# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 879397' #TrackingRef 'AlkynylSn2Si3_ChemComm.cif' _chemical_name_systematic ; 1-Ethynyl-2,2,4,4,5,5-hexakis(2,4,6-trimethylpheny)- 3-methyl-2,4,5-trisila-1,3-distannabicyclo[1.1.1]pentane ; _audit_creation_method SHELXL-97 _chemical_name_common ; 1-Ethynyl-2,2,4,4,5,5-hexakis(2,4,6-trimethylpheny)-3-methyl- 2,4,5-trisila-1,3-distannabicyclo(1.1.1)pentane ; _chemical_melting_point ? _chemical_formula_moiety 'C57 H70 Si3 Sn2, 1.5(C7 H8)' _chemical_formula_sum 'C67.50 H82 Si3 Sn2' _chemical_formula_weight 1214.98 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' Si Si 0.0817 0.0704 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.170(2) _cell_length_b 18.307(4) _cell_length_c 19.714(4) _cell_angle_alpha 64.00(3) _cell_angle_beta 80.10(3) _cell_angle_gamma 86.56(3) _cell_volume 3568.8(16) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 30550 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 25.00 _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.131 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1258 _exptl_absorpt_coefficient_mu 0.783 _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 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Stadi with CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30550 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12505 _reflns_number_gt 9367 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis Red' _computing_data_reduction 'CrysAlis Red' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Ortep 32' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0975P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12505 _refine_ls_number_parameters 655 _refine_ls_number_restraints 82 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1466 _refine_ls_wR_factor_gt 0.1381 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.994 _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 C93 C 0.7834(14) 0.0288(10) 0.2474(13) 0.255(18) Uiso 0.50 1 d PDU . . H93A H 0.7962 0.0775 0.1985 0.383 Uiso 0.50 1 calc PR . . H93B H 0.8588 -0.0020 0.2545 0.383 Uiso 0.50 1 calc PR . . H93C H 0.7598 0.0447 0.2892 0.383 Uiso 0.50 1 calc PR . . C94 C 0.6835(9) -0.0237(6) 0.2475(7) 0.125(6) Uiso 0.50 1 d PGDU . . C95 C 0.5869(11) 0.0123(5) 0.2090(7) 0.105(5) Uiso 0.50 1 d PGDU . . H95 H 0.5833 0.0698 0.1829 0.126 Uiso 0.50 1 calc PR . . C96 C 0.4956(10) -0.0359(7) 0.2087(7) 0.113(6) Uiso 0.50 1 d PGDU . . H96 H 0.4296 -0.0113 0.1824 0.135 Uiso 0.50 1 calc PR . . C97 C 0.5010(11) -0.1201(7) 0.2468(8) 0.110(5) Uiso 0.50 1 d PGDU . . H97 H 0.4386 -0.1530 0.2466 0.132 Uiso 0.50 1 calc PR . . C98 C 0.5976(12) -0.1561(5) 0.2853(7) 0.120(6) Uiso 0.50 1 d PGDU . . H98 H 0.6012 -0.2136 0.3114 0.143 Uiso 0.50 1 calc PR . . C99 C 0.6888(10) -0.1079(7) 0.2857(7) 0.107(5) Uiso 0.50 1 d PGDU . . H99 H 0.7548 -0.1325 0.3120 0.128 Uiso 0.50 1 calc PR . . C81 C 0.1316(17) 0.1476(12) 0.0910(7) 0.138(8) Uiso 0.50 1 d PDU . . H81A H 0.1792 0.1051 0.1253 0.207 Uiso 0.50 1 calc PR . . H81B H 0.0459 0.1305 0.1046 0.207 Uiso 0.50 1 calc PR . . H81C H 0.1396 0.1980 0.0959 0.207 Uiso 0.50 1 calc PR . . C82 C 0.3447(15) 0.1838(12) -0.0933(10) 0.204(11) Uiso 0.50 1 d PGDU . . H82 H 0.4295 0.1899 -0.1122 0.245 Uiso 0.50 1 calc PR . . C83 C 0.263(2) 0.1876(11) -0.1407(7) 0.197(11) Uiso 0.50 1 d PGDU . . H83 H 0.2924 0.1964 -0.1920 0.236 Uiso 0.50 1 calc PR . . C84 C 0.139(2) 0.1785(12) -0.1132(8) 0.187(10) Uiso 0.50 1 d PGDU . . H84 H 0.0836 0.1811 -0.1455 0.224 Uiso 0.50 1 calc PR . . C85 C 0.0966(13) 0.1657(10) -0.0382(9) 0.142(7) Uiso 0.50 1 d PGDU . . H85 H 0.0118 0.1595 -0.0194 0.170 Uiso 0.50 1 calc PR . . C86 C 0.1780(11) 0.1619(7) 0.0092(7) 0.107(5) Uiso 0.50 1 d PGDU . . C87 C 0.3021(11) 0.1709(10) -0.0184(9) 0.155(8) Uiso 0.50 1 d PGDU . . H87 H 0.3577 0.1683 0.0140 0.186 Uiso 0.50 1 calc PR . . C71 C 0.3667(18) 0.8060(14) 0.0310(10) 0.192(12) Uiso 0.50 1 d PDU . . H71A H 0.3464 0.8323 -0.0208 0.288 Uiso 0.50 1 calc PR . . H71B H 0.3585 0.7469 0.0509 0.288 Uiso 0.50 1 calc PR . . H71C H 0.4506 0.8204 0.0295 0.288 Uiso 0.50 1 calc PR . . C72 C 0.2369(13) 0.7802(7) 0.1573(7) 0.098(5) Uiso 0.50 1 d PGDU . . H72 H 0.2609 0.7250 0.1762 0.118 Uiso 0.50 1 calc PR . . C73 C 0.2811(13) 0.8347(8) 0.0825(7) 0.184(10) Uiso 0.50 1 d PGDU . . C74 C 0.2460(18) 0.9155(8) 0.0548(8) 0.187(10) Uiso 0.50 1 d PGDU . . H74 H 0.2762 0.9527 0.0037 0.224 Uiso 0.50 1 calc PR . . C75 C 0.1668(19) 0.9416(8) 0.1019(11) 0.196(11) Uiso 0.50 1 d PGDU . . H75 H 0.1429 0.9968 0.0830 0.236 Uiso 0.50 1 calc PR . . C76 C 0.1227(16) 0.8871(10) 0.1767(11) 0.204(11) Uiso 0.50 1 d PGDU . . H76 H 0.0686 0.9050 0.2089 0.245 Uiso 0.50 1 calc PR . . C77 C 0.1577(14) 0.8064(9) 0.2044(7) 0.117(6) Uiso 0.50 1 d PGDU . . H77 H 0.1276 0.7691 0.2555 0.141 Uiso 0.50 1 calc PR . . Sn1 Sn 0.10044(3) 0.350725(19) 0.328964(18) 0.03860(11) Uani 1 1 d D . . Sn2 Sn 0.38671(3) 0.348758(18) 0.291772(17) 0.03748(11) Uani 1 1 d D A . Si1 Si 0.25151(12) 0.28603(8) 0.42719(7) 0.0373(3) Uani 1 1 d . A . Si2 Si 0.24830(12) 0.47654(7) 0.25848(7) 0.0362(3) Uani 1 1 d . A . Si3 Si 0.23066(12) 0.28606(8) 0.24592(7) 0.0382(3) Uani 1 1 d . A . C10 C 0.2650(4) 0.5416(3) 0.3099(3) 0.0383(10) Uani 1 1 d . . . C11 C 0.1770(5) 0.5434(3) 0.3712(3) 0.0420(11) Uani 1 1 d . A . C12 C 0.1988(5) 0.5922(3) 0.4060(3) 0.0460(12) Uani 1 1 d . . . H12 H 0.1403 0.5924 0.4471 0.055 Uiso 1 1 calc R A . C13 C 0.3022(5) 0.6403(3) 0.3828(3) 0.0490(12) Uani 1 1 d . A . C14 C 0.3868(5) 0.6396(3) 0.3233(3) 0.0470(12) Uani 1 1 d . . . H14 H 0.4583 0.6725 0.3068 0.056 Uiso 1 1 calc R A . C15 C 0.3694(5) 0.5912(3) 0.2861(3) 0.0415(11) Uani 1 1 d . A . C16 C 0.0597(5) 0.4942(3) 0.4017(3) 0.0451(11) Uani 1 1 d . . . H16A H 0.0768 0.4371 0.4330 0.068 Uiso 1 1 calc R A . H16B H 0.0220 0.4983 0.3588 0.068 Uiso 1 1 calc R . . H16C H 0.0042 0.5152 0.4329 0.068 Uiso 1 1 calc R . . C17 C 0.3203(7) 0.6943(4) 0.4204(4) 0.0715(18) Uani 1 1 d . . . H17A H 0.4075 0.7022 0.4172 0.107 Uiso 1 1 calc R A . H17B H 0.2821 0.6686 0.4743 0.107 Uiso 1 1 calc R . . H17C H 0.2831 0.7470 0.3943 0.107 Uiso 1 1 calc R . . C18 C 0.4673(5) 0.5939(3) 0.2224(3) 0.0509(13) Uani 1 1 d . . . H18A H 0.5111 0.5425 0.2394 0.076 Uiso 1 1 calc R A . H18B H 0.5241 0.6389 0.2083 0.076 Uiso 1 1 calc R . . H18C H 0.4305 0.6020 0.1780 0.076 Uiso 1 1 calc R . . C20 C 0.2378(4) 0.5439(3) 0.1538(3) 0.0377(10) Uani 1 1 d . . . C21 C 0.1369(5) 0.5956(3) 0.1363(3) 0.0455(11) Uani 1 1 d . A . C22 C 0.1224(5) 0.6455(4) 0.0618(3) 0.0538(13) Uani 1 1 d . . . H22 H 0.0535 0.6794 0.0520 0.065 Uiso 1 1 calc R A . C23 C 0.2084(6) 0.6468(4) 0.0003(3) 0.0578(14) Uani 1 1 d . A . C24 C 0.3077(5) 0.5967(3) 0.0171(3) 0.0509(13) Uani 1 1 d . . . H24 H 0.3666 0.5971 -0.0241 0.061 Uiso 1 1 calc R A . C25 C 0.3250(5) 0.5459(3) 0.0915(3) 0.0415(11) Uani 1 1 d . A . C26 C 0.0388(5) 0.5977(4) 0.1996(3) 0.0535(13) Uani 1 1 d . . . H26A H -0.0199 0.6397 0.1770 0.080 Uiso 1 1 calc R A . H26B H 0.0763 0.6100 0.2349 0.080 Uiso 1 1 calc R . . H26C H -0.0030 0.5447 0.2275 0.080 Uiso 1 1 calc R . . C27 C 0.1931(7) 0.7041(5) -0.0816(3) 0.077(2) Uani 1 1 d . . . H27A H 0.2359 0.7557 -0.0974 0.116 Uiso 1 1 calc R A . H27B H 0.1066 0.7142 -0.0844 0.116 Uiso 1 1 calc R . . H27C H 0.2272 0.6793 -0.1157 0.116 Uiso 1 1 calc R . . C28 C 0.4382(5) 0.4958(3) 0.1006(3) 0.0456(12) Uani 1 1 d . . . H28A H 0.4176 0.4400 0.1117 0.068 Uiso 1 1 calc R A . H28B H 0.4738 0.4955 0.1428 0.068 Uiso 1 1 calc R . . H28C H 0.4970 0.5193 0.0532 0.068 Uiso 1 1 calc R . . C30 C 0.2272(4) 0.3328(3) 0.1389(3) 0.0390(10) Uani 1 1 d . . . C31 C 0.1318(5) 0.3812(3) 0.1037(3) 0.0437(11) Uani 1 1 d . A . C32 C 0.1338(5) 0.4083(3) 0.0253(3) 0.0502(12) Uani 1 1 d . . . H32 H 0.0678 0.4393 0.0029 0.060 Uiso 1 1 calc R A . C33 C 0.2290(5) 0.3915(4) -0.0209(3) 0.0518(13) Uani 1 1 d . A . C34 C 0.3239(5) 0.3457(3) 0.0134(3) 0.0479(12) Uani 1 1 d . . . H34 H 0.3910 0.3347 -0.0174 0.057 Uiso 1 1 calc R A . C35 C 0.3234(5) 0.3152(3) 0.0922(3) 0.0414(11) Uani 1 1 d . A . C36 C 0.0241(5) 0.4066(3) 0.1455(3) 0.0489(12) Uani 1 1 d . . . H36A H 0.0506 0.4467 0.1605 0.073 Uiso 1 1 calc R A . H36B H -0.0113 0.3590 0.1912 0.073 Uiso 1 1 calc R . . H36C H -0.0368 0.4307 0.1119 0.073 Uiso 1 1 calc R . . C37 C 0.2304(6) 0.4217(5) -0.1051(3) 0.075(2) Uani 1 1 d . . . H37A H 0.2887 0.4672 -0.1334 0.112 Uiso 1 1 calc R A . H37B H 0.1491 0.4400 -0.1171 0.112 Uiso 1 1 calc R . . H37C H 0.2544 0.3777 -0.1199 0.112 Uiso 1 1 calc R . . C38 C 0.4295(5) 0.2648(3) 0.1236(3) 0.0483(12) Uani 1 1 d . . . H38A H 0.4674 0.2889 0.1505 0.072 Uiso 1 1 calc R A . H38B H 0.4891 0.2633 0.0815 0.072 Uiso 1 1 calc R . . H38C H 0.4012 0.2094 0.1592 0.072 Uiso 1 1 calc R . . C40 C 0.2205(5) 0.1708(3) 0.2843(3) 0.0449(12) Uani 1 1 d . . . C41 C 0.1119(6) 0.1366(3) 0.2815(3) 0.0530(13) Uani 1 1 d . A . C42 C 0.1012(7) 