36 C39 156.6(3) . . . . ?
C34 C35 S3 C41 -168.3(2) . . . . ?
C30 C35 S3 C41 17.0(3) . . . . ?
O4 C40 C41 C42 177.4(2) . . . . ?
C45 C40 C41 C42 -11.4(4) . . . . ?
O4 C40 C41 S3 -4.5(4) . . . . ?
C45 C40 C41 S3 166.7(2) . . . . ?
C35 S3 C41 C40 -75.5(3) . . . . ?
C35 S3 C41 C42 102.7(2) . . . . ?
C40 C41 C42 C43 3.4(4) . . . . ?
S3 C41 C42 C43 -174.8(2) . . . . ?
C41 C42 C43 C44 4.8(4) . . . . ?
C41 C42 C43 C46 -173.1(3) . . . . ?
C42 C43 C44 C45 -5.1(4) . . . . ?
C46 C43 C44 C45 172.8(3) . . . . ?
O4 C40 C45 C44 -177.3(2) . . . . ?
C41 C40 C45 C44 11.3(4) . . . . ?
O4 C40 C45 S4 7.1(4) . . . . ?
C41 C40 C45 S4 -164.4(2) . . . . ?
C43 C44 C45 C40 -2.9(4) . . . . ?
C43 C44 C45 S4 172.6(2) . . . . ?
C44 C43 C46 C49 -95.0(3) . . . . ?
C42 C43 C46 C49 82.9(3) . . . . ?
C44 C43 C46 C47 146.0(3) . . . . ?
C42 C43 C46 C47 -36.1(4) . . . . ?
C44 C43 C46 C48 24.7(4) . . . . ?
C42 C43 C46 C48 -157.4(3) . . . . ?
C45 C40 O4 Si2 107.8(3) . . . . ?
C41 C40 O4 Si2 -81.0(3) . . . . ?
C40 O4 Si2 C54 4.6(3) . . . . ?
C40 O4 Si2 C57 -114.6(2) . . . . ?
C40 O4 Si2 C51 124.6(2) . . . . ?
O4 Si2 C51 C52 29.5(3) . . . . ?
C54 Si2 C51 C52 147.2(2) . . . . ?
C57 Si2 C51 C52 -83.4(3) . . . . ?
O4 Si2 C51 C50 156.8(2) . . . . ?
C54 Si2 C51 C50 -85.5(3) . . . . ?
C57 Si2 C51 C50 43.9(3) . . . . ?
O4 Si2 C54 C53 -71.7(2) . . . . ?
C57 Si2 C54 C53 41.4(3) . . . . ?
C51 Si2 C54 C53 171.9(2) . . . . ?
O4 Si2 C54 C55 160.9(2) . . . . ?
C57 Si2 C54 C55 -86.1(2) . . . . ?
C51 Si2 C54 C55 44.4(3) . . . . ?
O4 Si2 C57 C56 -61.3(2) . . . . ?
C54 Si2 C57 C56 -177.5(2) . . . . ?
C51 Si2 C57 C56 53.5(3) . . . . ?
O4 Si2 C57 C58 171.4(2) . . . . ?
C54 Si2 C57 C58 55.1(3) . . . . ?
C51 Si2 C57 C58 -73.9(3) . . . . ?
C59 C60 C61 C62 177.4(5) . . . . ?
C60 C61 C62 C63 179.4(5) . . . . ?
C64 C65 C66 C67 -177.5(12) . . . . ?
C65 C66 C67 C68 178.0(16) . . . . ?
C5 C6 S4 C45 93.1(2) . . . . ?
C1 C6 S4 C45 -88.9(2) . . . . ?
C5 C6 S4 Pb1 -177.8(2) . . . . ?
C1 C6 S4 Pb1 0.3(2) . . . . ?
C40 C45 S4 C6 141.4(2) . . . . ?
C44 C45 S4 C6 -34.2(3) . . . . ?
C40 C45 S4 Pb1 47.8(2) . . . . ?
C44 C45 S4 Pb1 -127.8(2) . . . . ?

_refine_diff_density_max         1.635
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.105

####################################################################### 
# 
# 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_ydkr_a_a
_database_code_depnum_ccdc_archive 'CCDC 2016539'
loop_
_audit_author_name
_audit_author_address
'Takuya Kuwabara'
;Chuo Univesity
Japan
;
_audit_update_record             
;
2020-07-15 deposited with the CCDC.	2020-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H86 O4 S4 Si2 Sn'
_chemical_formula_weight         1150.37

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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                   13.3770(12)
_cell_length_b                   17.7497(15)
_cell_length_c                   25.887(2)
_cell_angle_alpha                90
_cell_angle_beta                 102.696(2)
_cell_angle_gamma                90
_cell_volume                     5996.3(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    18360
_cell_measurement_theta_min      1.9370
_cell_measurement_theta_max      31.2209

