# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1274 data_global # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof. Klaus Jurkschat' _publ_contact_author_address ; Lehrstuhl f\"ur Anorganische Chemie II Universit\"at Dortmund Otto-Hahn-Str. 6 44227 Dortmund Germany ; _publ_contact_author_phone '49-231-755-3800' _publ_contact_author_fax '49-231-755-3797' _publ_contact_author_email 'kjur@platon.chemie.uni-dortmund.de' _publ_requested_journal 'Chemical Communications' _publ_requested_coeditor_name 'Prof. Edwin C. Constable' _publ_requested_category ? _publ_contact_letter ; ; #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Tetraorganodistannoxanes: Formation of a Novel cis - Ladder ; _publ_section_title_footnote ? loop_ _publ_author_name _publ_author_address 'Marcus Schulte' ; Lehrstuhl f\"ur Anorganische Chemie II Universit\"at Dortmund Otto-Hahn-Str. 6 44227 Dortmund Germany ; 'Klaus Jurkschat' ; Lehrstuhl f\"ur Anorganische Chemie II Universit\"at Dortmund Otto-Hahn-Str. 6 44227 Dortmund Germany ; 'Markus Sch\"urmann' ; Lehrstuhl f\"ur Anorganische Chemie II Universit\"at Dortmund Otto-Hahn-Str. 6 44227 Dortmund Germany ; 'Dainis Dakternieks' ; School of Biological and Chemical Sciences Deakin University Geelong Vic. 3217 Australia ; data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; cis-\m~2~-Cl-\m~3~-O-[1,3-Bis(trimethylsilylmethyl)-1,3-dichloro-1,3- distanna-2-oxa-5,8-disila-5,5,8,8-tetramethyl-cyclo-6-nonine]-dimer ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H76 Cl4 O2 Si8 Sn4' _chemical_formula_weight 1334.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.240(1) _cell_length_b 15.536(1) _cell_length_c 16.387(1) _cell_angle_alpha 78.643(1) _cell_angle_beta 75.868(1) _cell_angle_gamma 68.096(1) _cell_volume 3011.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 291(1) _cell_measurement_reflns_used 40282 _cell_measurement_theta_min 4.09 _cell_measurement_theta_max 25.68 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 2.000 _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 291(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_method ; 714 frames via \w-rotation (\D\w=1\%) and two times 5s 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 40574 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.09 _diffrn_reflns_theta_max 25.68 _reflns_number_total 10574 _reflns_number_gt 7455 _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-Plus (Sheldrick, 1991)' _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^)+(0.0427P)^2^+0.0908P] 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 10574 _refine_ls_number_parameters 472 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0822 _refine_ls_wR_factor_gt 0.0748 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.67967(3) 0.28844(2) 0.047783(19) 0.05350(10) Uani 1 1 d . . . Sn2 Sn 0.84349(2) 0.128052(19) 0.191964(18) 0.04344(9) Uani 1 1 d . . . Sn3 Sn 0.64641(2) 0.308552(19) 0.281735(18) 0.04263(9) Uani 1 1 d . . . Sn4 Sn 0.77948(2) 0.14256(2) 0.429912(18) 0.04593(9) Uani 1 1 d . . . Cl1 Cl 0.52661(11) 0.42290(9) 0.10441(8) 0.0762(4) Uani 1 1 d . . . Cl2 Cl 0.86312(10) 0.13064(9) 0.02728(7) 0.0647(3) Uani 1 1 d . . . Cl3 Cl 0.92204(11) -0.00514(8) 0.37869(8) 0.0709(3) Uani 1 1 d . . . Cl4 Cl 0.62386(17) 0.29575(13) 0.43991(13) 0.1223(7) Uani 1 1 d . . . Si1 Si 0.83752(13) 0.43052(11) -0.04343(10) 0.0776(5) Uani 1 1 d . . . Si2 Si 1.05323(10) 0.21883(10) 0.16148(9) 0.0574(3) Uani 1 1 d . . . Si3 Si 0.68093(12) 0.50792(9) 0.32635(9) 0.0606(4) Uani 1 1 d . . . Si4 Si 0.87839(12) 0.27365(10) 0.52728(9) 0.0628(4) Uani 1 1 d . . . Si5 Si 0.57590(12) 0.19470(11) -0.07240(9) 0.0675(4) Uani 1 1 d . . . Si6 Si 0.83463(12) -0.09384(10) 0.19744(10) 0.0678(4) Uani 1 1 d . . . Si7 Si 0.36372(11) 0.34072(11) 0.34576(10) 0.0701(4) Uani 1 1 d . . . Si8 Si 0.63709(12) 0.04395(10) 0.60199(9) 0.0650(4) Uani 1 1 d . . . O1 O 0.7275(2) 0.25529(18) 0.16155(16) 0.0436(6) Uani 1 1 d . . . O2 O 0.7781(2) 0.19158(18) 0.30647(16) 0.0429(6) Uani 1 1 d . . . C1 C 0.7548(4) 0.3630(4) -0.0583(3) 0.0721(15) Uani 1 1 d . . . H1A H 0.8026 0.3181 -0.0971 0.145(3) Uiso 1 1 calc R . . H1B H 0.6960 0.4062 -0.0869 0.145(3) Uiso 1 1 calc R . . C2 C 0.9292(6) 0.4512(5) -0.1461(4) 0.125(3) Uani 1 1 d . . . H2A H 0.9747 0.4833 -0.1378 0.145(3) Uiso 1 1 calc R . . H2B H 0.8844 0.4886 -0.1870 0.145(3) Uiso 1 1 calc R . . H2C H 0.9755 0.3924 -0.1662 0.145(3) Uiso 1 1 calc R . . C3 C 0.7456(6) 0.5429(4) -0.0014(4) 0.111(2) Uani 1 1 d . . . H3A H 0.7902 0.5764 0.0060 0.145(3) Uiso 1 1 calc R . . H3B H 0.7012 