Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Michael Mehring' ; Lehrstuhl fur Anorganische Chemie II Universitat Dortmund Otto-Hahn-Str. 6 44227 Dortmund Germany ; 'Giuseppina Gabriele' ; Lehrstuhl fur Anorganische Chemie II Universitat Dortmund Otto-Hahn-Str. 6 44227 Dortmund Germany ; 'Sotiris Hadjikakou' ; Department of Chemistry Universitiy of Ioannina 45110 Ioannina Greece ; 'Markus Schurmann' ; Lehrstuhl fur Anorganische Chemie II Universitat Dortmund Otto-Hahn-Str. 6 44227 Dortmund Germany ; 'Dainis Dakternieks' ; School of Biological and Chemical Sciences Deakin University Geelong Vic. 3217 Australia ; 'Klaus Jurkschat' ; Lehrstuhl fur Anorganische Chemie II Universitat Dortmund Otto-Hahn-Str. 6 44227 Dortmund Germany ; _publ_contact_author_name 'Prof. Klaus Jurkschat' _publ_contact_author_address ; Lehrstuhl fur Anorganische Chemie II Universitat Dortmund Otto-Hahn-Str. 6 44227 Dortmund Germany ; _publ_contact_author_phone '49-231-755-3800' _publ_contact_author_fax '49-231-755-5048' _publ_contact_author_email 'kjur@platon.chemie.uni-dortmund.de' _publ_requested_journal 'Chemical Communications' _publ_requested_coeditor_name 'Dr. S. Thomas' _publ_requested_category ? _publ_contact_letter ? #============================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; From organotin oxo clusters to hydrogen-bonded inorganic-organic hybrids ; _publ_section_title_footnote ? # 3. TEXT _publ_section_exptl_refinement ; Intensity data for the colorless crystals were collected on a Nonius KappaCCD diffractometer with graphite-monochromated MoK\a (0.71073 \%A) radiation at 173(1) K (1, 1ú4THF, 1ú3CH2Cl2). The data collection covered almost the whole sphere of reciprocal space with 3 sets at different \k-angles and 242(1) 262 (1ú4THF), and 291 (1ú3CH2Cl2) frames via (-rotation (\D/\w=1\%) at two times 5s (1ú3CH2Cl2), 10s (1ú4THF) and 100s (1) per frame. The crystal-to- detector distance was 3.4 cm. Crystal decay was monitored by repeating the initial frames at the end of data collection. The data were not corrected for absorption effects. Analyzing the duplicate reflections there was no indication for any decay. The structures were solved by direct methods SHELXS97 and successive difference Fourier syntheses. Refinement applied full-matrix least-squares methods SHELXL97. The H atoms were placed in geometrically calculated positions using a riding model (C-H~prim.~ 0.96 \%A, C-H~sec.~ 0.97 \%A; H~aryl~ C-H 0.93 \%A) constrained at 1.2 times U~eq~ of the carrier atom. All phenyl groups (refined as regular hexagons with AFIX 66) and one solvent molecule thf are disordered with occupancies of 0.3 (C(11') > C(16'), C(41') > C(46')), 0.5 (C(21) > C(26), C(21') > C(26'), C(31) > C(36), C(31') > C(36'), C(63), C(63'), C(64), C(64')), and 0.7 (C(11) > C(16), C(41) > C(46)), whereas C(11) > C(46), O(51), O(61), C(62) and C(65) were refined anisotropically and C(11') > C(46'), C(51') > C(55)', C(63) C(64), C(63'), and C(64') were refined isotropically. ; _publ_section_references ; Otwinowski, Z. & Minor, W. (1997). "Processing of X-Ray Diffraction Data Collected in Oscillation Mode", in Methods in Enzymology, Volume 276, Macromolecular Crystallography, Part A, edited by Carter, C.W. & Sweet, R.M., pp. 307-326. Academic Press. Sheldrick, G.M. (1990). SHELXS97. Acta Cryst. A46, 467-473. Sheldrick, G.M. (1997). SHELXTL. Release 5.1 Software Reference Manual, Bruker AXS, Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELXL97. Program for Crystal Structure Refinement. University of Gottingen, Germany. ; # 4. CHEMICAL DATA data_(1) _database_code_CSD 178297 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H52 I4 O8 Sn8' _chemical_formula_weight 2262.06 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' 'Sn' 'Sn' -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.8313(4) _cell_length_b 18.5471(5) _cell_length_c 21.8859(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.5531(9) _cell_angle_gamma 90.00 _cell_volume 6190.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 40285 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 25.32 _exptl_crystal_description 'parallel epipede' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not determined' _exptl_crystal_density_diffrn 2.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4160 _exptl_absorpt_coefficient_mu 5.213 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ; 3 sets at different \k-angles and 242 frames via \w-rotation (\D/\w=1\%) at two times 100s per frame ; _diffrn_detector_area_resol_mean '19 vertical, 18 horizontal' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 40285 _diffrn_reflns_av_R_equivalents 0.061 _diffrn_reflns_av_sigmaI/netI 0.1821 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.32 _reflns_number_total 11147 _reflns_number_gt 5688 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius KappaCCD' _computing_cell_refinement ; DENZO and SCALEPACK (Otwinowski & Minor, 1997) ; _computing_data_reduction ; DENZO and SCALEPACK (Otwinowski & Minor, 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11147 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1522 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I -0.19025(5) 0.26648(4) -0.12695(4) 0.0334(2) Uani 1 1 d . . . I2 I -0.70048(5) 0.17099(4) -0.43387(4) 0.0353(2) Uani 1 1 d . . . I3 I -0.26190(5) -0.01534(4) -0.34637(5) 0.0366(2) Uani 1 1 d . . . I4 I -0.40029(5) 0.45132(4) -0.42885(4) 0.0330(2) Uani 1 1 d . . . Sn1 Sn -0.28364(5) 0.13607(4) -0.17575(4) 0.0259(2) Uani 1 1 d . . . Sn2 Sn -0.47290(5) 0.12931(4) -0.28880(4) 0.0248(2) Uani 1 1 d . . . Sn3 Sn -0.42372(5) 0.30318(4) -0.25776(4) 0.0236(2) Uani 1 1 d . . . Sn4 Sn -0.61250(5) 0.29882(4) -0.37372(4) 0.0253(2) Uani 1 1 d . . . Sn5 Sn -0.17534(5) 0.11914(4) -0.30004(4) 0.0265(2) Uani 1 1 d . . . Sn6 Sn -0.39828(5) 0.15414(4) -0.43048(4) 0.0235(2) Uani 1 1 d . . . Sn7 Sn -0.26446(5) 0.28098(4) -0.34867(4) 0.0224(2) Uani 1 1 d . . . Sn8 Sn -0.47977(5) 0.31730(4) -0.48454(4) 0.0248(2) Uani 1 1 d . . . O1 O -0.3756(4) 0.1951(3) -0.2381(3) 0.0226(19) Uani 1 1 d . . . O2 O -0.5157(4) 0.2366(3) -0.3159(4) 0.0215(19) Uani 1 1 d . . . O3 O -0.3715(5) 0.0566(4) -0.2334(4) 0.027(2) Uani 1 1 d . . . O4 O -0.5155(4) 0.3763(4) -0.3202(4) 0.025(2) Uani 1 1 d . . . O5 O -0.2796(4) 0.1701(3) -0.3579(3) 0.0183(19) Uani 1 1 d . . . O6 O -0.3859(4) 0.2629(4) -0.4194(3) 0.0205(19) Uani 1 1 d . . . O7 O -0.1536(4) 0.2327(3) -0.2813(4) 0.0215(19) Uani 1 1 d . . . O8 O -0.5087(4) 0.2034(3) -0.4962(3) 0.0223(19) Uani 1 1 d . . . C1 C -0.1761(7) 0.0952(6) -0.2057(5) 0.029(3) Uani 1 1 d . . . H1A H -0.1225 0.1139 -0.1775 0.035 Uiso 1 1 calc R . . H1B H -0.1749 0.0432 -0.2007 0.035 Uiso 1 1 calc R . . C2 C -0.4714(7) 0.0937(5) -0.3798(5) 0.019(3) Uani 1 1 d . . . H2A H -0.5316 0.0917 -0.4056 0.023 Uiso 1 1 calc R . . H2B H -0.4491 0.0448 -0.3758 0.023 Uiso 1 1 calc R . . C3 C -0.3111(7) 0.3422(6) -0.2835(5) 0.021(3) Uani 1 1 d . . . H3A H -0.3244 0.3902 -0.3010 0.025 Uiso 1 1 calc R . . H3B H -0.2638 0.3469 -0.2450 0.025 Uiso 1 1 calc R . . C4 C -0.5980(7) 0.3402(6) -0.4607(6) 0.029(3) Uani 1 1 d . . . H4A H -0.6461 0.3219 -0.4945 0.035 Uiso 1 1 calc R . . H4B H -0.6044 0.3921 -0.4599 0.035 Uiso 1 1 calc R . . C11 C -0.3165(7) 0.1106(6) -0.0903(6) 0.023(3) Uani 1 1 d . . . C12 C -0.3109(8) 0.0408(7) -0.0677(6) 0.035(3) Uani 1 1 d . . . H12 H -0.3010 0.0034 -0.0933 0.042 Uiso 1 1 calc R . . C13 C -0.3195(8) 0.0256(7) -0.0083(6) 0.035(3) Uani 1 1 d . . . H13 H -0.3115 -0.0212 0.0075 0.042 Uiso 1 1 calc R . . C14 C -0.3397(8) 0.0794(7) 0.0270(7) 0.043(4) Uani 1 1 d . . . H14 H -0.3470 0.0687 0.0668 0.051 Uiso 1 1 calc R . . C15 C -0.3496(7) 0.1487(7) 0.0061(6) 0.032(3) Uani 1 1 d . . . H15 H -0.3655 0.1845 0.0307 0.038 Uiso 1 1 calc R . . C16 C -0.3359(7) 0.1653(6) -0.0525(6) 0.029(3) Uani 1 1 d . . . H16 H -0.3396 0.2129 -0.0664 0.035 Uiso 1 1 calc R . . C21 C -0.5622(8) 0.1045(6) -0.2337(6) 0.032(3) Uani 1 1 d . . . C22 C -0.5336(8) 0.0653(6) -0.1788(7) 0.037(3) Uani 1 1 d . . . H22 H -0.4778 0.0450 -0.1685 0.044 Uiso 1 1 calc R . . C23 C -0.5864(8) 0.0555(6) -0.1388(7) 0.038(4) Uani 1 1 d . . . H23 H -0.5668 0.0286 -0.1018 0.045 Uiso 1 1 calc R . . C24 C -0.6688(10) 0.0861(7) -0.1542(7) 0.046(4) Uani 1 1 d . . . H24 H -0.7043 0.0800 -0.1270 0.055 Uiso 1 1 calc R . . C25 C -0.6994(8) 0.1253(7) -0.2084(7) 0.043(4) Uani 1 1 d . . . H25 H -0.7550 0.1457 -0.2182 0.051 Uiso 1 1 calc R . . C26 C -0.6449(8) 0.1340(6) -0.2495(6) 0.035(3) Uani 1 1 d . . . H26 H -0.6649 0.1597 -0.2871 0.042 Uiso 1 1 calc R . . C31 C -0.4656(8) 0.3216(6) -0.1745(6) 0.026(3) Uani 1 1 d . . . C32 C -0.4137(8) 0.3503(6) -0.1197(6) 0.030(3) Uani 1 1 d . . . H32 H -0.3572 0.3658 -0.1179 0.036 Uiso 1 1 calc R . . C33 C -0.4456(9) 0.3561(6) -0.0669(6) 0.038(4) Uani 1 1 d . . . H33 H -0.4093 0.3745 -0.0295 0.045 Uiso 1 1 calc R . . C34 C -0.5273(9) 0.3361(7) -0.0682(7) 0.047(4) Uani 1 1 d . . . H34 H -0.5476 0.3421 -0.0324 0.056 Uiso 1 1 calc R . . C35 C -0.5795(8) 0.3075(7) -0.1205(7) 0.039(4) Uani 1 1 d . . . H35 H -0.6356 0.2921 -0.1210 0.047 Uiso 1 1 calc R . . C36 C -0.5487(8) 0.3006(6) -0.1758(7) 0.041(4) Uani 1 1 d . . . H36 H -0.5854 0.2817 -0.2128 0.049 Uiso 1 1 calc R . . C41 C -0.7075(8) 0.3330(6) -0.3268(6) 0.027(3) Uani 1 1 d . . . C42 C -0.7809(8) 0.2924(6) -0.3273(6) 0.035(3) Uani 1 1 d . . . H42 H -0.7887 0.2480 -0.3478 0.042 Uiso 1 1 calc R . . C43 C -0.8426(9) 0.3163(7) -0.2981(6) 0.043(4) Uani 1 1 d . . . H43 H -0.8913 0.2878 -0.2988 0.051 Uiso 1 1 calc R . . C44 C -0.8326(8) 0.3825(7) -0.2677(7) 0.045(4) Uani 1 1 d . . . H44 H -0.8746 0.3998 -0.2488 0.055 Uiso 1 1 calc R . . C45 C -0.7581(9) 0.4219(7) -0.2664(7) 0.045(4) Uani 1 1 d . . . H45 H -0.7490 0.4657 -0.2450 0.055 Uiso 1 1 calc R . . C46 C -0.6981(8) 0.3980(6) -0.2956(6) 0.031(3) Uani 1 1 d . . . H46 H -0.6492 0.4264 -0.2946 0.038 Uiso 1 1 calc R . . C51 C -0.0664(7) 0.1035(6) -0.3379(6) 0.032(3) Uani 1 1 d . . . C52 C -0.0241(8) 0.0378(6) -0.3321(6) 0.041(4) Uani 1 1 d . . . H52 H -0.0467 -0.0002 -0.3135 0.049 Uiso 1 1 calc R . . C53 C 0.0499(8) 0.0254(7) -0.3524(7) 0.048(4) Uani 1 1 d . . . H53 H 0.0760 -0.0199 -0.3481 0.058 Uiso 1 1 calc R . . C54 C 0.0848(8) 0.0820(7) -0.3794(7) 0.040(4) Uani 1 1 d . . . H54 H 0.1369 0.0760 -0.3909 0.048 Uiso 1 1 calc R . . C55 C 0.0416(8) 0.1466(7) -0.3889(6) 0.036(3) Uani 1 1 d . . . H55 H 0.0610 0.1833 -0.4108 0.043 Uiso 1 1 calc R . . C56 C -0.0315(8) 0.1578(6) -0.3659(6) 0.036(3) Uani 1 1 d . . . H56 H -0.0571 0.2033 -0.3696 0.043 Uiso 1 1 calc R . . C61 C -0.3480(8) 0.1087(6) -0.5033(6) 0.030(3) Uani 1 1 d . . . C62 C -0.2573(9) 0.0996(6) -0.4950(6) 0.036(3) Uani 1 1 d . . . H62 H -0.2178 0.1151 -0.4578 0.044 Uiso 1 1 calc R . . C63 C -0.2268(10) 0.0677(7) -0.5422(8) 0.049(4) Uani 1 1 d . . . H63 H -0.1671 0.0614 -0.5371 0.059 Uiso 1 1 calc R . . C64 C -0.2847(10) 0.0461(6) -0.5951(8) 0.044(4) Uani 1 1 d . . . H64 H -0.2643 0.0255 -0.6272 0.052 Uiso 1 1 calc R . . C65 C -0.3727(10) 0.0533(6) -0.6040(7) 0.050(4) Uani 1 1 d . . . H65 H -0.4109 0.0361 -0.6411 0.060 Uiso 1 1 calc R . . C66 C -0.4058(9) 0.0854(6) -0.5588(6) 0.035(3) Uani 1 1 d . . . H66 H -0.4659 0.0914 -0.5655 0.042 Uiso 1 1 calc R . . C71 C -0.1869(7) 0.3159(6) -0.4074(6) 0.026(3) Uani 1 1 d . . . C72 C -0.1056(8) 0.3486(6) -0.3825(7) 0.039(4) Uani 1 1 d . . . H72 H -0.0876 0.3611 -0.3398 0.047 Uiso 1 1 calc R . . C73 C -0.0511(9) 0.3626(7) -0.4222(8) 0.050(4) Uani 1 1 d . . . H73 H 0.0034 0.3840 -0.4056 0.060 Uiso 1 1 calc R . . C74 C -0.0776(10) 0.3448(7) -0.4851(9) 0.055(4) Uani 1 1 d . . . H74 H -0.0400 0.3537 -0.5105 0.066 Uiso 1 1 calc R . . C75 C -0.1580(9) 0.3141(7) -0.5122(8) 0.050(4) Uani 1 1 d . . . H75 H -0.1755 0.3029 -0.5551 0.060 Uiso 1 1 calc R . . C76 C -0.2121(8) 0.3005(5) -0.4731(6) 0.026(3) Uani 1 1 d . . . H76 H -0.2671 0.2804 -0.4908 0.031 Uiso 1 1 calc R . . C81 C -0.4488(7) 0.3308(6) -0.5729(6) 0.027(3) Uani 1 1 d . . . C82 C -0.4517(7) 0.2711(7) -0.6117(6) 0.032(3) Uani 1 1 d . . . H82 H -0.4634 0.2259 -0.5976 0.039 Uiso 1 1 calc R . . C83 C -0.4371(8) 0.2781(8) -0.6725(7) 0.049(4) Uani 1 1 d . . . H83 H -0.4384 0.2380 -0.6982 0.059 Uiso 1 1 calc R . . C84 C -0.4205(7) 0.3468(8) -0.6928(7) 0.040(4) Uani 1 1 d . . . H84 H -0.4097 0.3522 -0.7323 0.048 Uiso 1 1 calc R . . C85 C -0.4200(8) 0.4052(8) -0.6561(8) 0.049(4) Uani 1 1 d . . . H85 H -0.4112 0.4506 -0.6713 0.059 Uiso 1 1 calc R . . C86 C -0.4328(8) 0.3981(7) -0.5942(7) 0.040(4) Uani 1 1 d . . . H86 H -0.4304 0.4385 -0.5685 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0314(5) 0.0393(5) 0.0276(6) 0.0022(4) 0.0048(4) -0.0023(4) I2 0.0300(5) 0.0384(5) 0.0379(6) -0.0031(4) 0.0096(4) -0.0028(4) I3 0.0384(5) 0.0302(5) 0.0438(7) 0.0030(4) 0.0152(5) 0.0018(4) I4 0.0349(5) 0.0315(5) 0.0296(6) 0.0020(4) 0.0033(4) -0.0018(4) Sn1 0.0255(5) 0.0319(5) 0.0216(6) 0.0048(4) 0.0084(4) 0.0027(4) Sn2 0.0252(5) 0.0278(5) 0.0233(6) 0.0010(4) 0.0099(4) -0.0015(4) Sn3 0.0253(5) 0.0265(5) 