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_F_000             2432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1800
_exptl_crystal_size_mid          0.1700
_exptl_crystal_size_min          0.1000
_exptl_absorpt_coefficient_mu    0.648
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8793
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_device_type  'Rigaku VariMax Saturn'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            48104
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.033
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             13722
_reflns_number_gt                11958
_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       'RIGAKU CrystalClear'
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Yadokari-XG 2009(Wakita Nemoto et al.)'
_computing_publication_material  'Yadokari-XG 2009(Wakita,Nemoto et al.)'
_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)+(0.0428P)²+0.4685P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13722
_refine_ls_number_parameters     646
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.0899
_refine_ls_wR_factor_gt          0.0856
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.004
_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
Sn1 Sn 0.74872(2) 0.29139(2) 0.25233(2) 0.01507(5) Uani 1 1 d . . . . .
O1 O 0.78207(10) 0.36175(9) 0.19668(5) 0.0210(3) Uani 1 1 d . . . . .
C1 C 0.86596(14) 0.38417(11) 0.18186(7) 0.0135(4) Uani 1 1 d . . . . .
O2 O 0.70101(10) 0.38231(8) 0.28858(5) 0.0164(3) Uani 1 1 d . . . . .
C2 C 0.85986(14) 0.41620(10) 0.13132(7) 0.0134(4) Uani 1 1 d . . . . .
C3 C 0.94855(14) 0.43733(10) 0.11512(7) 0.0139(4) Uani 1 1 d . . . . .
H1 H 0.942051 0.458581 0.081708 0.017 Uiso 1 1 calc R U . . .
C4 C 1.04690(14) 0.42804(10) 0.14683(8) 0.0142(4) Uani 1 1 d . . . . .
C5 C 1.05210(14) 0.39966(10) 0.19776(7) 0.0135(4) Uani 1 1 d . . . . .
H2 H 1.115859 0.394689 0.220684 0.016 Uiso 1 1 calc R U . . .
C6 C 0.96507(14) 0.37866(10) 0.21517(7) 0.0124(4) Uani 1 1 d . . . . .
C7 C 1.14527(15) 0.44843(12) 0.12888(8) 0.0193(4) Uani 1 1 d . . . . .
C8 C 1.12404(16) 0.47234(13) 0.07073(8) 0.0235(5) Uani 1 1 d . . . . .
H3 H 1.088386 0.432649 0.049024 0.035 Uiso 1 1 calc R U . . .
H4 H 1.187723 0.482310 0.060703 0.035 Uiso 1 1 calc R U . . .
H5 H 1.082674 0.517065 0.065948 0.035 Uiso 1 1 calc R U . . .
C9 C 1.21700(17) 0.37957(14) 0.13571(10) 0.0339(6) Uani 1 1 d . . . . .
H6 H 1.184339 0.339209 0.113605 0.051 Uiso 1 1 calc R U . . .
H7 H 1.231665 0.363701 0.172046 0.051 Uiso 1 1 calc R U . . .
H8 H 1.279724 0.392865 0.125731 0.051 Uiso 1 1 calc R U . . .
C10 C 1.20017(18) 0.51317(14) 0.16286(9) 0.0338(6) Uani 1 1 d . . . . .
H9 H 1.261080 0.526367 0.151054 0.051 Uiso 1 1 calc R U . . .
H10 H 1.218290 0.497626 0.199238 0.051 Uiso 1 1 calc R U . . .
H11 H 1.155508 0.556076 0.159558 0.051 Uiso 1 1 calc R U . . .
S1 S 0.74319(4) 0.42558(3) 0.08271(2) 0.01500(10) Uani 1 1 d . . . . .
C11 C 0.59506(14) 0.39256(10) 0.13785(7) 0.0113(4) Uani 1 1 d . . . . .
C12 C 0.65107(14) 0.44962(11) 0.12045(7) 0.0130(4) Uani 1 1 d . . . . .
C13 C 0.64021(14) 0.52408(11) 0.13567(7) 0.0130(4) Uani 1 1 d . . . . .
H12 H 0.675759 0.562080 0.122656 0.016 Uiso 1 1 calc R U . . .
C14 C 0.57682(14) 0.54253(10) 0.17012(7) 0.0122(4) Uani 1 1 d . . . . .
C15 C 0.53221(14) 0.48327(10) 0.19251(7) 0.0126(4) Uani 1 1 d . . . . .
H13 H 0.494190 0.493722 0.217715 0.015 Uiso 1 1 calc R U . . .
C16 C 0.54356(14) 0.40903(10) 0.17784(7) 0.0115(4) Uani 1 1 d . . . . .
O3 O 0.59902(10) 0.31927(7) 0.12243(5) 0.0139(3) Uani 1 1 d . . . . .
Si1 Si 0.53667(4) 0.27585(3) 0.06704(2) 0.01225(11) Uani 1 1 d . . . . .
C17 C 0.49582(18) 0.15341(12) 0.13100(8) 0.0250(5) Uani 1 1 d . . . . .
H14 H 0.444989 0.125033 0.143664 0.037 Uiso 1 1 calc R U . . .
H15 H 0.540299 0.178136 0.160234 0.037 Uiso 1 1 calc R U . . .
H16 H 0.535280 0.120040 0.114121 0.037 Uiso 1 1 calc R U . . .
C18 C 0.44312(16) 0.21232(11) 0.09115(8) 0.0193(4) Uani 1 1 d . . . . .
H17 H 0.404638 0.244883 0.110412 0.023 Uiso 1 1 calc R U . . .
C19 C 0.36301(18) 0.17422(14) 0.04731(9) 0.0322(6) Uani 1 1 d . . . . .
H18 H 0.395994 0.137343 0.029632 0.048 Uiso 1 1 calc R U . . .
H19 H 0.330704 0.211480 0.022257 0.048 Uiso 1 1 calc R U . . .
H20 H 0.312247 0.150036 0.062656 0.048 Uiso 1 1 calc R U . . .
C20 C 0.72635(16) 0.19391(12) 0.08311(8) 0.0213(4) Uani 1 1 d . . . . .
H21 H 0.700839 0.153319 0.101073 0.032 Uiso 1 1 calc R U . . .
H22 H 0.753556 0.232666 0.108129 0.032 Uiso 1 1 calc R U . . .
H23 H 0.779458 0.175477 0.066809 0.032 Uiso 1 1 calc R U . . .
C21 C 0.63845(14) 0.22642(11) 0.04031(7) 0.0142(4) Uani 1 1 d . . . . .
H24 H 0.669743 0.265229 0.022040 0.017 Uiso 1 1 calc R U . . .
C22 C 0.59481(16) 0.16733(12) -0.00205(8) 0.0216(4) Uani 1 1 d . . . . .
H25 H 0.648483 0.149306 -0.018100 0.032 Uiso 1 1 calc R U . . .
H26 H 0.541760 0.189786 -0.028644 0.032 Uiso 1 1 calc R U . . .
H27 H 0.566927 0.125996 0.014130 0.032 Uiso 1 1 calc R U . . .
C23 C 0.52716(16) 0.39454(12) -0.01162(8) 0.0209(4) Uani 1 1 d . . . . .
H28 H 0.483804 0.418042 -0.041798 0.031 Uiso 1 1 calc R U . . .
H29 H 0.579793 0.366261 -0.022820 0.031 Uiso 1 1 calc R U . . .
H30 H 0.558032 0.432546 0.013196 0.031 Uiso 1 1 calc R U . . .
C24 C 0.46295(15) 0.34141(11) 0.01488(7) 0.0174(4) Uani 1 1 d . . . . .
H31 H 0.427166 0.308374 -0.013565 0.021 Uiso 1 1 calc R U . . .
C25 C 0.37781(16) 0.38608(12) 0.03255(9) 0.0251(5) Uani 1 1 d . . . . .
H32 H 0.407891 0.420183 0.060429 0.038 Uiso 1 1 calc R U . . .
H33 H 0.333013 0.351825 0.045171 0.038 Uiso 1 1 calc R U . . .
H34 H 0.339373 0.414115 0.003081 0.038 Uiso 1 1 calc R U . . .
C26 C 0.55968(15) 0.62355(11) 0.18694(8) 0.0154(4) Uani 1 1 d . . . . .
C27 C 0.44405(16) 0.63951(12) 0.17750(10) 0.0275(5) Uani 1 1 d . . . . .
H35 H 0.433452 0.691053 0.186179 0.041 Uiso 1 1 calc R U . . .
H36 H 0.413910 0.606891 0.199458 0.041 Uiso 1 1 calc R U . . .
H37 H 0.412623 0.630542 0.140970 0.041 Uiso 1 1 calc R U . . .
C28 C 0.60731(17) 0.68185(11) 0.15619(8) 0.0230(5) Uani 1 1 d . . . . .
H38 H 0.592736 0.731562 0.167159 0.034 Uiso 1 1 calc R U . . .
H39 H 0.578991 0.676114 0.118974 0.034 Uiso 1 1 calc R U . . .
H40 H 0.680147 0.674511 0.163107 0.034 Uiso 1 1 calc R U . . .
C29 C 0.60727(17) 0.63182(12) 0.24634(8) 0.0227(5) Uani 1 1 d . . . . .
H41 H 0.678083 0.617284 0.253155 0.034 Uiso 1 1 calc R U . . .
H42 H 0.571351 0.600037 0.266183 0.034 Uiso 1 1 calc R U . . .
H43 H 0.602108 0.683320 0.256788 0.034 Uiso 1 1 calc R U . . .
S2 S 0.50916(4) 0.33113(3) 0.21414(2) 0.01275(10) Uani 1 1 d . . . . .
C30 C 0.61720(14) 0.39274(10) 0.30728(7) 0.0121(4) Uani 1 1 d . . . . .
C31 C 0.51799(14) 0.37373(10) 0.27703(7) 0.0119(4) Uani 1 1 d . . . . .
C32 C 0.43012(14) 0.38664(10) 0.29593(7) 0.0126(4) Uani 1 1 d . . . . .
H44 H 0.366826 0.373228 0.275030 0.015 Uiso 1 1 calc R U . . .
C33 C 0.43408(14) 0.41934(10) 0.34568(7) 0.0127(4) Uani 1 1 d . . . . .
C34 C 0.53103(14) 0.43956(10) 0.37461(7) 0.0125(4) Uani 1 1 d . . . . .
H45 H 0.536030 0.462727 0.407306 0.015 Uiso 1 1 calc R U . . .
C35 C 0.62102(14) 0.42675(10) 0.35695(7) 0.0122(4) Uani 1 1 d . . . . .
C36 C 0.33554(14) 0.43313(11) 0.36498(8) 0.0158(4) Uani 1 1 d . . . . .
C37 C 0.26733(16) 0.48932(13) 0.32777(9) 0.0262(5) Uani 1 1 d . . . . .
H46 H 0.303982 0.535652 0.326971 0.039 Uiso 1 1 calc R U . . .
H47 H 0.206217 0.498867 0.340408 0.039 Uiso 1 1 calc R U . . .
H48 H 0.249250 0.468488 0.292733 0.039 Uiso 1 1 calc R U . . .
C38 C 0.27677(17) 0.35880(12) 0.36517(9) 0.0286(5) Uani 1 1 d . . . . .
H49 H 0.262439 0.337391 0.330265 0.043 Uiso 1 1 calc R U . . .
H50 H 0.213559 0.368325 0.375804 0.043 Uiso 1 1 calc R U . . .
H51 H 0.317583 0.324244 0.389567 0.043 Uiso 1 1 calc R U . . .
C39 C 0.35657(15) 0.46581(11) 0.42120(8) 0.0188(4) Uani 1 1 d . . . . .
H52 H 0.399696 0.431878 0.445106 0.028 Uiso 1 1 calc R U . . .
H53 H 0.292934 0.472343 0.432029 0.028 Uiso 1 1 calc R U . . .
H54 H 0.390229 0.513642 0.421635 0.028 Uiso 1 1 calc R U . . .
S3 S 0.73540(4) 0.45212(3) 0.40395(2) 0.01405(10) Uani 1 1 d . . . . .
C40 C 0.88359(13) 0.41169(10) 0.35100(7) 0.0108(4) Uani 1 1 d . . . . .
C41 C 0.82775(14) 0.47113(11) 0.36569(7) 0.0116(4) Uani 1 1 d . . . . .
C42 C 0.84190(14) 0.54411(10) 0.34863(7) 0.0128(4) Uani 1 1 d . . . . .
H55 H 0.806594 0.583735 0.359970 0.015 Uiso 1 1 calc R U . . .
C43 C 0.90795(14) 0.55901(10) 0.31488(7) 0.0125(4) Uani 1 1 d . . . . .
C44 C 0.95216(14) 0.49737(10) 0.29518(7) 0.0125(4) Uani 1 1 d . . . . .
H56 H 0.992036 0.505208 0.270422 0.015 Uiso 1 1 calc R U . . .
C45 C 0.93808(13) 0.42469(10) 0.31163(7) 0.0108(4) Uani 1 1 d . . . . .
O4 O 0.87805(10) 0.33970(7) 0.36891(5) 0.0127(3) Uani 1 1 d . . . . .
Si2 Si 0.94216(4) 0.30770(3) 0.42882(2) 0.01212(11) Uani 1 1 d . . . . .
C46 C 0.99811(18) 0.17641(12) 0.37913(8) 0.0251(5) Uani 1 1 d . . . . .
H57 H 1.052028 0.148420 0.368879 0.038 Uiso 1 1 calc R U . . .
H58 H 0.950344 0.193452 0.348038 0.038 Uiso 1 1 calc R U . . .
H59 H 0.963349 0.144688 0.399578 0.038 Uiso 1 1 calc R U . . .
C47 C 1.04377(15) 0.24451(11) 0.41249(8) 0.0184(4) Uani 1 1 d . . . . .
H60 H 1.079243 0.274324 0.390143 0.022 Uiso 1 1 calc R U . . .
C48 C 1.12670(17) 0.21839(13) 0.46009(9) 0.0288(5) Uani 1 1 d . . . . .
H61 H 1.096406 0.186224 0.482249 0.043 Uiso 1 1 calc R U . . .
H62 H 1.156649 0.261488 0.480042 0.043 Uiso 1 1 calc R U . . .
H63 H 1.178843 0.191146 0.447693 0.043 Uiso 1 1 calc R U . . .
C49 C 0.75436(16) 0.22618(12) 0.41612(8) 0.0227(5) Uani 1 1 d . . . . .
H64 H 0.780026 0.188562 0.395739 0.034 Uiso 1 1 calc R U . . .
H65 H 0.722728 0.265981 0.393133 0.034 Uiso 1 1 calc R U . . .
H66 H 0.704718 0.203883 0.433183 0.034 Uiso 1 1 calc R U . . .
C50 C 0.84354(15) 0.25842(11) 0.45830(7) 0.0161(4) Uani 1 1 d . . . . .
H67 H 0.813672 0.297048 0.477380 0.019 Uiso 1 1 calc R U . . .
C51 C 0.88809(17) 0.19741(12) 0.49960(8) 0.0231(5) Uani 1 1 d . . . . .
H68 H 0.835515 0.180025 0.516667 0.035 Uiso 1 1 calc R U . . .
H69 H 0.943493 0.218424 0.525584 0.035 Uiso 1 1 calc R U . . .
H70 H 0.912923 0.155918 0.482199 0.035 Uiso 1 1 calc R U . . .
C52 C 1.02265(17) 0.37333(13) 0.53032(8) 0.0240(5) Uani 1 1 d . . . . .
H71 H 1.075487 0.335760 0.537762 0.036 Uiso 1 1 calc R U . . .
H72 H 0.962379 0.354860 0.540556 0.036 Uiso 1 1 calc R U . . .
H73 H 1.045899 0.418342 0.549849 0.036 Uiso 1 1 calc R U . . .
C53 C 0.99730(14) 0.39099(11) 0.47071(7) 0.0149(4) Uani 1 1 d . . . . .
H74 H 0.943377 0.429410 0.465238 0.018 Uiso 1 1 calc R U . . .
C54 C 1.09023(15) 0.42757(12) 0.45461(8) 0.0208(4) Uani 1 1 d . . . . .
H75 H 1.109265 0.472494 0.475050 0.031 Uiso 1 1 calc R U . . .
H76 H 1.072712 0.440139 0.417649 0.031 Uiso 1 1 calc R U . . .
H77 H 1.146668 0.392879 0.461081 0.031 Uiso 1 1 calc R U . . .
C55 C 0.93218(15) 0.63889(11) 0.29871(8) 0.0159(4) Uani 1 1 d . . . . .
C56 C 0.87612(17) 0.69955(11) 0.32309(8) 0.0215(4) Uani 1 1 d . . . . .
H78 H 0.803504 0.692458 0.311469 0.032 Uiso 1 1 calc R U . . .
H79 H 0.894530 0.748342 0.312141 0.032 Uiso 1 1 calc R U . . .