0.5302 0.0522 0.145(3) Uiso 1 1 calc R . . H3C H 0.6982 0.5799 -0.0407 0.145(3) Uiso 1 1 calc R . . C4 C 0.9265(5) 0.3577(4) 0.0326(4) 0.0751(15) Uani 1 1 d . . . C5 C 0.9791(4) 0.3047(4) 0.0819(3) 0.0687(14) Uani 1 1 d . . . C6 C 1.2053(4) 0.1868(4) 0.1212(4) 0.0834(17) Uani 1 1 d . . . H6A H 1.2242 0.1606 0.0688 0.145(3) Uiso 1 1 calc R . . H6B H 1.2444 0.1416 0.1621 0.145(3) Uiso 1 1 calc R . . H6C H 1.2258 0.2415 0.1119 0.145(3) Uiso 1 1 calc R . . C7 C 1.0143(4) 0.2732(4) 0.2612(3) 0.0767(16) Uani 1 1 d . . . H7A H 1.0282 0.3312 0.2495 0.145(3) Uiso 1 1 calc R . . H7B H 1.0575 0.2318 0.3015 0.145(3) Uiso 1 1 calc R . . H7C H 0.9370 0.2847 0.2839 0.145(3) Uiso 1 1 calc R . . C8 C 1.0136(3) 0.1125(3) 0.1754(3) 0.0567(12) Uani 1 1 d . . . H8A H 1.0416 0.0722 0.2241 0.145(3) Uiso 1 1 calc R . . H8B H 1.0527 0.0795 0.1262 0.145(3) Uiso 1 1 calc R . . C11 C 0.6846(4) 0.4332(3) 0.2495(3) 0.0583(12) Uani 1 1 d . . . H11A H 0.7589 0.4164 0.2159 0.145(3) Uiso 1 1 calc R . . H11B H 0.6356 0.4735 0.2116 0.145(3) Uiso 1 1 calc R . . C12 C 0.7452(6) 0.5964(4) 0.2681(5) 0.121(3) Uani 1 1 d . . . H12A H 0.7391 0.6386 0.3061 0.145(3) Uiso 1 1 calc R . . H12B H 0.7077 0.6307 0.2223 0.145(3) Uiso 1 1 calc R . . H12C H 0.8220 0.5653 0.2458 0.145(3) Uiso 1 1 calc R . . C13 C 0.5362(5) 0.5647(4) 0.3813(4) 0.0940(19) Uani 1 1 d . . . H13A H 0.5022 0.5182 0.4043 0.145(3) Uiso 1 1 calc R . . H13B H 0.4948 0.6096 0.3415 0.145(3) Uiso 1 1 calc R . . H13C H 0.5371 0.5956 0.4262 0.145(3) Uiso 1 1 calc R . . C14 C 0.7619(5) 0.4329(4) 0.4072(4) 0.0716(15) Uani 1 1 d . . . C15 C 0.8102(5) 0.3758(4) 0.4578(4) 0.0737(15) Uani 1 1 d . . . C16 C 1.0169(5) 0.2759(4) 0.5307(4) 0.106(2) Uani 1 1 d . . . H16A H 1.0538 0.2899 0.4742 0.145(3) Uiso 1 1 calc R . . H16B H 1.0604 0.2160 0.5550 0.145(3) Uiso 1 1 calc R . . H16C H 1.0079 0.3230 0.5647 0.145(3) Uiso 1 1 calc R . . C17 C 0.7908(5) 0.2731(4) 0.6355(4) 0.103(2) Uani 1 1 d . . . H17A H 0.7933 0.3207 0.6638 0.145(3) Uiso 1 1 calc R . . H17B H 0.8185 0.2132 0.6675 0.145(3) Uiso 1 1 calc R . . H17C H 0.7157 0.2852 0.6310 0.145(3) Uiso 1 1 calc R . . C18 C 0.8975(4) 0.1690(3) 0.4789(3) 0.0584(12) Uani 1 1 d . . . H18A H 0.9216 0.1163 0.5212 0.145(3) Uiso 1 1 calc R . . H18B H 0.9607 0.1635 0.4329 0.145(3) Uiso 1 1 calc R . . C21 C 0.5813(4) 0.2121(4) 0.0360(3) 0.0670(14) Uani 1 1 d . . . H21A H 0.6075 0.1508 0.0675 0.145(3) Uiso 1 1 calc R . . H21B H 0.5060 0.2432 0.0638 0.145(3) Uiso 1 1 calc R . . C22 C 0.5441(7) 0.3053(5) -0.1406(4) 0.151(3) Uani 1 1 d . . . H22A H 0.5367 0.2955 -0.1946 0.145(3) Uiso 1 1 calc R . . H22B H 0.6028 0.3298 -0.1483 0.145(3) Uiso 1 1 calc R . . H22C H 0.4759 0.3488 -0.1148 0.145(3) Uiso 1 1 calc R . . C23 C 0.7081(5) 0.1159(5) -0.1235(4) 0.119(3) Uani 1 1 d . . . H23A H 0.7226 0.0545 -0.0930 0.145(3) Uiso 1 1 calc R . . H23B H 0.7665 0.1384 -0.1236 0.145(3) Uiso 1 1 calc R . . H23C H 0.7044 0.1136 -0.1808 0.145(3) Uiso 1 1 calc R . . C24 C 0.4678(7) 0.1494(8) -0.0655(5) 0.200(5) Uani 1 1 d . . . H24A H 0.4787 0.1230 -0.1165 0.145(3) Uiso 1 1 calc R . . H24B H 0.3975 0.1989 -0.0582 0.145(3) Uiso 1 1 calc R . . H24C H 0.4693 0.1019 -0.0179 0.145(3) Uiso 1 1 calc R . . C31 C 0.7615(4) 0.0290(3) 0.2215(3) 0.0523(11) Uani 1 1 d . . . H31A H 0.7317 0.0264 0.2818 0.145(3) Uiso 1 1 calc R . . H31B H 0.6985 0.0544 0.1930 0.145(3) Uiso 1 1 calc R . . C32 C 0.9863(4) -0.1333(4) 0.1956(4) 0.0869(17) Uani 1 1 d . . . H32A H 1.0185 -0.1991 0.1910 0.145(3) Uiso 1 1 calc R . . H32B H 0.9985 -0.1211 0.2469 0.145(3) Uiso 1 1 calc R . . H32C H 1.0202 -0.1001 0.1479 0.145(3) Uiso 1 1 calc R . . C33 C 0.8137(6) -0.1055(5) 0.0930(5) 0.137(3) Uani 1 1 d . . . H33A H 0.8483 -0.0687 0.0494 0.145(3) Uiso 1 1 calc R . . H33B H 0.7358 -0.0839 0.0926 0.145(3) Uiso 1 1 calc R . . H33C H 0.8461 -0.1698 0.0830 0.145(3) Uiso 1 1 calc R . . C34 C 0.7764(6) -0.1701(4) 0.2832(5) 0.143(3) Uani 1 1 d . . . H34A H 0.8258 -0.2336 0.2823 0.145(3) Uiso 1 1 calc R . . H34B H 0.7055 -0.1659 0.2743 0.145(3) Uiso 1 1 calc R . . H34C H 0.7677 -0.1500 0.3370 0.145(3) Uiso 1 1 calc R . . C41 C 0.5062(3) 0.2684(3) 0.2965(3) 0.0535(11) Uani 1 1 d . . . H41A H 0.5017 0.2602 0.2404 0.145(3) Uiso 1 1 calc R . . H41B H 0.5225 0.2072 0.3291 0.145(3) Uiso 1 1 calc R . . C42 C 0.3398(6) 0.4660(4) 0.3189(6) 0.150(4) Uani 1 1 d . . . H42A H 0.2671 0.5006 0.3469 0.145(3) Uiso 1 1 calc R . . H42B H 0.3455 0.4819 0.2587 0.145(3) Uiso 1 1 calc R . . H42C H 0.3943 0.4811 0.3370 0.145(3) Uiso 1 1 calc R . . C43 C 0.2658(5) 0.3125(5) 0.3010(5) 0.121(3) Uani 1 1 d . . . H43A H 0.2770 0.2470 