0.0202(5) -0.0002(4) 0.0078(4) 0.0001(4) Sn4 0.0220(5) 0.0319(5) 0.0230(6) 0.0008(4) 0.0078(4) 0.0016(4) Sn5 0.0245(5) 0.0300(5) 0.0266(6) 0.0039(4) 0.0098(4) 0.0037(4) Sn6 0.0233(5) 0.0268(5) 0.0211(6) -0.0015(4) 0.0073(4) -0.0011(4) Sn7 0.0215(5) 0.0248(5) 0.0215(6) 0.0005(4) 0.0068(4) -0.0004(4) Sn8 0.0230(5) 0.0313(5) 0.0202(6) 0.0030(4) 0.0060(4) 0.0021(4) O1 0.027(5) 0.020(4) 0.017(5) 0.003(4) 0.000(4) 0.004(4) O2 0.023(4) 0.015(4) 0.027(5) -0.002(4) 0.008(4) -0.005(3) O3 0.025(5) 0.035(5) 0.019(5) 0.006(4) 0.001(4) 0.000(4) O4 0.019(4) 0.032(5) 0.020(5) 0.005(4) -0.003(4) 0.006(4) O5 0.015(4) 0.012(4) 0.021(5) 0.004(3) -0.007(4) 0.006(3) O6 0.020(4) 0.029(4) 0.007(5) 0.010(4) -0.005(4) 0.007(3) O7 0.020(4) 0.017(4) 0.025(5) 0.008(4) 0.001(4) 0.006(3) O8 0.035(5) 0.019(4) 0.011(5) 0.000(4) 0.002(4) 0.009(4) C1 0.017(7) 0.051(8) 0.014(8) 0.008(6) -0.005(6) 0.011(6) C2 0.021(7) 0.024(6) 0.015(7) -0.004(5) 0.008(6) -0.004(5) C3 0.022(7) 0.032(7) 0.012(7) 0.000(5) 0.012(6) -0.004(5) C4 0.028(7) 0.031(7) 0.028(9) 0.006(6) 0.006(6) 0.016(6) C11 0.015(7) 0.033(8) 0.012(8) 0.000(6) -0.013(5) 0.004(6) C12 0.039(8) 0.046(9) 0.018(9) 0.006(7) 0.003(7) 0.005(7) C13 0.038(8) 0.036(8) 0.026(10) 0.013(7) 0.001(7) 0.002(7) C14 0.042(9) 0.047(10) 0.044(11) 0.012(8) 0.022(8) -0.012(8) C15 0.024(7) 0.046(9) 0.026(9) -0.012(7) 0.006(7) -0.007(6) C16 0.015(7) 0.029(8) 0.037(10) 0.004(7) -0.005(6) -0.014(6) C21 0.038(9) 0.033(8) 0.030(9) -0.008(7) 0.019(7) 0.000(7) C22 0.028(8) 0.048(9) 0.036(10) 0.002(8) 0.012(7) -0.002(7) C23 0.034(9) 0.046(9) 0.033(10) 0.008(7) 0.009(7) -0.006(7) C24 0.060(11) 0.043(9) 0.049(11) 0.003(8) 0.039(9) -0.009(8) C25 0.023(8) 0.041(9) 0.069(12) 0.009(8) 0.023(8) 0.005(7) C26 0.034(8) 0.031(8) 0.048(10) 0.010(7) 0.025(7) -0.004(7) C31 0.025(8) 0.033(8) 0.017(8) -0.004(6) -0.002(6) 0.000(6) C32 0.036(8) 0.025(7) 0.035(10) 0.007(7) 0.020(7) 0.008(6) C33 0.044(9) 0.055(9) 0.012(8) -0.011(7) 0.005(7) 0.007(8) C34 0.044(10) 0.076(11) 0.026(10) -0.015(8) 0.017(8) 0.001(8) C35 0.034(8) 0.054(9) 0.033(10) 0.014(8) 0.013(8) 0.002(7) C36 0.041(9) 0.048(9) 0.035(10) -0.017(7) 0.015(7) -0.006(7) C41 0.028(8) 0.026(7) 0.026(9) 0.008(6) 0.005(6) 0.004(6) C42 0.036(8) 0.035(8) 0.026(9) -0.009(6) -0.004(7) 0.013(7) C43 0.043(9) 0.057(10) 0.037(10) 0.000(8) 0.026(8) 0.012(8) C44 0.030(9) 0.064(10) 0.051(11) 0.000(8) 0.026(8) 0.020(8) C45 0.064(11) 0.036(8) 0.047(11) -0.013(7) 0.034(9) -0.002(8) C46 0.033(8) 0.037(8) 0.030(9) 0.000(7) 0.018(7) -0.009(6) C51 0.026(8) 0.027(8) 0.045(10) 0.004(7) 0.014(7) 0.004(6) C52 0.043(9) 0.032(8) 0.045(11) 0.003(7) 0.007(8) -0.011(7) C53 0.027(9) 0.047(9) 0.077(13) -0.017(9) 0.025(9) 0.008(7) C54 0.020(8) 0.055(10) 0.048(11) 0.001(8) 0.016(7) 0.012(8) C55 0.037(9) 0.047(9) 0.028(9) -0.013(7) 0.017(7) -0.018(7) C56 0.037(8) 0.031(8) 0.041(10) -0.002(7) 0.011(7) 0.008(7) C61 0.032(8) 0.030(8) 0.032(9) 0.005(6) 0.013(7) -0.006(6) C62 0.049(10) 0.034(8) 0.027(9) 0.003(7) 0.010(7) 0.005(7) C63 0.049(10) 0.063(11) 0.047(12) -0.002(9) 0.035(9) 0.001(9) C64 0.061(11) 0.036(9) 0.053(12) 0.003(8) 0.049(10) 0.013(8) C65 0.063(12) 0.038(9) 0.047(12) 0.001(8) 0.012(9) -0.003(8) C66 0.054(9) 0.028(8) 0.028(9) 0.007(7) 0.018(8) 0.008(7) C71 0.004(6) 0.044(8) 0.029(9) 0.012(7) 0.002(6) 0.003(6) C72 0.032(8) 0.053(9) 0.034(10) 0.003(7) 0.010(7) 0.010(7) C73 0.030(9) 0.054(10) 0.072(14) 0.015(10) 0.023(9) 0.002(7) C74 0.051(11) 0.059(11) 0.065(14) 0.022(10) 0.034(10) 0.008(9) C75 0.047(10) 0.057(10) 0.059(12) 0.012(8) 0.039(9) 0.013(8) C76 0.036(8) 0.017(7) 0.023(8) 0.004(6) 0.007(7) 0.000(6) C81 0.016(7) 0.026(7) 0.038(9) 0.003(7) 0.006(6) 0.000(6) C82 0.034(8) 0.047(9) 0.020(9) -0.002(7) 0.014(7) 0.003(7) C83 0.047(9) 0.054(10) 0.045(11) -0.017(8) 0.011(8) 0.021(8) C84 0.017(7) 0.065(11) 0.041(10) 0.005(9) 0.012(7) -0.007(7) C85 0.053(10) 0.043(10) 0.053(12) 0.021(9) 0.017(9) 0.012(8) C86 0.045(9) 0.043(9) 0.037(10) 0.011(7) 0.018(8) 0.001(7) _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 I1 Sn1 2.8861(11) . Y I1 O8 3.514(7) 4_666 Y I1 Sn3 4.0800(12) . Y I1 I3 4.1296(11) 2_454 Y I2 Sn4 2.8829(12) . Y I2 Sn2 4.1862(12) . Y I3 Sn5 2.8951(12) . Y I3 Sn6 3.9748(12) . Y I4 Sn8 2.9026(11) . Y I4 Sn7 3.9574(11) . Y I4 I4 4.2017(16) 3_464 Y Sn1 O1 2.028(7) . Y Sn1 C1 2.122(11) . Y Sn1 C11 2.126(12) . Y Sn1 O3 2.181(7) . Y Sn2 O1 2.043(7) . Y Sn2 C2 2.105(11) . Y Sn2 O2 2.135(6) . Y Sn2 C21 2.139(12) . Y Sn2 O3 2.196(7) . Y Sn3 O2 2.067(7) . Y Sn3 C31 2.128(12) . Y Sn3 C3 2.135(10) . Y Sn3 O1 2.147(6) . Y Sn3 O4 2.180(7) . Y Sn4 O2 2.058(7) . Y Sn4 C4 2.121(12) . Y Sn4 C41 2.132(12) . Y Sn4 O4 2.197(7) . Y Sn5 O5 2.025(6) . Y Sn5 C1 2.116(11) . Y Sn5 C51 2.124(12) . Y Sn5 O7 2.155(6) . Y Sn6 O6 2.036(7) . Y Sn6 C2 2.124(10) . Y Sn6 O5 2.131(7) . Y Sn6 C61 2.136(13) . Y Sn6 O8 2.148(7) . Y Sn7 O5 2.075(6) . Y Sn7 C71 2.103(11) . Y Sn7 C3 2.106(10) . Y Sn7 O6 2.147(7) . Y Sn7 O7 2.160(7) . Y Sn8 O6 2.030(6) . Y Sn8 C4 2.116(10) . Y Sn8 C81 2.133(13) . Y Sn8 O8 2.162(6) . Y C11 C12 1.379(14) . ? C11 C16 1.394(15) . ? C12 C13 1.374(17) . ? C13 C14 1.352(17) . ? C14 C15 1.359(15) . ? C15 C16 1.392(16) . ? C21 C22 1.374(16) . ? C21 C26 1.375(15) . ? C22 C23 1.374(16) . ? C23 C24 1.379(16) . ? C24 C25 1.365(17) . ? C25 C26 1.412(16) . ? C31 C36 1.365(15) . ? C31 C32 1.366(15) . ? C32 C33 1.385(16) . ? C33 C34 1.339(16) . ? C34 C35 1.329(17) . ? C35 C36 1.426(17) . ? C41 C46 1.373(15) . ? C41 C42 1.383(15) . ? C42 C43 1.376(16) . ? C43 C44 1.386(16) . ? C44 C45 1.381(16) . ? C45 C46 1.355(15) . ? C51 C56 1.370(15) . ? C51 C52 1.380(15) . ? C52 C53 1.380(16) . ? C53 C54 1.389(17) . ? C54 C55 1.368(15) . ? C55 C56 1.396(15) . ? C61 C66 1.379(17) . ? C61 C62 1.409(15) . ? C62 C63 1.385(17) . ? C63 C64 1.330(18) . ? C64 C65 1.359(17) . ? C65 C66 1.374(17) . ? C71 C72 1.395(15) . ? C71 C76 1.416(16) . ? C72 C73 1.403(17) . ? C73 C74 1.369(19) . ? C74 C75 1.376(18) . ? C75 C76 1.385(16) . ? C81 C86 1.380(15) . ? C81 C82 1.389(15) . ? C82 C83 1.416(17) . ? C83 C84 1.397(17) . ? C84 C85 1.347(17) . ? C85 C86 1.430(18) . ? 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 Sn1 I1 O8 131.34(11) . 4_666 Y Sn1 I1 Sn3 66.57(3) . . Y O8 I1 Sn3 159.07(11) 4_666 . Y Sn1 I1 I3 135.44(3) . 2_454 Y O8 I1 I3 92.19(11) 4_666 2_454 Y Sn3 I1 I3 68.90(2) . 2_454 Y Sn4 I2 Sn2 66.00(3) . . Y Sn5 I3 Sn6 68.18(3) . . Y Sn8 I4 Sn7 68.00(2) . . Y Sn8 I4 I4 84.36(3) . 3_464 Y Sn7 I4 I4 151.97(3) . 3_464 Y O1 Sn1 C1 118.5(4) . . Y O1 Sn1 C11 114.2(4) . . Y C1 Sn1 C11 126.8(4) . . Y O1 Sn1 O3 75.2(3) . . Y C1 Sn1 O3 91.1(4) . . Y C11 Sn1 O3 95.2(4) . . Y O1 Sn1 I1 90.06(19) . . Y C1 Sn1 I1 92.3(3) . . Y C11 Sn1 I1 94.7(3) . . Y O3 Sn1 I1 164.62(19) . . Y O1 Sn2 C2 120.2(3) . . Y O1 Sn2 O2 74.4(3) . . Y C2 Sn2 O2 96.5(3) . . Y O1 Sn2 C21 109.7(4) . . Y C2 Sn2 C21 130.0(4) . . Y O2 Sn2 C21 98.5(4) . . Y O1 Sn2 O3 74.5(3) . . Y C2 Sn2 O3 97.9(4) . . Y O2 Sn2 O3 148.9(3) . . Y C21 Sn2 O3 93.0(4) . . Y O1 Sn2 I2 132.22(18) . . Y C2 Sn2 I2 64.3(3) . . Y O2 Sn2 I2 58.15(19) . . Y C21 Sn2 I2 84.4(4) . . Y O3 Sn2 I2 152.28(19) . . Y O2 Sn3 C31 107.1(4) . . Y O2 Sn3 C3 122.7(4) . . Y C31 Sn3 C3 130.2(4) . . Y O2 Sn3 O1 73.7(3) . . Y C31 Sn3 O1 98.8(4) . . Y C3 Sn3 O1 95.4(3) . . Y O2 Sn3 O4 75.2(3) . . Y C31 Sn3 O4 97.4(4) . . Y C3 Sn3 O4 95.0(4) . . Y O1 Sn3 O4 147.9(3) . . Y O2 Sn3 I1 133.54(18) . . Y C31 Sn3 I1 81.8(3) . . Y C3 Sn3 I1 65.1(3) . . Y O1 Sn3 I1 59.84(18) . . Y O4 Sn3 I1 150.45(18) . . Y O2 Sn4 C4 120.8(3) . . Y O2 Sn4 C41 112.1(4) . . Y C4 Sn4 C41 125.8(4) . . Y O2 Sn4 O4 74.9(2) . . Y C4 Sn4 O4 90.8(4) . . Y C41 Sn4 O4 91.8(4) . . Y O2 Sn4 I2 90.49(18) . . Y C4 Sn4 I2 92.5(3) . . Y C41 Sn4 I2 98.5(3) . . Y O4 Sn4 I2 164.59(17) . . Y O5 Sn5 C1 119.5(3) . . Y O5 Sn5 C51 115.5(4) . . Y C1 Sn5 C51 124.7(4) . . Y O5 Sn5 O7 74.0(2) . . Y C1 Sn5 O7 93.5(4) . . Y C51 Sn5 O7 95.9(4) . . Y O5 Sn5 I3 87.30(18) . . Y C1 Sn5 I3 92.0(3) . . Y C51 Sn5 I3 95.9(3) . . Y O7 Sn5 I3 160.86(18) . . Y O6 Sn6 C2 120.6(3) . . Y O6 Sn6 O5 74.7(2) . . Y C2 Sn6 O5 100.3(3) . . Y O6 Sn6 C61 115.9(4) . . Y C2 Sn6 C61 123.1(4) . . Y O5 Sn6 C61 100.4(4) . . Y O6 Sn6 O8 72.1(3) . . Y C2 Sn6 O8 96.6(3) . . Y O5 Sn6 O8 146.8(2) . . Y C61 Sn6 O8 93.8(4) . . Y O6 Sn6 I3 134.90(18) . . Y C2 Sn6 I3 69.2(3) . . Y O5 Sn6 I3 60.23(17) . . Y C61 Sn6 I3 76.7(3) . . Y O8 Sn6 I3 152.90(18) . . Y O5 Sn7 C71 108.5(4) . . Y O5 Sn7 C3 123.3(3) . . Y C71 Sn7 C3 128.0(4) . . Y O5 Sn7 O6 73.6(2) . . Y C71 Sn7 O6 99.4(4) . . Y C3 Sn7 O6 99.4(3) . . Y O5 Sn7 O7 72.9(2) . . Y C71 Sn7 O7 92.5(3) . . Y C3 Sn7 O7 97.5(4) . . Y O6 Sn7 O7 146.5(2) . . Y O5 Sn7 I4 135.52(18) . . Y C71 Sn7 I4 79.6(3) . . Y C3 Sn7 I4 67.8(3) . . Y O6 Sn7 I4 61.94(18) . . Y O7 Sn7 I4 151.52(17) . . Y O6 Sn8 C4 117.1(4) . . Y O6 Sn8 C81 113.1(3) . . Y C4 Sn8 C81 129.3(4) . . Y O6 Sn8 O8 71.9(3) . . Y C4 Sn8 O8 93.0(4) . . Y C81 Sn8 O8 95.8(4) . . Y O6 Sn8 I4 88.7(2) . . Y C4 Sn8 I4 92.1(3) . . Y C81 Sn8 I4 95.8(3) . . Y O8 Sn8 I4 160.16(19) . . Y Sn1 O1 Sn2 110.1(3) . . Y Sn1 O1 Sn3 142.3(4) . . Y Sn2 O1 Sn3 105.9(3) . . Y Sn4 O2 Sn3 109.2(3) . . Y Sn4 O2 Sn2 145.3(3) . . Y Sn3 O2 Sn2 105.5(3) . . Y Sn1 O3 Sn2 99.4(3) . . Y Sn3 O4 Sn4 100.4(3) . . Y Sn5 O5 Sn7 110.4(3) . . Y Sn5 O5 Sn6 144.1(3) . . Y Sn7 O5 Sn6 105.4(3) . . Y Sn8 O6 Sn6 112.3(3) . . Y Sn8 O6 Sn7 140.7(3) . . Y Sn6 O6 Sn7 106.2(3) . . Y Sn5 O7 Sn7 102.5(3) . . Y Sn6 O8 Sn8 103.2(3) . . Y Sn5 C1 Sn1 116.2(5) . . Y Sn2 C2 Sn6 118.3(5) . . Y Sn7 C3 Sn3 117.7(5) . . Y Sn8 C4 Sn4 117.7(5) . . Y C12 C11 C16 118.3(12) . . ? C12 C11 Sn1 121.0(9) . . ? C16 C11 Sn1 120.3(9) . . ? C13 C12 C11 121.2(12) . . ? C14 C13 C12 119.1(13) . . ? C13 C14 C15 122.1(14) . . ? C14 C15 C16 119.0(12) . . ? C15 C16 C11 120.0(11) . . ? C22 C21 C26 119.9(12) . . ? C22 C21 Sn2 119.7(9) . . ? C26 C21 Sn2 120.1(10) . . ? C21 C22 C23 120.9(12) . . ? C22 C23 C24 119.1(13) . . ? C25 C24 C23 121.6(13) . . ? C24 C25 C26 118.7(12) . . ? C21 C26 C25 119.8(12) . . ? C36 C31 C32 118.6(12) . . ? C36 C31 Sn3 117.2(9) . . ? C32 C31 Sn3 124.2(9) . . ? C31 C32 C33 119.6(12) . . ? C34 C33 C32 121.8(13) . . ? C35 C34 C33 120.3(14) . . ? C34 C35 C36 119.4(12) . . ? C31 C36 C35 120.2(13) . . ? C46 C41 C42 117.5(11) . . ? C46 C41 Sn4 120.3(9) . . ? C42 C41 Sn4 122.3(9) . . ? C43 C42 C41 121.4(12) . . ? C42 C43 C44 120.3(12) . . ? C45 C44 C43 117.8(12) . . ? C46 C45 C44 121.4(12) . . ? C45 C46 C41 121.7(11) . . ? C56 C51 C52 116.5(11) . . ? C56 C51 Sn5 122.8(9) . . ? C52 C51 Sn5 120.6(9) . . ? C51 C52 C53 123.4(12) . . ? C52 C53 C54 118.8(12) . . ? C55 C54 C53 119.1(12) . . ? C54 C55 C56 120.3(12) . . ? C51 C56 C55 121.7(11) . . ? C66 C61 C62 119.2(12) . . ? C66 C61 Sn6 119.3(9) . . ? C62 C61 Sn6 121.5(10) . . ? C63 C62 C61 120.1(13) . . ? C64 C63 C62 118.7(14) . . ? C63 C64 C65 122.4(14) . . ? C64 C65 C66 120.9(14) . . ? C65 C66 C61 118.6(13) . . ? C72 C71 C76 117.6(11) . . ? C72 C71 Sn7 121.7(10) . . ? C76 C71 Sn7 120.5(8) . . ? C71 C72 C73 119.7(13) . . ? C74 C73 C72 120.3(14) . . ? C73 C74 C75 122.1(15) . . ? C74 C75 C76 117.7(15) . . ? C75 C76 C71 122.5(12) . . ? C86 C81 C82 119.5(12) . . ? C86 C81 Sn8 121.3(9) . . ? C82 C81 Sn8 118.9(9) . . ? C81 C82 C83 121.1(12) . . ? C84 C83 C82 118.3(12) . . ? C85 C84 C83 121.0(14) . . ? C84 C85 C86 120.8(13) . . ? C81 C86 C85 119.3(13) . . ? 