H80 H 0.895072 0.696022 0.360990 0.032 Uiso 1 1 calc R U . . .
C57 C 1.04846(16) 0.65267(12) 0.31740(9) 0.0265(5) Uani 1 1 d . . . . .
H81 H 1.064117 0.703467 0.309179 0.040 Uiso 1 1 calc R U . . .
H82 H 1.085008 0.618232 0.299680 0.040 Uiso 1 1 calc R U . . .
H83 H 1.068570 0.644887 0.354950 0.040 Uiso 1 1 calc R U . . .
C58 C 0.90324(17) 0.64552(12) 0.23806(8) 0.0229(5) Uani 1 1 d . . . . .
H84 H 0.832333 0.632625 0.225605 0.034 Uiso 1 1 calc R U . . .
H85 H 0.944913 0.611789 0.222824 0.034 Uiso 1 1 calc R U . . .
H86 H 0.914389 0.696305 0.227868 0.034 Uiso 1 1 calc R U . . .
S4 S 0.97585(4) 0.34287(3) 0.28014(2) 0.01259(10) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 O1 2.0291(14) . ?
Sn1 O2 2.0385(13) . ?
O1 C1 1.324(2) . ?
C1 C2 1.412(3) . ?
C1 C6 1.417(3) . ?
O2 C30 1.328(2) . ?
C2 C3 1.394(3) . ?
C2 S1 1.7842(19) . ?
C3 C4 1.399(3) . ?
C4 C5 1.399(3) . ?
C4 C7 1.532(3) . ?
C5 C6 1.389(3) . ?
C6 S4 1.7737(19) . ?
C7 C8 1.529(3) . ?
C7 C10 1.533(3) . ?
C7 C9 1.540(3) . ?
S1 C12 1.7845(19) . ?
C11 O3 1.365(2) . ?
C11 C12 1.392(3) . ?
C11 C16 1.395(2) . ?
C12 C13 1.396(3) . ?
C13 C14 1.398(3) . ?
C14 C15 1.397(3) . ?
C14 C26 1.534(3) . ?
C15 C16 1.389(2) . ?
C16 S2 1.7879(19) . ?
O3 Si1 1.6793(13) . ?
Si1 C21 1.8753(19) . ?
Si1 C24 1.8880(19) . ?
Si1 C18 1.890(2) . ?
C17 C18 1.528(3) . ?
C18 C19 1.536(3) . ?
C20 C21 1.540(3) . ?
C21 C22 1.537(3) . ?
C23 C24 1.535(3) . ?
C24 C25 1.537(3) . ?
C26 C28 1.528(3) . ?
C26 C29 1.536(3) . ?
C26 C27 1.538(3) . ?
S2 C31 1.7753(18) . ?
C30 C35 1.411(3) . ?
C30 C31 1.425(2) . ?
C31 C32 1.388(2) . ?
C32 C33 1.403(3) . ?
C33 C34 1.395(3) . ?
C33 C36 1.528(3) . ?
C34 C35 1.397(2) . ?
C35 S3 1.7904(19) . ?
C36 C39 1.534(3) . ?
C36 C38 1.536(3) . ?
C36 C37 1.539(3) . ?
S3 C41 1.7771(19) . ?
C40 O4 1.367(2) . ?
C40 C41 1.393(3) . ?
C40 C45 1.396(2) . ?
C41 C42 1.395(3) . ?
C42 C43 1.398(3) . ?
C43 C44 1.393(3) . ?
C43 C55 1.533(3) . ?
C44 C45 1.384(2) . ?
C45 S4 1.7917(18) . ?
O4 Si2 1.6966(13) . ?
Si2 C50 1.8791(19) . ?
Si2 C47 1.881(2) . ?
Si2 C53 1.8853(19) . ?
C46 C47 1.532(3) . ?
C47 C48 1.537(3) . ?
C49 C50 1.540(3) . ?
C50 C51 1.546(3) . ?
C52 C53 1.538(3) . ?
C53 C54 1.539(3) . ?
C55 C56 1.526(3) . ?
C55 C58 1.537(3) . ?
C55 C57 1.544(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
O1 Sn1 O2 88.82(6) . . ?
C1 O1 Sn1 136.31(12) . . ?
O1 C1 C2 120.61(17) . . ?
O1 C1 C6 122.81(17) . . ?
C2 C1 C6 116.58(17) . . ?
C30 O2 Sn1 130.76(12) . . ?
C3 C2 C1 120.48(17) . . ?
C3 C2 S1 115.67(14) . . ?
C1 C2 S1 123.67(15) . . ?
C2 C3 C4 123.00(17) . . ?
C5 C4 C3 116.17(17) . . ?
C5 C4 C7 120.19(17) . . ?
C3 C4 C7 123.63(17) . . ?
C6 C5 C4 122.08(17) . . ?
C5 C6 C1 121.52(17) . . ?
C5 C6 S4 120.31(14) . . ?
C1 C6 S4 118.17(14) . . ?
C8 C7 C4 112.21(16) . . ?
C8 C7 C10 108.59(17) . . ?
C4 C7 C10 109.76(18) . . ?
C8 C7 C9 108.03(18) . . ?
C4 C7 C9 109.43(17) . . ?
C10 C7 C9 108.74(19) . . ?
C2 S1 C12 103.79(9) . . ?
O3 C11 C12 122.71(16) . . ?
O3 C11 C16 118.29(16) . . ?
C12 C11 C16 118.45(17) . . ?
C11 C12 C13 120.05(17) . . ?
C11 C12 S1 119.25(14) . . ?
C13 C12 S1 120.54(15) . . ?
C12 C13 C14 121.15(17) . . ?
C15 C14 C13 117.56(17) . . ?
C15 C14 C26 118.94(17) . . ?
C13 C14 C26 123.38(17) . . ?
C16 C15 C14 121.25(17) . . ?
C15 C16 C11 120.21(17) . . ?
C15 C16 S2 122.26(14) . . ?
C11 C16 S2 117.02(14) . . ?
C11 O3 Si1 130.02(12) . . ?
O3 Si1 C21 105.38(8) . . ?
O3 Si1 C24 114.28(8) . . ?
C21 Si1 C24 109.39(9) . . ?
O3 Si1 C18 103.45(8) . . ?
C21 Si1 C18 115.46(9) . . ?
C24 Si1 C18 108.93(9) . . ?
C17 C18 C19 109.93(18) . . ?
C17 C18 Si1 113.00(14) . . ?
C19 C18 Si1 115.08(15) . . ?
C22 C21 C20 111.59(16) . . ?
C22 C21 Si1 112.95(13) . . ?
C20 C21 Si1 114.29(13) . . ?
C23 C24 C25 109.87(17) . . ?
C23 C24 Si1 116.27(13) . . ?
C25 C24 Si1 114.19(14) . . ?
C28 C26 C14 112.42(16) . . ?
C28 C26 C29 109.16(16) . . ?
C14 C26 C29 108.59(15) . . ?
C28 C26 C27 108.21(17) . . ?
C14 C26 C27 109.59(16) . . ?
C29 C26 C27 108.81(17) . . ?
C31 S2 C16 100.35(9) . . ?
O2 C30 C35 121.82(16) . . ?
O2 C30 C31 121.69(16) . . ?
C35 C30 C31 116.41(16) . . ?
C32 C31 C30 121.71(17) . . ?
C32 C31 S2 120.19(14) . . ?
C30 C31 S2 118.09(14) . . ?
C31 C32 C33 121.86(17) . . ?
C34 C33 C32 116.26(17) . . ?
C34 C33 C36 123.39(17) . . ?
C32 C33 C36 120.33(16) . . ?
C33 C34 C35 123.29(17) . . ?
C34 C35 C30 120.43(17) . . ?
C34 C35 S3 113.95(14) . . ?
C30 C35 S3 125.53(14) . . ?
C33 C36 C39 112.28(16) . . ?
C33 C36 C38 110.02(16) . . ?
C39 C36 C38 107.99(17) . . ?
C33 C36 C37 109.54(16) . . ?
C39 C36 C37 107.97(16) . . ?
C38 C36 C37 108.97(17) . . ?
C41 S3 C35 105.31(8) . . ?
O4 C40 C41 122.89(16) . . ?
O4 C40 C45 118.55(16) . . ?
C41 C40 C45 118.13(17) . . ?
C40 C41 C42 119.91(17) . . ?
C40 C41 S3 119.24(14) . . ?
C42 C41 S3 120.80(14) . . ?
C41 C42 C43 121.47(17) . . ?
C44 C43 C42 117.26(17) . . ?
C44 C43 C55 119.62(17) . . ?
C42 C43 C55 123.12(17) . . ?
C45 C44 C43 121.46(17) . . ?
C44 C45 C40 120.44(17) . . ?
C44 C45 S4 122.97(14) . . ?
C40 C45 S4 116.29(14) . . ?
C40 O4 Si2 124.67(11) . . ?
O4 Si2 C50 105.55(8) . . ?
O4 Si2 C47 103.85(8) . . ?
C50 Si2 C47 114.85(9) . . ?
O4 Si2 C53 108.58(8) . . ?
C50 Si2 C53 110.62(9) . . ?
C47 Si2 C53 112.72(9) . . ?
C46 C47 C48 109.99(17) . . ?
C46 C47 Si2 112.26(14) . . ?
C48 C47 Si2 115.44(14) . . ?
C49 C50 C51 110.55(17) . . ?
C49 C50 Si2 112.87(13) . . ?
C51 C50 Si2 114.12(14) . . ?
C52 C53 C54 110.17(16) . . ?
C52 C53 Si2 112.93(14) . . ?
C54 C53 Si2 114.34(13) . . ?
C56 C55 C43 112.78(16) . . ?
C56 C55 C58 109.40(16) . . ?
C43 C55 C58 109.21(16) . . ?
C56 C55 C57 108.15(17) . . ?
C43 C55 C57 108.66(16) . . ?
C58 C55 C57 108.56(17) . . ?
C6 S4 C45 99.72(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
Sn1 O1 C1 C2 160.50(14) . . . . ?
Sn1 O1 C1 C6 -20.4(3) . . . . ?
O1 C1 C2 C3 -177.75(17) . . . . ?
C6 C1 C2 C3 3.1(3) . . . . ?
O1 C1 C2 S1 -2.8(3) . . . . ?
C6 C1 C2 S1 177.98(14) . . . . ?
C1 C2 C3 C4 0.4(3) . . . . ?
S1 C2 C3 C4 -174.88(15) . . . . ?
C2 C3 C4 C5 -3.4(3) . . . . ?
C2 C3 C4 C7 177.79(18) . . . . ?
C3 C4 C5 C6 2.8(3) . . . . ?
C7 C4 C5 C6 -178.32(17) . . . . ?
C4 C5 C6 C1 0.7(3) . . . . ?
C4 C5 C6 S4 179.93(14) . . . . ?
O1 C1 C6 C5 177.21(18) . . . . ?
C2 C1 C6 C5 -3.6(3) . . . . ?
O1 C1 C6 S4 -2.0(3) . . . . ?
C2 C1 C6 S4 177.11(14) . . . . ?
C5 C4 C7 C8 175.37(18) . . . . ?
C3 C4 C7 C8 -5.8(3) . . . . ?
C5 C4 C7 C10 -63.8(2) . . . . ?
C3 C4 C7 C10 115.0(2) . . . . ?
C5 C4 C7 C9 55.5(2) . . . . ?
C3 C4 C7 C9 -125.7(2) . . . . ?
C3 C2 S1 C12 -146.86(15) . . . . ?
C1 C2 S1 C12 38.00(18) . . . . ?
O3 C11 C12 C13 177.03(16) . . . . ?
C16 C11 C12 C13 -11.6(3) . . . . ?
O3 C11 C12 S1 -7.5(2) . . . . ?
C16 C11 C12 S1 163.86(14) . . . . ?
C2 S1 C12 C11 -92.50(16) . . . . ?
C2 S1 C12 C13 82.95(16) . . . . ?
C11 C12 C13 C14 2.7(3) . . . . ?
S1 C12 C13 C14 -172.74(14) . . . . ?
C12 C13 C14 C15 5.7(3) . . . . ?
C12 C13 C14 C26 -178.24(17) . . . . ?
C13 C14 C15 C16 -5.1(3) . . . . ?
C26 C14 C15 C16 178.64(16) . . . . ?
C14 C15 C16 C11 -3.8(3) . . . . ?
C14 C15 C16 S2 167.75(14) . . . . ?
O3 C11 C16 C15 -176.04(16) . . . . ?
C12 C11 C16 C15 12.2(3) . . . . ?
O3 C11 C16 S2 11.9(2) . . . . ?
C12 C11 C16 S2 -159.81(14) . . . . ?
C12 C11 O3 Si1 -82.1(2) . . . . ?
C16 C11 O3 Si1 106.50(18) . . . . ?
C11 O3 Si1 C21 128.65(16) . . . . ?
C11 O3 Si1 C24 8.54(18) . . . . ?
C11 O3 Si1 C18 -109.73(16) . . . . ?
O3 Si1 C18 C17 -61.88(15) . . . . ?
C21 Si1 C18 C17 52.69(17) . . . . ?
C24 Si1 C18 C17 176.19(14) . . . . ?
O3 Si1 C18 C19 170.72(16) . . . . ?
C21 Si1 C18 C19 -74.71(18) . . . . ?
C24 Si1 C18 C19 48.79(18) . . . . ?
O3 Si1 C21 C22 165.23(13) . . . . ?
C24 Si1 C21 C22 -71.48(16) . . . . ?
C18 Si1 C21 C22 51.77(17) . . . . ?
O3 Si1 C21 C20 36.22(16) . . . . ?
C24 Si1 C21 C20 159.50(14) . . . . ?
C18 Si1 C21 C20 -77.24(16) . . . . ?
O3 Si1 C24 C23 68.16(16) . . . . ?
C21 Si1 C24 C23 -49.68(17) . . . . ?
C18 Si1 C24 C23 -176.73(14) . . . . ?
O3 Si1 C24 C25 -61.43(17) . . . . ?
C21 Si1 C24 C25 -179.27(14) . . . . ?
C18 Si1 C24 C25 53.68(17) . . . . ?
C15 C14 C26 C28 -176.12(17) . . . . ?
C13 C14 C26 C28 7.9(3) . . . . ?
C15 C14 C26 C29 63.0(2) . . . . ?
C13 C14 C26 C29 -113.0(2) . . . . ?
C15 C14 C26 C27 -55.7(2) . . . . ?
C13 C14 C26 C27 128.25(19) . . . . ?
C15 C16 S2 C31 -23.73(17) . . . . ?
C11 C16 S2 C31 148.12(14) . . . . ?
Sn1 O2 C30 C35 135.81(15) . . . . ?
Sn1 O2 C30 C31 -47.5(2) . . . . ?
O2 C30 C31 C32 -178.10(17) . . . . ?
C35 C30 C31 C32 -1.3(3) . . . . ?
O2 C30 C31 S2 2.9(2) . . . . ?
C35 C30 C31 S2 179.77(13) . . . . ?
C16 S2 C31 C32 110.88(16) . . . . ?
C16 S2 C31 C30 -70.13(16) . . . . ?
C30 C31 C32 C33 0.3(3) . . . . ?
S2 C31 C32 C33 179.23(14) . . . . ?
C31 C32 C33 C34 1.3(3) . . . . ?
C31 C32 C33 C36 179.61(17) . . . . ?
C32 C33 C34 C35 -1.9(3) . . . . ?
C36 C33 C34 C35 179.85(17) . . . . ?
C33 C34 C35 C30 0.9(3) . . . . ?
C33 C34 C35 S3 -175.77(15) . . . . ?
O2 C30 C35 C34 177.52(17) . . . . ?
C31 C30 C35 C34 0.7(3) . . . . ?
O2 C30 C35 S3 -6.2(3) . . . . ?
C31 C30 C35 S3 176.94(14) . . . . ?
C34 C33 C36 C39 -4.4(3) . . . . ?
C32 C33 C36 C39 177.33(17) . . . . ?
C34 C33 C36 C38 -124.7(2) . . . . ?
C32 C33 C36 C38 57.0(2) . . . . ?
C34 C33 C36 C37 115.5(2) . . . . ?
C32 C33 C36 C37 -62.7(2) . . . . ?
C34 C35 S3 C41 -154.98(14) . . . . ?
C30 C35 S3 C41 28.55(19) . . . . ?
O4 C40 C41 C42 175.93(16) . . . . ?
C45 C40 C41 C42 -11.7(3) . . . . ?
O4 C40 C41 S3 -6.5(2) . . . . ?
C45 C40 C41 S3 165.83(13) . . . . ?
C35 S3 C41 C40 -84.85(16) . . . . ?
C35 S3 C41 C42 92.66(16) . . . . ?
C40 C41 C42 C43 2.9(3) . . . . ?
S3 C41 C42 C43 -174.58(14) . . . . ?
C41 C42 C43 C44 5.5(3) . . . . ?
C41 C42 C43 C55 -175.03(16) . . . . ?
C42 C43 C44 C45 -5.1(3) . . . . ?
C55 C43 C44 C45 175.42(16) . . . . ?
C43 C44 C45 C40 -3.7(3) . . . . ?
C43 C44 C45 S4 169.81(14) . . . . ?
O4 C40 C45 C44 -175.12(16) . . . . ?
C41 C40 C45 C44 12.2(3) . . . . ?
O4 C40 C45 S4 10.9(2) . . . . ?
C41 C40 C45 S4 -161.79(13) . . . . ?
C41 C40 O4 Si2 -80.7(2) . . . . ?
C45 C40 O4 Si2 106.93(17) . . . . ?
C40 O4 Si2 C50 130.61(15) . . . . ?
C40 O4 Si2 C47 -108.20(15) . . . . ?
C40 O4 Si2 C53 11.98(16) . . . . ?
O4 Si2 C47 C46 -63.53(15) . . . . ?
C50 Si2 C47 C46 51.21(17) . . . . ?
C53 Si2 C47 C46 179.15(13) . . . . ?
O4 Si2 C47 C48 169.32(15) . . . . ?
C50 Si2 C47 C48 -75.93(17) . . . . ?
C53 Si2 C47 C48 52.00(18) . . . . ?
O4 Si2 C50 C49 27.78(16) . . . . ?
C47 Si2 C50 C49 -85.96(16) . . . . ?
C53 Si2 C50 C49 145.05(14) . . . . ?
O4 Si2 C50 C51 155.09(13) . . . . ?
C47 Si2 C50 C51 41.35(17) . . . . ?
C53 Si2 C50 C51 -87.64(16) . . . . ?
O4 Si2 C53 C52 159.39(14) . . . . ?
C50 Si2 C53 C52 44.00(17) . . . . ?
C47 Si2 C53 C52 -86.13(16) . . . . ?
O4 Si2 C53 C54 -73.59(15) . . . . ?
C50 Si2 C53 C54 171.02(14) . . . . ?
C47 Si2 C53 C54 40.90(17) . . . . ?
C44 C43 C55 C56 179.05(17) . . . . ?
C42 C43 C55 C56 -0.4(3) . . . . ?
C44 C43 C55 C58 57.2(2) . . . . ?
C42 C43 C55 C58 -122.20(19) . . . . ?
C44 C43 C55 C57 -61.0(2) . . . . ?
C42 C43 C55 C57 119.5(2) . . . . ?
C5 C6 S4 C45 102.58(16) . . . . ?
C1 C6 S4 C45 -78.15(16) . . . . ?
C44 C45 S4 C6 -28.14(17) . . . . ?
C40 C45 S4 C6 145.66(14) . . . . ?