0.0524(4) 0.3077(4) 0.0681(19) Uani 1 1 d . . . H42 H 0.0273 0.0300 0.3067 0.082 Uiso 1 1 calc R A . C43 C 0.1961(8) 0.0002(4) 0.3353(4) 0.072(2) Uani 1 1 d . A . C44 C 0.3019(7) 0.0344(3) 0.3378(3) 0.0626(16) Uani 1 1 d . . . H44 H 0.3674 -0.0001 0.3565 0.075 Uiso 1 1 calc R A . C45 C 0.3151(6) 0.1167(3) 0.3142(3) 0.0506(13) Uani 1 1 d . A . C46 C 0.0062(6) 0.1880(4) 0.2508(4) 0.0644(16) Uani 1 1 d . . . H46A H -0.0133 0.2250 0.2749 0.097 Uiso 1 1 calc R A . H46B H -0.0645 0.1529 0.2623 0.097 Uiso 1 1 calc R . . H46C H 0.0275 0.2197 0.1953 0.097 Uiso 1 1 calc R . . C47 C 0.1844(10) -0.0901(4) 0.3610(5) 0.103(3) Uani 1 1 d . . . H47A H 0.1007 -0.1038 0.3614 0.155 Uiso 1 1 calc R A . H47B H 0.2046 -0.1194 0.4126 0.155 Uiso 1 1 calc R . . H47C H 0.2401 -0.1059 0.3257 0.155 Uiso 1 1 calc R . . C48 C 0.4352(6) 0.1435(3) 0.3212(3) 0.0569(14) Uani 1 1 d . . . H48A H 0.4266 0.1510 0.3681 0.085 Uiso 1 1 calc R A . H48B H 0.4614 0.1949 0.2769 0.085 Uiso 1 1 calc R . . H48C H 0.4960 0.1020 0.3233 0.085 Uiso 1 1 calc R . . C50 C 0.2525(5) 0.1709(3) 0.4800(3) 0.0398(10) Uani 1 1 d . . . C51 C 0.1541(5) 0.1194(3) 0.4897(3) 0.0426(11) Uani 1 1 d . A . C52 C 0.1650(5) 0.0361(3) 0.5271(3) 0.0503(13) Uani 1 1 d . . . H52 H 0.0975 0.0028 0.5343 0.060 Uiso 1 1 calc R A . C53 C 0.2683(6) -0.0011(3) 0.5543(3) 0.0562(14) Uani 1 1 d . A . C54 C 0.3648(6) 0.0488(3) 0.5456(3) 0.0557(14) Uani 1 1 d . . . H54 H 0.4371 0.0246 0.5644 0.067 Uiso 1 1 calc R A . C55 C 0.3579(5) 0.1333(3) 0.5099(3) 0.0440(11) Uani 1 1 d . A . C56 C 0.0357(5) 0.1503(3) 0.4609(3) 0.0474(12) Uani 1 1 d . . . H56A H 0.0481 0.1698 0.4052 0.071 Uiso 1 1 calc R A . H56B H 0.0072 0.1950 0.4739 0.071 Uiso 1 1 calc R . . H56C H -0.0252 0.1061 0.4848 0.071 Uiso 1 1 calc R . . C57 C 0.2780(7) -0.0924(4) 0.5921(5) 0.079(2) Uani 1 1 d . . . H57A H 0.1964 -0.1171 0.6114 0.118 Uiso 1 1 calc R A . H57B H 0.3233 -0.1086 0.6347 0.118 Uiso 1 1 calc R . . H57C H 0.3207 -0.1108 0.5547 0.118 Uiso 1 1 calc R . . C58 C 0.4659(5) 0.1821(3) 0.5046(3) 0.0535(13) Uani 1 1 d . . . H58A H 0.5318 0.1453 0.5248 0.080 Uiso 1 1 calc R A . H58B H 0.4427 0.2131 0.5345 0.080 Uiso 1 1 calc R . . H58C H 0.4934 0.2196 0.4510 0.080 Uiso 1 1 calc R . . C60 C 0.2595(4) 0.3312(3) 0.4971(3) 0.0365(10) Uani 1 1 d . . . C61 C 0.1632(4) 0.3138(3) 0.5584(3) 0.0402(10) Uani 1 1 d . A . C62 C 0.1655(5) 0.3429(3) 0.6131(3) 0.0461(12) Uani 1 1 d . . . H62 H 0.0992 0.3307 0.6539 0.055 Uiso 1 1 calc R A . C63 C 0.2638(5) 0.3895(3) 0.6088(3) 0.0476(12) Uani 1 1 d . A . C64 C 0.3580(5) 0.4064(3) 0.5486(3) 0.0445(11) Uani 1 1 d . . . H64 H 0.4253 0.4380 0.5450 0.053 Uiso 1 1 calc R A . C65 C 0.3587(4) 0.3790(3) 0.4929(3) 0.0387(10) Uani 1 1 d . A . C66 C 0.0526(5) 0.2640(3) 0.5680(3) 0.0479(12) Uani 1 1 d . . . H66A H -0.0066 0.2624 0.6115 0.072 Uiso 1 1 calc R A . H66B H 0.0771 0.2086 0.5772 0.072 Uiso 1 1 calc R . . H66C H 0.0158 0.2888 0.5214 0.072 Uiso 1 1 calc R . . C67 C 0.2655(6) 0.4200(4) 0.6684(4) 0.0668(17) Uani 1 1 d . . . H67A H 0.3426 0.4488 0.6580 0.100 Uiso 1 1 calc R A . H67B H 0.2569 0.3739 0.7192 0.100 Uiso 1 1 calc R . . H67C H 0.1980 0.4572 0.6667 0.100 Uiso 1 1 calc R . . C68 C 0.4677(5) 0.4030(3) 0.4298(3) 0.0433(11) Uani 1 1 d . . . H68A H 0.4440 0.4441 0.3822 0.065 Uiso 1 1 calc R A . H68B H 0.4978 0.3551 0.4227 0.065 Uiso 1 1 calc R . . H68C H 0.5319 0.4255 0.4438 0.065 Uiso 1 1 calc R . . C1 C 0.6000(14) 0.3501(15) 0.2662(14) 0.035(5) Uani 0.458(13) 1 d PDU A 1 H1A H 0.6307 0.3030 0.3070 0.052 Uiso 0.458(13) 1 calc PR A 1 H1B H 0.6316 0.4002 0.2637 0.052 Uiso 0.458(13) 1 calc PR A 1 H1C H 0.6267 0.3477 0.2172 0.052 Uiso 0.458(13) 1 calc PR A 1 C1' C -0.1121(14) 0.3551(13) 0.3544(13) 0.044(4) Uani 0.542(13) 1 d PDU A 2 H1'1 H -0.1475 0.3072 0.3546 0.066 Uiso 0.542(13) 1 calc PR A 2 H1'2 H -0.1405 0.4045 0.3147 0.066 Uiso 0.542(13) 1 calc PR A 2 H1'3 H -0.1372 0.3554 0.4044 0.066 Uiso 0.542(13) 1 calc PR A 2 C2 C -0.0792(13) 0.3449(16) 0.3595(14) 0.047(5) Uani 0.50 1 d PDU A 1 C3 C -0.1838(13) 0.3455(10) 0.3751(9) 0.076(4) Uani 0.50 1 d PDU A 1 H3 H -0.2697 0.3460 0.3879 0.092 Uiso 0.50 1 calc PR A 1 C2' C 0.5669(13) 0.3442(13) 0.2642(12) 0.035(4) Uani 0.50 1 d PDU A 2 C3' C 0.6645(16) 0.3413(10) 0.2525(9) 0.075(4) Uani 0.50 1 d PDU A 2 H3' H 0.7506 0.3388 0.2423 0.090 Uiso 0.50 1 calc PR A 2 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 0.0349(2) 0.0471(2) 0.03897(19) -0.02421(15) -0.00247(13) -0.00314(14) Sn2 0.0351(2) 0.04304(19) 0.03853(19) -0.02238(14) -0.00310(13) -0.00102(13) Si1 0.0366(7) 0.0425(7) 0.0367(7) -0.0210(5) -0.0037(5) -0.0045(5) Si2 0.0361(7) 0.0407(6) 0.0361(6) -0.0217(5) -0.0018(5) -0.0009(5) Si3 0.0385(7) 0.0428(7) 0.0393(7) -0.0236(5) -0.0053(5) -0.0014(5) C10 0.038(3) 0.043(2) 0.038(2) -0.022(2) -0.008(2) 0.006(2) C11 0.047(3) 0.044(2) 0.038(2) -0.022(2) -0.009(2) 0.011(2) C12 0.051(3) 0.049(3) 0.043(3) -0.027(2) -0.006(2) 0.009(2) C13 0.057(3) 0.051(3) 0.054(3) -0.034(2) -0.019(3) 0.012(2) C14 0.049(3) 0.049(3) 0.053(3) -0.030(2) -0.017(2) 0.002(2) C15 0.039(3) 0.046(3) 0.043(3) -0.022(2) -0.011(2) 0.005(2) C16 0.046(3) 0.053(3) 0.041(3) -0.027(2) 0.000(2) 0.002(2) C17 0.077(5) 0.077(4) 0.093(5) -0.063(4) -0.026(4) 0.010(3) C18 0.044(3) 0.062(3) 0.052(3) -0.032(3) 0.001(2) -0.008(2) C20 0.036(3) 0.044(2) 0.036(2) -0.021(2) -0.0057(19) -0.0029(19) C21 0.043(3) 0.053(3) 0.044(3) -0.024(2) -0.005(2) -0.002(2) C22 0.046(3) 0.068(3) 0.048(3) -0.025(3) -0.013(2) 0.004(3) C23 0.060(4) 0.066(3) 0.045(3) -0.020(3) -0.010(3) -0.004(3) C24 0.050(3) 0.063(3) 0.041(3) -0.026(2) 0.002(2) -0.010(3) C25 0.043(3) 0.044(2) 0.041(3) -0.023(2) -0.004(2) -0.007(2) C26 0.046(3) 0.065(3) 0.052(3) -0.029(3) -0.009(2) 0.012(3) C27 0.075(5) 0.097(5) 0.045(3) -0.018(3) -0.014(3) 0.004(4) C28 0.047(3) 0.050(3) 0.041(3) -0.024(2) 0.004(2) -0.004(2) C30 0.038(3) 0.045(2) 0.040(2) -0.024(2) -0.006(2) -0.005(2) C31 0.038(3) 0.051(3) 0.046(3) -0.025(2) -0.006(2) -0.004(2) C32 0.041(3) 0.065(3) 0.048(3) -0.027(3) -0.012(2) 0.001(2) C33 0.047(3) 0.072(3) 0.041(3) -0.028(3) -0.004(2) -0.005(3) C34 0.043(3) 0.062(3) 0.045(3) -0.030(2) 0.000(2) -0.003(2) C35 0.039(3) 0.045(3) 0.046(3) -0.026(2) -0.004(2) -0.005(2) C36 0.043(3) 0.065(3) 0.048(3) -0.032(3) -0.011(2) 0.008(2) C37 0.060(4) 0.121(6) 0.042(3) -0.036(3) -0.008(3) 0.010(4) C38 0.043(3) 0.059(3) 0.047(3) -0.028(2) -0.005(2) 0.006(2) C40 0.054(3) 0.047(3) 0.039(3) -0.026(2) 0.002(2) -0.007(2) C41 0.059(4) 0.057(3) 0.050(3) -0.032(3) 0.002(3) -0.010(3) C42 0.075(5) 0.070(4) 0.067(4) -0.043(3) 0.020(3) -0.034(4) C43 0.099(6) 0.047(3) 0.063(4) -0.029(3) 0.018(4) -0.012(3) C44 0.080(5) 0.050(3) 0.056(3) -0.026(3) 0.000(3) 0.002(3) C45 0.065(4) 0.047(3) 0.041(3) -0.022(2) -0.002(2) 0.002(2) C46 0.055(4) 0.079(4) 0.070(4) -0.041(3) -0.003(3) -0.021(3) C47 0.145(8) 0.049(4) 0.102(6) -0.034(4) 0.032(6) -0.029(4) C48 0.059(4) 0.054(3) 0.059(3) -0.027(3) -0.012(3) 0.012(3) C50 0.043(3) 0.043(2) 0.037(2) -0.022(2) -0.001(2) -0.003(2) C51 0.043(3) 0.050(3) 0.039(2) -0.024(2) 0.001(2) -0.012(2) C52 0.052(3) 0.051(3) 0.052(3) -0.028(2) -0.001(2) -0.011(2) C53 0.063(4) 0.046(3) 0.055(3) -0.020(2) 0.000(3) -0.006(3) C54 0.052(3) 0.052(3) 0.060(3) -0.020(3) -0.014(3) 0.000(3) C55 0.043(3) 0.047(3) 0.043(3) -0.020(2) -0.006(2) -0.004(2) C56 0.042(3) 0.053(3) 0.053(3) -0.028(2) -0.006(2) -0.011(2) C57 0.069(5) 0.050(3) 0.105(5) -0.021(3) -0.016(4) -0.003(3) C58 0.042(3) 0.052(3) 0.066(3) -0.023(3) -0.014(3) 0.000(2) C60 0.037(3) 0.037(2) 0.041(2) -0.0206(19) -0.008(2) -0.0010(18) C61 0.034(3) 0.047(3) 0.043(3) -0.022(2) -0.004(2) -0.002(2) C62 0.039(3) 0.059(3) 0.048(3) -0.031(2) -0.004(2) -0.001(2) C63 0.044(3) 0.058(3) 0.054(3) -0.036(3) -0.010(2) 0.002(2) C64 0.037(3) 0.050(3) 0.057(3) -0.031(2) -0.011(2) -0.003(2) C65 0.033(3) 0.042(2) 0.043(3) -0.020(2) -0.007(2) -0.0003(19) C66 0.038(3) 0.059(3) 0.053(3) -0.032(2) 0.001(2) -0.008(2) C67 0.058(4) 0.098(5) 0.073(4) -0.066(4) -0.005(3) -0.003(3) C68 0.039(3) 0.050(3) 0.044(3) -0.024(2) -0.003(2) -0.010(2) C1 0.010(7) 0.049(7) 0.046(7) -0.022(5) -0.002(6) -0.009(6) C1' 0.034(8) 0.051(7) 0.050(7) -0.023(5) -0.009(7) 0.011(6) C2 0.033(7) 0.070(9) 0.049(7) -0.034(6) -0.013(6) 0.010(6) C3 0.074(8) 0.100(8) 0.069(7) -0.046(6) -0.023(6) 0.007(7) C2' 0.022(7) 0.053(6) 0.042(6) -0.026(5) -0.012(6) -0.006(6) C3' 0.070(8) 0.098(8) 0.066(7) -0.040(6) -0.021(6) 0.003(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 C93 C94 1.5153 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C94 C95 1.3900 . ? C94 C99 1.3900 . ? C95 C96 1.3900 . ? C95 H95 0.9500 . ? C96 C97 1.3900 . ? C96 H96 0.9500 . ? C97 C98 1.3900 . ? C97 H97 0.9500 . ? C98 C99 1.3900 . ? C98 H98 0.9500 . ? C99 H99 0.9500 . ? C81 C86 1.5153 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 C83 1.3900 . ? C82 C87 1.3900 . ? C82 H82 0.9500 . ? C83 C84 1.3900 . ? C83 H83 0.9500 . ? C84 C85 1.3900 . ? C84 H84 0.9500 . ? C85 C86 1.3900 . ? C85 H85 0.9500 . ? C86 C87 1.3900 . ? C87 H87 0.9500 . ? C71 C73 1.5153 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C73 1.3900 . ? C72 C77 1.3900 . ? C72 H72 0.9500 . ? C73 C74 1.3900 . ? C74 C75 1.3900 . ? C74 H74 0.9500 . ? C75 C76 1.3900 . ? C75 H75 0.9500 . ? C76 C77 1.3900 . ? C76 H76 0.9500 . ? C77 H77 0.9500 . ? Sn1 C2 1.988(14) . ? Sn1 C1' 2.345(15) . ? Sn1 Si2 2.6123(17) . ? Sn1 Si3 2.6213(15) . ? Sn1 Si1 2.6217(17) . ? Sn1 Sn2 3.1571(9) . ? Sn2 C2' 1.999(15) . ? Sn2 C1 2.348(15) . ? Sn2 Si1 2.6191(17) . ? Sn2 Si2 2.6197(16) . ? Sn2 Si3 2.6199(15) . ? Si1 C50 1.898(5) . ? Si1 C60 1.908(5) . ? Si2 C20 1.904(5) . ? Si2 C10 1.906(5) . ? Si3 C30 1.904(5) . ? Si3 C40 1.907(5) . ? C10 C15 1.403(7) . ? C10 C11 1.432(7) . ? C11 C12 1.397(7) . ? C11 C16 1.512(7) . ? C12 C13 1.380(8) . ? C12 H12 0.9500 . ? C13 C14 1.379(8) . ? C13 C17 1.512(7) . ? C14 C15 1.415(7) . ? C14 H14 0.9500 . ? C15 C18 1.501(7) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C20 C21 1.416(7) . ? C20 C25 1.418(7) . ? C21 C22 1.381(7) . ? C21 C26 1.525(7) . ? C22 C23 1.403(8) . ? C22 H22 0.9500 . ? C23 C24 1.386(9) . ? C23 C27 1.525(8) . ? C24 C25 1.391(7) . ? C24 H24 0.9500 . ? C25 C28 1.506(7) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C30 C35 1.409(7) . ? C30 C31 1.417(7) . ? C31 C32 1.397(7) . ? C31 C36 1.507(7) . ? C32 C33 1.389(8) . ? C32 H32 0.9500 . ? C33 C34 1.389(8) . ? C33 C37 1.499(8) . ? C34 C35 1.399(7) . ? C34 H34 0.9500 . ? C35 C38 1.503(7) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C40 C41 1.419(8) . ? C40 C45 1.422(8) . ? C41 C42 1.401(8) . ? C41 C46 1.502(9) . ? C42 C43 1.398(11) . ? C42 H42 0.9500 . ? C43 C44 1.388(10) . ? C43 C47 1.508(8) . ? C44 C45 1.377(8) . ? C44 H44 0.9500 . ? C45 C48 1.504(9) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C50 C55 1.412(7) . ? C50 C51 1.423(7) . ? C51 C52 1.382(7) . ? C51 C56 1.511(8) . ? C52 C53 1.372(9) . ? C52 H52 0.9500 . ? C53 C54 1.394(8) . ? C53 C57 1.508(8) . ? C54 C55 1.394(7) . ? C54 H54 0.9500 . ? C55 C58 1.505(7) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C60 C61 1.406(7) . ? C60 C65 1.421(6) . ? C61 C62 1.401(7) . ? C61 C66 1.516(7) . ? C62 C63 1.399(7) . ? C62 H62 0.9500 . ? C63 C64 1.378(7) . ? C63 C67 1.510(7) . ? C64 C65 1.391(7) . ? C64 H64 0.9500 . ? C65 C68 1.512(7) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1' H1'1 0.9800 . ? C1' H1'2 0.9800 . ? C1' H1'3 0.9800 . ? C2 C3 1.156(9) . ? C3 H3 0.9500 . ? C2' C3' 1.079(17) . ? C3' H3' 0.9500 . ? 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 C94 C93 H93A 109.5 . . ? C94 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C94 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C95 C94 C99 120.0 . . ? C95 C94 C93 120.01(6) . . ? C99 C94 C93 119.99(6) . . ? C96 C95 C94 120.0 . . ? C96 C95 H95 120.0 . . ? C94 C95 H95 120.0 . . ? C95 C96 C97 120.0 . . ? C95 C96 H96 120.0 . . ? C97 C96 H96 120.0 . . ? C98 C97 C96 120.0 . . ? C98 C97 H97 120.0 . . ? C96 C97 H97 120.0 . . ? C97 C98 C99 120.0 . . ? C97 C98 H98 120.0 . . ? C99 C98 H98 120.0 . . ? C98 C99 C94 120.0 . . ? C98 C99 H99 120.0 . . ? C94 C99 H99 120.0 . . ? C86 C81 H81A 109.5 . . ? C86 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C86 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C83 C82 C87 120.0 . . ? C83 C82 H82 120.0 . . ? C87 C82 H82 120.0 . . ? C84 C83 C82 120.0 . . ? C84 C83 H83 120.0 . . ? C82 C83 H83 120.0 . . ? C85 C84 C83 120.0 . . ? C85 C84 H84 120.0 . . ? C83 C84 H84 120.0 . . ? C84 C85 C86 120.0 . . ? C84 C85 H85 120.0 . . ? C86 C85 H85 120.0 . . ? C87 C86 C85 120.0 . . ? C87 C86 C81 120.00(6) . . ? C85 C86 C81 120.00(6) . . ? C86 C87 C82 120.0 . . ? C86 C87 H87 120.0 . . ? C82 C87 H87 120.0 . . ? C73 C71 H71A 109.5 . . ? C73 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C73 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C73 C72 C77 120.0 . . ? C73 C72 H72 120.0 . . ? C77 C72 H72 120.0 . . ? C74 C73 C72 120.0 . . ? C74 C73 C71 120.01(7) . . ? C72 C73 C71 119.99(6) . . ? C73 C74 C75 120.0 . . ? C73 C74 H74 120.0 . . ? C75 C74 H74 120.0 . . ? C74 C75 C76 120.0 . . ? C74 C75 H75 120.0 . . ? C76 C75 H75 120.0 . . ? C77 C76 C75 120.0 . . ? C77 C76 H76 120.0 . . ? C75 C76 H76 120.0 . . ? C76 C77 C72 120.0 . . ? C76 C77 H77 120.0 . . ? C72 C77 H77 120.0 . . ? C2 Sn1 C1' 5.4(11) . . ? C2 Sn1 Si2 130.3(7) . . ? C1' Sn1 Si2 125.8(5) . . ? C2 Sn1 Si3 127.4(9) . . ? C1' Sn1 Si3 127.2(7) . . ? Si2 Sn1 Si3 87.57(5) . . ? C2 Sn1 Si1 123.3(7) . . ? C1' Sn1 Si1 128.1(6) . . ? Si2 Sn1 Si1 87.43(5) . . ? Si3 Sn1 Si1 87.35(5) . . ? C2 Sn1 Sn2 175.9(7) . . ? C1' Sn1 Sn2 178.7(5) . . ? Si2 Sn1 Sn2 52.99(4) . . ? Si3 Sn1 Sn2 52.94(4) . . ? Si1 Sn1 Sn2 52.92(4) . . ? C2' Sn2 C1 5.4(12) . . ? C2' Sn2 Si1 128.9(6) . . ? C1 Sn2 Si1 126.2(6) . . ? C2' Sn2 Si2 128.7(6) . . ? C1 Sn2 Si2 126.1(6) . . ? Si1 Sn2 Si2 87.33(5) . . ? C2' Sn2 Si3 123.5(6) . . ? C1 Sn2 Si3 129.0(6) . . ? Si1 Sn2 Si3 87.43(5) . . ? Si2 Sn2 Si3 87.45(5) . . ? C2' Sn2 Sn1 176.5(6) . . ? C1 Sn2 Sn1 178.1(6) . . ? Si1 Sn2 Sn1 52.99(4) . . ? Si2 Sn2 Sn1 52.78(4) . . ? Si3 Sn2 Sn1 52.98(3) . . ? C50 Si1 C60 109.3(2) . . ? C50 Si1 Sn2 115.19(15) . . ? C60 Si1 Sn2 119.61(15) . . ? C50 Si1 Sn1 117.42(16) . . ? C60 Si1 Sn1 117.80(15) . . ? Sn2 Si1 Sn1 74.09(4) . . ? C20 Si2 C10 110.3(2) . . ? C20 Si2 Sn1 116.57(15) . . ? C10 Si2 Sn1 117.89(15) . . ? C20 Si2 Sn2 118.49(16) . . ? C10 Si2 Sn2 115.57(15) . . ? Sn1 Si2 Sn2 74.23(4) . . ? C30 Si3 C40 108.1(2) . . ? C30 Si3 Sn2 117.01(15) . . ? C40 Si3 Sn2 118.82(18) . . ? C30 Si3 Sn1 119.09(16) . . ? C40 Si3 Sn1 116.88(16) . . ? Sn2 Si3 Sn1 74.08(4) . . ? C15 C10 C11 117.9(4) . . ? C15 C10 Si2 118.2(4) . . ? C11 C10 Si2 123.9(4) . . ? C12 C11 C10 119.5(5) . . ? C12 C11 C16 117.0(4) . . ? C10 C11 C16 123.5(4) . . ? C13 C12 C11 122.3(5) . . ? C13 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? C14 C13 C12 118.5(5) . . ? C14 C13 C17 120.8(5) . . ? C12 C13 C17 120.6(5) . . ? C13 C14 C15 121.5(5) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C10 C15 C14 120.2(5) . . ? C10 C15 C18 122.2(4) . . ? C14 C15 C18 117.5(5) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 C20 C25 117.3(4) . . ? C21 C20 Si2 118.5(4) . . ? C25 C20 Si2 124.2(4) . . ? C22 C21 C20 121.8(5) . . ? C22 C21 C26 117.2(5) . . ? C20 C21 C26 121.0(4) . . ? C21 C22 C23 120.7(5) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C24 C23 C22 117.8(5) . . ? C24 C23 C27 122.1(6) . . ? C22 C23 C27 120.1(6) . . ? C23 C24 C25 122.8(5) . . ? C23 C24 H24 118.6 . . ? C25 C24 H24 118.6 . . ? C24 C25 C20 119.5(5) . . ? C24 C25 C28 116.7(4) . . ? C20 C25 C28 123.8(4) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C35 C30 C31 117.8(4) . . ? C35 C30 Si3 117.8(4) . . ? C31 C30 Si3 124.3(4) . . ? C32 C31 C30 120.0(5) . . ? C32 C31 C36 115.9(5) . . ? C30 C31 C36 124.2(4) . . ? C33 C32 C31 122.3(5) . . ? C33 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? C32 C33 C34 117.7(5) . . ? C32 C33 C37 121.6(5) . . ? C34 C33 C37 120.7(5) . . ? C33 C34 C35 121.8(5) . . ? C33 C34 H34 119.1 . . ? C35 C34 H34 119.1 . . ? C34 C35 C30 120.4(5) . . ? C34 C35 C38 117.4(5) . . ? C30 C35 C38 122.2(4) . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C33 C37 H37A 109.5 . . ? C33 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C33 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C41 C40 C45 117.6(5) . . ? C41 C40 Si3 117.7(4) . . ? C45 C40 Si3 124.7(4) . . ? C42 C41 C40 119.7(6) . . ? C42 C41 C46 118.1(6) . . ? C40 C41 C46 122.1(5) . . ? C43 C42 C41 121.9(6) . . ? C43 C42 H42 119.0 . . ? C41 C42 H42 119.0 . . ? C44 C43 C42 117.7(5) . . ? C44 C43 C47 121.1(8) . . ? C42 C43 C47 121.2(7) . . ? C45 C44 C43 122.2(7) . . ? C45 C44 H44 118.9 . . ? C43 C44 H44 118.9 . . ? C44 C45 C40 120.8(6) . . ? C44 C45 C48 115.3(5) . . ? C40 C45 C48 123.9(5) . . ? C41 C46 H46A 109.5 . . ? C41 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C41 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C43 C47 H47A 109.5 . . ? C43 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C43 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C55 C50 C51 117.5(4) . . ? C55 C50 Si1 118.5(4) . . ? C51 C50 Si1 124.0(4) . . ? C52 C51 C50 119.6(5) . . ? C52 C51 C56 116.6(4) . . ? C50 C51 C56 123.8(4) . . ? C53 C52 C51 123.4(5) . . ? C53 C52 H52 118.3 . . ? C51 C52 H52 118.3 . . ? C52 C53 C54 117.4(5) . . ? C52 C53 C57 121.7(5) . . ? C54 C53 C57 121.0(6) . . ? C53 C54 C55 121.7(6) . . ? C53 C54 H54 119.1 . . ? C55 C54 H54 119.1 . . ? C54 C55 C50 120.3(5) . . ? C54 C55 C58 117.8(5) . . ? C50 C55 C58 121.8(4) . . ? C51 C56 H56A 109.5 . . ? C51 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C51 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C53 C57 H57A 109.5 . . ? C53 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C53 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C61 C60 C65 117.6(4) . . ? C61 C60 Si1 118.0(3) . . ? C65 C60 Si1 124.3(4) . . ? C62 C61 C60 120.9(4) . . ? C62 C61 C66 117.1(4) . . ? C60 C61 C66 122.0(4) . . ? C63 C62 C61 121.1(5) . . ? C63 C62 H62 119.5 . . ? C61 C62 H62 119.5 . . ? C64 C63 C62 117.9(5) . . ? C64 C63 C67 121.6(5) . . ? C62 C63 C67 120.6(5) . . ? C63 C64 C65 122.7(5) . . ? C63 C64 H64 118.6 . . ? C65 C64 H64 118.6 . . ? C64 C65 C60 119.9(4) . . ? C64 C65 C68 116.8(4) . . ? C60 C65 C68 123.3(4) . . ? C61 C66 H66A 109.5 . . ? C61 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C61 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C63 C67 H67A 109.5 . . ? C63 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C63 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? Sn2 C1 H1A 109.5 . . ? Sn2 C1 H1B 109.5 . . ? Sn2 C1 H1C 109.5 . . ? Sn1 C1' H1'1 109.5 . . ? Sn1 C1' H1'2 109.5 . . ? H1'1 C1' H1'2 109.5 . . ? Sn1 C1' H1'3 109.5 . . ? H1'1 C1' H1'3 109.5 . . ? H1'2 C1' H1'3 109.5 . . ? C3 C2 Sn1 177(2) . . ? C2 C3 H3 180.0 . . ? C3' C2' Sn2 177(2) . . ? C2' C3' H3' 180.