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 O8 I1 Sn1 O1 172.4(3) 4_666 . . . ? Sn3 I1 Sn1 O1 5.3(2) . . . . ? I3 I1 Sn1 O1 7.3(2) 2_454 . . . ? O8 I1 Sn1 C1 -69.1(3) 4_666 . . . ? Sn3 I1 Sn1 C1 123.8(3) . . . . ? I3 I1 Sn1 C1 125.8(3) 2_454 . . . ? O8 I1 Sn1 C11 58.0(3) 4_666 . . . ? Sn3 I1 Sn1 C11 -109.0(3) . . . . ? I3 I1 Sn1 C11 -107.0(3) 2_454 . . . ? O8 I1 Sn1 O3 -171.9(8) 4_666 . . . ? Sn3 I1 Sn1 O3 21.1(7) . . . . ? I3 I1 Sn1 O3 23.1(8) 2_454 . . . ? Sn4 I2 Sn2 O1 -9.5(3) . . . . ? Sn4 I2 Sn2 C2 -118.0(3) . . . . ? Sn4 I2 Sn2 O2 -1.5(2) . . . . ? Sn4 I2 Sn2 C21 102.1(3) . . . . ? Sn4 I2 Sn2 O3 -172.0(4) . . . . ? Sn1 I1 Sn3 O2 -6.4(3) . . . . ? O8 I1 Sn3 O2 -158.3(4) 4_666 . . . ? I3 I1 Sn3 O2 175.1(3) 2_454 . . . ? Sn1 I1 Sn3 C31 99.4(3) . . . . ? O8 I1 Sn3 C31 -52.5(4) 4_666 . . . ? I3 I1 Sn3 C31 -79.1(3) 2_454 . . . ? Sn1 I1 Sn3 C3 -118.7(3) . . . . ? O8 I1 Sn3 C3 89.3(4) 4_666 . . . ? I3 I1 Sn3 C3 62.8(3) 2_454 . . . ? Sn1 I1 Sn3 O1 -5.8(2) . . . . ? O8 I1 Sn3 O1 -157.7(4) 4_666 . . . ? I3 I1 Sn3 O1 175.7(2) 2_454 . . . ? Sn1 I1 Sn3 O4 -170.1(4) . . . . ? O8 I1 Sn3 O4 38.0(5) 4_666 . . . ? I3 I1 Sn3 O4 11.5(4) 2_454 . . . ? Sn2 I2 Sn4 O2 1.4(2) . . . . ? Sn2 I2 Sn4 C4 122.2(3) . . . . ? Sn2 I2 Sn4 C41 -111.0(3) . . . . ? Sn2 I2 Sn4 O4 20.2(8) . . . . ? Sn6 I3 Sn5 O5 2.2(2) . . . . ? Sn6 I3 Sn5 C1 121.6(3) . . . . ? Sn6 I3 Sn5 C51 -113.1(4) . . . . ? Sn6 I3 Sn5 O7 14.8(6) . . . . ? Sn5 I3 Sn6 O6 -5.4(3) . . . . ? Sn5 I3 Sn6 C2 -118.4(3) . . . . ? Sn5 I3 Sn6 O5 -2.4(2) . . . . ? Sn5 I3 Sn6 C61 108.0(3) . . . . ? Sn5 I3 Sn6 O8 179.8(4) . . . . ? Sn8 I4 Sn7 O5 -3.3(3) . . . . ? I4 I4 Sn7 O5 -13.5(3) 3_464 . . . ? Sn8 I4 Sn7 C71 102.6(3) . . . . ? I4 I4 Sn7 C71 92.4(4) 3_464 . . . ? Sn8 I4 Sn7 C3 -118.8(3) . . . . ? I4 I4 Sn7 C3 -128.9(3) 3_464 . . . ? Sn8 I4 Sn7 O6 -4.1(2) . . . . ? I4 I4 Sn7 O6 -14.2(2) 3_464 . . . ? Sn8 I4 Sn7 O7 178.5(4) . . . . ? I4 I4 Sn7 O7 168.3(4) 3_464 . . . ? Sn7 I4 Sn8 O6 3.8(2) . . . . ? I4 I4 Sn8 O6 179.1(2) 3_464 . . . ? Sn7 I4 Sn8 C4 120.9(3) . . . . ? I4 I4 Sn8 C4 -63.9(3) 3_464 . . . ? Sn7 I4 Sn8 C81 -109.2(3) . . . . ? I4 I4 Sn8 C81 66.0(3) 3_464 . . . ? Sn7 I4 Sn8 O8 16.1(6) . . . . ? I4 I4 Sn8 O8 -168.7(6) 3_464 . . . ? C1 Sn1 O1 Sn2 90.4(5) . . . . ? C11 Sn1 O1 Sn2 -81.8(5) . . . . ? O3 Sn1 O1 Sn2 7.3(3) . . . . ? I1 Sn1 O1 Sn2 -177.0(3) . . . . ? C1 Sn1 O1 Sn3 -107.9(7) . . . . ? C11 Sn1 O1 Sn3 79.9(7) . . . . ? O3 Sn1 O1 Sn3 169.0(7) . . . . ? I1 Sn1 O1 Sn3 -15.3(6) . . . . ? C2 Sn2 O1 Sn1 -97.5(5) . . . . ? O2 Sn2 O1 Sn1 174.1(4) . . . . ? C21 Sn2 O1 Sn1 80.4(5) . . . . ? O3 Sn2 O1 Sn1 -7.2(3) . . . . ? I2 Sn2 O1 Sn1 -178.87(12) . . . . ? C2 Sn2 O1 Sn3 94.0(4) . . . . ? O2 Sn2 O1 Sn3 5.6(3) . . . . ? C21 Sn2 O1 Sn3 -88.1(5) . . . . ? O3 Sn2 O1 Sn3 -175.7(4) . . . . ? I2 Sn2 O1 Sn3 12.6(5) . . . . ? O2 Sn3 O1 Sn1 -168.0(7) . . . . ? C31 Sn3 O1 Sn1 -62.7(7) . . . . ? C3 Sn3 O1 Sn1 69.5(7) . . . . ? O4 Sn3 O1 Sn1 177.9(5) . . . . ? I1 Sn3 O1 Sn1 12.5(5) . . . . ? O2 Sn3 O1 Sn2 -5.8(3) . . . . ? C31 Sn3 O1 Sn2 99.5(4) . . . . ? C3 Sn3 O1 Sn2 -128.4(4) . . . . ? O4 Sn3 O1 Sn2 -20.0(7) . . . . ? I1 Sn3 O1 Sn2 174.6(4) . . . . ? C4 Sn4 O2 Sn3 85.8(5) . . . . ? C41 Sn4 O2 Sn3 -81.7(5) . . . . ? O4 Sn4 O2 Sn3 4.0(3) . . . . ? I2 Sn4 O2 Sn3 178.9(3) . . . . ? C4 Sn4 O2 Sn2 -97.4(7) . . . . ? C41 Sn4 O2 Sn2 95.1(7) . . . . ? O4 Sn4 O2 Sn2 -179.2(7) . . . . ? I2 Sn4 O2 Sn2 -4.3(6) . . . . ? C31 Sn3 O2 Sn4 89.2(4) . . . . ? C3 Sn3 O2 Sn4 -90.5(5) . . . . ? O1 Sn3 O2 Sn4 -176.4(4) . . . . ? O4 Sn3 O2 Sn4 -4.1(3) . . . . ? I1 Sn3 O2 Sn4 -175.82(10) . . . . ? C31 Sn3 O2 Sn2 -88.9(4) . . . . ? C3 Sn3 O2 Sn2 91.4(4) . . . . ? O1 Sn3 O2 Sn2 5.6(3) . . . . ? O4 Sn3 O2 Sn2 177.8(4) . . . . ? I1 Sn3 O2 Sn2 6.1(4) . . . . ? O1 Sn2 O2 Sn4 177.3(7) . . . . ? C2 Sn2 O2 Sn4 57.7(7) . . . . ? C21 Sn2 O2 Sn4 -74.5(7) . . . . ? O3 Sn2 O2 Sn4 174.9(5) . . . . ? I2 Sn2 O2 Sn4 3.5(5) . . . . ? O1 Sn2 O2 Sn3 -5.8(3) . . . . ? C2 Sn2 O2 Sn3 -125.5(4) . . . . ? C21 Sn2 O2 Sn3 102.4(4) . . . . ? O3 Sn2 O2 Sn3 -8.3(7) . . . . ? I2 Sn2 O2 Sn3 -179.7(4) . . . . ? O1 Sn1 O3 Sn2 -6.4(3) . . . . ? C1 Sn1 O3 Sn2 -125.6(4) . . . . ? C11 Sn1 O3 Sn2 107.3(4) . . . . ? I1 Sn1 O3 Sn2 -22.7(9) . . . . ? O1 Sn2 O3 Sn1 6.4(3) . . . . ? C2 Sn2 O3 Sn1 125.7(3) . . . . ? O2 Sn2 O3 Sn1 8.9(7) . . . . ? C21 Sn2 O3 Sn1 -103.2(4) . . . . ? I2 Sn2 O3 Sn1 173.01(16) . . . . ? O2 Sn3 O4 Sn4 3.7(3) . . . . ? C31 Sn3 O4 Sn4 -102.1(4) . . . . ? C3 Sn3 O4 Sn4 126.2(4) . . . . ? O1 Sn3 O4 Sn4 17.7(6) . . . . ? I1 Sn3 O4 Sn4 171.48(14) . . . . ? O2 Sn4 O4 Sn3 -3.7(3) . . . . ? C4 Sn4 O4 Sn3 -125.5(4) . . . . ? C41 Sn4 O4 Sn3 108.7(4) . . . . ? I2 Sn4 O4 Sn3 -23.2(10) . . . . ? C1 Sn5 O5 Sn7 88.1(5) . . . . ? C51 Sn5 O5 Sn7 -85.9(5) . . . . ? O7 Sn5 O5 Sn7 3.1(3) . . . . ? I3 Sn5 O5 Sn7 178.8(3) . . . . ? C1 Sn5 O5 Sn6 -97.4(7) . . . . ? C51 Sn5 O5 Sn6 88.7(7) . . . . ? O7 Sn5 O5 Sn6 177.7(7) . . . . ? I3 Sn5 O5 Sn6 -6.6(6) . . . . ? C71 Sn7 O5 Sn5 83.8(5) . . . . ? C3 Sn7 O5 Sn5 -90.9(5) . . . . ? O6 Sn7 O5 Sn5 178.5(4) . . . . ? O7 Sn7 O5 Sn5 -3.1(3) . . . . ? I4 Sn7 O5 Sn5 177.79(10) . . . . ? C71 Sn7 O5 Sn6 -92.9(4) . . . . ? C3 Sn7 O5 Sn6 92.4(5) . . . . ? O6 Sn7 O5 Sn6 1.8(3) . . . . ? O7 Sn7 O5 Sn6 -179.8(4) . . . . ? I4 Sn7 O5 Sn6 1.1(5) . . . . ? O6 Sn6 O5 Sn5 -176.6(7) . . . . ? C2 Sn6 O5 Sn5 64.2(7) . . . . ? C61 Sn6 O5 Sn5 -62.4(7) . . . . ? O8 Sn6 O5 Sn5 -176.3(5) . . . . ? I3 Sn6 O5 Sn5 5.5(5) . . . . ? O6 Sn6 O5 Sn7 -1.9(3) . . . . ? C2 Sn6 O5 Sn7 -121.0(4) . . . . ? C61 Sn6 O5 Sn7 112.3(4) . . . . ? O8 Sn6 O5 Sn7 -1.6(7) . . . . ? I3 Sn6 O5 Sn7 -179.8(4) . . . . ? C4 Sn8 O6 Sn6 89.4(5) . . . . ? C81 Sn8 O6 Sn6 -83.1(5) . . . . ? O8 Sn8 O6 Sn6 5.5(3) . . . . ? I4 Sn8 O6 Sn6 -178.8(3) . . . . ? C4 Sn8 O6 Sn7 -102.1(6) . . . . ? C81 Sn8 O6 Sn7 85.4(7) . . . . ? O8 Sn8 O6 Sn7 174.0(6) . . . . ? I4 Sn8 O6 Sn7 -10.4(5) . . . . ? C2 Sn6 O6 Sn8 -92.6(5) . . . . ? O5 Sn6 O6 Sn8 174.3(4) . . . . ? C61 Sn6 O6 Sn8 80.0(5) . . . . ? O8 Sn6 O6 Sn8 -5.5(3) . . . . ? I3 Sn6 O6 Sn8 176.92(11) . . . . ? C2 Sn6 O6 Sn7 95.0(4) . . . . ? O5 Sn6 O6 Sn7 1.9(3) . . . . ? C61 Sn6 O6 Sn7 -92.5(5) . . . . ? O8 Sn6 O6 Sn7 -178.0(4) . . . . ? I3 Sn6 O6 Sn7 4.5(5) . . . . ? O5 Sn7 O6 Sn8 -170.8(6) . . . . ? C71 Sn7 O6 Sn8 -64.2(6) . . . . ? C3 Sn7 O6 Sn8 67.1(6) . . . . ? O7 Sn7 O6 Sn8 -173.6(4) . . . . ? I4 Sn7 O6 Sn8 8.6(4) . . . . ? O5 Sn7 O6 Sn6 -1.9(3) . . . . ? C71 Sn7 O6 Sn6 104.7(4) . . . . ? C3 Sn7 O6 Sn6 -124.0(4) . . . . ? O7 Sn7 O6 Sn6 -4.7(6) . . . . ? I4 Sn7 O6 Sn6 177.5(4) . . . . ? O5 Sn5 O7 Sn7 -2.9(3) . . . . ? C1 Sn5 O7 Sn7 -122.5(4) . . . . ? C51 Sn5 O7 Sn7 112.0(4) . . . . ? I3 Sn5 O7 Sn7 -15.9(8) . . . . ? O5 Sn7 O7 Sn5 2.8(3) . . . . ? C71 Sn7 O7 Sn5 -105.7(4) . . . . ? C3 Sn7 O7 Sn5 125.4(4) . . . . ? O6 Sn7 O7 Sn5 5.6(6) . . . . ? I4 Sn7 O7 Sn5 -178.52(13) . . . . ? O6 Sn6 O8 Sn8 4.9(3) . . . . ? C2 Sn6 O8 Sn8 125.0(4) . . . . ? O5 Sn6 O8 Sn8 4.6(6) . . . . ? C61 Sn6 O8 Sn8 -111.0(4) . . . . ? I3 Sn6 O8 Sn8 -178.89(15) . . . . ? O6 Sn8 O8 Sn6 -5.0(3) . . . . ? C4 Sn8 O8 Sn6 -122.5(4) . . . . ? C81 Sn8 O8 Sn6 107.5(4) . . . . ? I4 Sn8 O8 Sn6 -17.9(8) . . . . ? O5 Sn5 C1 Sn1 -5.6(7) . . . . ? C51 Sn5 C1 Sn1 167.8(5) . . . . ? O7 Sn5 C1 Sn1 68.0(6) . . . . ? I3 Sn5 C1 Sn1 -93.6(5) . . . . ? O1 Sn1 C1 Sn5 -0.7(7) . . . . ? C11 Sn1 C1 Sn5 170.3(5) . . . . ? O3 Sn1 C1 Sn5 73.0(6) . . . . ? I1 Sn1 C1 Sn5 -92.0(5) . . . . ? O1 Sn2 C2 Sn6 -21.7(7) . . . . ? O2 Sn2 C2 Sn6 54.1(5) . . . . ? C21 Sn2 C2 Sn6 160.9(5) . . . . ? O3 Sn2 C2 Sn6 -98.3(5) . . . . ? I2 Sn2 C2 Sn6 104.0(5) . . . . ? O6 Sn6 C2 Sn2 -32.3(7) . . . . ? O5 Sn6 C2 Sn2 45.9(5) . . . . ? C61 Sn6 C2 Sn2 155.6(5) . . . . ? O8 Sn6 C2 Sn2 -105.4(5) . . . . ? I3 Sn6 C2 Sn2 98.4(5) . . . . ? O5 Sn7 C3 Sn3 -28.8(7) . . . . ? C71 Sn7 C3 Sn3 157.6(5) . . . . ? O6 Sn7 C3 Sn3 47.6(6) . . . . ? O7 Sn7 C3 Sn3 -103.3(5) . . . . ? I4 Sn7 C3 Sn3 102.0(5) . . . . ? O2 Sn3 C3 Sn7 -25.3(7) . . . . ? C31 Sn3 C3 Sn7 155.1(5) . . . . ? O1 Sn3 C3 Sn7 48.8(6) . . . . ? O4 Sn3 C3 Sn7 -100.9(5) . . . . ? I1 Sn3 C3 Sn7 101.9(5) . . . . ? O6 Sn8 C4 Sn4 -3.9(7) . . . . ? C81 Sn8 C4 Sn4 167.2(5) . . . . ? O8 Sn8 C4 Sn4 67.3(6) . . . . ? I4 Sn8 C4 Sn4 -93.5(5) . . . . ? O2 Sn4 C4 Sn8 -1.4(7) . . . . ? C41 Sn4 C4 Sn8 164.2(5) . . . . ? O4 Sn4 C4 Sn8 71.5(6) . . . . ? I2 Sn4 C4 Sn8 -93.5(5) . . . . ? O1 Sn1 C11 C12 129.9(8) . . . . ? C1 Sn1 C11 C12 -41.5(11) . . . . ? O3 Sn1 C11 C12 53.9(9) . . . . ? I1 Sn1 C11 C12 -137.9(9) . . . . ? O1 Sn1 C11 C16 -56.6(9) . . . . ? C1 Sn1 C11 C16 132.0(8) . . . . ? O3 Sn1 C11 C16 -132.6(8) . . . . ? I1 Sn1 C11 C16 35.6(8) . . . . ? C16 C11 C12 C13 -3.3(17) . . . . ? Sn1 C11 C12 C13 170.3(9) . . . . ? C11 C12 C13 C14 4.5(19) . . . . ? C12 C13 C14 C15 -1.7(19) . . . . ? C13 C14 C15 C16 -2.1(18) . . . . ? C14 C15 C16 C11 3.2(17) . . . . ? C12 C11 C16 C15 -0.6(16) . . . . ? Sn1 C11 C16 C15 -174.3(8) . . . . ? O1 Sn2 C21 C22 -64.7(10) . . . . ? C2 Sn2 C21 C22 112.9(10) . . . . ? O2 Sn2 C21 C22 -141.2(9) . . . . ? O3 Sn2 C21 C22 9.9(10) . . . . ? I2 Sn2 C21 C22 162.2(10) . . . . ? O1 Sn2 C21 C26 108.5(10) . . . . ? C2 Sn2 C21 C26 -73.9(11) . . . . ? O2 Sn2 C21 C26 32.0(10) . . . . ? O3 Sn2 C21 C26 -176.9(9) . . . . ? I2 Sn2 C21 C26 -24.5(9) . . . . ? C26 C21 C22 C23 -0.7(19) . . . . ? Sn2 C21 C22 C23 172.6(9) . . . . ? C21 C22 C23 C24 -0.4(19) . . . . ? C22 C23 C24 C25 1(2) . . . . ? C23 C24 C25 C26 0(2) . . . . ? C22 C21 C26 C25 1.5(18) . . . . ? Sn2 C21 C26 C25 -171.7(9) . . . . ? C24 C25 C26 C21 -1.3(19) . . . . ? O2 Sn3 C31 C36 -11.5(10) . . . . ? C3 Sn3 C31 C36 168.1(8) . . . . ? O1 Sn3 C31 C36 -87.1(9) . . . . ? O4 Sn3 C31 C36 65.2(9) . . . . ? I1 Sn3 C31 C36 -144.7(9) . . . . ? O2 Sn3 C31 C32 165.8(9) . . . . ? C3 Sn3 C31 C32 -14.6(12) . . . . ? O1 Sn3 C31 C32 90.2(10) . . . . ? O4 Sn3 C31 C32 -117.5(9) . . . . ? I1 Sn3 C31 C32 32.6(9) . . . . ? C36 C31 C32 C33 1.1(17) . . . . ? Sn3 C31 C32 C33 -176.1(8) . . . . ? C31 C32 C33 C34 -1.7(18) . . . . ? C32 C33 C34 C35 2(2) . . . . ? C33 C34 C35 C36 -2(2) . . . . ? C32 C31 C36 C35 -1.0(18) . . . . ? Sn3 C31 C36 C35 176.4(9) . . . . ? C34 C35 C36 C31 1.5(19) . . . . ? O2 Sn4 C41 C46 92.4(10) . . . . ? C4 Sn4 C41 C46 -74.3(11) . . . . ? O4 Sn4 C41 C46 18.0(10) . . . . ? I2 Sn4 C41 C46 -173.6(9) . . . . ? O2 Sn4 C41 C42 -88.9(10) . . . . ? C4 Sn4 C41 C42 104.4(10) . . . . ? O4 Sn4 C41 C42 -163.3(10) . . . . ? I2 Sn4 C41 C42 5.1(10) . . . . ? C46 C41 C42 C43 0.4(18) . . . . ? Sn4 C41 C42 C43 -178.3(9) . . . . ? C41 C42 C43 C44 0(2) . . . . ? C42 C43 C44 C45 -2(2) . . . . ? C43 C44 C45 C46 2(2) . . . . ? C44 C45 C46 C41 -1(2) . . . . ? C42 C41 C46 C45 0.0(18) . . . . ? Sn4 C41 C46 C45 178.7(10) . . . . ? O5 Sn5 C51 C56 49.1(12) . . . . ? C1 Sn5 C51 C56 -124.4(11) . . . . ? O7 Sn5 C51 C56 -26.0(11) . . . . ? I3 Sn5 C51 C56 139.0(11) . . . . ? O5 Sn5 C51 C52 -134.5(10) . . . . ? C1 Sn5 C51 C52 51.9(12) . . . . ? O7 Sn5 C51 C52 150.4(10) . . . . ? I3 Sn5 C51 C52 -44.7(11) . . . . ? C56 C51 C52 C53 0(2) . . . . ? Sn5 C51 C52 C53 -176.1(11) . . . . ? C51 C52 C53 C54 1(2) . . . . ? C52 C53 C54 C55 -4(2) . . . . ? C53 C54 C55 C56 6(2) . . . . ? C52 C51 C56 C55 1.7(19) . . . . ? Sn5 C51 C56 C55 178.2(9) . . . . ? C54 C55 C56 C51 -5(2) . . . . ? O6 Sn6 C61 C66 -106.4(9) . . . . ? C2 Sn6 C61 C66 65.9(11) . . . . ? O5 Sn6 C61 C66 175.6(9) . . . . ? O8 Sn6 C61 C66 -34.5(9) . . . . ? I3 Sn6 C61 C66 119.8(9) . . . . ? O6 Sn6 C61 C62 76.0(10) . . . . ? C2 Sn6 C61 C62 -111.7(9) . . . . ? O5 Sn6 C61 C62 -2.0(10) . . . . ? O8 Sn6 C61 C62 147.9(9) . . . . ? I3 Sn6 C61 C62 -57.8(9) . . . . ? C66 C61 C62 C63 0.1(18) . . . . ? Sn6 C61 C62 C63 177.7(9) . . . . ? C61 C62 C63 C64 0(2) . . . . ? C62 C63 C64 C65 -1(2) . . . . ? C63 C64 C65 C66 2(2) . . . . ? C64 C65 C66 C61 -1.7(19) . . . . ? C62 C61 C66 C65 0.7(18) . . . . ? Sn6 C61 C66 C65 -177.0(9) . . . . ? O5 Sn7 C71 C72 -117.6(9) . . . . ? C3 Sn7 C71 C72 56.8(11) . . . . ? O6 Sn7 C71 C72 166.7(9) . . . . ? O7 Sn7 C71 C72 -44.7(9) . . . . ? I4 Sn7 C71 C72 107.7(9) . . . . ? O5 Sn7 C71 C76 56.3(9) . . . . ? C3 Sn7 C71 C76 -129.4(9) . . . . ? O6 Sn7 C71 C76 -19.5(9) . . . . ? O7 Sn7 C71 C76 129.1(9) . . . . ? I4 Sn7 C71 C76 -78.4(8) . . . . ? C76 C71 C72 C73 -2.3(17) . . . . ? Sn7 C71 C72 C73 171.7(9) . . . . ? C71 C72 C73 C74 0.5(19) . . . . ? C72 C73 C74 C75 1(2) . . . . ? C73 C74 C75 C76 -1(2) . . . . ? C74 C75 C76 C71 -1.0(18) . . . . ? C72 C71 C76 C75 2.5(17) . . . . ? Sn7 C71 C76 C75 -171.6(8) . . . . ? O6 Sn8 C81 C86 -113.8(9) . . . . ? C4 Sn8 C81 C86 74.9(11) . . . . ? O8 Sn8 C81 C86 173.5(9) . . . . ? I4 Sn8 C81 C86 -22.7(10) . . . . ? O6 Sn8 C81 C82 71.3(9) . . . . ? C4 Sn8 C81 C82 -100.1(10) . . . . ? O8 Sn8 C81 C82 -1.5(9) . . . . ? I4 Sn8 C81 C82 162.4(8) . . . . ? C86 C81 C82 C83 1.0(18) . . . . ? Sn8 C81 C82 C83 176.0(9) . . . . ? C81 C82 C83 C84 -0.7(18) . . . . ? C82 C83 C84 C85 -1.2(19) . . . . ? C83 C84 C85 C86 3(2) . . . . ? C82 C81 C86 C85 0.4(18) . . . . ? Sn8 C81 C86 C85 -174.5(9) . . . . ? C84 C85 C86 C81 -2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.32 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.746 _refine_diff_density_min -0.971 _refine_diff_density_rms 0.233 data_(1u4THF) _database_code_CSD 178298 audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H84 I4 O12 Sn8' _chemical_formula_weight 2550.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_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 27.7234(13) _cell_length_b 20.1467(11) _cell_length_c 15.6854(10) _cell_angle_alpha 90.00 _cell_angle_beta 114.5854(17) _cell_angle_gamma 90.00 _cell_volume 7966.