_refine_diff_density_max         0.480
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.105

####################################################################### 
# 
# 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_2-Pb_Thia_Bn
_database_code_depnum_ccdc_archive 'CCDC 2021967'
loop_
_audit_author_name
_audit_author_address
'Takuya Kuwabara'
;Chuo Univesity
Japan
;
_audit_update_record             
;
2020-08-06 deposited with the CCDC.	2020-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C61 H66 O4 Pb S4'
_chemical_formula_weight         1198.56

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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                   22.413(3)
_cell_length_b                   20.959(2)
_cell_length_c                   12.5139(14)
_cell_angle_alpha                90
_cell_angle_beta                 108.6460(10)
_cell_angle_gamma                90
_cell_volume                     5570.1(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    9580
_cell_measurement_theta_min      2.5939
_cell_measurement_theta_max      31.2920

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_F_000             2440
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1400
_exptl_crystal_size_mid          0.1380
_exptl_crystal_size_min          0.0920
_exptl_absorpt_coefficient_mu    3.224
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8697
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_device_type  'Rigaku VariMax Saturn'
_diffrn_measurement_method       'omega scans'
_diffrn_reflns_number            22455
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.003
_diffrn_reflns_theta_max         27.436
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6294
_reflns_number_gt                5736
_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       'RIGAKU CrystalClear'
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Yadokari-XG 2009(Wakita Nemoto et al.)'
_computing_publication_material  'Yadokari-XG 2009(Wakita,Nemoto et al.)'
_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)+(0.0351P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6294
_refine_ls_number_parameters     338
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_ref         0.0695
_refine_ls_wR_factor_gt          0.0669
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_restrained_S_all      1.117
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Pb1 Pb 0.500000 0.39774(2) 0.750000 0.02191(6) Uani 1 2 d S T P . .
O1 O 0.47255(10) 0.32427(15) 0.62387(19) 0.0476(8) Uani 1 1 d . . . . .
C1 C 0.44366(14) 0.29544(14) 0.5299(2) 0.0219(6) Uani 1 1 d . . . . .
C2 C 0.47660(13) 0.27132(13) 0.4594(2) 0.0168(6) Uani 1 1 d . . . . .
C3 C 0.44683(13) 0.23335(12) 0.3665(2) 0.0174(6) Uani 1 1 d . . . . .
H3 H 0.470499 0.216941 0.323932 0.021 Uiso 1 1 calc R U . . .
C4 C 0.38305(13) 0.21900(13) 0.3350(2) 0.0191(6) Uani 1 1 d . . . . .
C5 C 0.34903(13) 0.24708(12) 0.3991(2) 0.0182(6) Uani 1 1 d . . . . .
H5 H 0.305784 0.240476 0.377966 0.022 Uiso 1 1 calc R U . . .
C6 C 0.37774(13) 0.28444(13) 0.4930(2) 0.0178(6) Uani 1 1 d . . . . .
S1 S 0.55573(3) 0.29525(3) 0.47834(6) 0.01719(14) Uani 1 1 d . . . . .
C7 C 0.34987(14) 0.17409(14) 0.2382(3) 0.0246(7) Uani 1 1 d . . . . .
C8 C 0.30129(18) 0.21111(18) 0.1443(3) 0.0477(11) Uani 1 1 d . . . . .
H8 H 0.270328 0.229331 0.173378 0.072 Uiso 1 1 calc R U . . .
H8A H 0.281075 0.182647 0.083368 0.072 Uiso 1 1 calc R U . . .
H8B H 0.322059 0.244539 0.117341 0.072 Uiso 1 1 calc R U . . .
C9 C 0.39641(15) 0.14124(16) 0.1894(3) 0.0325(8) Uani 1 1 d . . . . .
H9 H 0.417129 0.172763 0.158107 0.049 Uiso 1 1 calc R U . . .
H9A H 0.374115 0.111992 0.131290 0.049 Uiso 1 1 calc R U . . .
H9B H 0.427163 0.118363 0.248126 0.049 Uiso 1 1 calc R U . . .
C10 C 0.31705(18) 0.12119(17) 0.2835(3) 0.0409(9) Uani 1 1 d . . . . .
H10 H 0.347805 0.098005 0.341748 0.061 Uiso 1 1 calc R U . . .
H10A H 0.296034 0.092606 0.223260 0.061 Uiso 1 1 calc R U . . .
H10B H 0.286782 0.139886 0.313756 0.061 Uiso 1 1 calc R U . . .
S2 S 0.33049(3) 0.32296(3) 0.56351(6) 0.01704(14) Uani 1 1 d . . . . .
C11 C 0.38256(12) 0.30134(12) 0.7923(2) 0.0144(5) Uani 1 1 d . . . . .
C12 C 0.34824(12) 0.27551(13) 0.6880(2) 0.0152(5) Uani 1 1 d . . . . .
C13 C 0.32884(13) 0.21216(13) 0.6820(2) 0.0172(6) Uani 1 1 d . . . . .
H13 H 0.305147 0.195462 0.612518 0.021 Uiso 1 1 calc R U . . .
C14 C 0.34381(13) 0.17297(13) 0.7768(2) 0.0178(6) Uani 1 1 d . . . . .
C15 C 0.38026(13) 0.19955(13) 0.8790(2) 0.0179(6) Uani 1 1 d . . . . .
H15 H 0.391884 0.174175 0.943351 0.022 Uiso 1 1 calc R U . . .
C16 C 0.39986(12) 0.26320(13) 0.8876(2) 0.0160(5) Uani 1 1 d . . . . .
O2 O 0.40122(8) 0.36492(8) 0.79883(16) 0.0160(4) Uani 1 1 d . . . . .
C17 C 0.35299(14) 0.40991(13) 0.8025(3) 0.0210(6) Uani 1 1 d . . . . .
H17 H 0.343942 0.405848 0.872966 0.025 Uiso 1 1 calc R U . . .
H17A H 0.314528 0.402045 0.740762 0.025 Uiso 1 1 calc R U . . .
C18 C 0.37780(13) 0.47555(13) 0.7924(2) 0.0185(6) Uani 1 1 d . . . . .
C19 C 0.41394(14) 0.50797(14) 0.8870(3) 0.0240(6) Uani 1 1 d . . . . .
H19 H 0.421866 0.489608 0.957796 0.029 Uiso 1 1 calc R U . . .
C20 C 0.43873(15) 0.56797(14) 0.8775(3) 0.0285(7) Uani 1 1 d . . . . .
H20 H 0.462954 0.589616 0.941515 0.034 Uiso 1 1 calc R U . . .
C21 C 0.42691(17) 0.59497(14) 0.7717(3) 0.0310(8) Uani 1 1 d . . . . .
H21 H 0.442554 0.635316 0.764820 0.037 Uiso 1 1 calc R U . . .
C22 C 0.39198(16) 0.56225(15) 0.6765(3) 0.0297(7) Uani 1 1 d . . . . .
H22 H 0.384911 0.580250 0.605545 0.036 Uiso 1 1 calc R U . . .
C23 C 0.36743(14) 0.50267(14) 0.6863(3) 0.0250(7) Uani 1 1 d . . . . .
H23 H 0.343996 0.480731 0.621962 0.030 Uiso 1 1 calc R U . . .
C24 C 0.31627(15) 0.10544(13) 0.7683(3) 0.0229(6) Uani 1 1 d . . . . .
C25 C 0.31658(19) 0.07224(16) 0.6592(3) 0.0409(9) Uani 1 1 d . . . . .
H25 H 0.299809 0.029929 0.656841 0.061 Uiso 1 1 calc R U . . .
H25A H 0.358969 0.069916 0.657129 0.061 Uiso 1 1 calc R U . . .
H25B H 0.291155 0.096117 0.595417 0.061 Uiso 1 1 calc R U . . .
C26 C 0.2477(2) 0.11165(17) 0.7655(5) 0.0583(13) Uani 1 1 d . . . . .
H26 H 0.246367 0.130764 0.834381 0.087 Uiso 1 1 calc R U . . .
H26A H 0.228691 0.070117 0.757356 0.087 Uiso 1 1 calc R U . . .
H26B H 0.225013 0.137950 0.702840 0.087 Uiso 1 1 calc R U . . .
C27 C 0.3529(2) 0.06370(16) 0.8670(3) 0.0528(12) Uani 1 1 d . . . . .
H27 H 0.349892 0.081261 0.935887 0.079 Uiso 1 1 calc R U . . .
H27A H 0.396333 0.062161 0.870510 0.079 Uiso 1 1 calc R U . . .
H27B H 0.335708 0.021358 0.856717 0.079 Uiso 1 1 calc R U . . .
C28 C 0.5354(6) 0.1060(5) 0.9266(10) 0.0476(17) Uani 0.5 1 d . . P A -1
H28 H 0.570386 0.134696 0.938641 0.071 Uiso 0.5 1 calc R U P A -1
H29 H 0.549213 0.067934 0.970091 0.071 Uiso 0.5 1 calc R U P A -1
H30 H 0.503128 0.126250 0.949776 0.071 Uiso 0.5 1 calc R U P A -1
C29 C 0.5095(3) 0.0890(2) 0.8023(4) 0.0476(17) Uani 0.5 1 d G . P A -1
C30 C 0.4913(4) 0.13714(17) 0.7219(5) 0.057(4) Uani 0.5 1 d G . P A -1
H31 H 0.494475 0.179647 0.744369 0.068 Uiso 0.5 1 calc R U P A -1
C31 C 0.4685(4) 0.1217(2) 0.6080(5) 0.042(3) Uani 0.5 1 d G . P A -1
H32 H 0.456334 0.153920 0.554230 0.050 Uiso 0.5 1 calc R U P A -1
C32 C 0.4638(3) 0.0582(2) 0.5744(4) 0.0407(18) Uani 0.5 1 d G . P A -1
H33 H 0.448462 0.047887 0.498217 0.049 Uiso 0.5 1 calc R U P A -1
C33 C 0.4819(3) 0.01009(16) 0.6548(5) 0.0328(15) Uani 0.5 1 d G . P A -1
H34 H 0.478732 -0.032418 0.632343 0.039 Uiso 0.5 1 calc R U P A -1
C34 C 0.5047(4) 0.0255(2) 0.7687(4) 0.030(2) Uani 0.5 1 d G . P A -1
H35 H 0.516873 -0.006692 0.822483 0.036 Uiso 0.5 1 calc R U P A -1