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C99 C94 C95 C96 0.0 . . . . ? C93 C94 C95 C96 179.6(8) . . . . ? C94 C95 C96 C97 0.0 . . . . ? C95 C96 C97 C98 0.0 . . . . ? C96 C97 C98 C99 0.0 . . . . ? C97 C98 C99 C94 0.0 . . . . ? C95 C94 C99 C98 0.0 . . . . ? C93 C94 C99 C98 -179.6(8) . . . . ? C87 C82 C83 C84 0.0 . . . . ? C82 C83 C84 C85 0.0 . . . . ? C83 C84 C85 C86 0.0 . . . . ? C84 C85 C86 C87 0.0 . . . . ? C84 C85 C86 C81 -179.8(8) . . . . ? C85 C86 C87 C82 0.0 . . . . ? C81 C86 C87 C82 179.8(8) . . . . ? C83 C82 C87 C86 0.0 . . . . ? C77 C72 C73 C74 0.0 . . . . ? C77 C72 C73 C71 -179.6(8) . . . . ? C72 C73 C74 C75 0.0 . . . . ? C71 C73 C74 C75 179.6(8) . . . . ? C73 C74 C75 C76 0.0 . . . . ? C74 C75 C76 C77 0.0 . . . . ? C75 C76 C77 C72 0.0 . . . . ? C73 C72 C77 C76 0.0 . . . . ? Si2 Sn1 Sn2 Si1 119.95(6) . . . . ? Si3 Sn1 Sn2 Si1 -119.87(5) . . . . ? Si3 Sn1 Sn2 Si2 120.18(5) . . . . ? Si1 Sn1 Sn2 Si2 -119.95(6) . . . . ? Si2 Sn1 Sn2 Si3 -120.18(5) . . . . ? Si1 Sn1 Sn2 Si3 119.87(5) . . . . ? C2' Sn2 Si1 C50 -63.0(8) . . . . ? C1 Sn2 Si1 C50 -68.9(8) . . . . ? Si2 Sn2 Si1 C50 156.96(18) . . . . ? Si3 Sn2 Si1 C50 69.39(18) . . . . ? Sn1 Sn2 Si1 C50 113.27(18) . . . . ? C2' Sn2 Si1 C60 70.5(8) . . . . ? C1 Sn2 Si1 C60 64.5(8) . . . . ? Si2 Sn2 Si1 C60 -69.62(18) . . . . ? Si3 Sn2 Si1 C60 -157.18(18) . . . . ? Sn1 Sn2 Si1 C60 -113.31(18) . . . . ? C2' Sn2 Si1 Sn1 -176.2(8) . . . . ? C1 Sn2 Si1 Sn1 177.8(7) . . . . ? Si2 Sn2 Si1 Sn1 43.69(4) . . . . ? Si3 Sn2 Si1 Sn1 -43.87(4) . . . . ? C2 Sn1 Si1 C50 67.5(10) . . . . ? C1' Sn1 Si1 C50 70.4(8) . . . . ? Si2 Sn1 Si1 C50 -154.37(17) . . . . ? Si3 Sn1 Si1 C50 -66.68(17) . . . . ? Sn2 Sn1 Si1 C50 -110.53(17) . . . . ? C2 Sn1 Si1 C60 -66.5(10) . . . . ? C1' Sn1 Si1 C60 -63.5(8) . . . . ? Si2 Sn1 Si1 C60 71.65(17) . . . . ? Si3 Sn1 Si1 C60 159.34(17) . . . . ? Sn2 Sn1 Si1 C60 115.49(17) . . . . ? C2 Sn1 Si1 Sn2 178.0(10) . . . . ? C1' Sn1 Si1 Sn2 -179.0(8) . . . . ? Si2 Sn1 Si1 Sn2 -43.84(4) . . . . ? Si3 Sn1 Si1 Sn2 43.85(4) . . . . ? C2 Sn1 Si2 C20 -68.8(11) . . . . ? C1' Sn1 Si2 C20 -65.0(8) . . . . ? Si3 Sn1 Si2 C20 70.72(17) . . . . ? Si1 Sn1 Si2 C20 158.17(17) . . . . ? Sn2 Sn1 Si2 C20 114.39(18) . . . . ? C2 Sn1 Si2 C10 65.8(11) . . . . ? C1' Sn1 Si2 C10 69.6(8) . . . . ? Si3 Sn1 Si2 C10 -154.63(17) . . . . ? Si1 Sn1 Si2 C10 -67.18(17) . . . . ? Sn2 Sn1 Si2 C10 -110.97(18) . . . . ? C2 Sn1 Si2 Sn2 176.8(11) . . . . ? C1' Sn1 Si2 Sn2 -179.4(8) . . . . ? Si3 Sn1 Si2 Sn2 -43.66(4) . . . . ? Si1 Sn1 Si2 Sn2 43.79(4) . . . . ? C2' Sn2 Si2 C20 63.9(8) . . . . ? C1 Sn2 Si2 C20 69.9(8) . . . . ? Si1 Sn2 Si2 C20 -155.91(17) . . . . ? Si3 Sn2 Si2 C20 -68.37(17) . . . . ? Sn1 Sn2 Si2 C20 -112.06(17) . . . . ? C2' Sn2 Si2 C10 -70.2(8) . . . . ? C1 Sn2 Si2 C10 -64.2(8) . . . . ? Si1 Sn2 Si2 C10 69.97(17) . . . . ? Si3 Sn2 Si2 C10 157.51(17) . . . . ? Sn1 Sn2 Si2 C10 113.81(17) . . . . ? C2' Sn2 Si2 Sn1 176.0(8) . . . . ? C1 Sn2 Si2 Sn1 -178.1(7) . . . . ? Si1 Sn2 Si2 Sn1 -43.85(4) . . . . ? Si3 Sn2 Si2 Sn1 43.70(4) . . . . ? C2' Sn2 Si3 C30 -64.8(8) . . . . ? C1 Sn2 Si3 C30 -64.8(8) . . . . ? Si1 Sn2 Si3 C30 158.85(18) . . . . ? Si2 Sn2 Si3 C30 71.41(18) . . . . ? Sn1 Sn2 Si3 C30 114.97(18) . . . . ? C2' Sn2 Si3 C40 67.9(8) . . . . ? C1 Sn2 Si3 C40 67.9(8) . . . . ? Si1 Sn2 Si3 C40 -68.43(18) . . . . ? Si2 Sn2 Si3 C40 -155.87(18) . . . . ? Sn1 Sn2 Si3 C40 -112.31(18) . . . . ? C2' Sn2 Si3 Sn1 -179.8(7) . . . . ? C1 Sn2 Si3 Sn1 -179.7(7) . . . . ? Si1 Sn2 Si3 Sn1 43.88(4) . . . . ? Si2 Sn2 Si3 Sn1 -43.55(4) . . . . ? C2 Sn1 Si3 C30 72.7(9) . . . . ? C1' Sn1 Si3 C30 66.0(6) . . . . ? Si2 Sn1 Si3 C30 -68.74(17) . . . . ? Si1 Sn1 Si3 C30 -156.28(17) . . . . ? Sn2 Sn1 Si3 C30 -112.44(17) . . . . ? C2 Sn1 Si3 C40 -60.1(9) . . . . ? C1' Sn1 Si3 C40 -66.9(6) . . . . ? Si2 Sn1 Si3 C40 158.4(2) . . . . ? Si1 Sn1 Si3 C40 70.8(2) . . . . ? Sn2 Sn1 Si3 C40 114.7(2) . . . . ? C2 Sn1 Si3 Sn2 -174.8(8) . . . . ? C1' Sn1 Si3 Sn2 178.4(6) . . . . ? Si2 Sn1 Si3 Sn2 43.70(4) . . . . ? Si1 Sn1 Si3 Sn2 -43.83(4) . . . . ? C20 Si2 C10 C15 -63.5(4) . . . . ? Sn1 Si2 C10 C15 159.3(3) . . . . ? Sn2 Si2 C10 C15 74.3(4) . . . . ? C20 Si2 C10 C11 116.2(4) . . . . ? Sn1 Si2 C10 C11 -21.1(5) . . . . ? Sn2 Si2 C10 C11 -106.1(4) . . . . ? C15 C10 C11 C12 -1.4(7) . . . . ? Si2 C10 C11 C12 179.0(4) . . . . ? C15 C10 C11 C16 179.0(5) . . . . ? Si2 C10 C11 C16 -0.6(7) . . . . ? C10 C11 C12 C13 0.9(8) . . . . ? C16 C11 C12 C13 -179.5(5) . . . . ? C11 C12 C13 C14 -0.1(8) . . . . ? C11 C12 C13 C17 178.1(5) . . . . ? C12 C13 C14 C15 0.0(8) . . . . ? C17 C13 C14 C15 -178.2(5) . . . . ? C11 C10 C15 C14 1.3(7) . . . . ? Si2 C10 C15 C14 -179.1(4) . . . . ? C11 C10 C15 C18 180.0(5) . . . . ? Si2 C10 C15 C18 -0.4(7) . . . . ? C13 C14 C15 C10 -0.6(8) . . . . ? C13 C14 C15 C18 -179.3(5) . . . . ? C10 Si2 C20 C21 -64.0(4) . . . . ? Sn1 Si2 C20 C21 73.9(4) . . . . ? Sn2 Si2 C20 C21 159.7(3) . . . . ? C10 Si2 C20 C25 115.9(4) . . . . ? Sn1 Si2 C20 C25 -106.1(4) . . . . ? Sn2 Si2 C20 C25 -20.4(5) . . . . ? C25 C20 C21 C22 0.7(7) . . . . ? Si2 C20 C21 C22 -179.3(4) . . . . ? C25 C20 C21 C26 -179.8(5) . . . . ? Si2 C20 C21 C26 0.1(6) . . . . ? C20 C21 C22 C23 -0.2(8) . . . . ? C26 C21 C22 C23 -179.7(5) . . . . ? C21 C22 C23 C24 -0.2(9) . . . . ? C21 C22 C23 C27 -178.1(6) . . . . ? C22 C23 C24 C25 0.1(9) . . . . ? C27 C23 C24 C25 177.9(6) . . . . ? C23 C24 C25 C20 0.5(8) . . . . ? C23 C24 C25 C28 -179.3(5) . . . . ? C21 C20 C25 C24 -0.8(7) . . . . ? Si2 C20 C25 C24 179.2(4) . . . . ? C21 C20 C25 C28 178.9(4) . . . . ? Si2 C20 C25 C28 -1.1(7) . . . . ? C40 Si3 C30 C35 -63.2(4) . . . . ? Sn2 Si3 C30 C35 74.2(4) . . . . ? Sn1 Si3 C30 C35 160.3(3) . . . . ? C40 Si3 C30 C31 114.0(4) . . . . ? Sn2 Si3 C30 C31 -108.6(4) . . . . ? Sn1 Si3 C30 C31 -22.5(5) . . . . ? C35 C30 C31 C32 1.4(7) . . . . ? Si3 C30 C31 C32 -175.7(4) . . . . ? C35 C30 C31 C36 -178.8(5) . . . . ? Si3 C30 C31 C36 4.0(7) . . . . ? C30 C31 C32 C33 -2.0(8) . . . . ? C36 C31 C32 C33 178.2(5) . . . . ? C31 C32 C33 C34 0.4(8) . . . . ? C31 C32 C33 C37 -179.4(6) . . . . ? C32 C33 C34 C35 1.7(8) . . . . ? C37 C33 C34 C35 -178.5(6) . . . . ? C33 C34 C35 C30 -2.2(8) . . . . ? C33 C34 C35 C38 178.7(5) . . . . ? C31 C30 C35 C34 0.6(7) . . . . ? Si3 C30 C35 C34 178.0(4) . . . . ? C31 C30 C35 C38 179.6(4) . . . . ? Si3 C30 C35 C38 -3.0(6) . . . . ? C30 Si3 C40 C41 -65.0(4) . . . . ? Sn2 Si3 C40 C41 158.5(3) . . . . ? Sn1 Si3 C40 C41 72.6(4) . . . . ? C30 Si3 C40 C45 113.6(4) . . . . ? Sn2 Si3 C40 C45 -22.9(5) . . . . ? Sn1 Si3 C40 C45 -108.8(4) . . . . ? C45 C40 C41 C42 0.1(7) . . . . ? Si3 C40 C41 C42 178.8(4) . . . . ? C45 C40 C41 C46 -179.8(5) . . . . ? Si3 C40 C41 C46 -1.1(7) . . . . ? C40 C41 C42 C43 -1.6(9) . . . . ? C46 C41 C42 C43 178.4(6) . . . . ? C41 C42 C43 C44 1.5(9) . . . . ? C41 C42 C43 C47 -178.1(6) . . . . ? C42 C43 C44 C45 0.0(9) . . . . ? C47 C43 C44 C45 179.6(6) . . . . ? C43 C44 C45 C40 -1.5(9) . . . . ? C43 C44 C45 C48 179.7(6) . . . . ? C41 C40 C45 C44 1.4(7) . . . . ? Si3 C40 C45 C44 -177.2(4) . . . . ? C41 C40 C45 C48 -179.8(5) . . . . ? Si3 C40 C45 C48 1.6(7) . . . . ? C60 Si1 C50 C55 -65.8(4) . . . . ? Sn2 Si1 C50 C55 72.2(4) . . . . ? Sn1 Si1 C50 C55 156.6(3) . . . . ? C60 Si1 C50 C51 115.9(4) . . . . ? Sn2 Si1 C50 C51 -106.1(4) . . . . ? Sn1 Si1 C50 C51 -21.7(5) . . . . ? C55 C50 C51 C52 -0.3(7) . . . . ? Si1 C50 C51 C52 178.0(4) . . . . ? C55 C50 C51 C56 -179.8(5) . . . . ? Si1 C50 C51 C56 -1.5(7) . . . . ? C50 C51 C52 C53 -1.8(8) . . . . ? C56 C51 C52 C53 177.8(5) . . . . ? C51 C52 C53 C54 2.2(9) . . . . ? C51 C52 C53 C57 -177.6(6) . . . . ? C52 C53 C54 C55 -0.7(9) . . . . ? C57 C53 C54 C55 179.2(6) . . . . ? C53 C54 C55 C50 -1.3(9) . . . . ? C53 C54 C55 C58 