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 30090 _cell_measurement_theta_min 3.31 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not determined' _exptl_crystal_density_diffrn 2.126 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4800 _exptl_absorpt_coefficient_mu 4.068 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ; 3 sets at different \k-angles and 262 frames via \w-rotation (\D/\w=1\%) at two times 10s per frame ; _diffrn_detector_area_resol_mean '19 vertical, 18 horizontal' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 30090 _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_av_sigmaI/netI 0.0897 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6985 _reflns_number_gt 3892 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius KappaCCD' _computing_cell_refinement ; DENZO and SCALEPACK (Otwinowski & Minor, 1997) ; _computing_data_reduction ; DENZO and SCALEPACK (Otwinowski & Minor, 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0848P)^2^+60.2237P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6985 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1485 _refine_ls_R_factor_gt 0.0723 _refine_ls_wR_factor_ref 0.1878 _refine_ls_wR_factor_gt 0.1660 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.14157(4) -0.09058(6) -0.05326(10) 0.1039(5) Uani 1 1 d . A . I2 I -0.12554(4) -0.38983(5) -0.18830(8) 0.0816(4) Uani 1 1 d . A . Sn1 Sn 0.13654(3) -0.23373(5) -0.06253(7) 0.0585(3) Uani 1 1 d . . . Sn2 Sn 0.02474(4) -0.32129(5) -0.12487(7) 0.0562(3) Uani 1 1 d . . . Sn3 Sn -0.00801(3) -0.16068(4) -0.14147(7) 0.0526(3) Uani 1 1 d . . . Sn4 Sn -0.11897(3) -0.24847(5) -0.19542(7) 0.0563(3) Uani 1 1 d . . . O1 O 0.0570(3) -0.2271(4) -0.1116(5) 0.048(2) Uani 1 1 d . A . O2 O -0.0404(3) -0.2555(4) -0.1642(6) 0.048(2) Uani 1 1 d . A . O3 O 0.1064(3) -0.3338(4) -0.0903(6) 0.065(3) Uani 1 1 d . A . O4 O -0.0912(3) -0.1463(4) -0.1953(6) 0.060(2) Uani 1 1 d . A . C1 C 0.1720(5) -0.2404(7) -0.1594(10) 0.066(4) Uani 1 1 d . . . H1A H 0.1953 -0.2787 -0.1428 0.080 Uiso 1 1 calc R . . H1B H 0.1940 -0.2014 -0.1517 0.080 Uiso 1 1 calc R . . C2 C 0.0000 -0.3776(9) -0.2500 0.058(5) Uani 1 2 d S . . H2A H -0.0291 -0.4061 -0.2540 0.069 Uiso 0.50 1 calc PR . . H2B H 0.0291 -0.4061 -0.2460 0.069 Uiso 0.50 1 calc PR . . C3 C 0.0000 -0.1058(8) -0.2500 0.060(5) Uani 1 2 d S . . H3A H -0.0308 -0.0773 -0.2782 0.072 Uiso 0.50 1 calc PR . . H3B H 0.0308 -0.0773 -0.2218 0.072 Uiso 0.50 1 calc PR . . C11 C 0.1750(5) -0.2562(7) 0.0885(7) 0.045(5) Uani 0.70 1 d PG A 1 C12 C 0.1692(6) -0.3184(6) 0.1215(9) 0.075(7) Uani 0.70 1 d PG A 1 H12A H 0.1492 -0.3509 0.0797 0.090 Uiso 0.70 1 calc PR A 1 C13 C 0.1933(6) -0.3319(7) 0.2170(10) 0.079(7) Uani 0.70 1 d PG A 1 H13A H 0.1894 -0.3735 0.2391 0.095 Uiso 0.70 1 calc PR A 1 C14 C 0.2232(6) -0.2832(9) 0.2795(7) 0.075(7) Uani 0.70 1 d PG A 1 H14A H 0.2393 -0.2923 0.3434 0.090 Uiso 0.70 1 calc PR A 1 C15 C 0.2290(5) -0.2211(8) 0.2465(9) 0.080(9) Uani 0.70 1 d PG A 1 H15A H 0.2490 -0.1885 0.2883 0.095 Uiso 0.70 1 calc PR A 1 C16 C 0.2049(5) -0.2075(6) 0.1510(10) 0.052(5) Uani 0.70 1 d PG A 1 H16A H 0.2088 -0.1659 0.1289 0.062 Uiso 0.70 1 calc PR A 1 C21 C 0.0262(7) -0.3519(10) 0.0109(12) 0.046(7) Uani 0.50 1 d PG A 1 C22 C 0.0568(8) -0.4068(10) 0.0547(14) 0.074(9) Uani 0.50 1 d PG A 1 H22A H 0.0762 -0.4286 0.0270 0.088 Uiso 0.50 1 calc PR A 1 C23 C 0.0585(10) -0.4290(11) 0.1397(15) 0.13(2) Uani 0.50 1 d PG A 1 H23A H 0.0790 -0.4658 0.1690 0.159 Uiso 0.50 1 calc PR A 1 C24 C 0.0295(11) -0.3964(13) 0.1810(13) 0.123(17) Uani 0.50 1 d PG A 1 H24A H 0.0306 -0.4113 0.2380 0.148 Uiso 0.50 1 calc PR A 1 C25 C -0.0011(8) -0.3415(11) 0.1373(12) 0.082(11) Uani 0.50 1 d PG A 1 H25A H -0.0205 -0.3197 0.1650 0.098 Uiso 0.50 1 calc PR A 1 C26 C -0.0028(7) -0.3192(8) 0.0522(13) 0.061(8) Uani 0.50 1 d PG A 1 H26A H -0.0233 -0.2825 0.0230 0.073 Uiso 0.50 1 calc PR A 1 C31 C 0.0110(7) -0.1172(10) -0.0133(11) 0.056(8) Uani 0.50 1 d PG A 1 C32 C 0.0516(8) -0.1428(11) 0.0667(14) 0.092(14) Uani 0.50 1 d PG A 1 H32A H 0.0708 -0.1794 0.0622 0.110 Uiso 0.50 1 calc PR A 1 C33 C 0.0635(9) -0.1135(13) 0.1535(11) 0.114(14) Uani 0.50 1 d PG A 1 H33A H 0.0907 -0.1306 0.2070 0.137 Uiso 0.50 1 calc PR A 1 C34 C 0.0348(10) -0.0587(12) 0.1602(13) 0.102(13) Uani 0.50 1 d PG A 1 H34A H 0.0428 -0.0392 0.2182 0.122 Uiso 0.50 1 calc PR A 1 C35 C -0.0058(9) -0.0332(9) 0.0802(17) 0.100(12) Uani 0.50 1 d PG A 1 H35A H -0.0250 0.0035 0.0847 0.120 Uiso 0.50 1 calc PR A 1 C36 C -0.0177(6) -0.0624(9) -0.0065(14) 0.065(8) Uani 0.50 1 d PG A 1 H36A H -0.0449 -0.0453 -0.0601 0.078 Uiso 0.50 1 calc PR A 1 C41 C -0.1384(6) -0.2212(8) -0.0787(10) 0.048(5) Uani 0.70 1 d PG A 1 C42 C -0.1514(7) -0.2717(6) -0.0315(14) 0.102(9) Uani 0.70 1 d PG A 1 H42A H -0.1509 -0.3157 -0.0490 0.123 Uiso 0.70 1 calc PR A 1 C43 C -0.1653(8) -0.2564(9) 0.0418(13) 0.130(13) Uani 0.70 1 d PG A 1 H43A H -0.1740 -0.2902 0.0733 0.157 Uiso 0.70 1 calc PR A 1 C44 C -0.1662(8) -0.1906(11) 0.0679(12) 0.092(9) Uani 0.70 1 d PG A 1 H44A H -0.1755 -0.1804 0.1170 0.110 Uiso 0.70 1 calc PR A 1 C45 C -0.1532(8) -0.1402(8) 0.0208(13) 0.126(13) Uani 0.70 1 d PG A 1 H45A H -0.1537 -0.0962 0.0383 0.151 Uiso 0.70 1 calc PR A 1 C46 C -0.1393(7) -0.1554(7) -0.0525(12) 0.095(9) Uani 0.70 1 d PG A 1 H46A H -0.1306 -0.1217 -0.0840 0.114 Uiso 0.70 1 calc PR A 1 C11' C 0.1766(14) -0.2225(19) 0.077(2) 0.043(13) Uiso 0.30 1 d PG A 2 C12' C 0.1771(19) -0.2822(17) 0.122(3) 0.10(3) Uiso 0.30 1 d PG A 2 H12B H 0.1602 -0.3193 0.0866 0.119 Uiso 0.30 1 calc PR A 2 C13' C 0.203(3) -0.287(2) 0.219(3) 0.16(4) Uiso 0.30 1 d PG A 2 H13B H 0.2032 -0.3265 0.2487 0.191 Uiso 0.30 1 calc PR A 2 C14' C 0.228(2) -0.231(3) 0.271(2) 0.11(3) Uiso 0.30 1 d PG A 2 H14B H 0.2453 -0.2340 0.3361 0.138 Uiso 0.30 1 calc PR A 2 C15' C 0.2276(18) -0.171(2) 0.226(3) 0.10(2) Uiso 0.30 1 d PG A 2 H15B H 0.2445 -0.1343 0.2614 0.120 Uiso 0.30 1 calc PR A 2 C16' C 0.2018(17) -0.1671(17) 0.129(3) 0.09(2) Uiso 0.30 1 d PG A 2 H16B H 0.2015 -0.1271 0.0993 0.112 Uiso 0.30 1 calc PR A 2 C21' C 0.0238(12) -0.3702(17) -0.012(2) 0.104(18) Uiso 0.50 1 d PG A 2 C22' C 0.0252(11) -0.4390(17) -0.005(2) 0.121(14) Uiso 0.50 1 d PG A 2 H22B H 0.0243 -0.4648 -0.0548 0.145 Uiso 0.50 1 calc PR A 2 C23' C 0.0278(11) -0.4691(13) 0.076(3) 0.131(16) Uiso 0.50 1 d PG A 2 H23B H 0.0287 -0.5151 0.0813 0.158 Uiso 0.50 1 calc PR A 2 C24' C 0.0290(15) -0.430(2) 0.151(2) 0.15(3) Uiso 0.50 1 d PG A 2 H24B H 0.0308 -0.4505 0.2053 0.183 Uiso 0.50 1 calc PR A 2 C25' C 0.0277(15) -0.362(2) 0.143(3) 0.22(4) Uiso 0.50 1 d PG A 2 H25B H 0.0286 -0.3357 0.1931 0.264 Uiso 0.50 1 calc PR A 2 C26' C 0.0251(13) -0.3315(13) 0.062(3) 0.14(2) Uiso 0.50 1 d PG A 2 H26B H 0.0242 -0.2854 0.0570 0.169 Uiso 0.50 1 calc PR A 2 C31' C 0.0093(9) -0.1404(11) 0.0079(12) 0.052(9) Uiso 0.50 1 d PG A 2 C32' C 0.0514(8) -0.1711(10) 0.0803(15) 0.065(10) Uiso 0.50 1 d PG A 2 H32B H 0.0756 -0.1962 0.0672 0.079 Uiso 0.50 1 calc PR A 2 C33' C 0.0572(7) -0.1643(10) 0.1723(13) 0.071(9) Uiso 0.50 1 d PG A 2 H33B H 0.0854 -0.1848 0.2207 0.086 Uiso 0.50 1 calc PR A 2 C34' C 0.0209(8) -0.1268(10) 0.1918(12) 0.072(8) Uiso 0.50 1 d PG A 2 H34B H 0.0249 -0.1223 0.2534 0.087 Uiso 0.50 1 calc PR A 2 C35' C -0.0212(7) -0.0962(11) 0.1194(16) 0.104(12) Uiso 0.50 1 d PG A 2 H35B H -0.0454 -0.0711 0.1325 0.125 Uiso 0.50 1 calc PR A 2 C36' C -0.0270(7) -0.1030(11) 0.0274(13) 0.089(10) Uiso 0.50 1 d PG A 2 H36B H -0.0552 -0.0824 -0.0210 0.107 Uiso 0.50 1 calc PR A 2 C41' C -0.1313(15) -0.245(2) -0.071(3) 0.041(16) Uiso 0.30 1 d PG A 2 C42' C -0.1112(17) -0.2830(18) 0.010(3) 0.10(2) Uiso 0.30 1 d PG A 2 H42B H -0.0930 -0.3221 0.0114 0.122 Uiso 0.30 1 calc PR A 2 C43' C -0.118(2) -0.263(3) 0.089(3) 0.18(4) Uiso 0.30 1 d PG A 2 H43B H -0.1048 -0.2886 0.1430 0.217 Uiso 0.30 1 calc PR A 2 C44' C -0.145(2) -0.204(3) 0.087(3) 0.12(4) Uiso 0.30 1 d PG A 2 H44B H -0.1501 -0.1911 0.1394 0.147 Uiso 0.30 1 calc PR A 2 C45' C -0.1655(19) -0.166(2) 0.006(4) 0.10(2) Uiso 0.30 1 d PG A 2 H45B H -0.1837 -0.1271 0.0042 0.116 Uiso 0.30 1 calc PR A 2 C46' C -0.1585(15) -0.186(2) -0.073(3) 0.079(19) Uiso 0.30 1 d PG A 2 H46B H -0.1720 -0.1606 -0.1274 0.094 Uiso 0.30 1 calc PR A 2 O51 O -0.1498(7) -0.0424(9) -0.2049(13) 0.170(7) Uani 1 1 d . . . C52 C -0.1345(17) 0.029(2) -0.220(3) 0.272(19) Uiso 1 1 d . A . H52A H -0.1226 0.0556 -0.1632 0.326 Uiso 1 1 calc R . . H52B H -0.1079 0.0300 -0.2451 0.326 Uiso 1 1 calc R . . C53 C -0.1884(17) 0.051(2) -0.292(3) 0.28(2) Uiso 1 1 d . . . H53A H -0.1944 0.0360 -0.3540 0.336 Uiso 1 1 calc R A . H53B H -0.1916 0.0992 -0.2927 0.336 Uiso 1 1 calc R . . C54 C -0.2283(17) 0.018(2) -0.258(3) 0.28(2) Uiso 1 1 d . A . H54A H -0.2645 0.0235 -0.3050 0.336 Uiso 1 1 calc R . . H54B H -0.2254 0.0376 -0.1997 0.336 Uiso 1 1 calc R . . C55 C -0.2112(17) -0.057(2) -0.246(3) 0.273(19) Uiso 1 1 d . A . H55A H -0.2241 -0.0805 -0.3046 0.328 Uiso 1 1 calc R . . H55B H -0.2214 -0.0794 -0.2013 0.328 Uiso 1 1 calc R . . O61 O 0.1538(5) -0.4532(5) -0.0405(8) 0.094(3) Uani 1 1 d . . . C62 C 0.2057(8) -0.4596(12) -0.0435(19) 0.163(11) Uani 1 1 d . A . H62A H 0.2334 -0.4605 0.0198 0.195 Uiso 1 1 calc R B 1 H62B H 0.2119 -0.4218 -0.0759 0.195 Uiso 1 1 calc R B 1 C63 C 0.2073(17) -0.522(2) -0.093(3) 0.123(14) Uiso 0.50 1 d P A 1 H63A H 0.2393 -0.5470 -0.0589 0.147 Uiso 0.50 1 calc PR A 1 H63B H 0.2038 -0.5132 -0.1562 0.147 Uiso 0.50 1 calc PR A 1 C64 C 0.1539(17) -0.558(2) -0.093(3) 0.091(12) Uiso 0.50 1 d P A 1 H64A H 0.1330 -0.5782 -0.1532 0.109 Uiso 0.50 1 calc PR A 1 H64B H 0.1641 -0.5932 -0.0454 0.109 Uiso 0.50 1 calc PR A 1 C63' C 0.208(3) -0.547(3) 0.001(5) 0.22(3) Uiso 0.50 1 d P A 2 H63C H 0.2424 -0.5680 0.0224 0.265 Uiso 0.50 1 calc PR A 2 H63D H 0.1927 -0.5520 0.0463 0.265 Uiso 0.50 1 calc PR A 2 C64' C 0.183(2) -0.559(3) -0.066(5) 0.14(2) Uiso 0.50 1 d P A 2 H64C H 0.1754 -0.6058 -0.0739 0.167 Uiso 0.50 1 calc PR A 2 H64D H 0.1958 -0.5435 -0.1111 0.167 Uiso 0.50 1 calc PR A 2 C65 C 0.1268(7) -0.5129(8) -0.0735(13) 0.097(6) Uani 1 1 d . A . H65A H 0.1157 -0.5300 -0.0267 0.116 Uiso 1 1 calc R C 1 H65B H 0.0950 -0.5037 -0.1297 0.116 Uiso 1 1 calc R C 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0567(6) 0.0749(8) 0.1623(13) -0.0453(8) 0.0277(7) -0.0129(5) I2 0.0661(6) 0.0696(7) 0.1063(9) 0.0194(6) 0.0331(6) -0.0066(5) Sn1 0.0378(5) 0.0728(7) 0.0576(6) -0.0102(5) 0.0127(5) 0.0058(4) Sn2 0.0493(5) 0.0560(6) 0.0613(6) 0.0085(5) 0.0210(5) 0.0076(4) Sn3 0.0383(5) 0.0534(6) 0.0641(6) -0.0051(5) 0.0193(4) 0.0026(4) Sn4 0.0390(5) 0.0686(7) 0.0606(6) 0.0116(5) 0.0200(5) -0.0004(4) O1 0.040(4) 0.057(5) 0.041(5) -0.008(4) 0.010(4) 0.005(4) O2 0.032(4) 0.058(5) 0.053(5) 0.010(4) 0.019(4) -0.001(4) O3 0.057(5) 0.061(6) 0.076(6) 0.003(5) 0.025(5) 0.007(4) O4 0.038(5) 0.069(6) 0.071(6) 0.012(5) 0.022(4) -0.006(4) C1 0.035(7) 0.085(11) 0.073(10) -0.005(8) 0.016(7) 0.005(7) C2 0.058(11) 0.045(11) 0.063(12) 0.000 0.017(10) 0.000 C3 0.046(10) 0.025(9) 0.105(16) 0.000 0.027(11) 0.000 C11 0.045(11) 0.030(12) 0.068(13) 0.015(11) 0.031(10) -0.005(8) C12 0.080(16) 0.060(16) 0.072(17) -0.005(12) 0.017(13) 0.015(13) C13 0.068(15) 0.12(2) 0.045(13) 0.023(13) 0.017(12) -0.001(14) C14 0.041(12) 0.11(2) 0.068(16) -0.010(15) 0.022(12) -0.001(12) C15 0.056(15) 0.12(3) 0.058(16) -0.011(16) 0.016(12) 0.017(13) C16 0.038(10) 0.076(16) 0.047(12) -0.006(11) 0.023(9) -0.002(10) C21 0.045(16) 0.035(14) 0.066(19) 0.002(16) 0.030(14) 0.021(11) C22 0.10(2) 0.058(18) 0.08(2) 0.036(17) 0.049(19) 0.044(17) C23 0.18(4) 0.18(4) 0.06(2) 0.08(3) 0.07(3) 0.15(4) C24 0.16(4) 0.15(4) 0.07(2) 0.05(3) 0.05(3) 0.11(3) C25 0.09(2) 0.15(3) 0.019(14) 0.020(17) 0.036(15) 0.05(2) C26 0.027(14) 0.063(18) 0.08(2) 0.032(16) 0.016(14) 0.033(12) C31 0.048(16) 0.053(18) 0.09(2) 0.037(17) 0.046(16) 0.027(13) C32 0.16(4) 0.08(3) 0.06(2) 0.02(2) 0.07(2) 0.07(3) C33 0.13(3) 0.14(4) 0.031(19) 0.02(2) -0.016(19) 0.02(3) C34 0.18(4) 0.12(3) 0.05(2) -0.03(2) 0.09(3) -0.01(3) C35 0.09(3) 0.07(2) 0.11(3) 0.00(2) 0.01(2) 0.008(19) C36 0.078(19) 0.027(15) 0.08(2) -0.008(15) 0.025(17) -0.005(13) C41 0.038(11) 0.043(14) 0.050(13) 0.003(10) 0.008(9) 0.005(12) C42 0.11(2) 0.068(16) 0.16(3) 0.054(17) 0.08(2) 0.030(14) C43 0.18(3) 0.12(3) 0.16(3) 0.07(2) 0.14(3) 0.06(2) C44 0.077(19) 0.12(2) 0.076(18) 0.025(18) 0.030(14) 0.007(18) C45 0.21(4) 0.10(2) 0.12(2) -0.05(2) 0.12(3) -0.07(2) C46 0.14(2) 0.075(17) 0.11(2) -0.045(15) 0.092(19) -0.060(16) O51 0.141(14) 0.137(14) 0.223(19) 0.015(13) 0.065(13) 0.011(11) O61 0.081(8) 0.069(8) 0.116(9) -0.006(7) 0.026(7) 0.018(6) C62 0.083(15) 0.120(19) 0.22(3) -0.016(19) -0.003(16) 0.015(13) C65 0.096(13) 0.068(12) 0.141(17) -0.019(11) 0.066(12) -0.008(10) _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 I1 Sn1 2.8881(16) . ? I1 Sn3 4.0411(13) . ? I2 Sn4 2.8588(14) . ? I2 Sn2 4.0994(13) . ? Sn1 C11' 2.01(3) . ? Sn1 O1 2.015(7) . ? Sn1 C1 2.131(14) . ? Sn1 O3 2.155(9) . ? Sn1 C11 2.203(10) . ? Sn2 C21' 2.03(3) . ? Sn2 O1 2.072(8) . ? Sn2 O3 2.113(9) . ? Sn2 O2 2.114(7) . ? Sn2 C2 2.119(9) . ? Sn2 C21 2.202(13) . ? Sn3 C31 2.051(14) . ? Sn3 O2 2.078(7) . ? Sn3 C3 2.118(8) . ? Sn3 O4 2.120(8) . ? Sn3 O1 2.134(7) . ? Sn3 C31' 2.225(16) . ? Sn4 O2 2.029(7) . ? Sn4 C41' 2.12(4) . ? Sn4 C1 2.141(13) 2_554 ? Sn4 C41 2.184(13) . ? Sn4 O4 2.197(8) . ? O3 O61 2.697(13) . ? O4 O51 2.616(19) . ? C1 Sn4 2.141(13) 2_554 ? C2 Sn2 2.119(9) 2_554 ? C3 Sn3 2.118(8) 2_554 ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C11' C12' 1.3900 . ? C11' C16' 1.3900 . ? C12' C13' 1.3900 . ? C13' C14' 1.3900 . ? C14' C15' 1.3900 . ? C15' C16' 1.3900 . ? C21' C22' 1.3900 . ? C21' C26' 1.3900 . ? C22' C23' 1.3900 . ? C23' C24' 1.3900 . ? C24' C25' 1.3900 . ? C25' C26' 1.3900 . ? C31' C32' 1.3900 . ? C31' C36' 1.3900 . ? C32' C33' 1.3900 . ? C33' C34' 1.3900 . ? C34' C35' 1.3900 . ? C35' C36' 1.3900 . ? C41' C42' 1.3900 . ? C41' C46' 1.3900 . ? C42' C43' 1.3900 . ? C43' C44' 1.3900 . ? C44' C45' 1.3900 . ? C45' C46' 1.3900 . ? O51 C52 1.55(4) . ? O51 C55 1.57(4) . ? C52 C53 1.51(4) . ? C53 C54 1.55(5) . ? C54 C55 1.57(5) . ? O61 C65 1.396(18) . ? O61 C62 1.46(2) . ? C62 C63 1.48(4) . ? C62 C63' 1.89(7) . ? C63 C64 1.66(6) . ? C64 C65 1.30(4) . ? C63' C64' 1.02(7) . ? C64' C65 1.76(6) . ? 