_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
Pb1 O1 2.149(2) . ?
Pb1 O1 2.150(2) 2_656 ?
Pb1 O2 2.5716(19) . ?
Pb1 O2 2.5717(19) 2_656 ?
O1 C1 1.296(3) . ?
C1 C2 1.413(4) . ?
C1 C6 1.419(4) . ?
C2 C3 1.390(4) . ?
C2 S1 1.785(3) . ?
C3 C4 1.389(4) . ?
C4 C5 1.400(4) . ?
C4 C7 1.527(4) . ?
C5 C6 1.387(4) . ?
C6 S2 1.775(3) . ?
S1 C16 1.785(3) 2_656 ?
C7 C9 1.530(4) . ?
C7 C8 1.533(5) . ?
C7 C10 1.536(5) . ?
S2 C12 1.782(3) . ?
C11 C16 1.385(4) . ?
C11 O2 1.391(3) . ?
C11 C12 1.395(4) . ?
C12 C13 1.392(4) . ?
C13 C14 1.393(4) . ?
C14 C15 1.395(4) . ?
C14 C24 1.534(4) . ?
C15 C16 1.398(4) . ?
O2 C17 1.446(3) . ?
C17 C18 1.504(4) . ?
C18 C19 1.380(4) . ?
C18 C23 1.394(4) . ?
C19 C20 1.395(4) . ?
C20 C21 1.385(5) . ?
C21 C22 1.381(5) . ?
C22 C23 1.386(4) . ?
C24 C27 1.522(5) . ?
C24 C26 1.532(5) . ?
C24 C25 1.534(5) . ?
C28 C29 1.520(12) . ?
C29 C30 1.3900 . ?
C29 C34 1.3900 . ?
C30 C31 1.3900 . ?
C31 C32 1.3900 . ?
C32 C33 1.3900 . ?
C33 C34 1.3900 . ?

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
O1 Pb1 O1 88.48(16) . 2_656 ?
O1 Pb1 O2 85.23(8) . . ?
O1 Pb1 O2 72.53(7) 2_656 . ?
O1 Pb1 O2 72.53(7) . 2_656 ?
O1 Pb1 O2 85.23(7) 2_656 2_656 ?
O2 Pb1 O2 148.97(8) . 2_656 ?
C1 O1 Pb1 160.5(2) . . ?
O1 C1 C2 121.6(3) . . ?
O1 C1 C6 122.5(3) . . ?
C2 C1 C6 115.8(3) . . ?
C3 C2 C1 121.3(3) . . ?
C3 C2 S1 117.6(2) . . ?
C1 C2 S1 120.8(2) . . ?
C4 C3 C2 122.5(3) . . ?
C3 C4 C5 116.5(3) . . ?
C3 C4 C7 123.7(3) . . ?
C5 C4 C7 119.8(3) . . ?
C6 C5 C4 122.1(3) . . ?
C5 C6 C1 121.4(3) . . ?
C5 C6 S2 119.3(2) . . ?
C1 C6 S2 119.3(2) . . ?
C2 S1 C16 104.54(12) . 2_656 ?
C4 C7 C9 111.9(2) . . ?
C4 C7 C8 110.0(2) . . ?
C9 C7 C8 109.3(3) . . ?
C4 C7 C10 108.7(3) . . ?
C9 C7 C10 106.9(3) . . ?
C8 C7 C10 110.0(3) . . ?
C6 S2 C12 100.29(12) . . ?
C16 C11 O2 120.4(2) . . ?
C16 C11 C12 120.1(2) . . ?
O2 C11 C12 119.5(2) . . ?
C13 C12 C11 119.3(2) . . ?
C13 C12 S2 120.4(2) . . ?
C11 C12 S2 120.2(2) . . ?
C12 C13 C14 122.0(3) . . ?
C13 C14 C15 117.2(2) . . ?
C13 C14 C24 120.2(2) . . ?
C15 C14 C24 122.5(3) . . ?
C14 C15 C16 122.0(3) . . ?
C11 C16 C15 119.3(2) . . ?
C11 C16 S1 120.7(2) . 2_656 ?
C15 C16 S1 119.9(2) . 2_656 ?
C11 O2 C17 114.4(2) . . ?
C11 O2 Pb1 120.52(15) . . ?
C17 O2 Pb1 122.82(15) . . ?
O2 C17 C18 107.1(2) . . ?
C19 C18 C23 119.3(3) . . ?
C19 C18 C17 120.6(3) . . ?
C23 C18 C17 120.0(3) . . ?
C18 C19 C20 120.7(3) . . ?
C21 C20 C19 119.3(3) . . ?
C22 C21 C20 120.3(3) . . ?
C21 C22 C23 120.2(3) . . ?
C22 C23 C18 120.1(3) . . ?
C27 C24 C26 110.2(3) . . ?
C27 C24 C14 111.9(3) . . ?
C26 C24 C14 107.6(2) . . ?
C27 C24 C25 107.8(3) . . ?
C26 C24 C25 107.9(3) . . ?
C14 C24 C25 111.3(3) . . ?
C30 C29 C34 120.0 . . ?
C30 C29 C28 119.9(6) . . ?
C34 C29 C28 120.1(6) . . ?
C29 C30 C31 120.0 . . ?
C32 C31 C30 120.0 . . ?
C31 C32 C33 120.0 . . ?
C34 C33 C32 120.0 . . ?
C33 C34 C29 120.0 . . ?

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
Pb1 O1 C1 C2 118.8(6) . . . . ?
Pb1 O1 C1 C6 -63.0(8) . . . . ?
O1 C1 C2 C3 171.5(3) . . . . ?
C6 C1 C2 C3 -6.7(4) . . . . ?
O1 C1 C2 S1 -14.8(4) . . . . ?
C6 C1 C2 S1 166.9(2) . . . . ?
C1 C2 C3 C4 2.6(4) . . . . ?
S1 C2 C3 C4 -171.2(2) . . . . ?
C2 C3 C4 C5 2.6(4) . . . . ?
C2 C3 C4 C7 -176.0(3) . . . . ?
C3 C4 C5 C6 -3.5(4) . . . . ?
C7 C4 C5 C6 175.2(3) . . . . ?
C4 C5 C6 C1 -0.8(4) . . . . ?
C4 C5 C6 S2 175.5(2) . . . . ?
O1 C1 C6 C5 -172.4(3) . . . . ?
C2 C1 C6 C5 5.9(4) . . . . ?
O1 C1 C6 S2 11.3(4) . . . . ?
C2 C1 C6 S2 -170.5(2) . . . . ?
C3 C2 S1 C16 -119.9(2) . . . 2_656 ?
C1 C2 S1 C16 66.2(3) . . . 2_656 ?
C3 C4 C7 C9 6.5(4) . . . . ?
C5 C4 C7 C9 -172.1(3) . . . . ?
C3 C4 C7 C8 -115.2(3) . . . . ?
C5 C4 C7 C8 66.3(4) . . . . ?
C3 C4 C7 C10 124.3(3) . . . . ?
C5 C4 C7 C10 -54.2(4) . . . . ?
C5 C6 S2 C12 107.0(2) . . . . ?
C1 C6 S2 C12 -76.5(2) . . . . ?
C16 C11 C12 C13 3.4(4) . . . . ?
O2 C11 C12 C13 -179.1(2) . . . . ?
C16 C11 C12 S2 -175.7(2) . . . . ?
O2 C11 C12 S2 1.8(3) . . . . ?
C6 S2 C12 C13 -67.4(2) . . . . ?
C6 S2 C12 C11 111.6(2) . . . . ?
C11 C12 C13 C14 -1.5(4) . . . . ?
S2 C12 C13 C14 177.6(2) . . . . ?
C12 C13 C14 C15 -1.0(4) . . . . ?
C12 C13 C14 C24 174.3(3) . . . . ?
C13 C14 C15 C16 1.6(4) . . . . ?
C24 C14 C15 C16 -173.5(3) . . . . ?
O2 C11 C16 C15 179.7(2) . . . . ?
C12 C11 C16 C15 -2.8(4) . . . . ?
O2 C11 C16 S1 2.0(4) . . . 2_656 ?
C12 C11 C16 S1 179.5(2) . . . 2_656 ?
C14 C15 C16 C11 0.2(4) . . . . ?
C14 C15 C16 S1 177.9(2) . . . 2_656 ?
C16 C11 O2 C17 -100.8(3) . . . . ?
C12 C11 O2 C17 81.7(3) . . . . ?
C16 C11 O2 Pb1 95.9(3) . . . . ?
C12 C11 O2 Pb1 -81.6(3) . . . . ?
C11 O2 C17 C18 -172.0(2) . . . . ?
Pb1 O2 C17 C18 -9.1(3) . . . . ?
O2 C17 C18 C19 -87.1(3) . . . . ?
O2 C17 C18 C23 89.2(3) . . . . ?
C23 C18 C19 C20 1.6(4) . . . . ?
C17 C18 C19 C20 177.9(3) . . . . ?
C18 C19 C20 C21 -0.2(5) . . . . ?
C19 C20 C21 C22 -1.3(5) . . . . ?
C20 C21 C22 C23 1.3(5) . . . . ?
C21 C22 C23 C18 0.1(5) . . . . ?
C19 C18 C23 C22 -1.6(4) . . . . ?
C17 C18 C23 C22 -177.9(3) . . . . ?
C13 C14 C24 C27 162.0(3) . . . . ?
C15 C14 C24 C27 -23.0(4) . . . . ?
C13 C14 C24 C26 -76.8(4) . . . . ?
C15 C14 C24 C26 98.2(4) . . . . ?
C13 C14 C24 C25 41.2(4) . . . . ?
C15 C14 C24 C25 -143.7(3) . . . . ?
C34 C29 C30 C31 0.0 . . . . ?
C28 C29 C30 C31 179.0(8) . . . . ?
C29 C30 C31 C32 0.0 . . . . ?
C30 C31 C32 C33 0.0 . . . . ?
C31 C32 C33 C34 0.0 . . . . ?
C32 C33 C34 C29 0.0 . . . . ?
C30 C29 C34 C33 0.0 . . . . ?
C28 C29 C34 C33 -179.0(8) . . . . ?