178.8(5) . . . . ? C51 C50 C55 C54 1.7(7) . . . . ? Si1 C50 C55 C54 -176.7(4) . . . . ? C51 C50 C55 C58 -178.3(5) . . . . ? Si1 C50 C55 C58 3.2(7) . . . . ? C50 Si1 C60 C61 -62.8(4) . . . . ? Sn2 Si1 C60 C61 161.3(3) . . . . ? Sn1 Si1 C60 C61 74.6(4) . . . . ? C50 Si1 C60 C65 114.8(4) . . . . ? Sn2 Si1 C60 C65 -21.1(5) . . . . ? Sn1 Si1 C60 C65 -107.8(4) . . . . ? C65 C60 C61 C62 0.1(7) . . . . ? Si1 C60 C61 C62 177.8(4) . . . . ? C65 C60 C61 C66 179.5(5) . . . . ? Si1 C60 C61 C66 -2.7(6) . . . . ? C60 C61 C62 C63 -0.4(8) . . . . ? C66 C61 C62 C63 -179.9(5) . . . . ? C61 C62 C63 C64 0.4(8) . . . . ? C61 C62 C63 C67 -179.7(5) . . . . ? C62 C63 C64 C65 0.0(8) . . . . ? C67 C63 C64 C65 -180.0(5) . . . . ? C63 C64 C65 C60 -0.3(8) . . . . ? C63 C64 C65 C68 179.4(5) . . . . ? C61 C60 C65 C64 0.3(7) . . . . ? Si1 C60 C65 C64 -177.3(4) . . . . ? C61 C60 C65 C68 -179.4(4) . . . . ? Si1 C60 C65 C68 3.0(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 1.355 _refine_diff_density_min -0.670 _refine_diff_density_rms 0.118 data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 879398' #TrackingRef 'AlkynylSn2Si3_ChemComm.cif' _chemical_name_systematic ; 1-(prop-1-yn)-2,2,4,4,5,5-hexakis(2,4,6-trimethylphenyl)- 3-methyl-2,4,5-trisila-1,3-distannabicyclo[1.1.1]pentane ; _audit_creation_method SHELXL-97 _chemical_name_common ; 1-(prop-1-yn)-2,2,4,4,5,5-hexakis(2,4,6-trimethylphenyl)-3- methyl-2,4,5-trisila-1,3-distannabicyclo(1.1.1)pentane ; _chemical_melting_point ? _chemical_formula_moiety 'C58 H72 Si3 Sn2, C7 H8' _chemical_formula_sum 'C65 H80 Si3 Sn2' _chemical_formula_weight 1182.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.384(2) _cell_length_b 26.502(5) _cell_length_c 19.445(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.70(3) _cell_angle_gamma 90.00 _cell_volume 5864(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 40243 _cell_measurement_theta_min 3.24 _cell_measurement_theta_max 25.00 _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 0.951 _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 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Stadi with CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40243 _diffrn_reflns_av_R_equivalents 0.0872 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10267 _reflns_number_gt 8544 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis Red' _computing_data_reduction 'CrysAlis Red' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Ortep 32' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0605P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10267 _refine_ls_number_parameters 653 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1114 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn2 Sn 0.22530(2) 0.661084(9) 0.396454(12) 0.02637(9) Uani 1 1 d . . . Sn1 Sn 0.06915(2) 0.690486(9) 0.265638(12) 0.02617(9) Uani 1 1 d . . . Si3 Si 0.00333(9) 0.68581(4) 0.39332(5) 0.0258(2) Uani 1 1 d . . . Si2 Si 0.25730(9) 0.73664(4) 0.31215(5) 0.0266(2) Uani 1 1 d . . . Si1 Si 0.17969(9) 0.60499(4) 0.28893(5) 0.0272(2) Uani 1 1 d . . . C23 C 0.2406(3) 0.80179(13) 0.35235(19) 0.0305(9) Uani 1 1 d . . . C50 C 0.0782(3) 0.54904(13) 0.29968(19) 0.0309(8) Uani 1 1 d . . . C5 C -0.1068(3) 0.63586(14) 0.41721(19) 0.0292(8) Uani 1 1 d . . . C51 C 0.0182(3) 0.52990(14) 0.2409(2) 0.0346(9) Uani 1 1 d . . . C52 C -0.0654(4) 0.49186(15) 0.2461(2) 0.0385(10) Uani 1 1 d . . . H52 H -0.1056 0.4800 0.2057 0.046 Uiso 1 1 calc R . . C19 C 0.0321(3) 0.77492(14) 0.48229(18) 0.0306(8) Uani 1 1 d . . . C1 C -0.0424(4) 0.71273(17) 0.17964(19) 0.0397(10) Uani 1 1 d . . . H1A H -0.0945 0.7400 0.1937 0.060 Uiso 1 1 calc R . . H1B H -0.0896 0.6838 0.1639 0.060 Uiso 1 1 calc R . . H1C H 0.0062 0.7245 0.1421 0.060 Uiso 1 1 calc R . . C2 C 0.3329(3) 0.63964(14) 0.4813(2) 0.0334(9) Uani 1 1 d . . . C6 C -0.1824(3) 0.61098(13) 0.3690(2) 0.0309(9) Uani 1 1 d . . . C41 C 0.3112(3) 0.58720(14) 0.23640(19) 0.0301(8) Uani 1 1 d . . . C55 C 0.0537(3) 0.52629(13) 0.3637(2) 0.0327(9) Uani 1 1 d . . . C38 C 0.2728(4) 0.79732(15) 0.1760(2) 0.0402(10) Uani 1 1 d . . . H38A H 0.2793 0.8124 0.1303 0.060 Uiso 1 1 calc R . . H38B H 0.2737 0.8240 0.2109 0.060 Uiso 1 1 calc R . . H38C H 0.1990 0.7784 0.1780 0.060 Uiso 1 1 calc R . . C28 C 0.3311(4) 0.81756(15) 0.3995(2) 0.0378(10) Uani 1 1 d . . . C42 C 0.3372(4) 0.60740(14) 0.17149(19) 0.0358(9) Uani 1 1 d . . . C46 C 0.3933(3) 0.55222(14) 0.2653(2) 0.0350(9) Uani 1 1 d . . . C16 C -0.1748(4) 0.81865(16) 0.4343(2) 0.0413(10) Uani 1 1 d . . . H16 H -0.2458 0.8337 0.4176 0.050 Uiso 1 1 calc R . . C11 C -0.1813(3) 0.62044(14) 0.2925(2) 0.0343(9) Uani 1 1 d . . . H11A H -0.2446 0.6011 0.2697 0.051 Uiso 1 1 calc R . . H11B H -0.1055 0.6099 0.2748 0.051 Uiso 1 1 calc R . . H11C H -0.1932 0.6565 0.2835 0.051 Uiso 1 1 calc R . . C24 C 0.1451(4) 0.83432(14) 0.3404(2) 0.0355(9) Uani 1 1 d . . . C14 C -0.0377(3) 0.74842(13) 0.43285(18) 0.0292(8) Uani 1 1 d . . . C49 C 0.3744(4) 0.52737(16) 0.3337(2) 0.0426(10) Uani 1 1 d . . . H49A H 0.4385 0.5035 0.3438 0.064 Uiso 1 1 calc R . . H49B H 0.2994 0.5093 0.3322 0.064 Uiso 1 1 calc R . . H49C H 0.3733 0.5532 0.3698 0.064 Uiso 1 1 calc R . . C40 C 0.5074(4) 0.67116(15) 0.3237(2) 0.0381(10) Uani 1 1 d . . . H40A H 0.4911 0.6910 0.3649 0.057 Uiso 1 1 calc R . . H40B H 0.5897 0.6603 0.3255 0.057 Uiso 1 1 calc R . . H40C H 0.4561 0.6415 0.3219 0.057 Uiso 1 1 calc R . . C9 C -0.1995(4) 0.58742(15) 0.5067(2) 0.0400(10) Uani 1 1 d . . . H9 H -0.2053 0.5795 0.5541 0.048 Uiso 1 1 calc R . . C20 C -0.2256(3) 0.74668(15) 0.3585(2) 0.0442(11) Uani 1 1 d . . . H20A H -0.2927 0.7689 0.3485 0.066 Uiso 1 1 calc R . . H20B H -0.2538 0.7146 0.3771 0.066 Uiso 1 1 calc R . . H20C H -0.1835 0.7403 0.3161 0.066 Uiso 1 1 calc R . . C37 C 0.4846(3) 0.70313(15) 0.2602(2) 0.0346(9) Uani 1 1 d . . . C34 C 0.4578(4) 0.75773(17) 0.1393(2) 0.0424(10) Uani 1 1 d . . . H34 H 0.4472 0.7763 0.0978 0.051 Uiso 1 1 calc R . . C18 C -0.0036(4) 0.82194(15) 0.5047(2) 0.0398(10) Uani 1 1 d . . . H18 H 0.0447 0.8394 0.5375 0.048 Uiso 1 1 calc R . . C27 C 0.3196(4) 0.86324(16) 0.4341(2) 0.0452(11) Uani 1 1 d . . . H27 H 0.3800 0.8733 0.4660 0.054 Uiso 1 1 calc R . . C13 C -0.0409(4) 0.64684(17) 0.5429(2) 0.0462(11) Uani 1 1 d . . . H13A H -0.0538 0.6298 0.5867 0.069 Uiso 1 1 calc R . . H13B H -0.0606 0.6827 0.5471 0.069 Uiso 1 1 calc R . . H13C H 0.0418 0.6434 0.5309 0.069 Uiso 1 1 calc R . . C32 C 0.3853(3) 0.73373(14) 0.25111(19) 0.0301(8) Uani 1 1 d . . . C15 C -0.1443(3) 0.77139(14) 0.41038(19) 0.0321(9) Uani 1 1 d . . . C17 C -0.1058(4) 0.84435(15) 0.4813(2) 0.0434(11) Uani 1 1 d . . . C29 C 0.0444(4) 0.82302(15) 0.2911(2) 0.0398(10) Uani 1 1 d . . . H29A H 0.0751 0.8117 0.2471 0.060 Uiso 1 1 calc R . . H29B H -0.0027 0.8536 0.2837 0.060 Uiso 1 1 calc R . . H29C H -0.0047 0.7964 0.3103 0.060 Uiso 1 1 calc R . . C36 C 0.5670(4) 0.70092(17) 0.2090(2) 0.0453(11) Uani 1 1 d . . . H36 H 0.6346 0.6804 0.2163 0.054 Uiso 1 1 calc R . . C31 C 0.4371(4) 0.78600(17) 0.4155(2) 0.0465(11) Uani 1 1 d . . . H31A H 0.4919 0.8049 0.4455 0.070 Uiso 1 1 calc R . . H31B H 0.4756 0.7774 0.3726 0.070 Uiso 1 1 calc R . . H31C H 0.4134 0.7550 0.4387 0.070 Uiso 1 1 calc R . . C54 C -0.0284(4) 0.48780(14) 0.3670(2) 0.0399(10) Uani 1 1 d . . . H54 H -0.0422 0.4725 0.4102 0.048 Uiso 1 1 calc R . . C58 C 0.1126(4) 0.54120(15) 0.43070(19) 0.0384(10) Uani 1 1 d . . . H58A H 0.0766 0.5722 0.4477 0.058 Uiso 1 1 calc R . . H58B H 0.1965 0.5470 0.4237 0.058 Uiso 1 1 calc R . . H58C H 0.1032 0.5141 0.4644 0.058 Uiso 1 1 calc R . . C45 C 0.4950(4) 0.54041(18) 0.2316(2) 0.0466(11) Uani 1 1 d . . . H45 H 0.5492 0.5174 0.2524 0.056 Uiso 1 1 calc R . . C47 C 0.2581(4) 0.64442(16) 0.1339(2) 0.0411(10) Uani 1 1 d . . . H47A H 0.2609 0.6770 0.1578 0.062 Uiso 1 1 calc R . . H47B H 0.1773 0.6316 0.1327 0.062 Uiso 1 1 calc R . . H47C H 0.2847 0.6487 0.0868 0.062 Uiso 1 1 calc R . . C33 C 0.3750(3) 0.76209(14) 0.18958(19) 0.0318(9) Uani 1 1 d . . . C43 C 0.4407(4) 0.59419(18) 0.1394(2) 0.0487(11) Uani 1 1 d . . . H43 H 0.4566 0.6086 0.0959 0.058 Uiso 1 1 calc R . . C22 C 0.1456(3) 0.75477(15) 0.5133(2) 0.0373(9) Uani 1 1 d . . . H22A H 0.2078 0.7578 0.4798 0.056 Uiso 1 1 calc R . . H22B H 0.1355 0.7192 0.5256 0.056 Uiso 1 1 calc R . . H22C H 0.1672 0.7742 0.5546 0.056 Uiso 1 1 calc R . . C3 C 0.3943(4) 0.62766(16) 0.5252(2) 0.0459(11) Uani 1 1 d . . . C10 C -0.1181(3) 0.62308(15) 0.4871(2) 0.0349(9) Uani 1 1 d . . . C25 C 0.1394(4) 0.87946(15) 0.3764(2) 0.0446(11) Uani 1 1 d . . . H25 H 0.0739 0.9010 0.3676 0.054 Uiso 1 1 calc R . . C56 C 0.0376(4) 0.55069(17) 0.1700(2) 0.0459(11) Uani 1 1 d . . . H56A H 0.0106 0.5858 0.1678 0.069 Uiso 1 1 calc R . . H56B H -0.0066 0.5305 0.1359 0.069 Uiso 1 1 calc R . . H56C H 0.1215 0.5493 0.1603 0.069 Uiso 1 1 calc R . . C7 C -0.2628(3) 0.57576(14) 0.3914(2) 0.0371(10) Uani 