0.3144 0.145(3) Uiso 1 1 calc R . . H43B H 0.2784 0.3281 0.2406 0.145(3) Uiso 1 1 calc R . . H43C H 0.1911 0.3478 0.3248 0.145(3) Uiso 1 1 calc R . . C44 C 0.3437(6) 0.3088(7) 0.4617(4) 0.158(4) Uani 1 1 d . . . H44A H 0.2710 0.3462 0.4874 0.145(3) Uiso 1 1 calc R . . H44B H 0.3984 0.3197 0.4834 0.145(3) Uiso 1 1 calc R . . H44C H 0.3512 0.2440 0.4746 0.145(3) Uiso 1 1 calc R . . C51 C 0.6591(4) 0.0782(3) 0.4860(3) 0.0644(13) Uani 1 1 d . . . H51A H 0.5887 0.1204 0.4721 0.145(3) Uiso 1 1 calc R . . H51B H 0.6787 0.0225 0.4588 0.145(3) Uiso 1 1 calc R . . C52 C 0.7713(5) -0.0247(5) 0.6357(4) 0.125(3) Uani 1 1 d . . . H52A H 0.7580 -0.0538 0.6928 0.145(3) Uiso 1 1 calc R . . H52B H 0.8118 0.0160 0.6332 0.145(3) Uiso 1 1 calc R . . H52C H 0.8136 -0.0719 0.5987 0.145(3) Uiso 1 1 calc R . . C53 C 0.5671(6) 0.1516(5) 0.6543(4) 0.114(2) Uani 1 1 d . . . H53A H 0.5127 0.1953 0.6230 0.145(3) Uiso 1 1 calc R . . H53B H 0.6208 0.1787 0.6560 0.145(3) Uiso 1 1 calc R . . H53C H 0.5315 0.1367 0.7110 0.145(3) Uiso 1 1 calc R . . C54 C 0.5441(5) -0.0272(5) 0.6308(4) 0.110(2) Uani 1 1 d . . . H54A H 0.5781 -0.0825 0.6025 0.145(3) Uiso 1 1 calc R . . H54B H 0.4744 0.0089 0.6137 0.145(3) Uiso 1 1 calc R . . H54C H 0.5319 -0.0446 0.6910 0.145(3) 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 Sn1 0.0570(2) 0.0640(2) 0.03902(18) 0.00236(15) -0.01522(14) -0.02044(17) Sn2 0.04002(16) 0.04201(17) 0.04610(17) -0.00417(13) -0.00705(13) -0.01270(14) Sn3 0.04137(16) 0.03855(16) 0.04730(18) -0.00432(13) -0.01033(13) -0.01200(13) Sn4 0.05370(18) 0.04701(17) 0.03980(17) 0.00158(13) -0.01535(14) -0.01949(15) Cl1 0.0717(8) 0.0717(9) 0.0670(8) -0.0021(7) -0.0240(7) -0.0002(7) Cl2 0.0628(7) 0.0763(8) 0.0454(7) -0.0143(6) -0.0056(5) -0.0123(7) Cl3 0.0821(9) 0.0502(7) 0.0706(8) -0.0080(6) -0.0328(7) 0.0005(6) Cl4 0.1397(16) 0.1089(13) 0.1364(16) 0.0180(12) -0.0672(13) -0.0532(13) Si1 0.0754(10) 0.0767(10) 0.0726(10) 0.0257(8) -0.0200(8) -0.0304(9) Si2 0.0459(7) 0.0656(8) 0.0623(8) 0.0030(7) -0.0126(6) -0.0245(7) Si3 0.0767(9) 0.0419(7) 0.0700(9) -0.0001(6) -0.0275(8) -0.0224(7) Si4 0.0698(9) 0.0605(8) 0.0698(9) -0.0038(7) -0.0337(8) -0.0243(8) Si5 0.0590(9) 0.0900(11) 0.0585(9) -0.0195(8) -0.0148(7) -0.0233(8) Si6 0.0690(9) 0.0512(8) 0.0880(11) -0.0175(8) -0.0127(8) -0.0226(7) Si7 