_refine_diff_density_max         1.500
_refine_diff_density_min         -1.746
_refine_diff_density_rms         0.125

####################################################################### 
# 
# 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_4_Thia_TIPS_OH
_database_code_depnum_ccdc_archive 'CCDC 2021969'
loop_
_audit_author_name
_audit_author_address
'Takuya Kuwabara'
;Chuo Univesity
Japan
;
_audit_update_record             
;
2020-08-06 deposited with the CCDC.	2020-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C58 H88 O4 S4 Si2, C4 H8 O1'
_chemical_formula_sum            'C62 H96 O5 S4 Si2'
_chemical_formula_weight         1105.80

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   13.510(2)
_cell_length_b                   15.106(2)
_cell_length_c                   16.040(2)
_cell_angle_alpha                79.593(5)
_cell_angle_beta                 81.074(4)
_cell_angle_gamma                89.230(6)
_cell_volume                     3180.1(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8327
_cell_measurement_theta_min      2.4137
_cell_measurement_theta_max      31.2514

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_F_000             1200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1640
_exptl_crystal_size_mid          0.1410
_exptl_crystal_size_min          0.0640
_exptl_absorpt_coefficient_mu    0.232
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8616
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_device_type  'Rigaku VariMax Saturn'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            26240
_diffrn_reflns_av_unetI/netI     0.0807
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.053
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measured_fraction_theta_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             14039
_reflns_number_gt                10139
_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       'RIGAKU CrystalClear'
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Yadokari-XG 2009(Wakita Nemoto et al.)'
_computing_publication_material  'Yadokari-XG 2009(Wakita,Nemoto et al.)'
_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)+(0.0641P)²+0.1820P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14039
_refine_ls_number_parameters     684
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0598
_refine_ls_wR_factor_ref         0.1488
_refine_ls_wR_factor_gt          0.1317
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_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
O1 O 0.40070(14) 0.14621(11) 0.29415(10) 0.0220(4) Uani 1 1 d . . . . .
H63 H 0.446365 0.183681 0.283993 0.033 Uiso 1 1 calc R U . . .
O2 O 0.28796(13) 0.33858(11) 0.17433(12) 0.0223(4) Uani 1 1 d . . . . .
H64 H 0.259957 0.295502 0.162821 0.033 Uiso 1 1 calc R U . . .
C1 C 0.38441(18) 0.11125(16) 0.37945(15) 0.0180(5) Uani 1 1 d . . . . .
C2 C 0.43827(18) 0.13978(15) 0.43774(15) 0.0172(5) Uani 1 1 d . . . . .
C3 C 0.41321(19) 0.10658(16) 0.52550(15) 0.0190(5) Uani 1 1 d . . . . .
H3 H 0.449155 0.126760 0.563574 0.023 Uiso 1 1 calc R U . . .
C4 C 0.33596(19) 0.04421(16) 0.55727(15) 0.0196(5) Uani 1 1 d . . . . .
C5 C 0.28688(19) 0.01275(16) 0.49792(15) 0.0190(5) Uani 1 1 d . . . . .
H5 H 0.237278 -0.031474 0.517524 0.023 Uiso 1 1 calc R U . . .
C6 C 0.30984(19) 0.04555(16) 0.40977(15) 0.0187(5) Uani 1 1 d . . . . .
C7 C 0.3008(2) 0.02014(17) 0.65457(16) 0.0232(6) Uani 1 1 d . . . . .
C8 C 0.2540(2) 0.10444(18) 0.68451(17) 0.0311(7) Uani 1 1 d . . . . .
H8 H 0.199048 0.123336 0.654355 0.047 Uiso 1 1 calc R U . . .
H8A H 0.303507 0.151848 0.672859 0.047 Uiso 1 1 calc R U . . .
H8B H 0.230041 0.090828 0.745041 0.047 Uiso 1 1 calc R U . . .
S1 S 0.53771(5) 0.21985(4) 0.39899(4) 0.01871(14) Uani 1 1 d . . . . .
O3 O 0.50819(12) 0.33635(10) 0.23126(10) 0.0177(4) Uani 1 1 d . . . . .
C9 C 0.3889(2) -0.00847(18) 0.70254(16) 0.0282(6) Uani 1 1 d . . . . .
H9 H 0.438308 0.039140 0.689692 0.042 Uiso 1 1 calc R U . . .
H9A H 0.418244 -0.061632 0.684809 0.042 Uiso 1 1 calc R U . . .
H9B H 0.365439 -0.020859 0.763170 0.042 Uiso 1 1 calc R U . . .
C10 C 0.2224(2) -0.05609(19) 0.67740(17) 0.0323(7) Uani 1 1 d . . . . .
H10 H 0.205694 -0.072102 0.738660 0.048 Uiso 1 1 calc R U . . .
H10A H 0.249027 -0.107481 0.654499 0.048 Uiso 1 1 calc R U . . .
H10B H 0.163296 -0.036500 0.653376 0.048 Uiso 1 1 calc R U . . .
C11 C 0.46074(17) 0.36736(15) 0.30136(15) 0.0149(5) Uani 1 1 d . . . . .
C12 C 0.39887(18) 0.44245(16) 0.29344(15) 0.0177(5) Uani 1 1 d . . . . .
C13 C 0.34607(18) 0.46909(16) 0.36632(16) 0.0195(5) Uani 1 1 d . . . . .
H13 H 0.305635 0.519386 0.359536 0.023 Uiso 1 1 calc R U . . .
C14 C 0.35155(18) 0.42325(16) 0.44890(16) 0.0189(5) Uani 1 1 d . . . . .
C15 C 0.41330(18) 0.34859(16) 0.45581(16) 0.0193(5) Uani 1 1 d . . . . .
H15 H 0.419275 0.316609 0.510017 0.023 Uiso 1 1 calc R U . . .
C16 C 0.46647(18) 0.32042(15) 0.38373(15) 0.0166(5) Uani 1 1 d . . . . .
C17 C 0.2975(2) 0.45671(17) 0.52864(16) 0.0233(6) Uani 1 1 d . . . . .
Si1 Si 0.61179(5) 0.35549(4) 0.15745(4) 0.01694(15) Uani 1 1 d . . . . .
C18 C 0.2026(2) 0.50839(19) 0.51081(19) 0.0341(7) Uani 1 1 d . . . . .
H18 H 0.220454 0.562370 0.469576 0.051 Uiso 1 1 calc R U . . .
H18A H 0.168119 0.523792 0.563142 0.051 Uiso 1 1 calc R U . . .
H18B H 0.159594 0.471426 0.488549 0.051 Uiso 1 1 calc R U . . .
C19 C 0.3704(2) 0.5206(2) 0.55476(19) 0.0404(8) Uani 1 1 d . . . . .
H19 H 0.389457 0.569523 0.507950 0.061 Uiso 1 1 calc R U . . .
H19A H 0.428943 0.488177 0.568793 0.061 Uiso 1 1 calc R U . . .
H19B H 0.338058 0.543789 0.603815 0.061 Uiso 1 1 calc R U . . .
C20 C 0.2690(2) 0.37906(19) 0.60355(17) 0.0325(7) Uani 1 1 d . . . . .
H20 H 0.232823 0.401835 0.651423 0.049 Uiso 1 1 calc R U . . .
H20A H 0.328675 0.350138 0.619694 0.049 Uiso 1 1 calc R U . . .
H20B H 0.227672 0.336342 0.586676 0.049 Uiso 1 1 calc R U . . .
C21 C 0.57920(19) 0.30963(16) 0.06394(16) 0.0217(5) Uani 1 1 d . . . . .
H21 H 0.641677 0.306711 0.024350 0.026 Uiso 1 1 calc R U . . .
C22 C 0.5071(2) 0.36830(18) 0.01368(17) 0.0268(6) Uani 1 1 d . . . . .
H22 H 0.496486 0.342394 -0.034690 0.040 Uiso 1 1 calc R U . . .
H22A H 0.535413 0.427748 -0.006033 0.040 Uiso 1 1 calc R U . . .
H22B H 0.444312 0.371527 0.050266 0.040 Uiso 1 1 calc R U . . .
C23 C 0.5364(2) 0.21320(16) 0.09179(17) 0.0267(6) Uani 1 1 d . . . . .
H23 H 0.473428 0.213851 0.128845 0.040 Uiso 1 1 calc R U . . .
H23A H 0.582471 0.176078 0.121897 0.040 Uiso 1 1 calc R U . . .
H23B H 0.526487 0.189469 0.042015 0.040 Uiso 1 1 calc R U . . .
C24 C 0.64331(19) 0.47921(16) 0.12580(15) 0.0196(5) Uani 1 1 d . . . . .
H24 H 0.587725 0.506921 0.098360 0.024 Uiso 1 1 calc R U . . .
C25 C 0.7377(2) 0.49643(18) 0.05693(17) 0.0277(6) Uani 1 1 d . . . . .
H25 H 0.745040 0.559762 0.034491 0.042 Uiso 1 1 calc R U . . .
H25A H 0.731121 0.464709 0.011287 0.042 Uiso 1 1 calc R U . . .
H25B H 0.795623 0.475549 0.082177 0.042 Uiso 1 1 calc R U . . .
C26 C 0.6529(2) 0.52982(17) 0.19897(17) 0.0251(6) Uani 1 1 d . . . . .
H26 H 0.710274 0.508717 0.224878 0.038 Uiso 1 1 calc R U . . .
H26A H 0.593633 0.519292 0.241266 0.038 Uiso 1 1 calc R U . . .
H26B H 0.660626 0.593130 0.176568 0.038 Uiso 1 1 calc R U . . .
C27 C 0.71366(19) 0.28444(17) 0.20145(16) 0.0210(5) Uani 1 1 d . . . . .
H27 H 0.681432 0.227353 0.231503 0.025 Uiso 1 1 calc R U . . .
C28 C 0.7948(2) 0.26037(19) 0.13108(18) 0.0321(7) Uani 1 1 d . . . . .
H28 H 0.823851 0.314616 0.095441 0.048 Uiso 1 1 calc R U . . .
H28A H 0.765375 0.225317 0.096737 0.048 Uiso 1 1 calc R U . . .
H28B H 0.846025 0.226158 0.157119 0.048 Uiso 1 1 calc R U . . .
C29 C 0.7628(2) 0.32190(18) 0.26777(17) 0.0286(6) Uani 1 1 d . . . . .
H29 H 0.805928 0.277395 0.293205 0.043 Uiso 1 1 calc R U . . .
H29A H 0.711899 0.336913 0.311562 0.043 Uiso 1 1 calc R U . . .
H29B H 0.801513 0.374902 0.240160 0.043 Uiso 1 1 calc R U . . .
S2 S 0.38873(5) 0.50700(4) 0.19064(4) 0.02099(15) Uani 1 1 d . . . . .
C30 C 0.22429(18) 0.40899(15) 0.17362(15) 0.0174(5) Uani 1 1 d . . . . .
C31 C 0.12446(19) 0.40160(15) 0.16234(15) 0.0171(5) Uani 1 1 d . . . . .