1 1 d . . . H7 H -0.3133 0.5598 0.3583 0.045 Uiso 1 1 calc R . . C53 C -0.0909(4) 0.47089(15) 0.3097(2) 0.0445(11) Uani 1 1 d . . . C4 C 0.4757(5) 0.6114(2) 0.5839(3) 0.0760(17) Uani 1 1 d . . . H4A H 0.4546 0.6291 0.6260 0.114 Uiso 1 1 calc R . . H4B H 0.5570 0.6195 0.5729 0.114 Uiso 1 1 calc R . . H4C H 0.4684 0.5749 0.5909 0.114 Uiso 1 1 calc R . . C35 C 0.5548(4) 0.72736(19) 0.1475(2) 0.0484(11) Uani 1 1 d . . . C26 C 0.2235(4) 0.89450(15) 0.4238(2) 0.0459(11) Uani 1 1 d . . . C8 C -0.2722(3) 0.56304(15) 0.4597(2) 0.0402(10) Uani 1 1 d . . . C39 C 0.6448(4) 0.7225(3) 0.0921(3) 0.0783(18) Uani 1 1 d . . . H39A H 0.6233 0.7449 0.0536 0.117 Uiso 1 1 calc R . . H39B H 0.6468 0.6875 0.0758 0.117 Uiso 1 1 calc R . . H39C H 0.7224 0.7320 0.1110 0.117 Uiso 1 1 calc R . . C44 C 0.5201(4) 0.56116(19) 0.1684(2) 0.0526(12) Uani 1 1 d . . . C30 C 0.2109(6) 0.94271(17) 0.4645(3) 0.0702(16) Uani 1 1 d . . . H30A H 0.1865 0.9701 0.4335 0.105 Uiso 1 1 calc R . . H30B H 0.2864 0.9512 0.4871 0.105 Uiso 1 1 calc R . . H30C H 0.1515 0.9380 0.4995 0.105 Uiso 1 1 calc R . . C48 C 0.6330(5) 0.5490(3) 0.1334(3) 0.0826(18) Uani 1 1 d . . . H48A H 0.6900 0.5761 0.1423 0.124 Uiso 1 1 calc R . . H48B H 0.6176 0.5458 0.0838 0.124 Uiso 1 1 calc R . . H48C H 0.6647 0.5171 0.1515 0.124 Uiso 1 1 calc R . . C12 C -0.3597(4) 0.52406(19) 0.4812(3) 0.0612(14) Uani 1 1 d . . . H12A H -0.4387 0.5341 0.4651 0.092 Uiso 1 1 calc R . . H12B H -0.3577 0.5213 0.5315 0.092 Uiso 1 1 calc R . . H12C H -0.3398 0.4914 0.4611 0.092 Uiso 1 1 calc R . . C57 C -0.1857(5) 0.43176(18) 0.3154(3) 0.0686(15) Uani 1 1 d . . . H57A H -0.1590 0.4052 0.3472 0.103 Uiso 1 1 calc R . . H57B H -0.2030 0.4170 0.2700 0.103 Uiso 1 1 calc R . . H57C H -0.2568 0.4475 0.3328 0.103 Uiso 1 1 calc R . . C21 C -0.1381(5) 0.8970(2) 0.5046(3) 0.0776(18) Uani 1 1 d . . . H21A H -0.1309 0.8990 0.5549 0.116 Uiso 1 1 calc R . . H21B H -0.2192 0.9045 0.4898 0.116 Uiso 1 1 calc R . . H21C H -0.0850 0.9216 0.4843 0.116 Uiso 1 1 calc R . . C102 C 0.3844(10) 0.3557(3) 0.2485(6) 0.128(4) Uani 1 1 d . . . H102 H 0.4303 0.3282 0.2654 0.154 Uiso 1 1 calc R . . C105 C 0.2566(9) 0.4344(4) 0.2023(6) 0.119(3) Uani 1 1 d . . . H105 H 0.2099 0.4618 0.1861 0.143 Uiso 1 1 calc R . . C104 C 0.2214(8) 0.4082(4) 0.2562(7) 0.136(4) Uani 1 1 d . . . H104 H 0.1534 0.4192 0.2791 0.164 Uiso 1 1 calc R . . C101 C 0.4252(8) 0.3834(4) 0.1939(6) 0.128(4) Uani 1 1 d . . . H101 H 0.4977 0.3754 0.1735 0.154 Uiso 1 1 calc R . . C100 C 0.3568(10) 0.4232(3) 0.1700(5) 0.114(3) Uani 1 1 d . . . C103 C 0.2781(9) 0.3666(4) 0.2799(6) 0.145(4) Uani 1 1 d . . . H103 H 0.2480 0.3461 0.3154 0.174 Uiso 1 1 calc R . . C106 C 0.3927(14) 0.4496(5) 0.1132(7) 0.244(8) Uani 1 1 d . . . H70A H 0.4116 0.4258 0.0765 0.366 Uiso 1 1 calc R . . H70B H 0.4626 0.4695 0.1258 0.366 Uiso 1 1 calc R . . H70C H 0.3295 0.4721 0.0971 0.366 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 Sn2 0.02690(15) 0.02752(15) 0.02445(15) 0.00235(10) -0.00342(11) 0.00032(10) Sn1 0.02522(15) 0.02877(15) 0.02434(15) 0.00268(10) -0.00219(11) 0.00092(10) Si3 0.0257(5) 0.0275(5) 0.0242(5) 0.0012(4) -0.0006(4) -0.0013(4) Si2 0.0251(5) 0.0264(5) 0.0282(5) 0.0029(4) -0.0012(4) 0.0004(4) Si1 0.0300(6) 0.0256(5) 0.0259(5) 0.0014(4) -0.0013(4) 0.0011(4) C23 0.035(2) 0.0284(19) 0.028(2) 0.0021(16) 0.0052(17) -0.0012(17) C50 0.033(2) 0.0240(18) 0.035(2) -0.0015(17) 0.0024(17) 0.0044(16) C5 0.0247(19) 0.0295(19) 0.034(2) 0.0022(17) 0.0020(16) 0.0015(16) C51 0.038(2) 0.0273(19) 0.039(2) -0.0050(17) -0.0010(18) 0.0053(17) C52 0.037(2) 0.032(2) 0.046(3) -0.0095(19) -0.006(2) 0.0002(18) C19 0.037(2) 0.033(2) 0.0219(19) 0.0009(16) 0.0041(16) -0.0046(17) C1 0.038(2) 0.053(3) 0.027(2) 0.0066(19) -0.0020(18) 0.003(2) C2 0.038(2) 0.034(2) 0.027(2) 0.0011(17) -0.0098(18) 0.0033(18) C6 0.028(2) 0.0265(19) 0.038(2) 0.0013(17) -0.0013(17) 0.0047(16) C41 0.032(2) 0.0287(19) 0.030(2) -0.0065(16) -0.0023(16) 0.0008(16) C55 0.035(2) 0.0241(18) 0.039(2) 0.0012(17) 0.0032(18) 0.0068(17) C38 0.043(2) 0.042(2) 0.036(2) 0.0098(19) 0.0032(19) 0.006(2) C28 0.042(2) 0.038(2) 0.033(2) -0.0002(18) 0.0028(19) -0.0102(19) C42 0.044(2) 0.037(2) 0.027(2) -0.0043(18) 0.0047(18) -0.0023(19) C46 0.036(2) 0.034(2) 0.036(2) -0.0076(18) -0.0002(18) 0.0061(18) C16 0.036(2) 0.043(2) 0.045(3) -0.002(2) 0.005(2) 0.0085(19) C11 0.029(2) 0.032(2) 0.041(2) -0.0019(18) -0.0041(18) -0.0025(17) C24 0.042(2) 0.032(2) 0.033(2) 0.0084(17) 0.0099(19) -0.0003(18) C14 0.033(2) 0.0307(19) 0.0248(19) 0.0057(16) 0.0064(16) -0.0025(17) C49 0.042(2) 0.047(2) 0.039(2) 0.008(2) -0.006(2) 0.015(2) C40 0.031(2) 0.035(2) 0.048(3) 0.0013(19) -0.0077(19) 0.0062(18) C9 0.041(2) 0.042(2) 0.037(2) 0.0117(19) 0.0049(19) -0.004(2) C20 0.032(2) 0.042(2) 0.058(3) -0.003(2) -0.009(2) 0.010(2) C37 0.029(2) 0.038(2) 0.036(2) -0.0004(18) -0.0050(18) -0.0014(17) C34 0.035(2) 0.057(3) 0.036(2) 0.010(2) 0.0032(19) 0.001(2) C18 0.053(3) 0.037(2) 0.030(2) -0.0065(18) 0.002(2) -0.003(2) C27 0.060(3) 0.040(2) 0.035(2) -0.004(2) 0.003(2) -0.020(2) C13 0.055(3) 0.051(3) 0.032(2) 0.010(2) 0.000(2) -0.015(2) C32 0.026(2) 0.034(2) 0.031(2) 0.0012(17) -0.0011(16) -0.0035(16) C15 0.029(2) 0.037(2) 0.030(2) 0.0000(17) 0.0023(17) 0.0002(17) C17 0.051(3) 0.039(2) 0.041(3) -0.007(2) 0.008(2) 0.003(2) C29 0.037(2) 0.035(2) 0.048(3) 0.006(2) 0.005(2) 0.0079(19) C36 0.030(2) 0.057(3) 0.049(3) -0.005(2) -0.003(2) 0.014(2) C31 0.047(3) 0.048(3) 0.044(3) -0.010(2) -0.013(2) -0.010(2) C54 0.049(3) 0.029(2) 0.042(2) 0.0020(19) 0.013(2) -0.0018(19) C58 0.050(3) 0.032(2) 0.034(2) 0.0126(18) 0.0061(19) 0.0000(19) C45 0.042(3) 0.057(3) 0.041(3) -0.006(2) -0.002(2) 0.016(2) C47 0.051(3) 0.045(2) 0.027(2) 0.0032(19) 0.0025(19) 0.004(2) C33 0.028(2) 0.034(2) 0.034(2) -0.0003(17) 0.0001(17) -0.0041(17) C43 0.048(3) 0.064(3) 0.034(2) -0.003(2) 0.009(2) 0.001(2) C22 0.040(2) 0.041(2) 0.031(2) -0.0023(18) -0.0043(18) -0.0059(19) C3 0.050(3) 0.039(2) 0.048(3) -0.006(2) -0.003(2) 0.005(2) C10 0.032(2) 0.038(2) 0.035(2) 0.0053(18) 0.0007(18) -0.0006(18) C25 0.061(3) 0.030(2) 0.044(3) 0.0064(19) 0.017(2) 0.007(2) C56 0.055(3) 0.047(3) 0.035(2) -0.004(2) -0.011(2) -0.007(2) C7 0.029(2) 0.031(2) 0.050(3) 0.0016(19) -0.0065(19) -0.0031(17) C53 0.039(2) 0.029(2) 0.066(3) -0.009(2) 0.007(2) -0.0043(18) C4 0.092(4) 0.071(4) 0.063(3) -0.011(3) -0.035(3) 0.026(3) C35 0.037(2) 0.072(3) 0.036(2) -0.002(2) 0.007(2) 0.010(2) C26 0.071(3) 0.030(2) 0.037(2) -0.0033(19) 0.016(2) -0.002(2) C8 0.030(2) 0.040(2) 0.050(3) 0.011(2) 0.000(2) -0.0047(18) C39 0.047(3) 0.135(5) 0.053(3) 0.005(3) 0.012(3) 0.022(3) C44 0.044(3) 0.070(3) 0.045(3) -0.009(2) 0.007(2) 0.014(2) C30 0.114(5) 0.041(3) 0.057(3) -0.010(2) 0.017(3) -0.005(3) C48 0.058(3) 0.121(5) 0.070(4) -0.010(4) 0.024(3) 0.026(3) C12 0.047(3) 0.067(3) 0.069(3) 0.024(3) -0.003(3) -0.025(3) C57 0.067(4) 0.052(3) 0.088(4) -0.012(3) 0.011(3) -0.025(3) C21 0.084(4) 0.063(3) 0.085(4) -0.036(3) -0.009(3) 0.022(3) C102 0.149(9) 0.096(6) 0.135(8) -0.034(6) -0.083(7) 0.051(6) C105 0.092(7) 0.088(6) 0.176(10) -0.066(6) -0.020(6) 0.031(5) C104 0.075(6) 0.131(9) 0.202(12) -0.081(8) -0.008(7) -0.013(6) C101 0.114(7) 0.128(8) 0.139(8) -0.077(7) -0.038(7) 0.054(6) C100 0.167(10) 0.085(5) 0.090(6) -0.034(5) -0.012(6) -0.034(6) C103 0.116(7) 0.119(7) 0.197(10) -0.083(7) -0.073(7) 0.035(6) C106 0.38(2) 0.190(12) 0.160(11) -0.039(10) -0.024(13) -0.132(14) _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 Sn2 C2 2.104(4) . ? Sn2 Si1 2.6051(11) . ? Sn2 Si3 2.6095(11) . ? Sn2 Si2 2.6201(11) . ? Sn2 Sn1 3.1575(9) . ? Sn1 C1 2.152(4) . ? Sn1 Si2 2.6052(11) . ? Sn1 Si3 2.6175(12) . ? Sn1 Si1 2.6247(11) . ? Si3 C5 1.890(4) . ? Si3 C14 1.893(4) . ? Si2 C23 1.907(4) . ? Si2 C32 1.908(4) . ? Si1 C50 1.895(4) . ? Si1 C41 1.897(4) . ? C23 C24 1.402(5) . ? C23 C28 1.422(5) . ? C50 C51 1.409(5) . ? C50 C55 1.418(5) . ? C5 C10 1.409(5) . ? C5 C6 1.417(5) . ? C51 C52 1.392(5) . ? C51 C56 1.507(6) . ? C52 C53 1.393(6) . ? C52 H52 0.9500 . ? C19 C18 1.385(5) . ? C19 C14 1.415(5) . ? C19 C22 1.507(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.133(5) . ? C6 C7 1.386(5) . ? C6 C11 1.507(5) . ? C41 C42 1.410(5) . ? C41 C46 1.420(5) . ? C55 C54 1.387(5) . ? C55 C58 1.500(5) . ? C38 C33 1.509(5) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C28 C27 1.393(6) . ? C28 C31 1.494(6) . ? C42 C43 1.394(6) . ? C42 C47 1.506(5) . ? C46 C45 1.383(6) . ? C46 C49 1.507(6) . ? C16 C17 1.369(6) . ? C16 C15 1.384(5) . ? C16 H16 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C24 C25 1.388(5) . ? C24 C29 1.502(6) . ? C14 C15 1.416(5) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C40 C37 1.513(5) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C9 C8 1.376(6) . ? C9 C10 1.385(5) . ? C9 H9 0.9500 . ? C20 C15 1.499(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C37 C36 1.390(6) . ? C37 C32 1.398(5) . ? C34 