0.0454(8) 0.0822(10) 0.0855(11) -0.0207(9) -0.0073(7) -0.0227(8) Si8 0.0698(9) 0.0714(9) 0.0575(8) 0.0086(7) -0.0126(7) -0.0360(8) O1 0.0455(16) 0.0461(16) 0.0374(15) -0.0007(12) -0.0110(12) -0.0135(14) O2 0.0457(16) 0.0417(15) 0.0379(15) -0.0004(12) -0.0113(12) -0.0111(13) C1 0.074(3) 0.087(4) 0.050(3) 0.012(3) -0.017(3) -0.029(3) C2 0.111(5) 0.144(7) 0.103(5) 0.046(5) -0.009(4) -0.061(5) C3 0.122(6) 0.075(4) 0.127(6) 0.010(4) -0.037(5) -0.027(4) C4 0.072(4) 0.072(4) 0.085(4) 0.015(3) -0.020(3) -0.037(3) C5 0.068(3) 0.065(3) 0.074(4) 0.008(3) -0.017(3) -0.030(3) C6 0.055(3) 0.108(5) 0.088(4) -0.001(4) -0.005(3) -0.039(3) C7 0.072(3) 0.089(4) 0.085(4) -0.013(3) -0.014(3) -0.043(3) C8 0.041(2) 0.059(3) 0.068(3) -0.002(2) -0.012(2) -0.015(2) C11 0.067(3) 0.044(3) 0.065(3) 0.002(2) -0.014(2) -0.023(2) C12 0.159(7) 0.091(5) 0.155(7) 0.021(4) -0.071(6) -0.083(5) C13 0.096(4) 0.079(4) 0.097(5) -0.025(3) -0.030(4) -0.004(4) C14 0.093(4) 0.055(3) 0.084(4) -0.012(3) -0.037(3) -0.030(3) C15 0.094(4) 0.058(3) 0.085(4) -0.003(3) -0.046(3) -0.029(3) C16 0.107(5) 0.106(5) 0.141(6) 0.011(4) -0.065(5) -0.063(4) C17 0.126(6) 0.096(5) 0.086(5) -0.023(4) -0.024(4) -0.026(4) C18 0.060(3) 0.057(3) 0.064(3) -0.005(2) -0.030(2) -0.016(2) C21 0.065(3) 0.093(4) 0.053(3) -0.010(3) -0.008(2) -0.039(3) C22 0.219(10) 0.122(6) 0.109(6) -0.020(5) -0.104(6) -0.007(6) C23 0.098(5) 0.144(6) 0.108(5) -0.060(5) -0.039(4) 0.004(5) C24 0.187(9) 0.410(16) 0.103(6) -0.079(8) 0.014(6) -0.217(11) C31 0.051(3) 0.048(3) 0.059(3) -0.003(2) -0.011(2) -0.019(2) C32 0.079(4) 0.077(4) 0.088(4) -0.024(3) -0.005(3) -0.008(3) C33 0.152(7) 0.123(6) 0.162(7) -0.070(6) -0.075(6) -0.023(5) C34 0.125(6) 0.067(4) 0.220(9) -0.019(5) 0.035(6) -0.053(4) C41 0.050(3) 0.055(3) 0.062(3) -0.009(2) -0.016(2) -0.021(2) C42 0.102(6) 0.078(5) 0.242(10) -0.059(6) 0.022(6) -0.013(4) C43 0.067(4) 0.141(6) 0.173(7) -0.039(6) -0.040(4) -0.033(4) C44 0.102(6) 0.254(11) 0.083(5) -0.034(6) 0.020(4) -0.038(7) C51 0.077(3) 0.068(3) 0.060(3) 0.004(3) -0.015(3) -0.042(3) C52 0.093(5) 0.149(6) 0.099(5) 0.056(5) -0.034(4) -0.028(5) C53 0.140(6) 0.120(6) 0.092(5) -0.037(4) 0.001(4) -0.060(5) C54 0.125(6) 0.113(5) 0.110(5) 0.012(4) -0.010(4) -0.082(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O1 2.024(3) . Y