C32 C 0.06248(18) 0.47643(15) 0.16020(15) 0.0178(5) Uani 1 1 d . . . . .
H32 H -0.003533 0.470514 0.151840 0.021 Uiso 1 1 calc R U . . .
C33 C 0.09731(19) 0.56029(16) 0.17035(15) 0.0182(5) Uani 1 1 d . . . . .
C34 C 0.19657(19) 0.56521(16) 0.18270(15) 0.0189(5) Uani 1 1 d . . . . .
H34 H 0.221677 0.619900 0.189898 0.023 Uiso 1 1 calc R U . . .
C35 C 0.26001(18) 0.49157(16) 0.18475(15) 0.0180(5) Uani 1 1 d . . . . .
C36 C 0.0302(2) 0.64268(16) 0.17172(17) 0.0227(6) Uani 1 1 d . . . . .
C37 C 0.0177(2) 0.6671(2) 0.26172(18) 0.0364(7) Uani 1 1 d . . . . .
H37 H -0.024194 0.718845 0.263203 0.055 Uiso 1 1 calc R U . . .
H37A H 0.082153 0.680447 0.274887 0.055 Uiso 1 1 calc R U . . .
H37B H -0.012806 0.617302 0.303260 0.055 Uiso 1 1 calc R U . . .
C38 C -0.0742(2) 0.62529(19) 0.1517(2) 0.0446(9) Uani 1 1 d . . . . .
H38 H -0.068290 0.609808 0.095726 0.067 Uiso 1 1 calc R U . . .
H38A H -0.113504 0.678560 0.153260 0.067 Uiso 1 1 calc R U . . .
H38B H -0.106310 0.576592 0.193721 0.067 Uiso 1 1 calc R U . . .
C39 C 0.0781(2) 0.72268(18) 0.1068(2) 0.0400(8) Uani 1 1 d . . . . .
H39 H 0.087304 0.707986 0.050375 0.060 Uiso 1 1 calc R U . . .
H39A H 0.141969 0.736642 0.120912 0.060 Uiso 1 1 calc R U . . .
H39B H 0.035377 0.773824 0.108310 0.060 Uiso 1 1 calc R U . . .
S3 S 0.07876(5) 0.29910(4) 0.14247(4) 0.01988(14) Uani 1 1 d . . . . .
O4 O 0.20553(13) 0.13481(10) 0.17390(10) 0.0179(4) Uani 1 1 d . . . . .
C40 C 0.14671(18) 0.15175(15) 0.24676(15) 0.0162(5) Uani 1 1 d . . . . .
C41 C 0.15403(19) 0.09978(15) 0.32711(15) 0.0172(5) Uani 1 1 d . . . . .
C42 C 0.09807(19) 0.12294(16) 0.40045(15) 0.0191(5) Uani 1 1 d . . . . .
H42 H 0.101519 0.086420 0.453186 0.023 Uiso 1 1 calc R U . . .
C43 C 0.03735(19) 0.19808(16) 0.39844(15) 0.0190(5) Uani 1 1 d . . . . .
C44 C 0.03174(18) 0.24888(16) 0.31791(15) 0.0184(5) Uani 1 1 d . . . . .
H44 H -0.009163 0.299001 0.313918 0.022 Uiso 1 1 calc R U . . .
C45 C 0.08509(18) 0.22729(15) 0.24337(15) 0.0170(5) Uani 1 1 d . . . . .
C46 C -0.0162(2) 0.22763(17) 0.47987(16) 0.0224(6) Uani 1 1 d . . . . .
C47 C -0.0049(2) 0.1604(2) 0.56114(18) 0.0403(8) Uani 1 1 d . . . . .
H47 H -0.041568 0.180868 0.610138 0.061 Uiso 1 1 calc R U . . .
H47A H 0.064651 0.155373 0.567116 0.061 Uiso 1 1 calc R U . . .
H47B H -0.030743 0.102609 0.557252 0.061 Uiso 1 1 calc R U . . .
C48 C -0.1281(2) 0.23891(19) 0.47654(18) 0.0308(6) Uani 1 1 d . . . . .
H48 H -0.137500 0.283817 0.427925 0.046 Uiso 1 1 calc R U . . .
H48A H -0.160414 0.257327 0.528168 0.046 Uiso 1 1 calc R U . . .
H48B H -0.156718 0.182680 0.471422 0.046 Uiso 1 1 calc R U . . .
C49 C 0.0292(2) 0.3184(2) 0.48546(19) 0.0379(7) Uani 1 1 d . . . . .
H49 H 0.019445 0.361999 0.435999 0.057 Uiso 1 1 calc R U . . .
H49A H 0.099635 0.311885 0.487454 0.057 Uiso 1 1 calc R U . . .
H49B H -0.002984 0.338242 0.536419 0.057 Uiso 1 1 calc R U . . .
Si2 Si 0.19320(5) 0.07102(4) 0.10072(4) 0.01722(15) Uani 1 1 d . . . . .
C50 C 0.28950(19) -0.01924(16) 0.10955(16) 0.0211(5) Uani 1 1 d . . . . .
H50 H 0.268382 -0.058588 0.164995 0.025 Uiso 1 1 calc R U . . .
C51 C 0.3955(2) 0.01400(18) 0.1124(2) 0.0317(7) Uani 1 1 d . . . . .
H51 H 0.437439 -0.036733 0.125910 0.048 Uiso 1 1 calc R U . . .
H51A H 0.392835 0.050886 0.155534 0.048 Uiso 1 1 calc R U . . .
H51B H 0.422604 0.048652 0.057507 0.048 Uiso 1 1 calc R U . . .
C52 C 0.2910(2) -0.07939(18) 0.04163(18) 0.0319(7) Uani 1 1 d . . . . .
H52 H 0.321076 -0.046761 -0.013308 0.048 Uiso 1 1 calc R U . . .
H52A H 0.223697 -0.096752 0.038836 0.048 Uiso 1 1 calc R U . . .
H52B H 0.329276 -0.132218 0.056937 0.048 Uiso 1 1 calc R U . . .
C53 C 0.2075(2) 0.15336(17) -0.00348(16) 0.0224(5) Uani 1 1 d . . . . .
H53 H 0.157200 0.199577 0.005061 0.027 Uiso 1 1 calc R U . . .
C54 C 0.3089(2) 0.2034(2) -0.02676(18) 0.0386(8) Uani 1 1 d . . . . .
H54 H 0.360518 0.162558 -0.042511 0.058 Uiso 1 1 calc R U . . .
H54A H 0.323279 0.227132 0.021791 0.058 Uiso 1 1 calc R U . . .
H54B H 0.306355 0.251965 -0.074113 0.058 Uiso 1 1 calc R U . . .
C55 C 0.1830(3) 0.11358(18) -0.07949(17) 0.0348(7) Uani 1 1 d . . . . .
H55 H 0.183547 0.160788 -0.128462 0.052 Uiso 1 1 calc R U . . .
H55A H 0.117939 0.085240 -0.064727 0.052 Uiso 1 1 calc R U . . .
H55B H 0.232314 0.069809 -0.092873 0.052 Uiso 1 1 calc R U . . .
C56 C 0.06512(19) 0.01673(16) 0.12112(16) 0.0212(5) Uani 1 1 d . . . . .
H56 H 0.063456 -0.017803 0.075163 0.025 Uiso 1 1 calc R U . . .
C57 C 0.0434(2) -0.05150(17) 0.20613(17) 0.0281(6) Uani 1 1 d . . . . .
H57 H 0.040511 -0.020360 0.253574 0.042 Uiso 1 1 calc R U . . .
H57A H 0.095735 -0.095070 0.208506 0.042 Uiso 1 1 calc R U . . .
H57B H -0.019614 -0.081505 0.209168 0.042 Uiso 1 1 calc R U . . .
C58 C -0.0199(2) 0.08472(17) 0.11445(18) 0.0265(6) Uani 1 1 d . . . . .
H58 H -0.082268 0.053217 0.118747 0.040 Uiso 1 1 calc R U . . .
H58A H -0.007017 0.125083 0.060275 0.040 Uiso 1 1 calc R U . . .
H58B H -0.023704 0.118423 0.160152 0.040 Uiso 1 1 calc R U . . .
S4 S 0.23836(5) 0.00818(4) 0.33793(4) 0.01935(14) Uani 1 1 d . . . . .
O5 O 0.51236(18) 0.24186(16) 0.64600(14) 0.0483(6) Uani 1 1 d . . . . .
C59 C 0.6149(3) 0.2177(3) 0.6263(3) 0.0555(10) Uani 1 1 d . . . . .
H59 H 0.643909 0.249832 0.569997 0.067 Uiso 1 1 calc R U . . .
H59A H 0.619700 0.153626 0.626100 0.067 Uiso 1 1 calc R U . . .
C60 C 0.6694(3) 0.2422(2) 0.6934(2) 0.0498(9) Uani 1 1 d . . . . .
H60 H 0.701474 0.300997 0.674468 0.060 Uiso 1 1 calc R U . . .
H60A H 0.719701 0.197978 0.707658 0.060 Uiso 1 1 calc R U . . .
C61 C 0.5872(3) 0.2426(2) 0.7689(2) 0.0580(11) Uani 1 1 d . . . . .
H61 H 0.577768 0.183575 0.805085 0.070 Uiso 1 1 calc R U . . .
H61A H 0.601170 0.286318 0.803090 0.070 Uiso 1 1 calc R U . . .
C62 C 0.4995(3) 0.2680(3) 0.7262(3) 0.0806(14) Uani 1 1 d . . . . .
H62 H 0.439735 0.239232 0.761469 0.097 Uiso 1 1 calc R U . . .
H62A H 0.490971 0.332689 0.719075 0.097 Uiso 1 1 calc R 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
O1 C1 1.359(3) . ?
O2 C30 1.358(3) . ?
C1 C6 1.392(3) . ?
C1 C2 1.398(3) . ?
C2 C3 1.396(3) . ?
C2 S1 1.780(2) . ?
C3 C4 1.387(3) . ?
C4 C5 1.393(3) . ?
C4 C7 1.537(3) . ?
C5 C6 1.398(3) . ?
C6 S4 1.782(3) . ?
C7 C10 1.530(4) . ?
C7 C9 1.532(4) . ?
C7 C8 1.535(4) . ?
S1 C16 1.787(2) . ?
O3 C11 1.361(3) . ?
O3 Si1 1.6785(17) . ?
C11 C16 1.395(3) . ?
C11 C12 1.399(3) . ?
C12 C13 1.393(3) . ?
C12 S2 1.782(2) . ?
C13 C14 1.392(4) . ?
C14 C15 1.392(3) . ?
C14 C17 1.536(3) . ?
C15 C16 1.395(3) . ?
C17 C20 1.526(4) . ?
C17 C18 1.531(4) . ?
C17 C19 1.541(4) . ?
Si1 C21 1.874(3) . ?
Si1 C27 1.879(3) . ?
Si1 C24 1.882(2) . ?
C21 C22 1.532(4) . ?
C21 C23 1.537(3) . ?
C24 C26 1.534(3) . ?
C24 C25 1.543(3) . ?
C27 C29 1.530(4) . ?
C27 C28 1.537(3) . ?
S2 C35 1.777(3) . ?
C30 C35 1.394(3) . ?
C30 C31 1.397(3) . ?
C31 C32 1.396(3) . ?
C31 S3 1.773(2) . ?
C32 C33 1.403(3) . ?
C33 C34 1.391(3) . ?
C33 C36 1.531(3) . ?
C34 C35 1.394(3) . ?
C36 C39 1.523(4) . ?
C36 C38 1.530(4) . ?
C36 C37 1.537(4) . ?
S3 C45 1.792(2) . ?
O4 C40 1.370(3) . ?
O4 Si2 1.6756(17) . ?
C40 C41 1.400(3) . ?
C40 C45 1.401(3) . ?
C41 C42 1.394(3) . ?
C41 S4 1.782(2) . ?
C42 C43 1.390(3) . ?
C43 C44 1.391(3) . ?
C43 C46 1.529(3) . ?
C44 C45 1.387(3) . ?
C46 C48 1.527(4) . ?
C46 C47 1.528(4) . ?
C46 C49 1.533(4) . ?
Si2 C50 1.874(3) . ?
Si2 C53 1.880(3) . ?
Si2 C56 1.881(3) . ?
C50 C51 1.534(4) . ?
C50 C52 1.537(3) . ?
C53 C55 1.533(3) . ?
C53 C54 1.535(4) . ?
C56 C58 1.534(3) . ?
C56 C57 1.544(4) . ?
O5 C62 1.398(4) . ?
O5 C59 1.429(4) . ?
C59 C60 1.495(5) . ?
C60 C61 1.512(5) . ?
C61 C62 1.470(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C6 118.4(2) . . ?
O1 C1 C2 122.6(2) . . ?
C6 C1 C2 119.0(2) . . ?
C3 C2 C1 120.2(2) . . ?
C3 C2 S1 120.50(19) . . ?
C1 C2 S1 119.31(18) . . ?
C4 C3 C2 121.6(2) . . ?
C3 C4 C5 117.4(2) . . ?
C3 C4 C7 119.7(2) . . ?
C5 C4 C7 122.6(2) . . ?
C4 C5 C6 122.1(2) . . ?
C1 C6 C5 119.6(2) . . ?
C1 C6 S4 120.48(18) . . ?
C5 C6 S4 119.81(19) . . ?
C10 C7 C9 108.4(2) . . ?
C10 C7 C8 108.8(2) . . ?
C9 C7 C8 108.8(2) . . ?
C10 C7 C4 111.8(2) . . ?
C9 C7 C4 111.1(2) . . ?
C8 C7 C4 107.8(2) . . ?
C2 S1 C16 99.52(11) . . ?
C11 O3 Si1 140.62(15) . . ?
O3 C11 C16 120.4(2) . . ?
O3 C11 C12 121.5(2) . . ?