C35 1.372(6) . ? C34 C33 1.383(5) . ? C34 H34 0.9500 . ? C18 C17 1.372(6) . ? C18 H18 0.9500 . ? C27 C26 1.382(6) . ? C27 H27 0.9500 . ? C13 C10 1.513(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C32 C33 1.415(5) . ? C17 C21 1.516(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C36 C35 1.389(6) . ? C36 H36 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C54 C53 1.380(6) . ? C54 H54 0.9500 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C45 C44 1.384(6) . ? C45 H45 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C43 C44 1.368(6) . ? C43 H43 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C3 C4 1.512(6) . ? C25 C26 1.369(6) . ? C25 H25 0.9500 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C7 C8 1.377(6) . ? C7 H7 0.9500 . ? C53 C57 1.503(6) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C35 C39 1.515(6) . ? C26 C30 1.512(6) . ? C8 C12 1.503(5) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C44 C48 1.506(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C102 C101 1.382(13) . ? C102 C103 1.402(13) . ? C102 H102 0.9500 . ? C105 C104 1.328(13) . ? C105 C100 1.352(12) . ? C105 H105 0.9500 . ? C104 C103 1.352(13) . ? C104 H104 0.9500 . ? C101 C100 1.383(12) . ? C101 H101 0.9500 . ? C100 C106 1.378(13) . ? C103 H103 0.9500 . ? C106 H70A 0.9800 . ? C106 H70B 0.9800 . ? C106 H70C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Sn2 Si1 124.95(11) . . ? C2 Sn2 Si3 128.83(12) . . ? Si1 Sn2 Si3 87.40(4) . . ? C2 Sn2 Si2 127.49(11) . . ? Si1 Sn2 Si2 87.83(3) . . ? Si3 Sn2 Si2 86.90(4) . . ? C2 Sn2 Sn1 177.86(11) . . ? Si1 Sn2 Sn1 53.15(3) . . ? Si3 Sn2 Sn1 52.95(3) . . ? Si2 Sn2 Sn1 52.61(2) . . ? C1 Sn1 Si2 126.96(12) . . ? C1 Sn1 Si3 124.84(11) . . ? Si2 Sn1 Si3 87.05(4) . . ? C1 Sn1 Si1 129.75(12) . . ? Si2 Sn1 Si1 87.73(3) . . ? Si3 Sn1 Si1 86.83(3) . . ? C1 Sn1 Sn2 177.24(11) . . ? Si2 Sn1 Sn2 53.04(3) . . ? Si3 Sn1 Sn2 52.72(3) . . ? Si1 Sn1 Sn2 52.58(2) . . ? C5 Si3 C14 109.93(16) . . ? C5 Si3 Sn2 117.84(12) . . ? C14 Si3 Sn2 117.45(12) . . ? C5 Si3 Sn1 118.47(12) . . ? C14 Si3 Sn1 115.12(11) . . ? Sn2 Si3 Sn1 74.32(4) . . ? C23 Si2 C32 112.26(16) . . ? C23 Si2 Sn1 118.45(13) . . ? C32 Si2 Sn1 113.60(12) . . ? C23 Si2 Sn2 114.71(12) . . ? C32 Si2 Sn2 118.76(12) . . ? Sn1 Si2 Sn2 74.35(3) . . ? C50 Si1 C41 111.01(16) . . ? C50 Si1 Sn2 117.75(12) . . ? C41 Si1 Sn2 115.60(12) . . ? C50 Si1 Sn1 113.81(12) . . ? C41 Si1 Sn1 120.24(12) . . ? Sn2 Si1 Sn1 74.28(3) . . ? C24 C23 C28 118.0(3) . . ? C24 C23 Si2 125.1(3) . . ? C28 C23 Si2 116.8(3) . . ? C51 C50 C55 117.1(3) . . ? C51 C50 Si1 118.4(3) . . ? C55 C50 Si1 124.4(3) . . ? C10 C5 C6 117.0(3) . . ? C10 C5 Si3 119.0(3) . . ? C6 C5 Si3 123.9(3) . . ? C52 C51 C50 121.2(4) . . ? C52 C51 C56 116.8(4) . . ? C50 C51 C56 122.0(4) . . ? C51 C52 C53 120.9(4) . . ? C51 C52 H52 119.5 . . ? C53 C52 H52 119.5 . . ? C18 C19 C14 119.8(4) . . ? C18 C19 C22 116.7(3) . . ? C14 C19 C22 123.6(3) . . ? Sn1 C1 H1A 109.5 . . ? Sn1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sn1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 Sn2 177.2(4) . . ? C7 C6 C5 119.9(4) . . ? C7 C6 C11 116.5(3) . . ? C5 C6 C11 123.5(3) . . ? C42 C41 C46 116.7(4) . . ? C42 C41 Si1 125.3(3) . . ? C46 C41 Si1 118.0(3) . . ? C54 C55 C50 120.2(4) . . ? C54 C55 C58 116.0(4) . . ? C50 C55 C58 123.8(3) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C27 C28 C23 119.4(4) . . ? C27 C28 C31 118.3(4) . . ? C23 C28 C31 122.3(3) . . ? C43 C42 C41 120.5(4) . . ? C43 C42 C47 116.6(4) . . ? C41 C42 C47 122.9(4) . . ? C45 C46 C41 120.7(4) . . ? C45 C46 C49 117.6(4) . . ? C41 C46 C49 121.7(4) . . ? C17 C16 C15 122.0(4) . . ? C17 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C25 C24 C23 119.6(4) . . ? C25 C24 C29 116.6(4) . . ? C23 C24 C29 123.8(3) . . ? C19 C14 C15 117.1(3) . . ? C19 C14 Si3 124.8(3) . . ? C15 C14 Si3 118.1(3) . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C8 C9 C10 122.1(4) . . ? C8 C9 H9 118.9 . . ? C10 C9 H9 118.9 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C36 C37 C32 119.6(4) . . ? C36 C37 C40 117.3(4) . . ? C32 C37 C40 123.1(4) . . ? C35 C34 C33 122.0(4) . . ? C35 C34 H34 119.0 . . ? C33 C34 H34 119.0 . . ? C17 C18 C19 122.6(4) . . ? C17 C18 H18 118.7 . . ? C19 C18 H18 118.7 . . ? C26 C27 C28 122.4(4) . . ? C26 C27 H27 118.8 . . ? C28 C27 H27 118.8 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C37 C32 C33 117.5(4) . . ? C37 C32 Si2 125.0(3) . . ? C33 C32 Si2 117.3(3) . . ? C16 C15 C14 120.4(4) . . ? C16 C15 C20 117.8(3) . . ? C14 C15 C20 121.8(3) . . ? C16 C17 C18 118.0(4) . . ? C16 C17 C21 121.2(4) . . ? C18 C17 C21 120.7(4) . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C35 C36 C37 122.9(4) . . ? C35 C36 H36 118.5 . . ? C37 C36 H36 118.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C53 C54 C55 122.3(4) . . ? C53 C54 H54 118.9 . . ? C55 C54 H54 118.9 . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C46 C45 C44 121.9(4) . . ? C46 C45 H45 119.1 . . ? C44 C45 H45 119.1 . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C34 C33 C32 120.8(4) . . ? C34 C33 C38 117.8(3) . . ? C32 C33 C38 121.4(3) . . ? C44 C43 C42 122.3(4) . . ? C44 C43 H43 118.9 . . ? C42 C43 H43 118.9 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C2 C3 C4 179.6(6) . . ? C9 C10 C5 120.7(4) . . ? C9 C10 C13 117.8(4) . . ? C5 C10 C13 121.5(3) . . ? C26 C25 C24 123.2(4) . . ? C26 C25 H25 118.4 . . ? C24 C25 H25 118.4 . . ? C51 C56 H56A 109.5 . . ? C51 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C51 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C8 C7 C6 122.6(4) . . ? C8 C7 H7 118.7 . . ? C6 C7 H7 118.7 . . ? C54 C53 C52 118.1(4) . . ? C54 C53 C57 121.2(4) . . ? C52 C53 C57 120.7(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C34 C35 C36 117.1(4) . . ? C34 C35 C39 121.7(4) . . ? C36 C35 C39 121.1(4) . . ? C25 C26 C27 117.2(4) . . ? C25 C26 C30 121.6(5) . . ? C27 C26 C30 121.2(5) . . ? C9 C8 C7 117.6(4) . . ? C9 C8 C12 121.9(4) . . ? C7 C8 C12 120.6(4) . . ? C35 C39 H39A 109.5 . . ? C35 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C35 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C43 C44 C45 117.9(4) . . ? C43 C44 C48 120.9(5) . . ? C45 C44 C48 121.1(5) . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C53 C57 H57A 109.5 . . ? C53 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C53 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C17 C21 H21A 109.5 . . ? C17 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C17 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C101 C102 C103 122.8(9) . . ? C101 C102 H102 118.6 . . ? C103 C102 H102 118.6 . . ? C104 C105 C100 122.1(10) . . ? C104 C105 H105 119.0 . . ? C100 C105 H105 119.0 . . ? C105 C104 C103 122.9(11) . . ? C105 C104 H104 118.6 . . ? C103 C104 H104 118.6 . . ? C102 C101 C100 117.6(10) . . ? C102 C101 H101 121.2 . . ? C100 C101 H101 121.2 . . ? C105 C100 C106 122.4(13) . . ? C105 C100 C101 119.0(10) . . ? C106 C100 C101 118.6(13) . . ? C104 C103 C102 115.3(12) . . ? C104 C103 H103 122.3 . . ? C102 C103 H103 122.3 . . ? C100 C106 H70A 109.5 . . ? C100 C106 H70B 109.5 . . ? H70A C106 H70B 109.5 . . ? C100 C106 H70C 109.5 . . ? H70A C106 H70C 109.5 . . ? H70B C106 H70C 109.5 . . ? 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 Si1 Sn2 Sn1 Si2 -120.88(4) . . . . ? Si3 Sn2 Sn1 Si2 119.45(4) . . . . ? Si1 Sn2 Sn1 Si3 119.66(4) . . . . ? Si2 Sn2 Sn1 Si3 -119.45(4) . . . . ? Si3 Sn2 Sn1 Si1 -119.66(4) . . . . ? Si2 Sn2 Sn1 Si1 120.88(4) . . . . ? C2 Sn2 Si3 C5 -64.20(19) . . . . ? Si1 Sn2 Si3 C5 70.20(14) . . . . ? Si2 Sn2 Si3 C5 158.17(14) . . . . ? Sn1 Sn2 Si3 C5 114.31(14) . . . . ? C2 Sn2 Si3 C14 70.93(18) . . . . ? Si1 Sn2 Si3 C14 -154.67(13) . . . . ? Si2 Sn2 Si3 C14 -66.70(13) . . . . ? Sn1 Sn2 Si3 C14 -110.56(13) . . . . ? C2 Sn2 Si3 Sn1 -178.51(13) . . . . ? Si1 Sn2 Si3 Sn1 -44.11(3) . . . . ? Si2 Sn2 Si3 Sn1 43.85(3) . . . . ? C1 Sn1 Si3 C5 68.1(2) . . . . ? Si2 Sn1 Si3 C5 -157.72(13) . . . . ? Si1 Sn1 Si3 C5 -69.83(13) . . . . ? Sn2 Sn1 Si3 C5 -113.55(13) . . . . ? C1 Sn1 Si3 C14 -65.0(2) . . . . ? Si2 Sn1 Si3 C14 69.24(13) . . . . ? Si1 Sn1 Si3 C14 157.13(13) . . . . ? Sn2 Sn1 Si3 C14 113.41(13) . . . . ? C1 Sn1 Si3 Sn2 -178.40(15) . . . . ? Si2 Sn1 Si3 Sn2 -44.16(3) . . . . ? Si1 Sn1 Si3 Sn2 43.72(3) . . . . ? C1 Sn1 Si2 C23 66.5(2) . . . . ? Si3 Sn1 Si2 C23 -66.07(13) . . . . ? Si1 Sn1 Si2 C23 -153.01(13) . . . . ? Sn2 Sn1 Si2 C23 -110.00(13) . . . . ? C1 Sn1 Si2 C32 -68.44(19) . . . . ? Si3 Sn1 Si2 C32 158.95(13) . . . . ? Si1 Sn1 Si2 C32 72.01(13) . . . . ? Sn2 Sn1 Si2 C32 115.02(13) . . . . ? C1 Sn1 Si2 Sn2 176.54(14) . . . . ? Si3 Sn1 Si2 Sn2 43.93(3) . . . . ? Si1 Sn1 Si2 Sn2 -43.01(3) . . . . ? C2 Sn2 Si2 C23 -68.12(19) . . . . ? Si1 Sn2 Si2 C23 157.97(14) . . . . ? Si3 Sn2 Si2 C23 70.46(14) . . . . ? Sn1 Sn2 Si2 C23 114.56(14) . . . . ? C2 