Sn1 C21 2.122(4) . Y Sn1 C1 2.139(4) . Y Sn1 Cl1 2.4531(14) . Y Sn1 Cl2 2.7397(13) . Y Sn2 O1 2.058(3) . Y Sn2 C31 2.116(4) . Y Sn2 C8 2.128(4) . Y Sn2 O2 2.132(3) . Y Sn2 Cl2 2.6410(12) . Y Sn2 Cl3 3.4902(13) . Y Sn3 O2 2.049(3) . Y Sn3 C41 2.116(4) . Y Sn3 C11 2.117(4) . Y Sn3 O1 2.159(3) . Y Sn3 Cl4 2.512(2) . Y Sn3 Cl1 3.4973(13) . Y Sn4 O2 2.018(2) . Y Sn4 C18 2.116(4) . Y Sn4 C51 2.120(4) . Y Sn4 Cl4 2.503(2) . Y Sn4 Cl3 2.5072(13) . Y Si1 C4 1.841(6) . ? Si1 C1 1.856(5) . ? Si1 C3 1.866(6) . ? Si1 C2 1.867(6) . ? Si2 C5 1.846(6) . ? Si2 C7 1.859(5) . ? Si2 C6 1.863(5) . ? Si2 C8 1.870(4) . ? Si3 C14 1.848(6) . ? Si3 C11 1.854(5) . ? Si3 C13 1.862(6) . ? Si3 C12 1.867(5) . ? Si4 C15 1.830(6) . ? Si4 C18 1.855(5) . ? Si4 C16 1.862(5) . ? Si4 C17 1.868(6) . ? Si5 C24 1.788(7) . ? Si5 C22 1.819(7) . ? Si5 C23 1.831(6) . ? Si5 C21 1.870(5) . ? Si6 C33 1.851(7) . ? Si6 C31 1.862(4) . ? Si6 C34 1.862(6) . ? Si6 C32 1.863(6) . ? Si7 C42 1.831(7) . ? Si7 C44 1.846(7) . ? Si7 C43 1.851(6) . ? Si7 C41 1.872(5) . ? Si8 C53 1.846(6) . ? Si8 C51 1.852(5) . ? Si8 C52 1.854(6) . ? Si8 C54 1.868(5) . ? C4 C5 1.183(7) . Y C14 C15 1.196(6) . Y loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sn1 C21 112.47(15) . . Y O1 Sn1 C1 122.71(15) . . Y C21 Sn1 C1 122.94(19) . . Y O1 Sn1 Cl1 88.29(8) . . Y C21 Sn1 Cl1 96.97(15) . . Y C1 Sn1 Cl1 97.97(15) . . Y O1 Sn1 Cl2 76.28(8) . . Y C21 Sn1 Cl2 89.11(15) . . Y C1 Sn1 Cl2 90.49(15) . . Y Cl1 Sn1 Cl2 164.57(4) . . Y O1 Sn2 C31 106.59(14) . . Y O1 Sn2 C8 121.03(14) . . Y C31 Sn2 C8 131.83(17) . . Y O1 Sn2 O2 74.44(10) . . Y C31 Sn2 O2 98.28(14) . . Y C8 Sn2 O2 100.73(15) . . Y O1 Sn2 Cl2 78.11(8) . . Y C31 Sn2 Cl2 92.52(13) . . Y C8 Sn2 Cl2 90.56(13) . . Y O2 Sn2 Cl2 152.36(7) . . Y O1 Sn2 Cl3 135.69(8) . . Y C31 Sn2 Cl3 74.59(12) . . Y C8 Sn2 Cl3 76.32(13) . . Y O2 Sn2 Cl3 61.85(7) . . Y Cl2 Sn2 Cl3 145.79(4) . . Y O2 Sn3 C41 108.43(14) . . Y O2 Sn3 C11 114.02(15) . . Y C41 Sn3 C11 137.54(18) . . Y O2 Sn3 O1 74.03(10) . . Y C41 Sn3 O1 95.90(14) . . Y C11 Sn3 O1 95.62(15) . . Y O2 Sn3 Cl4 77.72(8) . . Y C41 Sn3 Cl4 90.10(13) . . Y C11 Sn3 Cl4 98.54(14) . . Y O1 Sn3 Cl4 151.59(8) . . Y O2 Sn3 Cl1 135.99(8) . . Y C41 Sn3 Cl1 74.80(13) . . Y C11 Sn3 Cl1 75.02(13) . . Y O1 Sn3 Cl1 62.06(7) . . Y Cl4 Sn3 