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 Sn1 I1 Sn3 67.21(3) . . ? Sn4 I2 Sn2 66.37(3) . . ? C11' Sn1 O1 115.4(11) . . ? C11' Sn1 C1 124.9(11) . . ? O1 Sn1 C1 119.2(4) . . ? C11' Sn1 O3 108.5(11) . . ? O1 Sn1 O3 73.4(3) . . ? C1 Sn1 O3 92.9(5) . . ? C11' Sn1 C11 18.7(10) . . ? O1 Sn1 C11 112.8(4) . . ? C1 Sn1 C11 126.4(5) . . ? O3 Sn1 C11 89.9(4) . . ? C11' Sn1 I1 80.8(11) . . ? O1 Sn1 I1 88.6(2) . . ? C1 Sn1 I1 94.1(4) . . ? O3 Sn1 I1 161.9(2) . . ? C11 Sn1 I1 99.2(4) . . ? C21' Sn2 O1 121.2(11) . . ? C21' Sn2 O3 96.8(9) . . ? O1 Sn2 O3 73.2(3) . . ? C21' Sn2 O2 103.9(10) . . ? O1 Sn2 O2 74.7(3) . . ? O3 Sn2 O2 147.5(3) . . ? C21' Sn2 C2 115.4(12) . . ? O1 Sn2 C2 122.9(4) . . ? O3 Sn2 C2 94.2(3) . . ? O2 Sn2 C2 99.0(3) . . ? C21' Sn2 C21 12.9(12) . . ? O1 Sn2 C21 109.0(6) . . ? O3 Sn2 C21 97.6(5) . . ? O2 Sn2 C21 97.3(4) . . ? C2 Sn2 C21 127.9(7) . . ? C21' Sn2 I2 70.7(8) . . ? O1 Sn2 I2 133.3(2) . . ? O3 Sn2 I2 153.5(2) . . ? O2 Sn2 I2 58.8(2) . . ? C2 Sn2 I2 71.95(9) . . ? C21 Sn2 I2 75.4(5) . . ? C31 Sn3 O2 118.5(7) . . ? C31 Sn3 C3 119.7(7) . . ? O2 Sn3 C3 121.6(4) . . ? C31 Sn3 O4 97.2(6) . . ? O2 Sn3 O4 74.7(3) . . ? C3 Sn3 O4 94.0(2) . . ? C31 Sn3 O1 101.7(5) . . ? O2 Sn3 O1 74.1(3) . . ? C3 Sn3 O1 98.2(3) . . ? O4 Sn3 O1 148.5(3) . . ? C31 Sn3 C31' 15.1(8) . . ? O2 Sn3 C31' 103.8(6) . . ? C3 Sn3 C31' 134.6(7) . . ? O4 Sn3 C31' 96.7(6) . . ? O1 Sn3 C31' 95.2(6) . . ? C31 Sn3 I1 73.0(6) . . ? O2 Sn3 I1 133.5(2) . . ? C3 Sn3 I1 69.93(8) . . ? O4 Sn3 I1 151.6(2) . . ? O1 Sn3 I1 59.4(2) . . ? C31' Sn3 I1 80.5(6) . . ? O2 Sn4 C41' 110.4(11) . . ? O2 Sn4 C1 117.1(4) . 2_554 ? C41' Sn4 C1 132.4(11) . 2_554 ? O2 Sn4 C41 115.5(5) . . ? C41' Sn4 C41 13.4(12) . . ? C1 Sn4 C41 124.9(6) 2_554 . ? O2 Sn4 O4 74.0(3) . . ? C41' Sn4 O4 99.0(11) . . ? C1 Sn4 O4 90.9(4) 2_554 . ? C41 Sn4 O4 88.4(5) . . ? O2 Sn4 I2 90.0(2) . . ? C41' Sn4 I2 87.9(11) . . ? C1 Sn4 I2 95.2(4) 2_554 . ? C41 Sn4 I2 100.1(4) . . ? O4 Sn4 I2 164.0(2) . . ? Sn1 O1 Sn2 109.6(3) . . ? Sn1 O1 Sn3 144.7(4) . . ? Sn2 O1 Sn3 105.2(3) . . ? Sn4 O2 Sn3 108.7(3) . . ? Sn4 O2 Sn2 144.6(4) . . ? Sn3 O2 Sn2 105.7(3) . . ? Sn2 O3 Sn1 102.9(4) . . ? Sn2 O3 O61 121.4(5) . . ? Sn1 O3 O61 132.4(5) . . ? Sn3 O4 Sn4 101.3(4) . . ? Sn3 O4 O51 132.7(6) . . ? Sn4 O4 O51 122.7(5) . . ? Sn1 C1 Sn4 116.5(5) . 2_554 ? Sn2 C2 Sn2 115.2(8) . 2_554 ? Sn3 C3 Sn3 117.1(7) 2_554 . ? C12 C11 C16 120.0 . . ? C12 C11 Sn1 120.4(7) . . ? C16 C11 Sn1 119.6(7) . . ? C13 C12 C11 120.0 . . ? C14 C13 C12 120.0 . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C15 C16 C11 120.0 . . ? C22 C21 C26 120.0 . . ? C22 C21 Sn2 117.5(8) . . ? C26 C21 Sn2 122.5(8) . . ? C23 C22 C21 120.0 . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? C24 C25 C26 120.0 . . ? C25 C26 C21 120.0 . . ? C32 C31 C36 120.0 . . ? C32 C31 Sn3 120.5(11) . . ? C36 C31 Sn3 119.5(11) . . ? C31 C32 C33 120.0 . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C35 C36 C31 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 Sn4 118.1(9) . . ? C46 C41 Sn4 121.9(9) . . ? C41 C42 C43 120.0 . . ? C44 C43 C42 120.0 . . ? C45 C44 C43 120.0 . . ? C44 C45 C46 120.0 . . ? C45 C46 C41 120.0 . . ? C12' C11' C16' 120.0 . . ? C12' C11' Sn1 110(2) . . ? C16' C11' Sn1 130(2) . . ? C13' C12' C11' 120.0 . . ? C12' C13' C14' 120.0 . . ? C15' C14' C13' 120.0 . . ? C16' C15' C14' 120.0 . . ? C15' C16' C11' 120.0 . . ? C22' C21' C26' 120.0 . . ? C22' C21' Sn2 123(2) . . ? C26' C21' Sn2 117(2) . . ? C23' C22' C21' 120.0 . . ? C24' C23' C22' 120.0 . . ? C23' C24' C25' 120.0 . . ? C26' C25' C24' 120.0 . . ? C25' C26' C21' 120.0 . . ? C32' C31' C36' 120.0 . . ? C32' C31' Sn3 121.2(11) . . ? C36' C31' Sn3 118.3(12) . . ? C31' C32' C33' 120.0 . . ? C32' C33' C34' 120.0 . . ? C35' C34' C33' 120.0 . . ? C34' C35' C36' 120.0 . . ? C35' C36' C31' 120.0 . . ? C42' C41' C46' 120.0 . . ? C42' C41' Sn4 132(2) . . ? C46' C41' Sn4 108(3) . . ? C41' C42' C43' 120.0 . . ? C44' C43' C42' 120.0 . . ? C45' C44' C43' 120.0 . . ? C44' C45' C46' 120.0 . . ? C45' C46' C41' 120.0 . . ? C52 O51 C55 115(3) . . ? C52 O51 O4 123.5(19) . . ? C55 O51 O4 114.8(19) . . ? C53 C52 O51 98(3) . . ? C52 C53 C54 104(3) . . ? C53 C54 C55 103(3) . . ? C54 C55 O51 96(3) . . ? C65 O61 C62 107.2(14) . . ? C65 O61 O3 122.6(10) . . ? C62 O61 O3 115.8(12) . . ? O61 C62 C63 110(2) . . ? O61 C62 C63' 87(3) . . ? C63 C62 C63' 53(3) . . ? C62 C63 C64 99(3) . . ? C65 C64 C63 107(3) . . ? C64' C63' C62 86(6) . . ? C63' C64' C65 99(7) . . ? C64 C65 O61 115(2) . . ? C64 C65 C64' 21(3) . . ? O61 C65 C64' 96(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sn3 I1 Sn1 C11' -114.2(11) . . . . ? Sn3 I1 Sn1 O1 1.8(2) . . . . ? Sn3 I1 Sn1 C1 121.0(3) . . . . ? Sn3 I1 Sn1 O3 8.3(8) . . . . ? Sn3 I1 Sn1 C11 -111.1(4) . . . . ? Sn4 I2 Sn2 C21' 118.2(12) . . . . ? Sn4 I2 Sn2 O1 3.1(3) . . . . ? Sn4 I2 Sn2 O3 -176.7(6) . . . . ? Sn4 I2 Sn2 O2 -2.5(3) . . . . ? Sn4 I2 Sn2 C2 -115.5(4) . . . . ? Sn4 I2 Sn2 C21 105.7(5) . . . . ? Sn1 I1 Sn3 C31 113.4(6) . . . . ? Sn1 I1 Sn3 O2 -0.1(3) . . . . ? Sn1 I1 Sn3 C3 -115.1(4) . . . . ? Sn1 I1 Sn3 O4 -173.6(5) . . . . ? Sn1 I1 Sn3 O1 -2.0(2) . . . . ? Sn1 I1 Sn3 C31' 99.9(6) . . . . ? Sn2 I2 Sn4 O2 2.2(2) . . . . ? Sn2 I2 Sn4 C41' -108.3(11) . . . . ? Sn2 I2 Sn4 C1 119.4(3) . . . 2_554 ? Sn2 I2 Sn4 C41 -113.7(4) . . . . ? Sn2 I2 Sn4 O4 7.6(8) . . . . ? C11' Sn1 O1 Sn2 -96.0(13) . . . . ? C1 Sn1 O1 Sn2 91.0(6) . . . . ? O3 Sn1 O1 Sn2 7.0(4) . . . . ? C11 Sn1 O1 Sn2 -75.7(5) . . . . ? I1 Sn1 O1 Sn2 -175.0(3) . . . . ? C11' Sn1 O1 Sn3 73.6(14) . . . . ? C1 Sn1 O1 Sn3 -99.5(8) . . . . ? O3 Sn1 O1 Sn3 176.6(8) . . . . ? C11 Sn1 O1 Sn3 93.8(8) . . . . ? I1 Sn1 O1 Sn3 -5.5(7) . . . . ? C21' Sn2 O1 Sn1 80.7(11) . . . . ? O3 Sn2 O1 Sn1 -7.2(4) . . . . ? O2 Sn2 O1 Sn1 177.8(4) . . . . ? C2 Sn2 O1 Sn1 -91.2(4) . . . . ? C21 Sn2 O1 Sn1 85.2(5) . . . . ? I2 Sn2 O1 Sn1 172.87(12) . . . . ? C21' Sn2 O1 Sn3 -93.1(11) . . . . ? O3 Sn2 O1 Sn3 179.1(4) . . . . ? O2 Sn2 O1 Sn3 4.1(3) . . . . ? C2 Sn2 O1 Sn3 95.0(4) . . . . ? C21 Sn2 O1 Sn3 -88.5(5) . . . . ? I2 Sn2 O1 Sn3 -0.9(5) . . . . ? C31 Sn3 O1 Sn1 -57.4(10) . . . . ? O2 Sn3 O1 Sn1 -174.0(8) . . . . ? C3 Sn3 O1 Sn1 65.4(8) . . . . ? O4 Sn3 O1 Sn1 177.0(6) . . . . ? C31' Sn3 O1 Sn1 -71.1(9) . . . . ? I1 Sn3 O1 Sn1 4.6(6) . . . . ? C31 Sn3 O1 Sn2 112.4(7) . . . . ? O2 Sn3 O1 Sn2 -4.2(3) . . . . ? C3 Sn3 O1 Sn2 -124.8(4) . . . . ? O4 Sn3 O1 Sn2 -13.2(8) . . . . ? C31' Sn3 O1 Sn2 98.7(7) . . . . ? I1 Sn3 O1 Sn2 174.4(4) . . . . ? C41' Sn4 O2 Sn3 -84.9(13) . . . . ? C1 Sn4 O2 Sn3 91.6(6) 2_554 . . . ? C41 Sn4 O2 Sn3 -71.3(6) . . . . ? O4 Sn4 O2 Sn3 9.0(3) . . . . ? I2 Sn4 O2 Sn3 -172.6(3) . . . . ? C41' Sn4 O2 Sn2 81.0(14) . . . . ? C1 Sn4 O2 Sn2 -102.6(8) 2_554 . . . ? C41 Sn4 O2 Sn2 94.5(9) . . . . ? O4 Sn4 O2 Sn2 174.8(8) . . . . ? I2 Sn4 O2 Sn2 -6.8(7) . . . . ? C31 Sn3 O2 Sn4 80.7(7) . . . . ? C3 Sn3 O2 Sn4 -94.4(4) . . . . ? O4 Sn3 O2 Sn4 -9.3(4) . . . . ? O1 Sn3 O2 Sn4 175.6(4) . . . . ? C31' Sn3 O2 Sn4 84.0(7) . . . . ? I1 Sn3 O2 Sn4 173.88(12) . . . . ? C31 Sn3 O2 Sn2 -90.8(6) . . . . ? C3 Sn3 O2 Sn2 94.0(4) . . . . ? O4 Sn3 O2 Sn2 179.2(4) . . . . ? O1 Sn3 O2 Sn2 4.1(3) . . . . ? C31' Sn3 O2 Sn2 -87.5(7) . . . . ? I1 Sn3 O2 Sn2 2.4(5) . . . . ? C21' Sn2 O2 Sn4 -51.2(13) . . . . ? O1 Sn2 O2 Sn4 -170.3(8) . . . . ? O3 Sn2 O2 Sn4 -179.3(6) . . . . ? C2 Sn2 O2 Sn4 67.9(8) . . . . ? C21 Sn2 O2 Sn4 -62.5(9) . . . . ? I2 Sn2 O2 Sn4 5.5(6) . . . . ? C21' Sn2 O2 Sn3 114.8(11) . . . . ? O1 Sn2 O2 Sn3 -4.2(3) . . . . ? O3 Sn2 O2 Sn3 -13.2(8) . . . . ? C2 Sn2 O2 Sn3 -126.0(4) . . . . ? C21 Sn2 O2 Sn3 103.6(7) . . . . ? I2 Sn2 O2 Sn3 171.6(4) . . . . ? C21' Sn2 O3 Sn1 -114.1(12) . . . . ? O1 Sn2 O3 Sn1 6.5(3) . . . . ? O2 Sn2 O3 Sn1 15.6(8) . . . . ? C2 Sn2 O3 Sn1 129.7(5) . . . . ? C21 Sn2 O3 Sn1 -101.1(7) . . . . ? I2 Sn2 O3 Sn1 -173.6(2) . . . . ? C21' Sn2 O3 O61 48.1(13) . . . . ? O1 Sn2 O3 O61 168.7(6) . . . . ? O2 Sn2 O3 O61 177.7(5) . . . . ? C2 Sn2 O3 O61 -68.1(6) . . . . ? C21 Sn2 O3 O61 61.1(8) . . . . ? I2 Sn2 O3 O61 -11.4(9) . . . . ? C11' Sn1 O3 Sn2 105.2(12) . . . . ? O1 Sn1 O3 Sn2 -6.7(3) . . . . ? C1 Sn1 O3 Sn2 -126.3(5) . . . . ? C11 Sn1 O3 Sn2 107.2(5) . . . . ? I1 Sn1 O3 Sn2 -13.4(11) . . . . ? C11' Sn1 O3 O61 -54.1(13) . . . . ? O1 Sn1 O3 O61 -166.0(7) . . . . ? C1 Sn1 O3 O61 74.4(7) . . . . ? C11 Sn1 O3 O61 -52.1(7) . . . . ? I1 Sn1 O3 O61 -172.7(5) . . . . ? C31 Sn3 O4 Sn4 -109.4(7) . . . . ? O2 Sn3 O4 Sn4 8.3(3) . . . . ? C3 Sn3 O4 Sn4 130.0(4) . . . . ? O1 Sn3 O4 Sn4 17.3(8) . . . . ? C31' Sn3 O4 Sn4 -94.2(7) . . . . ? I1 Sn3 O4 Sn4 -176.56(18) . . . . ? C31 Sn3 O4 O51 49.8(10) . . . . ? O2 Sn3 O4 O51 167.5(8) . . . . ? C3 Sn3 O4 O51 -70.8(8) . . . . ? O1 Sn3 O4 O51 176.5(7) . . . . ? C31' Sn3 O4 O51 65.0(10) . . . . ? I1 Sn3 O4 O51 -17.4(11) . . . . ? O2 Sn4 O4 Sn3 -8.5(3) . . . . ? C41' Sn4 O4 Sn3 100.3(12) . . . . ? C1 Sn4 O4 Sn3 -126.5(5) 2_554 . . . ? C41 Sn4 O4 Sn3 108.6(5) . . . . ? I2 Sn4 O4 Sn3 -14.1(11) . . . . ? O2 Sn4 O4 O51 -170.4(7) . . . . ? C41' Sn4 O4 O51 -61.6(13) . . . . ? C1 Sn4 O4 O51 71.6(7) 2_554 . . . ? C41 Sn4 O4 O51 -53.3(8) . . . . ? I2 Sn4 O4 O51 -176.1(7) . . . . ? C11' Sn1 C1 Sn4 -177.7(14) . . . 2_554 ? O1 Sn1 C1 Sn4 -5.4(9) . . . 2_554 ? O3 Sn1 C1 Sn4 67.3(7) . . . 2_554 ? C11 Sn1 C1 Sn4 159.3(6) . . . 2_554 ? I1 Sn1 C1 Sn4 -96.1(6) . . . 2_554 ? C21' Sn2 C2 Sn2 159.6(10) . . . 2_554 ? O1 Sn2 C2 Sn2 -28.1(3) . . . 2_554 ? O3 Sn2 C2 Sn2 -100.8(2) . . . 2_554 ? O2 Sn2 C2 Sn2 49.4(2) . . . 2_554 ? C21 Sn2 C2 Sn2 156.1(5) . . . 2_554 ? I2 Sn2 C2 Sn2 102.29(13) . . . 2_554 ? C31 Sn3 C3 Sn3 157.7(6) . . . 2_554 ? O2 Sn3 C3 Sn3 -27.2(3) . . . 2_554 ? O4 Sn3 C3 Sn3 -101.7(2) . . . 2_554 ? O1 Sn3 C3 Sn3 49.1(2) . . . 2_554 ? C31' Sn3 C3 Sn3 154.9(8) . . . 2_554 ? I1 Sn3 C3 Sn3 102.28(13) . . . 2_554 ? C11' Sn1 C11 C12 172(4) . . . . ? O1 Sn1 C11 C12 70.0(7) . . . . ? C1 Sn1 C11 C12 -95.6(8) . . . . ? O3 Sn1 C11 C12 -2.0(7) . . . . ? I1 Sn1 C11 C12 162.3(6) . . . . ? C11' Sn1 C11 C16 -7(4) . . . . ? O1 Sn1 C11 C16 -109.5(7) . . . . ? C1 Sn1 C11 C16 84.9(9) . . . . ? O3 Sn1 C11 C16 178.5(7) . . . . ? I1 Sn1 C11 C16 -17.2(8) . . . . ? C16 C11 C12 C13 0.0 . . . . ? Sn1 C11 C12 C13 -179.5(9) . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 C11 0.0 . . . . ? C12 C11 C16 C15 0.0 . . . . ? Sn1 C11 C16 C15 179.5(9) . . . . ? C21' Sn2 C21 C22 45(5) . . . . ? O1 Sn2 C21 C22 -116.9(11) . . . . ? O3 Sn2 C21 C22 -42.1(12) . . . . ? O2 Sn2 C21 C22 166.8(11) . . . . ? C2 Sn2 C21 C22 59.3(13) . . . . ? I2 Sn2 C21 C22 111.8(12) . . . . ? C21' Sn2 C21 C26 -134(5) . . . . ? O1 Sn2 C21 C26 64.3(13) . . . . ? O3 Sn2 C21 C26 139.1(12) . . . . ? O2 Sn2 C21 C26 -12.0(13) . . . . ? C2 Sn2 C21 C26 -119.5(11) . . . . ? I2 Sn2 C21 C26 -67.0(11) . . . . ? C26 C21 C22 C23 0.0 . . . . ? Sn2 C21 C22 C23 -178.9(16) . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C21 0.0 . . . . ? C22 C21 C26 C25 0.0 . . . . ? Sn2 C21 C26 C25 178.8(17) . . . . ? O2 Sn3 C31 C32 66.8(11) . . . . ? C3 Sn3 C31 C32 -118.0(10) . . . . ? O4 Sn3 C31 C32 143.3(10) . . . . ? O1 Sn3 C31 C32 -11.4(11) . . . . ? C31' Sn3 C31 C32 54(3) . . . . ? I1 Sn3 C31 C32 -64.0(10) . . . . ? O2 Sn3 C31 C36 -112.1(12) . . . . ? C3 Sn3 C31 C36 63.1(13) . . . . ? O4 Sn3 C31 C36 -35.7(12) . . . . ? O1 Sn3 C31 C36 169.7(11) . . . . ? C31' Sn3 C31 C36 -125(4) . . . . ? I1 Sn3 C31 C36 117.1(12) . . . . ? C36 C31 C32 C33 0.0 . . . . ? Sn3 C31 C32 C33 -178.9(15) . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C31 0.0 . . . . ? C32 C31 C36 C35 0.0 . . . . ? Sn3 C31 C36 C35 179.0(15) . . . . ? O2 Sn4 C41 C42 -97.8(9) . . . . ? C41' Sn4 C41 C42 -27(5) . . . . ? C1 Sn4 C41 C42 100.8(10) 2_554 . . . ? O4 Sn4 C41 C42 -169.2(9) . . . . ? I2 Sn4 C41 C42 -2.9(9) . . . . ? O2 Sn4 C41 C46 83.8(10) . . . . ? C41' Sn4 C41 C46 154(6) . . . . ? C1 Sn4 C41 C46 -77.6(11) 2_554 . . . ? O4 Sn4 C41 C46 12.3(9) . . . . ? I2 Sn4 C41 C46 178.7(9) . . . . ? C46 C41 C42 C43 0.0 . . . . ? Sn4 C41 C42 C43 -178.5(11) . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C46 0.0 . . . . ? C44 C45 C46 C41 0.0 . . . . ? C42 C41 C46 C45 0.0 . . . . ? Sn4 C41 C46 C45 178.4(11) . . . . ? O1 Sn1 C11' C12' 82(2) . . . . ? C1 Sn1 C11' C12' -105(2) . . . . ? O3 Sn1 C11' C12' 2(2) . . . . ? C11 Sn1 C11' C12' -4(4) . . . . ? I1 Sn1 C11' C12' 166(2) . . . . ? O1 Sn1 C11' C16' -98(3) . . . . ? C1 Sn1 C11' C16' 75(3) . . . . ? O3 Sn1 C11' C16' -178(2) . . . . ? C11 Sn1 C11' C16' 176(6) . . . . ? I1 Sn1 C11' C16' -14(3) . . . . ? C16' C11' C12' C13' 0.0 . . . . ? Sn1 C11' C12' C13' 180(3) . . . . ? C11' C12' C13' C14' 0.0 . . . . ? C12' C13' C14' C15' 0.0 . . . . ? C13' C14' C15' C16' 0.0 . . . . ? C14' C15' C16' C11' 0.0 . . . . ? C12' C11' C16' C15' 0.0 . . . . ? Sn1 C11' C16' C15' -180(3) . . . . ? O1 Sn2 C21' C22' -151.0(13) . . . . ? O3 Sn2 C21' C22' -76.5(16) . . . . ? O2 Sn2 C21' C22' 128.7(15) . . . . ? C2 Sn2 C21' C22' 21.4(18) . . . . ? C21 Sn2 C21' C22' -171(6) . . . . ? I2 Sn2 C21' C22' 79.4(16) . . . . ? O1 Sn2 C21' C26' 25.1(19) . . . . ? O3 Sn2 C21' C26' 99.6(16) . . . . ? O2 Sn2 C21' C26' -55.2(16) . . . . ? C2 Sn2 C21' C26' -162.5(14) . . . . ? C21 Sn2 C21' C26' 5(4) . . . . ? I2 Sn2 C21' C26' -104.5(17) . . . . ? C26' C21' C22' C23' 0.0 . . . . ? Sn2 C21' C22' C23' 176(2) . . . . ? C21' C22' C23' C24' 0.0 . . . . ? C22' C23' C24' C25' 0.0 . . . . ? C23' C24' C25' C26' 0.0 . . . . ? C24' C25' C26' C21' 0.0 . . . . ? C22' C21' C26' C25' 0.0 . . . . ? Sn2 C21' C26' C25' -176(2) . . . . ? C31 Sn3 C31' C32' -118(4) . . . . ? O2 Sn3 C31' C32' 73.5(11) . . . . ? C3 Sn3 C31' C32' -108.3(11) . . . . ? O4 Sn3 C31' C32' 149.3(10) . . . . ? O1 Sn3 C31' C32' -1.4(11) . . . . ? I1 Sn3 C31' C32' -59.2(10) . . . . ? C31 Sn3 C31' C36' 70(3) . . . . ? O2 Sn3 C31' C36' -98.4(11) . . . . ? C3 Sn3 C31' C36' 79.8(13) . . . . ? O4 Sn3 C31' C36' -22.5(11) . . . . ? O1 Sn3 C31' C36' -173.3(10) . . . . ? I1 Sn3 C31' C36' 129.0(11) . . . . ? C36' C31' C32' C33' 0.0 . . . . ? Sn3 C31' C32' C33' -171.7(15) . . . . ? C31' C32' C33' C34' 0.0 . . . . ? C32' C33' C34' C35' 0.0 . . . . ? C33' C34' C35' C36' 0.0 . . . . ? C34' C35' C36' C31' 0.0 . . . . ? C32' C31' C36' C35' 0.0 . . . . ? Sn3 C31' C36' C35' 172.0(14) . . . . ? O2 Sn4 C41' C42' -47(3) . . . . ? C1 Sn4 C41' C42' 137(2) 2_554 . . . ? C41 Sn4 C41' C42' -162(7) . . . . ? O4 Sn4 C41' C42' -124(3) . . . . ? I2 Sn4 C41' C42' 42(3) . . . . ? O2 Sn4 C41' C46' 122.2(19) . . . . ? C1 Sn4 C41' C46' -54(2) 2_554 . . . ? C41 Sn4 C41' C46' 8(4) . . . . ? O4 Sn4 C41' C46' 46(2) . . . . ? I2 Sn4 C41' C46' -148.6(19) . . . . ? C46' C41' C42' C43' 0.0 . . . . ? Sn4 C41' C42' C43' 169(3) . . . . ? C41' C42' C43' C44' 0.0 . . . . ? C42' C43' C44' C45' 0.0 . . . . ? C43' C44' C45' C46' 0.0 . . . . ? C44' C45' C46' C41' 0.0 . . . . ? C42' C41' C46' C45' 0.0 . . . . ? Sn4 C41' C46' C45' -171(3) . . . . ? Sn3 O4 O51 C52 34(3) . . . . ? Sn4 O4 O51 C52 -170(2) . . . . ? Sn3 O4 O51 C55 -176.1(19) . . . . ? Sn4 O4 O51 C55 -21(2) . . . . ? C55 O51 C52 C53 -13(4) . . . . ? O4 O51 C52 C53 136(2) . . . . ? O51 C52 C53 C54 38(4) . . . . ? C52 C53 C54 C55 -52(4) . . . . ? C53 C54 C55 O51 38(4) . . . . ? C52 O51 C55 C54 -16(4) . . . . ? O4 O51 C55 C54 -168(2) . . . . ? Sn2 O3 O61 C65 29.3(14) . . . . ? Sn1 O3 O61 C65 -174.5(11) . . . . ? Sn2 O3 O61 C62 163.8(13) . . . . ? Sn1 O3 O61 C62 -40.1(16) . . . . ? C65 O61 C62 C63 9(3) . . . . ? O3 O61 C62 C63 -132(2) . . . . ? C65 O61 C62 C63' -41(3) . . . . ? O3 O61 C62 C63' 178(2) . . . . ? O61 C62 C63 C64 -14(4) . . . . ? C63' C62 C63 C64 57(4) . . . . ? C62 C63 C64 C65 16(4) . . . . ? O61 C62 C63' C64' 78(6) . . . . ? C63 C62 C63' C64' -39(5) . . . . ? C62 C63' C64' C65 -66(4) . . . . ? C63 C64 C65 O61 -13(4) . . . . ? C63 C64 C65 C64' -42(8) . . . . ? C62 O61 C65 C64 4(3) . . . . ? O3 O61 C65 C64 141(2) . . . . ? C62 O61 C65 C64' 14(3) . . . . ? O3 O61 C65 C64' 152(2) . . . . ? C63' C64' C65 C64 -156(14) . . . . ? C63' C64' C65 O61 50(7) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 3.180 _refine_diff_density_min -2.907 _refine_diff_density_rms 0.181 _data_(1u3CH2Cl2) _database_code_CSD 178299 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H58 Cl6 I4 O8 Sn8' _chemical_formula_weight 2516.83 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.8847(2) _cell_length_b 19.7039(3) _cell_length_c 21.2582(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.4481(8) _cell_angle_gamma 90.00 _cell_volume 7220.71(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 63211 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 27.49 _exptl_crystal_description 'parallel epipede' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not determined' _exptl_crystal_density_diffrn 2.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4664 _exptl_absorpt_coefficient_mu 4.697 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ; 3 sets at different \k-angles and 291 frames via \w-rotation (\D/\w=1\%) at two times 5s per frame ; _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 63211 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.1018 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.49 _reflns_number_total 16361 _reflns_number_gt 9885 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius KappaCCD' _computing_cell_refinement ; DENZO and SCALEPACK (Otwinowski & Minor, 1997) ; _computing_data_reduction ; DENZO and SCALEPACK (Otwinowski & Minor, 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16361 _refine_ls_number_parameters 730 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1094 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0773 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.25932(3) -0.48243(3) 0.52887(2) 0.03505(14) Uani 1 1 d . . . I2 I 0.20058(3) -0.01981(3) 0.52435(2) 0.03417(14) Uani 1 1 d . . . I3 I 0.07482(3) -0.28680(2) 0.25538(2) 0.02748(13) Uani 1 1 d . . . I4 I 0.54673(3) -0.19517(3) 0.53496(2) 0.03840(15) Uani 1 1 d . . . Sn1 Sn 0.13548(3) -0.38951(2) 0.46945(2) 0.01997(12) Uani 1 1 d . . . Sn2 Sn 0.14400(3) -0.21996(2) 0.48243(2) 0.01724(11) Uani 1 1 d . . . Sn3 Sn 0.31011(3) -0.28200(2) 0.57638(2) 0.02039(12) Uani 1 1 d . . . Sn4 Sn 0.31969(3) -0.11264(3) 0.59170(2) 0.02379(13) Uani 1 1 d . . . Sn5 Sn 0.20457(3) -0.36919(2) 0.32554(2) 0.01767(12) Uani 1 1 d . . . Sn6 Sn 0.25249(3) -0.17619(2) 0.36676(2) 0.01688(12) Uani 1 1 d . . . Sn7 Sn 0.36624(3) -0.30872(2) 0.42745(2) 0.01786(12) Uani 1 1 d . . . Sn8 Sn 0.41773(3) -0.11555(3) 0.46264(2) 0.02349(13) Uani 1 1 d . . . Cl1 Cl 0.25706(17) 0.16787(12) 0.53729(11) 0.0595(7) Uani 1 1 d . . . Cl2 Cl 0.2224(2) 0.31093(16) 0.54264(18) 0.1098(13) Uani 1 1 d . . . Cl3 Cl -0.0149(3) 0.08166(19) 0.82499(18) 0.1282(16) Uani 1 1 d . . . Cl4 Cl -0.0767(2) 0.0786(2) 0.93514(13) 0.1035(12) Uani 1 1 d . . . Cl5 Cl 0.02491(17) 0.07895(14) 0.55873(13) 0.0703(8) Uani 1 1 d . . . Cl6 Cl 0.0358(2) 0.01612(19) 0.68456(14) 0.1110(14) Uani 1 1 d . . . O1 O 0.2048(3) -0.3093(2) 0.50780(19) 0.0179(11) Uani 1 1 d . . . O2 O 0.2540(3) -0.1918(2) 0.5447(2) 0.0204(11) Uani 1 1 d . . . O3 O 0.0686(3) -0.2985(2) 0.4287(2) 0.0193(11) Uani 1 1 d . . . O4 O 0.3906(3) -0.2022(2) 0.6200(2) 0.0260(12) Uani 1 1 d . . . O5 O 0.2587(3) -0.2838(2) 0.36758(19) 0.0175(11) Uani 1 1 d . . . O6 O 0.3571(3) -0.2015(2) 0.43046(19) 0.0175(10) Uani 1 1 d . . . O7 O 0.3094(3) -0.4046(2) 0.3961(2) 0.0198(11) Uani 1 1 d . . . O8 O 0.3021(3) -0.0810(2) 0.4063(2) 0.0233(12) Uani 1 1 d . . . C1 C 0.1330(4) -0.4234(3) 0.3734(3) 0.0227(17) Uani 1 1 d . . . H1A H 0.1483 -0.4708 0.3759 0.027 Uiso 1 1 calc R . . H1B H 0.0799 -0.4210 0.3466 0.027 Uiso 1 1 calc R . . C2 C 0.1509(4) -0.1649(3) 0.3990(3) 0.0207(17) Uani 1 1 d . . . H2A H 0.1452 -0.1171 0.4077 0.025 Uiso 1 1 calc R . . H2B H 0.1069 -0.1777 0.3633 0.025 Uiso 1 1 calc R . . C3 C 0.3868(4) -0.3265(4) 0.5281(3) 0.0234(17) Uani 1 1 d . . . H3A H 0.4388 -0.3107 0.5493 0.028 Uiso 1 1 calc R . . H3B H 0.3863 -0.3752 0.5347 0.028 Uiso 1 1 calc R . . C4 C 0.4015(5) -0.0685(4) 0.5479(3) 0.0307(19) Uani 1 1 d . . . H4A H 0.4513 -0.0674 0.5803 0.037 Uiso 1 1 calc R . . H4B H 0.3861 -0.0218 0.5371 0.037 Uiso 1 1 calc R . . C11 C 0.0623(5) -0.4116(3) 0.5299(3) 0.0253(17) Uani 1 1 d . . . C12 C 0.0864(7) -0.4451(8) 0.5861(5) 0.119(6) Uani 1 1 d . . . H12 H 0.1359 -0.4638 0.5971 0.143 Uiso 1 1 calc R . . C13 C 0.0407(7) -0.4533(8) 0.6290(5) 0.122(6) Uani 1 1 d . . . H13 H 0.0604 -0.4776 0.6674 0.146 Uiso 1 1 calc R . . C14 C -0.0275(6) -0.4284(4) 0.6175(4) 0.045(2) Uani 1 1 d . . . H14 H -0.0558 -0.4305 0.6483 0.055 Uiso 1 1 calc R . . C15 C -0.0560(7) -0.3999(7) 0.5603(7) 0.113(6) Uani 1 1 d . . . H15 H -0.1071 -0.3848 0.5487 0.136 Uiso 1 1 calc R . . C16 C -0.0103(6) -0.3919(7) 0.5168(5) 0.096(5) Uani 1 1 d . . . H16 H -0.0324 -0.3716 0.4766 0.115 Uiso 1 1 calc R . . C21 C 0.0752(4) -0.2010(3) 0.5474(3) 0.0225(17) Uani 1 1 d . . . C22 C -0.0025(5) -0.2167(6) 0.5315(4) 0.064(3) Uani 1 1 d . . . H22 H -0.0261 -0.2355 0.4909 0.077 Uiso 1 1 calc R . . C23 C -0.0459(6) -0.2046(6) 0.5754(5) 0.079(4) Uani 1 1 d . . . H23 H -0.0991 -0.2126 0.5627 0.095 Uiso 1 1 calc R . . C24 C -0.0127(6) -0.1817(5) 0.6360(4) 0.054(3) Uani 1 1 d . . . H24 H -0.0419 -0.1770 0.6660 0.065 Uiso 1 1 calc R . . C25 C 0.0632(6) -0.1655(5) 0.6529(4) 0.054(3) Uani 1 1 d . . . H25 H 0.0864 -0.1474 0.6939 0.065 Uiso 1 1 calc R . . C26 C 0.1066(5) -0.1761(4) 0.6084(3) 0.042(2) Uani 1 1 d . . . H26 H 0.1592 -0.1657 0.6208 0.050 Uiso 1 1 calc R . . C31 C 0.2893(5) -0.3130(4) 0.6661(3) 0.0280(19) Uani 1 1 d . . . C32 C 0.2154(6) -0.3201(6) 0.6719(4) 0.071(4) Uani 1 1 d . . . H32 H 0.1733 -0.3142 0.6356 0.085 Uiso 1 1 calc R . . C33 C 0.2029(8) -0.3365(7) 0.7330(5) 0.106(5) Uani 1 1 d . . . H33 H 0.1528 -0.3429 0.7368 0.128 Uiso 1 1 calc R . . C34 C 0.2637(8) -0.3427(5) 0.7855(5) 0.070(3) Uani 1 1 d . . . H34 H 0.2551 -0.3523 0.8258 0.084 Uiso 1 1 calc R . . C35 C 0.3382(7) -0.3350(5) 0.7810(4) 0.057(3) Uani 1 1 d . . . H35 H 0.3798 -0.3396 0.8178 0.069 Uiso 1 1 calc R . . C36 C 0.3510(5) -0.3202(4) 0.7200(3) 0.042(2) Uani 1 1 d . . . H36 H 0.4013 -0.3153 0.7162 0.050 Uiso 1 1 calc R . . C41 C 0.3060(4) -0.0956(4) 0.6877(3) 0.0263(18) Uani 1 1 d . . . C42 C 0.3448(6) -0.1397(4) 0.7364(3) 0.045(3) Uani 1 1 d . . . H42 H 0.3758 -0.1741 0.7272 0.054 Uiso 1 1 calc R . . C43 C 0.3366(7) -0.1314(4) 0.7998(4) 0.068(4) Uani 1 1 d . . . H43 H 0.3612 -0.1612 0.8328 0.081 Uiso 1 1 calc R . . C44 C 0.2924(7) -0.0796(5) 0.8130(4) 0.064(3) Uani 1 1 d . . . H44 H 0.2883 -0.0741 0.8554 0.077 Uiso 1 1 calc R . . C45 C 0.2540(6) -0.0355(5) 0.7654(4) 0.054(3) Uani 1 1 d . . . H45 H 0.2236 -0.0008 0.7750 0.065 Uiso 1 1 calc R . . C46 C 0.2617(5) -0.0440(4) 0.7025(3) 0.036(2) Uani 1 1 d . . . H46 H 0.2364 -0.0143 0.6698 0.043 Uiso 1 1 calc R . . C51 C 0.2483(4) -0.3973(3) 0.2451(3) 0.0234(17) Uani 1 1 d . . . C52 C 0.2081(5) -0.3850(4) 0.1810(3) 0.0303(19) Uani 1 1 d . . . H52 H 0.1586 -0.3663 0.1716 0.036 Uiso 1 1 calc R . . C53 C 0.2406(5) -0.4001(4) 0.1310(4) 0.040(2) Uani 1 1 d . . . H53 H 0.2124 -0.3926 0.0880 0.048 Uiso 1 1 calc R . . C54 C 0.3141(5) -0.4262(4) 0.1438(4) 0.043(2) Uani 1 1 d . . . H54 H 0.3362 -0.4351 0.1097 0.051 Uiso 1 1 calc R . . C55 C 0.3557(5) -0.4392(4) 0.2079(4) 0.041(2) Uani 1 1 d . . . H55 H 0.4053 -0.4576 0.2168 0.049 Uiso 1 1 calc R . . C56 C 0.3226(5) -0.4248(4) 0.2580(4) 0.032(2) Uani 1 1 d . . . H56 H 0.3503 -0.4335 0.3009 0.038 Uiso 1 1 calc R . . C61 C 0.2664(4) -0.1578(3) 0.2721(3) 0.0168(16) Uani 1 1 d . . . C62 C 0.2614(4) -0.0926(4) 0.2486(3) 0.0280(18) Uani 1 1 d . . . H62 H 0.2536 -0.0570 0.2749 0.034 Uiso 1 1 calc R . . C63 C 0.2679(5) -0.0788(4) 0.1862(3) 0.035(2) Uani 1 1 d . . . H63 H 0.2630 -0.0346 0.1704 0.042 Uiso 1 1 calc R . . C64 C 0.2817(5) -0.1313(4) 0.1480(4) 0.038(2) Uani 1 1 d . . . H64 H 0.2865 -0.1224 0.1062 0.046 Uiso 1 1 calc R . . C65 C 0.2885(5) -0.1963(4) 0.1712(4) 0.047(2) Uani 1 1 d . . . H65 H 0.2985 -0.2315 0.1454 0.056 Uiso 1 1 calc R . . C66 C 0.2806(5) -0.2102(4) 0.2328(3) 0.034(2) Uani 1 1 d . . . H66 H 0.2848 -0.2547 0.2481 0.041 Uiso 1 1 calc R . . C71 C 0.4557(4) -0.3189(4) 0.3793(3) 0.0246(18) Uani 1 1 d . . . C72 C 0.4745(5) -0.2676(4) 0.3427(3) 0.033(2) Uani 1 1 d . . . H72 H 0.4463 -0.2273 0.3358 0.040 Uiso 1 1 calc R . . C73 C 0.5373(6) -0.2776(5) 0.3161(4) 0.055(3) Uani 1 1 d . . . H73 H 0.5506 -0.2434 0.2910 0.065 Uiso 1 1 calc R . . C74 C 0.5794(5) -0.3358(6) 0.3258(4) 0.059(3) Uani 1 1 d . . . H74 H 0.6217 -0.3404 0.3084 0.070 Uiso 1 1 calc R . . C75 C 0.5601(5) -0.3873(5) 0.3609(4) 0.055(3) Uani 1 1 d . . . H75 H 0.5889 -0.4273 0.3673 0.066 Uiso 1 1 calc R . . C76 C 0.4972(5) -0.3803(4) 0.3872(4) 0.040(2) Uani 1 1 d . . . H76 H 0.4827 -0.4161 0.4099 0.049 Uiso 1 1 calc R . . C81 C 0.4699(5) -0.0742(4) 0.3912(3) 0.0246(18) Uani 1 1 d . . . C82 C 0.4301(5) -0.0236(4) 0.3509(3) 0.035(2) Uani 1 1 d . . . H82 H 0.3821 -0.0091 0.3549 0.042 Uiso 1 1 calc R . . C83 C 0.4626(6) 0.0060(5) 0.3038(4) 0.052(3) Uani 1 1 d . . . H83 H 0.4362 0.0400 0.2764 0.062 Uiso 1 1 calc R . . C84 C 0.5342(6) -0.0162(5) 0.2991(4) 0.042(2) Uani 1 1 d . . . H84 H 0.5558 0.0033 0.2682 0.050 Uiso 1 1 calc R . . C85 C 0.5736(6) -0.0658(4) 0.3386(4) 0.045(3) Uani 1 1 d . . . H85 H 0.6217 -0.0802 0.3346 0.054 Uiso 1 1 calc R . . C86 C 0.5414(5) -0.0953(4) 0.3854(4) 0.038(2) Uani 1 1 d . . . H86 H 0.5683 -0.1292 0.4127 0.046 Uiso 1 1 calc R . . C91 C 0.2885(7) 0.2521(5) 0.5365(7) 0.102(5) Uani 1 1 d . . . H91A H 0.3346 0.2583 0.5724 0.122 Uiso 1 1 calc R . . H91B H 0.3031 0.2598 0.4963 0.122 Uiso 1 1 calc R . . C92 C -0.0757(6) 0.1226(5) 0.8636(4) 0.069(3) Uani 1 1 d . . . H92A H -0.1278 0.1245 0.8347 0.083 Uiso 1 1 calc R . . H92B H -0.0578 0.1687 0.8742 0.083 Uiso 1 1 calc R . . C93 C 0.0262(7) 0.0031(6) 0.6017(4) 0.074(3) Uani 1 1 d . . . H93A H -0.0216 -0.0216 0.5830 0.089 Uiso 1 1 calc R . . H93B H 0.0689 -0.0248 0.5966 0.089 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0356(4) 0.0313(3) 0.0424(3) 0.0188(2) 0.0178(3) 