C16 C11 C12 117.9(2) . . ?
C13 C12 C11 120.2(2) . . ?
C13 C12 S2 119.01(19) . . ?
C11 C12 S2 120.73(19) . . ?
C14 C13 C12 122.5(2) . . ?
C13 C14 C15 116.7(2) . . ?
C13 C14 C17 121.7(2) . . ?
C15 C14 C17 121.5(2) . . ?
C14 C15 C16 121.9(2) . . ?
C15 C16 C11 120.8(2) . . ?
C15 C16 S1 118.46(18) . . ?
C11 C16 S1 120.64(18) . . ?
C20 C17 C18 108.5(2) . . ?
C20 C17 C14 111.5(2) . . ?
C18 C17 C14 112.0(2) . . ?
C20 C17 C19 108.6(2) . . ?
C18 C17 C19 108.6(2) . . ?
C14 C17 C19 107.5(2) . . ?
O3 Si1 C21 104.16(10) . . ?
O3 Si1 C27 107.19(10) . . ?
C21 Si1 C27 108.09(12) . . ?
O3 Si1 C24 111.53(10) . . ?
C21 Si1 C24 110.63(11) . . ?
C27 Si1 C24 114.64(12) . . ?
C22 C21 C23 109.5(2) . . ?
C22 C21 Si1 114.06(18) . . ?
C23 C21 Si1 111.39(17) . . ?
C26 C24 C25 109.9(2) . . ?
C26 C24 Si1 116.52(17) . . ?
C25 C24 Si1 111.26(17) . . ?
C29 C27 C28 109.7(2) . . ?
C29 C27 Si1 115.21(18) . . ?
C28 C27 Si1 113.07(18) . . ?
C35 S2 C12 101.74(11) . . ?
O2 C30 C35 118.7(2) . . ?
O2 C30 C31 122.4(2) . . ?
C35 C30 C31 118.9(2) . . ?
C32 C31 C30 120.3(2) . . ?
C32 C31 S3 119.66(19) . . ?
C30 C31 S3 119.86(18) . . ?
C31 C32 C33 121.6(2) . . ?
C34 C33 C32 116.7(2) . . ?
C34 C33 C36 120.4(2) . . ?
C32 C33 C36 122.9(2) . . ?
C33 C34 C35 122.7(2) . . ?
C34 C35 C30 119.7(2) . . ?
C34 C35 S2 119.37(19) . . ?
C30 C35 S2 120.61(19) . . ?
C39 C36 C38 108.7(2) . . ?
C39 C36 C33 110.3(2) . . ?
C38 C36 C33 112.4(2) . . ?
C39 C36 C37 108.6(2) . . ?
C38 C36 C37 107.9(2) . . ?
C33 C36 C37 108.8(2) . . ?
C31 S3 C45 100.31(11) . . ?
C40 O4 Si2 134.86(15) . . ?
O4 C40 C41 121.0(2) . . ?
O4 C40 C45 120.3(2) . . ?
C41 C40 C45 118.4(2) . . ?
C42 C41 C40 119.4(2) . . ?
C42 C41 S4 119.35(18) . . ?
C40 C41 S4 121.21(18) . . ?
C43 C42 C41 123.1(2) . . ?
C42 C43 C44 116.4(2) . . ?
C42 C43 C46 122.6(2) . . ?
C44 C43 C46 120.9(2) . . ?
C45 C44 C43 122.2(2) . . ?
C44 C45 C40 120.5(2) . . ?
C44 C45 S3 119.58(18) . . ?
C40 C45 S3 119.83(18) . . ?
C48 C46 C47 107.7(2) . . ?
C48 C46 C43 110.7(2) . . ?
C47 C46 C43 112.7(2) . . ?
C48 C46 C49 109.0(2) . . ?
C47 C46 C49 108.8(2) . . ?
C43 C46 C49 107.9(2) . . ?
O4 Si2 C50 107.43(10) . . ?
O4 Si2 C53 103.98(10) . . ?
C50 Si2 C53 116.17(12) . . ?
O4 Si2 C56 111.24(10) . . ?
C50 Si2 C56 108.92(11) . . ?
C53 Si2 C56 109.02(12) . . ?
C51 C50 C52 110.9(2) . . ?
C51 C50 Si2 114.89(18) . . ?
C52 C50 Si2 112.90(19) . . ?
C55 C53 C54 110.7(2) . . ?
C55 C53 Si2 114.08(18) . . ?
C54 C53 Si2 114.04(19) . . ?
C58 C56 C57 110.3(2) . . ?
C58 C56 Si2 113.41(17) . . ?
C57 C56 Si2 114.03(19) . . ?
C6 S4 C41 98.50(11) . . ?
C62 O5 C59 107.6(3) . . ?
O5 C59 C60 107.8(3) . . ?
C59 C60 C61 103.2(3) . . ?
C62 C61 C60 102.0(3) . . ?
O5 C62 C61 110.1(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
O1 C1 C2 C3 175.0(2) . . . . ?
C6 C1 C2 C3 -3.8(3) . . . . ?
O1 C1 C2 S1 -4.1(3) . . . . ?
C6 C1 C2 S1 177.05(17) . . . . ?
C1 C2 C3 C4 0.8(4) . . . . ?
S1 C2 C3 C4 179.94(18) . . . . ?
C2 C3 C4 C5 2.8(4) . . . . ?
C2 C3 C4 C7 -171.0(2) . . . . ?
C3 C4 C5 C6 -3.4(4) . . . . ?
C7 C4 C5 C6 170.1(2) . . . . ?
O1 C1 C6 C5 -175.7(2) . . . . ?
C2 C1 C6 C5 3.2(3) . . . . ?
O1 C1 C6 S4 0.4(3) . . . . ?
C2 C1 C6 S4 179.25(18) . . . . ?
C4 C5 C6 C1 0.5(4) . . . . ?
C4 C5 C6 S4 -175.64(19) . . . . ?
C3 C4 C7 C10 -174.5(2) . . . . ?
C5 C4 C7 C10 12.1(3) . . . . ?
C3 C4 C7 C9 -53.2(3) . . . . ?
C5 C4 C7 C9 133.4(3) . . . . ?
C3 C4 C7 C8 65.9(3) . . . . ?
C5 C4 C7 C8 -107.5(3) . . . . ?
C3 C2 S1 C16 -99.8(2) . . . . ?
C1 C2 S1 C16 79.3(2) . . . . ?
Si1 O3 C11 C16 -102.0(3) . . . . ?
Si1 O3 C11 C12 83.1(3) . . . . ?
O3 C11 C12 C13 175.7(2) . . . . ?
C16 C11 C12 C13 0.7(3) . . . . ?
O3 C11 C12 S2 -5.8(3) . . . . ?
C16 C11 C12 S2 179.12(17) . . . . ?
C11 C12 C13 C14 -0.3(4) . . . . ?
S2 C12 C13 C14 -178.77(18) . . . . ?
C12 C13 C14 C15 0.2(4) . . . . ?
C12 C13 C14 C17 176.5(2) . . . . ?
C13 C14 C15 C16 -0.6(4) . . . . ?
C17 C14 C15 C16 -176.8(2) . . . . ?
C14 C15 C16 C11 1.0(4) . . . . ?
C14 C15 C16 S1 -176.25(19) . . . . ?
O3 C11 C16 C15 -176.1(2) . . . . ?
C12 C11 C16 C15 -1.0(3) . . . . ?
O3 C11 C16 S1 1.0(3) . . . . ?
C12 C11 C16 S1 176.15(18) . . . . ?
C2 S1 C16 C15 66.6(2) . . . . ?
C2 S1 C16 C11 -110.6(2) . . . . ?
C13 C14 C17 C20 151.2(2) . . . . ?
C15 C14 C17 C20 -32.8(3) . . . . ?
C13 C14 C17 C18 29.3(3) . . . . ?
C15 C14 C17 C18 -154.6(2) . . . . ?
C13 C14 C17 C19 -89.9(3) . . . . ?
C15 C14 C17 C19 86.1(3) . . . . ?
C11 O3 Si1 C21 -156.4(2) . . . . ?
C11 O3 Si1 C27 89.2(3) . . . . ?
C11 O3 Si1 C24 -37.1(3) . . . . ?
O3 Si1 C21 C22 74.10(19) . . . . ?
C27 Si1 C21 C22 -172.13(17) . . . . ?
C24 Si1 C21 C22 -45.9(2) . . . . ?
O3 Si1 C21 C23 -50.5(2) . . . . ?
C27 Si1 C21 C23 63.3(2) . . . . ?
C24 Si1 C21 C23 -170.47(18) . . . . ?
O3 Si1 C24 C26 53.8(2) . . . . ?
C21 Si1 C24 C26 169.22(19) . . . . ?
C27 Si1 C24 C26 -68.2(2) . . . . ?
O3 Si1 C24 C25 -179.13(17) . . . . ?
C21 Si1 C24 C25 -63.7(2) . . . . ?
C27 Si1 C24 C25 58.8(2) . . . . ?
O3 Si1 C27 C29 -78.8(2) . . . . ?
C21 Si1 C27 C29 169.50(18) . . . . ?
C24 Si1 C27 C29 45.6(2) . . . . ?
O3 Si1 C27 C28 153.95(18) . . . . ?
C21 Si1 C27 C28 42.2(2) . . . . ?
C24 Si1 C27 C28 -81.7(2) . . . . ?
C13 C12 S2 C35 -64.5(2) . . . . ?
C11 C12 S2 C35 117.1(2) . . . . ?
O2 C30 C31 C32 -178.6(2) . . . . ?
C35 C30 C31 C32 1.5(3) . . . . ?
O2 C30 C31 S3 -3.4(3) . . . . ?
C35 C30 C31 S3 176.72(18) . . . . ?
C30 C31 C32 C33 -0.9(4) . . . . ?
S3 C31 C32 C33 -176.08(18) . . . . ?
C31 C32 C33 C34 0.0(4) . . . . ?
C31 C32 C33 C36 -177.6(2) . . . . ?
C32 C33 C34 C35 0.3(4) . . . . ?
C36 C33 C34 C35 177.9(2) . . . . ?
C33 C34 C35 C30 0.4(4) . . . . ?
C33 C34 C35 S2 174.04(18) . . . . ?
O2 C30 C35 C34 178.8(2) . . . . ?
C31 C30 C35 C34 -1.3(3) . . . . ?
O2 C30 C35 S2 5.3(3) . . . . ?
C31 C30 C35 S2 -174.87(17) . . . . ?
C12 S2 C35 C34 114.5(2) . . . . ?
C12 S2 C35 C30 -71.9(2) . . . . ?
C34 C33 C36 C39 55.2(3) . . . . ?
C32 C33 C36 C39 -127.3(3) . . . . ?
C34 C33 C36 C38 176.7(2) . . . . ?
C32 C33 C36 C38 -5.8(4) . . . . ?
C34 C33 C36 C37 -63.9(3) . . . . ?
C32 C33 C36 C37 113.6(3) . . . . ?
C32 C31 S3 C45 -117.6(2) . . . . ?
C30 C31 S3 C45 67.2(2) . . . . ?
Si2 O4 C40 C41 91.2(3) . . . . ?
Si2 O4 C40 C45 -95.3(3) . . . . ?
O4 C40 C41 C42 175.5(2) . . . . ?
C45 C40 C41 C42 1.9(3) . . . . ?
O4 C40 C41 S4 -1.2(3) . . . . ?
C45 C40 C41 S4 -174.84(18) . . . . ?
C40 C41 C42 C43 -2.6(4) . . . . ?
S4 C41 C42 C43 174.16(19) . . . . ?
C41 C42 C43 C44 2.2(4) . . . . ?
C41 C42 C43 C46 -174.3(2) . . . . ?
C42 C43 C44 C45 -1.2(4) . . . . ?
C46 C43 C44 C45 175.4(2) . . . . ?
C43 C44 C45 C40 0.6(4) . . . . ?
C43 C44 C45 S3 -176.97(19) . . . . ?
O4 C40 C45 C44 -174.7(2) . . . . ?
C41 C40 C45 C44 -0.9(4) . . . . ?
O4 C40 C45 S3 2.9(3) . . . . ?
C41 C40 C45 S3 176.67(17) . . . . ?
C31 S3 C45 C44 59.2(2) . . . . ?
C31 S3 C45 C40 -118.4(2) . . . . ?
C42 C43 C46 C48 -127.1(3) . . . . ?
C44 C43 C46 C48 56.5(3) . . . . ?
C42 C43 C46 C47 -6.4(4) . . . . ?
C44 C43 C46 C47 177.2(2) . . . . ?
C42 C43 C46 C49 113.7(3) . . . . ?
C44 C43 C46 C49 -62.6(3) . . . . ?
C40 O4 Si2 C50 -114.4(2) . . . . ?
C40 O4 Si2 C53 121.9(2) . . . . ?
C40 O4 Si2 C56 4.7(2) . . . . ?
O4 Si2 C50 C51 -47.7(2) . . . . ?
C53 Si2 C50 C51 68.2(2) . . . . ?
C56 Si2 C50 C51 -168.33(19) . . . . ?
O4 Si2 C50 C52 -176.28(17) . . . . ?
C53 Si2 C50 C52 -60.4(2) . . . . ?
C56 Si2 C50 C52 63.1(2) . . . . ?
O4 Si2 C53 C55 -171.1(2) . . . . ?
C50 Si2 C53 C55 71.1(2) . . . . ?
C56 Si2 C53 C55 -52.3(2) . . . . ?
O4 Si2 C53 C54 60.4(2) . . . . ?
C50 Si2 C53 C54 -57.4(2) . . . . ?
C56 Si2 C53 C54 179.1(2) . . . . ?
O4 Si2 C56 C58 62.4(2) . . . . ?
C50 Si2 C56 C58 -179.33(18) . . . . ?
C53 Si2 C56 C58 -51.7(2) . . . . ?
O4 Si2 C56 C57 -64.9(2) . . . . ?
C50 Si2 C56 C57 53.3(2) . . . . ?
C53 Si2 C56 C57 -178.98(18) . . . . ?
C1 C6 S4 C41 -78.9(2) . . . . ?
C5 C6 S4 C41 97.1(2) . . . . ?
C42 C41 S4 C6 -54.8(2) . . . . ?
C40 C41 S4 C6 121.9(2) . . . . ?
C62 O5 C59 C60 -7.6(4) . . . . ?
O5 C59 C60 C61 23.7(4) . . . . ?
C59 C60 C61 C62 -29.6(4) . . . . ?
C59 O5 C62 C61 -12.6(5) . . . . ?
C60 C61 C62 O5 26.9(5) . . . . ?

_refine_diff_density_max         0.475
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.081