Cl1 145.76(5) . . Y O2 Sn4 C18 113.73(15) . . Y O2 Sn4 C51 113.67(15) . . Y C18 Sn4 C51 132.57(18) . . Y O2 Sn4 Cl4 78.46(9) . . Y C18 Sn4 Cl4 100.79(13) . . Y C51 Sn4 Cl4 86.98(15) . . Y O2 Sn4 Cl3 86.29(8) . . Y C18 Sn4 Cl3 91.03(13) . . Y C51 Sn4 Cl3 93.50(15) . . Y Cl4 Sn4 Cl3 163.50(6) . . Y Sn1 Cl1 Sn3 77.50(3) . . Y Sn2 Cl2 Sn1 82.72(3) . . Y Sn4 Cl3 Sn2 77.11(3) . . Y Sn4 Cl4 Sn3 86.84(7) . . Y C4 Si1 C1 107.2(2) . . ? C4 Si1 C3 109.9(3) . . ? C1 Si1 C3 111.0(3) . . ? C4 Si1 C2 108.0(3) . . ? C1 Si1 C2 109.4(3) . . ? C3 Si1 C2 111.2(3) . . ? C5 Si2 C7 108.3(3) . . ? C5 Si2 C6 109.1(2) . . ? C7 Si2 C6 110.1(2) . . ? C5 Si2 C8 107.6(2) . . ? C7 Si2 C8 112.6(2) . . ? C6 Si2 C8 109.1(2) . . ? C14 Si3 C11 108.3(2) . . ? C14 Si3 C13 108.0(3) . . ? C11 Si3 C13 110.9(3) . . ? C14 Si3 C12 109.9(3) . . ? C11 Si3 C12 108.4(3) . . ? C13 Si3 C12 111.4(3) . . ? C15 Si4 C18 106.9(2) . . ? C15 Si4 C16 108.9(3) . . ? C18 Si4 C16 109.0(3) . . ? C15 Si4 C17 110.2(3) . . ? C18 Si4 C17 110.5(3) . . ? C16 Si4 C17 111.2(3) . . ? C24 Si5 C22 107.3(5) . . ? C24 Si5 C23 109.9(4) . . ? C22 Si5 C23 107.4(4) . . ? C24 Si5 C21 109.5(3) . . ? C22 Si5 C21 110.8(3) . . ? C23 Si5 C21 111.9(3) . . ? C33 Si6 C31 109.7(3) . . ? C33 Si6 C34 110.8(4) . . ? C31 Si6 C34 107.7(3) . . ? C33 Si6 C32 108.5(3) . . ? C31 Si6 C32 112.6(2) . . ? C34 Si6 C32 107.5(3) . . ? C42 Si7 C44 110.8(4) . . ? C42 Si7 C43 108.2(4) . . ? C44 Si7 C43 110.5(4) . . ? C42 Si7 C41 111.9(3) . . ? C44 Si7 C41 109.1(3) . . ? C43 Si7 C41 106.4(3) . . ? C53 Si8 C51 108.0(3) . . ? C53 Si8 C52 111.1(4) . . ? C51 Si8 C52 110.3(3) . . ? C53 Si8 C54 108.3(3) . . ? C51 Si8 C54 109.3(3) . . ? C52 Si8 C54 109.8(3) . . ? Sn1 O1 Sn2 121.20(13) . . ? Sn1 O1 Sn3 131.37(13) . . ? Sn2 O1 Sn3 104.52(11) . . ? Sn4 O2 Sn3 115.90(12) . . ? Sn4 O2 Sn2 133.72(13) . . ? Sn3 O2 Sn2 105.86(11) . . ? Si1 C1 Sn1 120.8(3) . . ? C5 C4 Si1 173.7(5) . . Y C4 C5 Si2 176.0(5) . . Y Si2 C8 Sn2 119.3(2) . . ? Si3 C11 Sn3 125.2(2) . . ? C15 C14 Si3 171.8(4) . . Y C14 C15 Si4 169.9(4) . . Y Si4 C18 Sn4 127.5(2) . . ? Si5 C21 Sn1 118.8(2) . . ? Si6 C31 Sn2 121.7(2) . . ? Si7 C41 Sn3 122.6(2) . . ? Si8 C51 Sn4 118.8(2) . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 0.841 _refine_diff_density_min -1.213 _refine_diff_density_rms 0.076