0.0091(3) I2 0.0462(4) 0.0293(3) 0.0300(3) -0.0011(2) 0.0153(3) 0.0022(3) I3 0.0248(3) 0.0336(3) 0.0211(2) -0.0013(2) 0.0010(2) 0.0040(2) I4 0.0232(3) 0.0641(4) 0.0264(3) 0.0032(3) 0.0039(2) -0.0086(3) Sn1 0.0224(3) 0.0199(3) 0.0198(2) 0.0017(2) 0.0093(2) -0.0023(2) Sn2 0.0171(3) 0.0195(3) 0.0158(2) 0.0007(2) 0.0057(2) 0.0000(2) Sn3 0.0179(3) 0.0298(3) 0.0138(2) 0.0018(2) 0.0048(2) 0.0019(2) Sn4 0.0244(3) 0.0316(3) 0.0177(2) -0.0083(2) 0.0096(2) -0.0089(2) Sn5 0.0206(3) 0.0175(3) 0.0158(2) -0.00176(19) 0.0063(2) -0.0024(2) Sn6 0.0200(3) 0.0164(2) 0.0150(2) 0.00085(19) 0.0059(2) -0.0009(2) Sn7 0.0172(3) 0.0221(3) 0.0146(2) 0.0017(2) 0.0049(2) 0.0018(2) Sn8 0.0259(3) 0.0285(3) 0.0187(2) -0.0067(2) 0.0105(2) -0.0118(2) Cl1 0.078(2) 0.0510(15) 0.0495(14) -0.0058(12) 0.0179(13) 0.0023(14) Cl2 0.115(3) 0.066(2) 0.142(3) -0.023(2) 0.023(3) 0.035(2) Cl3 0.197(5) 0.103(3) 0.112(3) -0.038(2) 0.089(3) -0.025(3) Cl4 0.092(3) 0.156(3) 0.0526(16) 0.0198(19) 0.0022(16) -0.048(2) Cl5 0.063(2) 0.0737(19) 0.0674(16) -0.0134(14) 0.0063(14) 0.0186(15) Cl6 0.133(3) 0.144(3) 0.0756(19) -0.040(2) 0.063(2) -0.077(3) O1 0.019(3) 0.017(2) 0.017(2) 0.001(2) 0.003(2) -0.001(2) O2 0.021(3) 0.020(3) 0.018(2) -0.001(2) 0.002(2) -0.002(2) O3 0.016(3) 0.020(3) 0.022(2) 0.000(2) 0.005(2) 0.000(2) O4 0.025(3) 0.036(3) 0.016(2) -0.005(2) 0.004(2) -0.004(2) O5 0.021(3) 0.014(2) 0.018(2) 0.0012(19) 0.006(2) 0.001(2) O6 0.018(3) 0.017(2) 0.015(2) 0.0014(19) 0.001(2) -0.001(2) O7 0.018(3) 0.019(3) 0.022(2) 0.000(2) 0.004(2) -0.001(2) O8 0.035(3) 0.015(2) 0.023(2) -0.003(2) 0.012(2) -0.004(2) C1 0.020(5) 0.027(4) 0.022(4) -0.003(3) 0.007(3) -0.005(3) C2 0.030(5) 0.021(4) 0.009(3) -0.004(3) 0.001(3) -0.006(3) C3 0.019(5) 0.029(4) 0.023(4) 0.002(3) 0.008(3) 0.003(3) C4 0.031(5) 0.042(5) 0.022(4) -0.010(4) 0.013(4) -0.013(4) C11 0.024(5) 0.022(4) 0.034(4) 0.001(3) 0.014(4) -0.003(4) C12 0.051(9) 0.234(17) 0.084(8) 0.107(10) 0.040(7) 0.063(9) C13 0.048(9) 0.262(19) 0.068(7) 0.104(10) 0.037(7) 0.035(10) C14 0.058(7) 0.046(6) 0.046(5) 0.008(4) 0.038(5) -0.007(5) C15 0.054(9) 0.156(13) 0.159(12) 0.097(11) 0.080(9) 0.050(8) C16 0.045(8) 0.161(12) 0.094(8) 0.096(9) 0.042(7) 0.035(8) C21 0.021(5) 0.019(4) 0.031(4) 0.001(3) 0.013(4) 0.004(3) C22 0.026(6) 0.124(10) 0.043(5) -0.033(6) 0.012(5) -0.015(6) C23 0.024(6) 0.159(12) 0.064(7) -0.041(7) 0.027(5) -0.016(7) C24 0.053(7) 0.069(7) 0.057(6) -0.003(5) 0.044(6) 0.008(6) C25 0.052(7) 0.086(8) 0.032(5) -0.019(5) 0.024(5) -0.009(6) C26 0.022(5) 0.081(7) 0.026(4) -0.007(4) 0.012(4) -0.015(5) C31 0.030(5) 0.034(5) 0.020(4) 0.002(3) 0.007(4) 0.001(4) C32 0.032(6) 0.142(10) 0.041(5) 0.053(6) 0.017(5) 0.008(6) C33 0.085(11) 0.190(14) 0.062(8) 0.059(9) 0.052(8) 0.040(10) C34 0.099(11) 0.084(8) 0.038(6) 0.006(6) 0.038(7) -0.001(8) C35 0.090(10) 0.052(6) 0.024(5) 0.006(4) 0.004(5) -0.010(6) C36 0.042(6) 0.055(6) 0.026(4) 0.009(4) 0.006(4) 0.007(5) C41 0.031(5) 0.033(4) 0.016(4) -0.006(3) 0.009(3) -0.014(4) C42 0.087(8) 0.032(5) 0.023(4) -0.005(4) 0.027(5) 0.002(5) C43 0.143(12) 0.040(6) 0.027(5) -0.001(4) 0.036(6) 0.013(6) C44 0.115(10) 0.056(7) 0.031(5) -0.013(5) 0.038(6) 0.003(6) C45 0.064(8) 0.069(7) 0.041(5) -0.016(5) 0.034(5) 0.006(6) C46 0.033(6) 0.049(5) 0.025(4) -0.007(4) 0.008(4) 0.009(4) C51 0.030(5) 0.014(4) 0.030(4) -0.004(3) 0.013(4) -0.008(3) C52 0.036(5) 0.036(5) 0.019(4) -0.003(3) 0.007(4) 0.006(4) C53 0.050(7) 0.043(5) 0.029(4) -0.004(4) 0.014(4) -0.003(5) C54 0.038(6) 0.065(6) 0.031(5) -0.017(4) 0.017(4) -0.016(5) C55 0.030(6) 0.056(6) 0.043(5) -0.021(4) 0.020(4) 0.004(4) C56 0.031(5) 0.038(5) 0.029(4) -0.011(4) 0.011(4) -0.002(4) C61 0.016(4) 0.025(4) 0.011(3) 0.004(3) 0.006(3) -0.001(3) C62 0.028(5) 0.037(5) 0.022(4) -0.004(3) 0.010(3) -0.005(4) C63 0.043(6) 0.032(5) 0.029(4) 0.013(4) 0.008(4) -0.014(4) C64 0.055(7) 0.040(5) 0.026(4) 0.007(4) 0.021(4) -0.007(4) C65 0.068(7) 0.043(5) 0.035(5) -0.002(4) 0.026(5) 0.010(5) C66 0.053(6) 0.031(5) 0.026(4) 0.004(4) 0.022(4) 0.005(4) C71 0.021(5) 0.039(5) 0.012(3) -0.007(3) 0.003(3) 0.001(4) C72 0.044(6) 0.033(5) 0.026(4) 0.000(4) 0.015(4) -0.008(4) C73 0.048(7) 0.085(8) 0.041(5) -0.016(5) 0.029(5) -0.027(6) C74 0.026(6) 0.118(10) 0.039(5) -0.028(6) 0.022(5) 0.000(6) C75 0.040(7) 0.089(8) 0.038(5) -0.007(5) 0.015(5) 0.035(6) C76 0.032(6) 0.057(6) 0.033(4) -0.005(4) 0.010(4) 0.012(5) C81 0.030(5) 0.025(4) 0.020(4) -0.009(3) 0.010(4) -0.018(4) C82 0.032(6) 0.046(5) 0.026(4) 0.001(4) 0.005(4) -0.015(4) C83 0.043(7) 0.081(7) 0.025(4) 0.017(5) -0.003(4) -0.029(6) C84 0.051(7) 0.060(6) 0.021(4) -0.016(4) 0.020(4) -0.034(5) C85 0.067(7) 0.037(5) 0.048(5) -0.016(4) 0.046(5) -0.018(5) C86 0.053(6) 0.028(4) 0.045(5) -0.008(4) 0.032(5) -0.012(4) C91 0.063(10) 0.060(8) 0.171(13) -0.039(8) 0.012(9) 0.004(7) C92 0.060(8) 0.100(9) 0.038(5) 0.003(6) -0.005(5) -0.028(7) C93 0.074(9) 0.103(9) 0.052(6) -0.010(6) 0.027(6) -0.008(7) _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 I1 Sn1 2.8919(7) . Y I1 Sn3 4.1174(7) . Y I2 Sn4 2.8824(8) . Y I2 Cl1 3.824(2) . Y I2 Cl5 3.926(3) . Y I2 Sn2 4.1099(7) . Y I3 Sn5 2.8984(7) . Y I3 O4 3.759(5) 4 Y I3 Sn6 4.0552(7) . Y I4 Sn8 2.8738(8) . Y I4 Sn7 4.0889(7) . Y Sn1 O1 2.040(4) . Y Sn1 C11 2.110(7) . Y Sn1 C1 2.138(6) . Y Sn1 O3 2.201(4) . Y Sn2 O1 2.064(4) . Y Sn2 C2 2.110(6) . Y Sn2 C21 2.113(7) . Y Sn2 O2 2.132(5) . Y Sn2 O3 2.167(4) . Y Sn3 O2 2.064(4) . Y Sn3 C3 2.111(6) . Y Sn3 O1 2.121(4) . Y Sn3 C31 2.127(7) . Y Sn3 O4 2.167(5) . Y Sn4 O2 2.045(4) . Y Sn4 C4 2.120(7) . Y Sn4 C41 2.146(6) . Y Sn4 O4 2.162(5) . Y Sn5 O5 2.027(4) . Y Sn5 C1 2.124(6) . Y Sn5 C51 2.134(7) . Y Sn5 O7 2.180(4) . Y Sn6 O6 2.058(4) . Y Sn6 C2 2.118(7) . Y Sn6 O5 2.122(4) . Y Sn6 C61 2.124(6) . Y Sn6 O8 2.148(4) . Y Sn7 O5 2.064(4) . Y Sn7 C3 2.101(6) . Y Sn7 O6 2.122(4) . Y Sn7 C71 2.125(7) . Y Sn7 O7 2.165(4) . Y Sn8 O6 2.028(4) . Y Sn8 C4 2.123(6) . Y Sn8 C81 2.144(7) . Y Sn8 O8 2.203(5) . Y Cl1 C91 1.754(11) . ? Cl2 C91 1.685(11) . ? Cl3 C92 1.726(11) . ? Cl3 Cl6 3.584(4) . Y Cl4 C92 1.755(9) . ? Cl5 C93 1.749(10) . ? Cl6 C93 1.744(9) . ? C11 C16 1.312(12) . ? C11 C12 1.332(11) . ? C12 C13 1.386(13) . ? C13 C14 1.276(13) . ? C14 C15 1.313(13) . ? C15 C16 1.398(12) . ? C21 C26 1.361(10) . ? C21 C22 1.376(11) . ? C22 C23 1.384(11) . ? C23 C24 1.345(12) . ? C24 C25 1.348(12) . ? C25 C26 1.389(10) . ? C31 C32 1.368(11) . ? C31 C36 1.370(10) . ? C32 C33 1.412(11) . ? C33 C34 1.340(15) . ? C34 C35 1.369(14) . ? C35 C36 1.406(11) . ? C41 C46 1.375(10) . ? C41 C42 1.387(10) . ? C42 C43 1.404(10) . ? C43 C44 1.364(12) . ? C44 C45 1.371(12) . ? C45 C46 1.390(10) . ? C51 C52 1.382(9) . ? C51 C56 1.395(10) . ? C52 C53 1.372(10) . ? C53 C54 1.370(11) . ? C54 C55 1.391(11) . ? C55 C56 1.378(9) . ? C61 C62 1.374(9) . ? C61 C66 1.392(9) . ? C62 C63 1.388(9) . ? C63 C64 1.378(10) . ? C64 C65 1.367(11) . ? C65 C66 1.383(10) . ? C71 C72 1.370(10) . ? C71 C76 1.407(10) . ? C72 C73 1.401(11) . ? C73 C74 1.356(13) . ? C74 C75 1.359(13) . ? C75 C76 1.389(11) . ? C81 C86 1.380(10) . ? C81 C82 1.382(10) . ? C82 C83 1.411(10) . ? C83 C84 1.382(12) . ? C84 C85 1.358(12) . ? C85 C86 1.401(10) . ? 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 Sn1 I1 Sn3 65.991(15) . . Y Sn4 I2 Cl1 115.58(5) . . Y Sn4 I2 Cl5 138.09(4) . . Y Cl1 I2 Cl5 73.53(6) . . Y Sn4 I2 Sn2 66.764(15) . . Y Cl1 I2 Sn2 171.35(4) . . Y Cl5 I2 Sn2 110.67(5) . . Y Sn5 I3 O4 141.25(7) . 4 Y Sn5 I3 Sn6 66.743(15) . . Y O4 I3 Sn6 150.30(7) 4 . Y Sn8 I4 Sn7 66.292(15) . . Y O1 Sn1 C11 109.0(2) . . Y O1 Sn1 C1 118.7(2) . . Y C11 Sn1 C1 131.2(3) . . Y O1 Sn1 O3 74.63(17) . . Y C11 Sn1 O3 92.8(2) . . Y C1 Sn1 O3 90.4(2) . . Y O1 Sn1 I1 90.14(12) . . Y C11 Sn1 I1 97.5(2) . . Y C1 Sn1 I1 92.2(2) . . Y O3 Sn1 I1 163.81(12) . . Y O1 Sn2 C2 120.9(2) . . Y O1 Sn2 C21 109.7(2) . . Y C2 Sn2 C21 129.3(3) . . Y O1 Sn2 O2 74.04(17) . . Y C2 Sn2 O2 97.9(2) . . Y C21 Sn2 O2 98.6(2) . . Y O1 Sn2 O3 74.89(17) . . Y C2 Sn2 O3 95.3(2) . . Y C21 Sn2 O3 94.7(2) . . Y O2 Sn2 O3 148.76(17) . . Y O1 Sn2 I2 132.80(12) . . Y C2 Sn2 I2 67.83(17) . . Y C21 Sn2 I2 80.89(19) . . Y O2 Sn2 I2 58.81(12) . . Y O3 Sn2 I2 151.91(12) . . Y O2 Sn3 C3 121.4(2) . . Y O2 Sn3 O1 74.27(17) . . Y C3 Sn3 O1 97.6(2) . . Y O2 Sn3 C31 110.7(2) . . Y C3 Sn3 C31 127.5(3) . . Y O1 Sn3 C31 102.0(2) . . Y O2 Sn3 O4 73.98(18) . . Y C3 Sn3 O4 93.8(2) . . Y O1 Sn3 O4 147.71(17) . . Y C31 Sn3 O4 94.6(2) . . Y O2 Sn3 I1 133.62(12) . . Y C3 Sn3 I1 67.2(2) . . Y O1 Sn3 I1 59.38(11) . . Y C31 Sn3 I1 82.2(2) . . Y O4 Sn3 I1 151.56(13) . . Y O2 Sn4 C4 118.2(2) . . Y O2 Sn4 C41 112.8(2) . . Y C4 Sn4 C41 128.4(3) . . Y O2 Sn4 O4 74.45(18) . . Y C4 Sn4 O4 92.0(3) . . Y C41 Sn4 O4 94.0(2) . . Y O2 Sn4 I2 89.36(13) . . Y C4 Sn4 I2 91.5(2) . . Y C41 Sn4 I2 96.7(2) . . Y O4 Sn4 I2 163.13(12) . . Y O5 Sn5 C1 119.0(2) . . Y O5 Sn5 C51 109.6(2) . . Y C1 Sn5 C51 130.5(2) . . Y O5 Sn5 O7 74.96(17) . . Y C1 Sn5 O7 91.6(2) . . Y C51 Sn5 O7 92.1(2) . . Y O5 Sn5 I3 89.11(12) . . Y C1 Sn5 I3 91.5(2) . . Y C51 Sn5 I3 98.4(2) . . Y O7 Sn5 I3 163.18(11) . . Y O6 Sn6 C2 121.4(2) . . Y O6 Sn6 O5 73.53(17) . . Y C2 Sn6 O5 98.6(2) . . Y O6 Sn6 C61 110.4(2) . . Y C2 Sn6 C61 128.0(2) . . Y O5 Sn6 C61 99.1(2) . . Y O6 Sn6 O8 75.24(17) . . Y C2 Sn6 O8 94.7(2) . . Y O5 Sn6 O8 148.59(17) . . Y C61 Sn6 O8 94.7(2) . . Y O6 Sn6 I3 133.47(12) . . Y C2 Sn6 I3 68.85(17) . . Y O5 Sn6 I3 59.94(12) . . Y C61 Sn6 I3 79.02(18) . . Y O8 Sn6 I3 151.12(13) . . Y O5 Sn7 C3 123.3(2) . . Y O5 Sn7 O6 73.43(17) . . Y C3 Sn7 O6 97.4(2) . . Y O5 Sn7 C71 115.0(2) . . Y C3 Sn7 C71 121.6(3) . . Y O6 Sn7 C71 100.5(2) . . Y O5 Sn7 O7 74.58(16) . . Y C3 Sn7 O7 96.3(2) . . Y O6 Sn7 O7 147.68(17) . . Y C71 Sn7 O7 96.9(2) . . Y O5 Sn7 I4 132.98(12) . . Y C3 Sn7 I4 67.9(2) . . Y O6 Sn7 I4 59.58(12) . . Y C71 Sn7 I4 74.78(18) . . Y O7 Sn7 I4 152.34(12) . . Y O6 Sn8 C4 118.1(2) . . Y O6 Sn8 C81 111.9(2) . . Y C4 Sn8 C81 128.5(3) . . Y O6 Sn8 O8 74.61(17) . . Y C4 Sn8 O8 90.4(2) . . Y C81 Sn8 O8 91.2(2) . . Y O6 Sn8 I4 90.31(13) . . Y C4 Sn8 I4 93.1(2) . . Y C81 Sn8 I4 98.5(2) . . Y O8 Sn8 I4 164.35(11) . . Y C91 Cl1 I2 173.5(4) . . Y C92 Cl3 Cl6 153.5(4) . . Y C93 Cl5 I2 76.9(4) . . Y C93 Cl6 Cl3 156.4(4) . . Y Sn1 O1 Sn2 109.5(2) . . Y Sn1 O1 Sn3 143.6(2) . . Y Sn2 O1 Sn3 105.84(18) . . Y Sn4 O2 Sn3 109.4(2) . . Y Sn4 O2 Sn2 144.8(2) . . Y Sn3 O2 Sn2 105.43(19) . . Y Sn2 O3 Sn1 100.25(18) . . Y Sn4 O4 Sn3 101.5(2) . . Y Sn5 O5 Sn7 109.34(19) . . Y Sn5 O5 Sn6 143.9(2) . . Y Sn7 O5 Sn6 106.33(19) . . Y Sn8 O6 Sn6 109.29(19) . . Y Sn8 O6 Sn7 143.4(2) . . Y Sn6 O6 Sn7 106.56(19) . . Y Sn7 O7 Sn5 100.35(17) . . Y Sn6 O8 Sn8 99.99(18) . . Y Sn5 C1 Sn1 116.0(3) . . Y Sn2 C2 Sn6 117.7(3) . . Y Sn7 C3 Sn3 117.8(3) . . Y Sn4 C4 Sn8 117.6(3) . . Y C16 C11 C12 113.8(8) . . ? C16 C11 Sn1 123.2(6) . . ? C12 C11 Sn1 122.9(7) . . ? C11 C12 C13 122.8(10) . . ? C14 C13 C12 122.0(10) . . ? C13 C14 C15 117.2(9) . . ? C14 C15 C16 120.7(10) . . ? C11 C16 C15 123.0(9) . . ? C26 C21 C22 116.6(7) . . ? C26 C21 Sn2 121.5(6) . . ? C22 C21 Sn2 121.7(6) . . ? C21 C22 C23 120.5(8) . . ? C24 C23 C22 121.3(9) . . ? C23 C24 C25 119.5(8) . . ? C24 C25 C26 119.2(8) . . ? C21 C26 C25 122.7(8) . . ? C32 C31 C36 119.7(7) . . ? C32 C31 Sn3 121.0(6) . . ? C36 C31 Sn3 119.1(6) . . ? C31 C32 C33 120.0(9) . . ? C34 C33 C32 119.7(11) . . ? C33 C34 C35 121.4(9) . . ? C34 C35 C36 119.1(9) . . ? C31 C36 C35 120.1(9) . . ? C46 C41 C42 119.7(6) . . ? C46 C41 Sn4 123.5(5) . . ? C42 C41 Sn4 116.8(5) . . ? C41 C42 C43 119.0(8) . . ? C44 C43 C42 119.9(9) . . ? C43 C44 C45 121.7(8) . . ? C44 C45 C46 118.3(8) . . ? C41 C46 C45 121.3(8) . . ? C52 C51 C56 118.7(7) . . ? C52 C51 Sn5 122.7(6) . . ? C56 C51 Sn5 118.5(5) . . ? C53 C52 C51 120.7(8) . . ? C54 C53 C52 120.6(8) . . ? C53 C54 C55 119.9(7) . . ? C56 C55 C54 119.5(8) . . ? C55 C56 C51 120.7(7) . . ? C62 C61 C66 118.8(6) . . ? C62 C61 Sn6 119.4(5) . . ? C66 C61 Sn6 121.8(5) . . ? C61 C62 C63 121.1(7) . . ? C64 C63 C62 119.4(7) . . ? C65 C64 C63 120.2(7) . . ? C64 C65 C66 120.4(7) . . ? C65 C66 C61 120.1(7) . . ? C72 C71 C76 120.0(7) . . ? C72 C71 Sn7 122.2(6) . . ? C76 C71 Sn7 117.7(5) . . ? C71 C72 C73 118.0(8) . . ? C74 C73 C72 122.1(9) . . ? C73 C74 C75 120.2(8) . . ? C74 C75 C76 119.9(9) . . ? C75 C76 C71 119.8(8) . . ? C86 C81 C82 120.0(7) . . ? C86 C81 Sn8 122.5(6) . . ? C82 C81 Sn8 117.6(6) . . ? C81 C82 C83 119.8(8) . . ? C84 C83 C82 119.0(8) . . ? C85 C84 C83 121.4(8) . . ? C84 C85 C86 119.6(9) . . ? C81 C86 C85 120.3(8) . . ? Cl2 C91 Cl1 114.7(7) . . ? Cl3 C92 Cl4 109.5(6) . . ? Cl6 C93 Cl5 112.7(6) . . ? 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 Sn3 I1 Sn1 O1 4.28(11) . . . . ? Sn3 I1 Sn1 C11 -104.96(19) . . . . ? Sn3 I1 Sn1 C1 122.98(18) . . . . ? Sn3 I1 Sn1 O3 23.8(4) . . . . ? Sn4 I2 Sn2 O1 -5.35(16) . . . . ? Cl1 I2 Sn2 O1 102.2(3) . . . . ? Cl5 I2 Sn2 O1 -140.07(16) . . . . ? Sn4 I2 Sn2 C2 -117.6(2) . . . . ? Cl1 I2 Sn2 C2 -10.0(4) . . . . ? Cl5 I2 Sn2 C2 107.7(2) . . . . ? Sn4 I2 Sn2 C21 103.2(2) . . . . ? Cl1 I2 Sn2 C21 -149.2(4) . . . . ? Cl5 I2 Sn2 C21 -31.5(2) . . . . ? Sn4 I2 Sn2 O2 -2.75(13) . . . . ? Cl1 I2 Sn2 O2 104.8(3) . . . . ? Cl5 I2 Sn2 O2 -137.47(14) . . . . ? Sn4 I2 Sn2 O3 -174.0(2) . . . . ? Cl1 I2 Sn2 O3 -66.4(4) . . . . ? Cl5 I2 Sn2 O3 51.3(2) . . . . ? Sn1 I1 Sn3 O2 -7.10(17) . . . . ? Sn1 I1 Sn3 C3 -119.4(2) . . . . ? Sn1 I1 Sn3 O1 -4.78(13) . . . . ? Sn1 I1 Sn3 C31 104.2(2) . . . . ? Sn1 I1 Sn3 O4 -170.6(2) . . . . ? Cl1 I2 Sn4 O2 -168.40(13) . . . . ? Cl5 I2 Sn4 O2 98.00(14) . . . . ? Sn2 I2 Sn4 O2 2.46(12) . . . . ? Cl1 I2 Sn4 C4 -50.22(18) . . . . ? Cl5 I2 Sn4 C4 -143.82(19) . . . . ? Sn2 I2 Sn4 C4 120.63(18) . . . . ? Cl1 I2 Sn4 C41 78.72(19) . . . . ? Cl5 I2 Sn4 C41 -14.9(2) . . . . ? Sn2 I2 Sn4 C41 -110.43(19) . . . . ? Cl1 I2 Sn4 O4 -152.3(4) . . . . ? Cl5 I2 Sn4 O4 114.1(4) . . . . ? Sn2 I2 Sn4 O4 18.6(4) . . . . ? O4 I3 Sn5 O5 169.68(16) 4 . . . ? Sn6 I3 Sn5 O5 2.51(12) . . . . ? O4 I3 Sn5 C1 -71.3(2) 4 . . . ? Sn6 I3 Sn5 C1 121.50(17) . . . . ? O4 I3 Sn5 C51 60.0(2) 4 . . . ? Sn6 I3 Sn5 C51 -107.15(18) . . . . ? O4 I3 Sn5 O7 -171.8(4) 4 . . . ? Sn6 I3 Sn5 O7 21.0(4) . . . . ? Sn5 I3 Sn6 O6 -3.19(16) . . . . ? O4 I3 Sn6 O6 -166.9(2) 4 . . . ? Sn5 I3 Sn6 C2 -116.94(18) . . . . ? O4 I3 Sn6 C2 79.4(2) 4 . . . ? Sn5 I3 Sn6 O5 -2.77(13) . . . . ? O4 I3 Sn6 O5 -166.47(19) 4 . . . ? Sn5 I3 Sn6 C61 104.64(19) . . . . ? O4 I3 Sn6 C61 -59.1(2) 4 . . . ? Sn5 I3 Sn6 O8 -175.7(2) . . . . ? O4 I3 Sn6 O8 20.6(3) 4 . . . ? Sn8 I4 Sn7 O5 -1.18(16) . . . . ? Sn8 I4 Sn7 C3 -116.8(2) . . . . ? Sn8 I4 Sn7 O6 -3.21(13) . . . . ? Sn8 I4 Sn7 C71 109.0(2) . . . . ? Sn8 I4 Sn7 O7 -175.4(2) . . . . ? Sn7 I4 Sn8 O6 2.89(12) . . . . ? Sn7 I4 Sn8 C4 121.01(19) . . . . ? Sn7 I4 Sn8 C81 -109.28(17) . . . . ? Sn7 I4 Sn8 O8 18.1(4) . . . . ? Sn4 I2 Cl1 C91 79(4) . . . . ? Cl5 I2 Cl1 C91 -145(4) . . . . ? Sn2 I2 Cl1 C91 -25(4) . . . . ? Sn4 I2 Cl5 C93 -34.2(4) . . . . ? Cl1 I2 Cl5 C93 -144.3(4) . . . . ? Sn2 I2 Cl5 C93 43.7(3) . . . . ? C92 Cl3 Cl6 C93 8.9(14) . . . . ? C11 Sn1 O1 Sn2 -80.8(3) . . . . ? C1 Sn1 O1 Sn2 88.7(3) . . . . ? O3 Sn1 O1 Sn2 6.82(17) . . . . ? I1 Sn1 O1 Sn2 -178.73(16) . . . . ? C11 Sn1 O1 Sn3 85.1(4) . . . . ? C1 Sn1 O1 Sn3 -105.5(4) . . . . ? O3 Sn1 O1 Sn3 172.7(4) . . . . ? I1 Sn1 O1 Sn3 -12.9(3) . . . . ? C2 Sn2 O1 Sn1 -94.0(3) . . . . ? C21 Sn2 O1 Sn1 82.7(3) . . . . ? O2 Sn2 O1 Sn1 176.3(2) . . . . ? O3 Sn2 O1 Sn1 -6.92(17) . . . . ? I2 Sn2 O1 Sn1 178.60(6) . . . . ? C2 Sn2 O1 Sn3 94.7(3) . . . . ? C21 Sn2 O1 Sn3 -88.6(3) . . . . ? O2 Sn2 O1 Sn3 4.96(17) . . . . ? O3 Sn2 O1 Sn3 -178.2(2) . . . . ? I2 Sn2 O1 Sn3 7.3(3) . . . . ? O2 Sn3 O1 Sn1 -171.2(4) . . . . ? C3 Sn3 O1 Sn1 68.2(4) . . . . ? C31 Sn3 O1 Sn1 -62.8(4) . . . . ? O4 Sn3 O1 Sn1 177.9(3) . . . . ? I1 Sn3 O1 Sn1 10.5(3) . . . . ? O2 Sn3 O1 Sn2 -5.11(17) . . . . ? C3 Sn3 O1 Sn2 -125.7(2) . . . . ? C31 Sn3 O1 Sn2 103.3(3) . . . . ? O4 Sn3 O1 Sn2 -16.0(4) . . . . ? I1 Sn3 O1 Sn2 176.6(2) . . . . ? C4 Sn4 O2 Sn3 90.5(3) . . . . ? C41 Sn4 O2 Sn3 -81.1(3) . . . . ? O4 Sn4 O2 Sn3 6.73(18) . . . . ? I2 Sn4 O2 Sn3 -178.07(17) . . . . ? C4 Sn4 O2 Sn2 -99.0(4) . . . . ? C41 Sn4 O2 Sn2 89.4(4) . . . . ? O4 Sn4 O2 Sn2 177.2(4) . . . . ? I2 Sn4 O2 Sn2 -7.6(4) . . . . ? C3 Sn3 O2 Sn4 -91.3(3) . . . . ? O1 Sn3 O2 Sn4 179.3(2) . . . . ? C31 Sn3 O2 Sn4 82.1(3) . . . . ? O4 Sn3 O2 Sn4 -6.74(18) . . . . ? I1 Sn3 O2 Sn4 -178.66(6) . . . . ? C3 Sn3 O2 Sn2 94.4(3) . . . . ? O1 Sn3 O2 Sn2 4.94(16) . . . . ? C31 Sn3 O2 Sn2 -92.2(3) . . . . ? O4 Sn3 O2 Sn2 178.9(2) . . . . ? I1 Sn3 O2 Sn2 7.0(3) . . . . ? O1 Sn2 O2 Sn4 -175.8(4) . . . . ? C2 Sn2 O2 Sn4 64.3(4) . . . . ? C21 Sn2 O2 Sn4 -67.6(4) . . . . ? O3 Sn2 O2 Sn4 178.2(3) . . . . ? I2 Sn2 O2 Sn4 6.2(3) . . . . ? O1 Sn2 O2 Sn3 -5.08(17) . . . . ? C2 Sn2 O2 Sn3 -125.0(2) . . . . ? C21 Sn2 O2 Sn3 103.1(2) . . . . ? O3 Sn2 O2 Sn3 -11.0(4) . . . . ? I2 Sn2 O2 Sn3 176.9(2) . . . . ? O1 Sn2 O3 Sn1 6.14(16) . . . . ? C2 Sn2 O3 Sn1 126.7(2) . . . . ? C21 Sn2 O3 Sn1 -103.1(2) . . . . ? O2 Sn2 O3 Sn1 12.1(4) . . . . ? I2 Sn2 O3 Sn1 177.53(9) . . . . ? O1 Sn1 O3 Sn2 -6.22(16) . . . . ? C11 Sn1 O3 Sn2 102.8(2) . . . . ? C1 Sn1 O3 Sn2 -125.9(2) . . . . ? I1 Sn1 O3 Sn2 -26.5(5) . . . . ? O2 Sn4 O4 Sn3 -6.17(16) . . . . ? C4 Sn4 O4 Sn3 -124.9(2) . . . . ? C41 Sn4 O4 Sn3 106.4(2) . . . . ? I2 Sn4 O4 Sn3 -22.9(5) . . . . ? O2 Sn3 O4 Sn4 6.13(16) . . . . ? C3 Sn3 O4 Sn4 127.8(2) . . . . ? O1 Sn3 O4 Sn4 17.0(4) . . . . ? C31 Sn3 O4 Sn4 -104.1(2) . . . . ? I1 Sn3 O4 Sn4 173.80(8) . . . . ? C1 Sn5 O5 Sn7 90.4(3) . . . . ? C51 Sn5 O5 Sn7 -79.7(3) . . . . ? O7 Sn5 O5 Sn7 7.11(17) . . . . ? I3 Sn5 O5 Sn7 -178.36(16) . . . . ? C1 Sn5 O5 Sn6 -98.7(4) . . . . ? C51 Sn5 O5 Sn6 91.1(4) . . . . ? O7 Sn5 O5 Sn6 178.0(4) . . . . ? I3 Sn5 O5 Sn6 -7.5(4) . . . . ? C3 Sn7 O5 Sn5 -94.5(3) . . . . ? O6 Sn7 O5 Sn5 177.4(2) . . . . ? C71 Sn7 O5 Sn5 83.4(3) . . . . ? O7 Sn7 O5 Sn5 -7.17(17) . . . . ? I4 Sn7 O5 Sn5 175.62(6) . . . . ? C3 Sn7 O5 Sn6 91.1(3) . . . . ? O6 Sn7 O5 Sn6 3.03(16) . . . . ? C71 Sn7 O5 Sn6 -91.0(3) . . . . ? O7 Sn7 O5 Sn6 178.4(2) . . . . ? I4 Sn7 O5 Sn6 1.2(3) . . . . ? O6 Sn6 O5 Sn5 -174.1(4) . . . . ? C2 Sn6 O5 Sn5 65.6(4) . . . . ? C61 Sn6 O5 Sn5 -65.4(4) . . . . ? O8 Sn6 O5 Sn5 179.6(3) . . . . ? I3 Sn6 O5 Sn5 6.2(3) . . . . ? O6 Sn6 O5 Sn7 -3.12(17) . . . . ? C2 Sn6 O5 Sn7 -123.4(2) . . . . ? C61 Sn6 O5 Sn7 105.6(2) . . . . ? O8 Sn6 O5 Sn7 -9.3(4) . . . . ? I3 Sn6 O5 Sn7 177.2(2) . . . . ? C4 Sn8 O6 Sn6 89.6(3) . . . . ? C81 Sn8 O6 Sn6 -77.5(3) . . . . ? O8 Sn8 O6 Sn6 7.48(17) . . . . ? I4 Sn8 O6 Sn6 -176.74(16) . . . . ? C4 Sn8 O6 Sn7 -102.3(4) . . . . ? C81 Sn8 O6 Sn7 90.7(4) . . . . ? O8 Sn8 O6 Sn7 175.6(4) . . . . ? I4 Sn8 O6 Sn7 -8.6(3) . . . . ? C2 Sn6 O6 Sn8 -94.2(3) . . . . ? O5 Sn6 O6 Sn8 175.7(2) . . . . ? C61 Sn6 O6 Sn8 81.9(3) . . . . ? O8 Sn6 O6 Sn8 -7.65(18) . . . . ? I3 Sn6 O6 Sn8 176.09(6) . . . . ? C2 Sn6 O6 Sn7 93.2(3) . . . . ? O5 Sn6 O6 Sn7 3.04(16) . . . . ? C61 Sn6 O6 Sn7 -90.8(2) . . . . ? O8 Sn6 O6 Sn7 179.7(2) . . . . ? I3 Sn6 O6 Sn7 3.4(3) . . . . ? O5 Sn7 O6 Sn8 -171.5(4) . . . . ? C3 Sn7 O6 Sn8 65.9(4) . . . . ? C71 Sn7 O6 Sn8 -58.3(4) . . . . ? O7 Sn7 O6 Sn8 -179.8(3) . . . . ? I4 Sn7 O6 Sn8 7.0(3) . . . . ? O5 Sn7 O6 Sn6 -3.13(17) . . . . ? C3 Sn7 O6 Sn6 -125.8(2) . . . . ? C71 Sn7 O6 Sn6 110.1(2) . . . . ? O7 Sn7 O6 Sn6 -11.5(4) . . . . ? I4 Sn7 O6 Sn6 175.3(2) . . . . ? O5 Sn7 O7 Sn5 6.39(15) . . . . ? C3 Sn7 O7 Sn5 129.3(2) . . . . ? O6 Sn7 O7 Sn5 14.7(4) . . . . ? C71 Sn7 O7 Sn5 -107.7(2) . . . . ? I4 Sn7 O7 Sn5 -178.00(9) . . . . ? O5 Sn5 O7 Sn7 -6.49(16) . . . . ? C1 Sn5 O7 Sn7 -126.2(2) . . . . ? C51 Sn5 O7 Sn7 103.2(2) . . . . ? I3 Sn5 O7 Sn7 -25.7(5) . . . . ? O6 Sn6 O8 Sn8 6.74(16) . . . . ? C2 Sn6 O8 Sn8 128.0(2) . . . . ? O5 Sn6 O8 Sn8 12.9(4) . . . . ? C61 Sn6 O8 Sn8 -103.2(2) . . . . ? I3 Sn6 O8 Sn8 -178.88(8) . . . . ? O6 Sn8 O8 Sn6 -6.86(16) . . . . ? C4 Sn8 O8 Sn6 -125.9(2) . . . . ? C81 Sn8 O8 Sn6 105.5(2) . . . . ? I4 Sn8 O8 Sn6 -22.7(5) . . . . ? O5 Sn5 C1 Sn1 -7.5(4) . . . . ? C51 Sn5 C1 Sn1 160.2(3) . . . . ? O7 Sn5 C1 Sn1 66.1(3) . . . . ? I3 Sn5 C1 Sn1 -97.4(3) . . . . ? O1 Sn1 C1 Sn5 0.0(4) . . . . ? C11 Sn1 C1 Sn5 166.7(3) . . . . ? O3 Sn1 C1 Sn5 72.6(3) . . . . ? I1 Sn1 C1 Sn5 -91.4(3) . . . . ? O1 Sn2 C2 Sn6 -26.2(4) . . . . ? C21 Sn2 C2 Sn6 157.9(3) . . . . ? O2 Sn2 C2 Sn6 49.9(3) . . . . ? O3 Sn2 C2 Sn6 -101.7(3) . . . . ? I2 Sn2 C2 Sn6 101.5(3) . . . . ? O6 Sn6 C2 Sn2 -27.0(4) . . . . ? O5 Sn6 C2 Sn2 48.9(3) . . . . ? C61 Sn6 C2 Sn2 157.7(3) . . . . ? O8 Sn6 C2 Sn2 -102.6(3) . . . . ? I3 Sn6 C2 Sn2 101.9(3) . . . . ? O5 Sn7 C3 Sn3 -24.1(5) . . . . ? O6 Sn7 C3 Sn3 50.9(4) . . . . ? C71 Sn7 C3 Sn3 158.1(3) . . . . ? O7 Sn7 C3 Sn3 -99.8(3) . . . . ? I4 Sn7 C3 Sn3 103.7(4) . . . . ? O2 Sn3 C3 Sn7 -29.6(5) . . . . ? O1 Sn3 C3 Sn7 46.6(4) . . . . ? C31 Sn3 C3 Sn7 158.2(3) . . . . ? O4 Sn3 C3 Sn7 -103.1(3) . . . . ? I1 Sn3 C3 Sn7 98.7(4) . . . . ? O2 Sn4 C4 Sn8 -5.8(5) . . . . ? C41 Sn4 C4 Sn8 164.3(3) . . . . ? O4 Sn4 C4 Sn8 67.6(4) . . . . ? I2 Sn4 C4 Sn8 -95.9(4) . . . . ? O6 Sn8 C4 Sn4 -2.2(5) . . . . ? C81 Sn8 C4 Sn4 162.3(3) . . . . ? O8 Sn8 C4 Sn4 70.5(4) . . . . ? I4 Sn8 C4 Sn4 -94.2(4) . . . . ? O1 Sn1 C11 C16 100.1(9) . . . . ? C1 Sn1 C11 C16 -67.6(10) . . . . ? O3 Sn1 C11 C16 25.4(9) . . . . ? I1 Sn1 C11 C16 -167.2(9) . . . . ? O1 Sn1 C11 C12 -77.7(10) . . . . ? C1 Sn1 C11 C12 114.6(10) . . . . ? O3 Sn1 C11 C12 -152.4(10) . . . . ? I1 Sn1 C11 C12 15.1(10) . . . . ? C16 C11 C12 C13 -5(2) . . . . ? Sn1 C11 C12 C13 172.9(12) . . . . ? C11 C12 C13 C14 -1(3) . . . . ? C12 C13 C14 C15 6(2) . . . . ? C13 C14 C15 C16 -6(2) . . . . ? C12 C11 C16 C15 5.4(19) . . . . ? Sn1 C11 C16 C15 -172.5(11) . . . . ? C14 C15 C16 C11 0(2) . . . . ? O1 Sn2 C21 C26 77.6(7) . . . . ? C2 Sn2 C21 C26 -106.1(7) . . . . ? O2 Sn2 C21 C26 1.6(7) . . . . ? O3 Sn2 C21 C26 153.2(6) . . . . ? I2 Sn2 C21 C26 -54.7(6) . . . . ? O1 Sn2 C21 C22 -98.9(7) . . . . ? C2 Sn2 C21 C22 77.5(8) . . . . ? O2 Sn2 C21 C22 -174.9(7) . . . . ? O3 Sn2 C21 C22 -23.3(7) . . . . ? I2 Sn2 C21 C22 128.8(7) . . . . ? C26 C21 C22 C23 2.4(15) . . . . ? Sn2 C21 C22 C23 179.1(8) . . . . ? C21 C22 C23 C24 -4.4(18) . . . . ? C22 C23 C24 C25 4.8(18) . . . . ? C23 C24 C25 C26 -3.2(16) . . . . ? C22 C21 C26 C25 -1.0(13) . . . . ? Sn2 C21 C26 C25 -177.6(7) . . . . ? C24 C25 C26 C21 1.4(15) . . . . ? O2 Sn3 C31 C32 54.9(8) . . . . ? C3 Sn3 C31 C32 -132.2(8) . . . . ? O1 Sn3 C31 C32 -22.7(8) . . . . ? O4 Sn3 C31 C32 129.4(8) . . . . ? I1 Sn3 C31 C32 -79.0(8) . . . . ? O2 Sn3 C31 C36 -119.6(6) . . . . ? C3 Sn3 C31 C36 53.3(7) . . . . ? O1 Sn3 C31 C36 162.9(6) . . . . ? O4 Sn3 C31 C36 -45.0(6) . . . . ? I1 Sn3 C31 C36 106.6(6) . . . . ? C36 C31 C32 C33 -1.5(16) . . . . ? Sn3 C31 C32 C33 -175.9(9) . . . . ? C31 C32 C33 C34 2(2) . . . . ? C32 C33 C34 C35 -2(2) . . . . ? C33 C34 C35 C36 0.2(17) . . . . ? C32 C31 C36 C35 0.1(13) . . . . ? Sn3 C31 C36 C35 174.6(6) . . . . ? C34 C35 C36 C31 0.6(14) . . . . ? O2 Sn4 C41 C46 -102.8(6) . . . . ? C4 Sn4 C41 C46 86.6(7) . . . . ? O4 Sn4 C41 C46 -177.6(6) . . . . ? I2 Sn4 C41 C46 -10.7(7) . . . . ? O2 Sn4 C41 C42 77.4(6) . . . . ? C4 Sn4 C41 C42 -93.1(7) . . . . ? O4 Sn4 C41 C42 2.6(6) . . . . ? I2 Sn4 C41 C42 169.6(6) . . . . ? C46 C41 C42 C43 1.4(13) . . . . ? Sn4 C41 C42 C43 -178.9(7) . . . . ? C41 C42 C43 C44 -1.5(15) . . . . ? C42 C43 C44 C45 1.3(17) . . . . ? C43 C44 C45 C46 -0.8(16) . . . . ? C42 C41 C46 C45 -0.9(13) . . . . ? Sn4 C41 C46 C45 179.3(6) . . . . ? C44 C45 C46 C41 0.6(14) . . . . ? O5 Sn5 C51 C52 -102.4(6) . . . . ? C1 Sn5 C51 C52 89.0(6) . . . . ? O7 Sn5 C51 C52 -177.2(6) . . . . ? I3 Sn5 C51 C52 -10.3(6) . . . . ? O5 Sn5 C51 C56 73.0(6) . . . . ? C1 Sn5 C51 C56 -95.6(6) . . . . ? O7 Sn5 C51 C56 -1.7(6) . . . . ? I3 Sn5 C51 C56 165.1(5) . . . . ? C56 C51 C52 C53 0.5(11) . . . . ? Sn5 C51 C52 C53 175.9(6) . . . . ? C51 C52 C53 C54 -1.5(12) . . . . ? C52 C53 C54 C55 1.8(13) . . . . ? C53 C54 C55 C56 -1.0(13) . . . . ? C54 C55 C56 C51 -0.1(12) . . . . ? C52 C51 C56 C55 0.3(11) . . . . ? Sn5 C51 C56 C55 -175.3(6) . . . . ? O6 Sn6 C61 C62 -108.1(6) . . . . ? C2 Sn6 C61 C62 67.6(7) . . . . ? O5 Sn6 C61 C62 176.2(6) . . . . ? O8 Sn6 C61 C62 -32.1(6) . . . . ? I3 Sn6 C61 C62 119.4(6) . . . . ? O6 Sn6 C61 C66 71.8(6) . . . . ? C2 Sn6 C61 C66 -112.5(6) . . . . ? O5 Sn6 C61 C66 -3.9(6) . . . . ? O8 Sn6 C61 C66 147.8(6) . . . . ? I3 Sn6 C61 C66 -60.7(6) . . . . ? C66 C61 C62 C63 2.0(11) . . . . ? Sn6 C61 C62 C63 -178.1(6) . . . . ? C61 C62 C63 C64 -1.8(12) . . . . ? C62 C63 C64 C65 0.4(13) . . . . ? C63 C64 C65 C66 0.9(14) . . . . ? C64 C65 C66 C61 -0.6(14) . . . . ? C62 C61 C66 C65 -0.8(12) . . . . ? Sn6 C61 C66 C65 179.3(6) . . . . ? O5 Sn7 C71 C72 56.6(6) . . . . ? C3 Sn7 C71 C72 -125.5(6) . . . . ? O6 Sn7 C71 C72 -19.9(6) . . . . ? O7 Sn7 C71 C72 132.8(6) . . . . ? I4 Sn7 C71 C72 -74.2(6) . . . . ? O5 Sn7 C71 C76 -124.8(5) . . . . ? C3 Sn7 C71 C76 53.1(7) . . . . ? O6 Sn7 C71 C76 158.7(5) . . . . ? O7 Sn7 C71 C76 -48.6(6) . . . . ? I4 Sn7 C71 C76 104.5(6) . . . . ? C76 C71 C72 C73 -2.3(11) . . . . ? Sn7 C71 C72 C73 176.3(6) . . . . ? C71 C72 C73 C74 -0.3(13) . . . . ? C72 C73 C74 C75 1.7(14) . . . . ? C73 C74 C75 C76 -0.3(14) . . . . ? C74 C75 C76 C71 -2.3(13) . . . . ? C72 C71 C76 C75 3.7(12) . . . . ? Sn7 C71 C76 C75 -175.0(6) . . . . ? O6 Sn8 C81 C86 -85.8(6) . . . . ? C4 Sn8 C81 C86 108.8(6) . . . . ? O8 Sn8 C81 C86 -159.7(6) . . . . ? I4 Sn8 C81 C86 7.9(6) . . . . ? O6 Sn8 C81 C82 95.6(5) . . . . ? C4 Sn8 C81 C82 -69.7(7) . . . . ? O8 Sn8 C81 C82 21.7(5) . . . . ? I4 Sn8 C81 C82 -170.6(5) . . . . ? C86 C81 C82 C83 0.4(11) . . . . ? Sn8 C81 C82 C83 179.0(6) . . . . ? C81 C82 C83 C84 -0.3(12) . . . . ? C82 C83 C84 C85 0.2(13) . . . . ? C83 C84 C85 C86 -0.2(12) . . . . ? C82 C81 C86 C85 -0.4(11) . . . . ? Sn8 C81 C86 C85 -178.9(5) . . . . ? C84 C85 C86 C81 0.3(12) . . . . ? I2 Cl1 C91 Cl2 141(3) . . . . ? Cl6 Cl3 C92 Cl4 137.2(6) . . . . ? Cl3 Cl6 C93 Cl5 57.7(13) . . . . ? I2 Cl5 C93 Cl6 122.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.135 _refine_diff_density_min -1.653 _refine_diff_density_rms 0.233