Sn2 Si2 C32 68.61(19) . . . . ? Si1 Sn2 Si2 C32 -65.29(13) . . . . ? Si3 Sn2 Si2 C32 -152.81(13) . . . . ? Sn1 Sn2 Si2 C32 -108.70(13) . . . . ? C2 Sn2 Si2 Sn1 177.31(14) . . . . ? Si1 Sn2 Si2 Sn1 43.41(3) . . . . ? Si3 Sn2 Si2 Sn1 -44.11(3) . . . . ? C2 Sn2 Si1 C50 72.19(19) . . . . ? Si3 Sn2 Si1 C50 -65.04(13) . . . . ? Si2 Sn2 Si1 C50 -152.04(13) . . . . ? Sn1 Sn2 Si1 C50 -109.01(13) . . . . ? C2 Sn2 Si1 C41 -62.36(19) . . . . ? Si3 Sn2 Si1 C41 160.41(13) . . . . ? Si2 Sn2 Si1 C41 73.42(13) . . . . ? Sn1 Sn2 Si1 C41 116.44(13) . . . . ? C2 Sn2 Si1 Sn1 -178.80(14) . . . . ? Si3 Sn2 Si1 Sn1 43.97(3) . . . . ? Si2 Sn2 Si1 Sn1 -43.03(3) . . . . ? C1 Sn1 Si1 C50 -64.2(2) . . . . ? Si2 Sn1 Si1 C50 157.20(13) . . . . ? Si3 Sn1 Si1 C50 70.04(14) . . . . ? Sn2 Sn1 Si1 C50 113.86(14) . . . . ? C1 Sn1 Si1 C41 71.1(2) . . . . ? Si2 Sn1 Si1 C41 -67.49(13) . . . . ? Si3 Sn1 Si1 C41 -154.65(13) . . . . ? Sn2 Sn1 Si1 C41 -110.83(14) . . . . ? C1 Sn1 Si1 Sn2 -178.11(14) . . . . ? Si2 Sn1 Si1 Sn2 43.34(3) . . . . ? Si3 Sn1 Si1 Sn2 -43.83(3) . . . . ? C32 Si2 C23 C24 113.9(3) . . . . ? Sn1 Si2 C23 C24 -21.6(4) . . . . ? Sn2 Si2 C23 C24 -106.6(3) . . . . ? C32 Si2 C23 C28 -68.0(3) . . . . ? Sn1 Si2 C23 C28 156.5(2) . . . . ? Sn2 Si2 C23 C28 71.6(3) . . . . ? C41 Si1 C50 C51 -66.7(3) . . . . ? Sn2 Si1 C50 C51 156.8(2) . . . . ? Sn1 Si1 C50 C51 72.7(3) . . . . ? C41 Si1 C50 C55 116.4(3) . . . . ? Sn2 Si1 C50 C55 -20.0(4) . . . . ? Sn1 Si1 C50 C55 -104.2(3) . . . . ? C14 Si3 C5 C10 -62.7(3) . . . . ? Sn2 Si3 C5 C10 75.5(3) . . . . ? Sn1 Si3 C5 C10 162.0(3) . . . . ? C14 Si3 C5 C6 115.3(3) . . . . ? Sn2 Si3 C5 C6 -106.4(3) . . . . ? Sn1 Si3 C5 C6 -19.9(3) . . . . ? C55 C50 C51 C52 2.8(5) . . . . ? Si1 C50 C51 C52 -174.2(3) . . . . ? C55 C50 C51 C56 -179.5(4) . . . . ? Si1 C50 C51 C56 3.5(5) . . . . ? C50 C51 C52 C53 -1.1(6) . . . . ? C56 C51 C52 C53 -178.9(4) . . . . ? C10 C5 C6 C7 -0.2(5) . . . . ? Si3 C5 C6 C7 -178.2(3) . . . . ? C10 C5 C6 C11 180.0(3) . . . . ? Si3 C5 C6 C11 1.9(5) . . . . ? C50 Si1 C41 C42 115.9(3) . . . . ? Sn2 Si1 C41 C42 -106.6(3) . . . . ? Sn1 Si1 C41 C42 -20.5(4) . . . . ? C50 Si1 C41 C46 -66.6(3) . . . . ? Sn2 Si1 C41 C46 70.9(3) . . . . ? Sn1 Si1 C41 C46 156.9(2) . . . . ? C51 C50 C55 C54 -1.6(5) . . . . ? Si1 C50 C55 C54 175.3(3) . . . . ? C51 C50 C55 C58 178.2(3) . . . . ? Si1 C50 C55 C58 -4.9(5) . . . . ? C24 C23 C28 C27 2.7(6) . . . . ? Si2 C23 C28 C27 -175.6(3) . . . . ? C24 C23 C28 C31 -179.4(4) . . . . ? Si2 C23 C28 C31 2.3(5) . . . . ? C46 C41 C42 C43 -1.9(6) . . . . ? Si1 C41 C42 C43 175.6(3) . . . . ? C46 C41 C42 C47 179.3(3) . . . . ? Si1 C41 C42 C47 -3.2(5) . . . . ? C42 C41 C46 C45 2.1(5) . . . . ? Si1 C41 C46 C45 -175.5(3) . . . . ? C42 C41 C46 C49 -179.0(4) . . . . ? Si1 C41 C46 C49 3.4(5) . . . . ? C28 C23 C24 C25 -2.4(5) . . . . ? Si2 C23 C24 C25 175.7(3) . . . . ? C28 C23 C24 C29 178.9(4) . . . . ? Si2 C23 C24 C29 -3.0(5) . . . . ? C18 C19 C14 C15 -2.1(5) . . . . ? C22 C19 C14 C15 177.7(3) . . . . ? C18 C19 C14 Si3 176.2(3) . . . . ? C22 C19 C14 Si3 -4.0(5) . . . . ? C5 Si3 C14 C19 116.9(3) . . . . ? Sn2 Si3 C14 C19 -21.6(3) . . . . ? Sn1 Si3 C14 C19 -106.2(3) . . . . ? C5 Si3 C14 C15 -64.9(3) . . . . ? Sn2 Si3 C14 C15 156.7(2) . . . . ? Sn1 Si3 C14 C15 72.0(3) . . . . ? C14 C19 C18 C17 0.7(6) . . . . ? C22 C19 C18 C17 -179.1(4) . . . . ? C23 C28 C27 C26 -0.7(6) . . . . ? C31 C28 C27 C26 -178.7(4) . . . . ? C36 C37 C32 C33 -1.2(5) . . . . ? C40 C37 C32 C33 179.5(3) . . . . ? C36 C37 C32 Si2 174.1(3) . . . . ? C40 C37 C32 Si2 -5.1(5) . . . . ? C23 Si2 C32 C37 117.1(3) . . . . ? Sn1 Si2 C32 C37 -105.1(3) . . . . ? Sn2 Si2 C32 C37 -20.6(4) . . . . ? C23 Si2 C32 C33 -67.5(3) . . . . ? Sn1 Si2 C32 C33 70.3(3) . . . . ? Sn2 Si2 C32 C33 154.8(2) . . . . ? C17 C16 C15 C14 -1.6(6) . . . . ? C17 C16 C15 C20 -179.5(4) . . . . ? C19 C14 C15 C16 2.6(5) . . . . ? Si3 C14 C15 C16 -175.8(3) . . . . ? C19 C14 C15 C20 -179.6(3) . . . . ? Si3 C14 C15 C20 2.0(5) . . . . ? C15 C16 C17 C18 0.1(6) . . . . ? C15 C16 C17 C21 177.4(4) . . . . ? C19 C18 C17 C16 0.4(6) . . . . ? C19 C18 C17 C21 -176.9(4) . . . . ? C32 C37 C36 C35 -1.1(6) . . . . ? C40 C37 C36 C35 178.3(4) . . . . ? C50 C55 C54 C53 -1.4(6) . . . . ? C58 C55 C54 C53 178.8(4) . . . . ? C41 C46 C45 C44 -1.2(6) . . . . ? C49 C46 C45 C44 179.8(4) . . . . ? C35 C34 C33 C32 -2.1(6) . . . . ? C35 C34 C33 C38 178.8(4) . . . . ? C37 C32 C33 C34 2.8(5) . . . . ? Si2 C32 C33 C34 -172.9(3) . . . . ? C37 C32 C33 C38 -178.2(3) . . . . ? Si2 C32 C33 C38 6.1(5) . . . . ? C41 C42 C43 C44 0.7(7) . . . . ? C47 C42 C43 C44 179.6(4) . . . . ? C8 C9 C10 C5 0.0(6) . . . . ? C8 C9 C10 C13 -178.8(4) . . . . ? C6 C5 C10 C9 0.5(6) . . . . ? Si3 C5 C10 C9 178.7(3) . . . . ? C6 C5 C10 C13 179.3(4) . . . . ? Si3 C5 C10 C13 -2.6(5) . . . . ? C23 C24 C25 C26 0.1(6) . . . . ? C29 C24 C25 C26 178.9(4) . . . . ? C5 C6 C7 C8 -0.7(6) . . . . ? C11 C6 C7 C8 179.2(4) . . . . ? C55 C54 C53 C52 3.2(6) . . . . ? C55 C54 C53 C57 -175.5(4) . . . . ? C51 C52 C53 C54 -2.0(6) . . . . ? C51 C52 C53 C57 176.8(4) . . . . ? C33 C34 C35 C36 -0.2(7) . . . . ? C33 C34 C35 C39 179.6(5) . . . . ? C37 C36 C35 C34 1.8(7) . . . . ? C37 C36 C35 C39 -178.0(5) . . . . ? C24 C25 C26 C27 1.9(6) . . . . ? C24 C25 C26 C30 -176.8(4) . . . . ? C28 C27 C26 C25 -1.5(6) . . . . ? C28 C27 C26 C30 177.2(4) . . . . ? C10 C9 C8 C7 -0.8(6) . . . . ? C10 C9 C8 C12 179.5(4) . . . . ? C6 C7 C8 C9 1.2(6) . . . . ? C6 C7 C8 C12 -179.2(4) . . . . ? C42 C43 C44 C45 0.3(7) . . . . ? C42 C43 C44 C48 -178.0(5) . . . . ? C46 C45 C44 C43 0.0(7) . . . . ? C46 C45 C44 C48 178.2(5) . . . . ? C100 C105 C104 C103 -4.6(15) . . . . ? C103 C102 C101 C100 -0.2(13) . . . . ? C104 C105 C100 C106 178.8(9) . . . . ? C104 C105 C100 C101 -0.4(13) . . . . ? C102 C101 C100 C105 2.6(11) . . . . ? C102 C101 C100 C106 -176.6(8) . . . . ? C105 C104 C103 C102 6.6(13) . . . . ? C101 C102 C103 C104 -4.2(12) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.875 _refine_diff_density_min -0.834 _refine_diff_density_rms 0.093 data_compound_5 _database_code_depnum_ccdc_archive 'CCDC 879399' #TrackingRef 'AlkynylSn2Si3_ChemComm.cif' _chemical_name_systematic ; 1,2-bis(2,2,4,4,5,5-hexakis(2,4,6-trimethylphenyl)- 3-methyl-2,4,5-trisila-1,3- distannabicylo[1.1.1]pentan)ethyne ; _audit_creation_method SHELXL-97 _chemical_name_common ; 1,2-bis(2,2,4,4,5,5-hexakis(2,4,6-trimethylphenyl)-3-methyl- 2,4,5-trisila-1,3-distannabicylo(1.1.1)pentan)ethyne ; _chemical_melting_point ? _chemical_formula_moiety 'C112 H138 Si6 Sn4, 0.5(C6 H6), 3(C7 H8), 2(C2 H3 N)' _chemical_formula_sum 'C140 H171 N2 Si6 Sn4' _chemical_formula_weight 2525.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.943(3) _cell_length_b 15.950(3) _cell_length_c 17.865(4) _cell_angle_alpha 113.74(3) _cell_angle_beta 108.71(3) _cell_angle_gamma 96.95(3) _cell_volume 3298.4(19) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 22218 _cell_measurement_theta_min 3.65 _cell_measurement_theta_max 25.00 _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1309 _exptl_absorpt_coefficient_mu 0.851 _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 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Stadi with CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22218 _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_sigmaI/netI 0.0691 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11460 _reflns_number_gt 8153 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis Red' _computing_data_reduction 'CrysAlis Red' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Ortep 32' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1121P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11460 _refine_ls_number_parameters 755 _refine_ls_number_restraints 123 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1812 _refine_ls_wR_factor_gt 0.1559 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.050 _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 Sn1 Sn 0.53243(3) 0.61213(3) 0.67269(2) 0.02862(14) Uani 1 1 d . . . Sn2 Sn 0.57312(3) 0.74838(3) 0.87483(2) 0.02941(14) Uani 1 1 d . . . Si1 Si 0.67116(12) 0.62289(11) 0.81857(10) 0.0301(3) Uani 1 1 d . . . Si2 Si 0.39760(12) 0.61759(10) 0.74689(10) 0.0299(3) Uani 1 1 d . . . Si3 Si 0.58504(12) 0.79829(10) 0.75397(9) 0.0288(3) Uani 1 1 d . . . C1 C 0.5076(4) 0.5247(3) 0.5369(3) 0.0162(9) Uani 1 1 d . . . C2 C 0.6007(5) 0.8420(4) 1.0123(3) 0.0411(14) Uani 1 1 d . . . H2A H 0.5529 0.8113 1.0299 0.062 Uiso 1 1 calc R . . H2B H 0.5875 0.9026 1.0175 0.062 Uiso 1 1 calc R . . H2C H 0.6741 0.8542 1.0517 0.062 Uiso 1 1 calc R . . C100 C 0.8172(4) 0.6742(4) 0.8507(4) 0.0340(13) Uani 1 1 d . . . C101 C 0.8868(5) 0.7102(4) 0.9421(4) 0.0376(13) Uani 1 1 d . . . C102 C 0.9943(5) 0.7540(4) 0.9721(4) 0.0438(15) Uani 1 1 d . . . H102 H 1.0391 0.7788 1.0335 0.053 Uiso 1 1 calc R . . C103 C 1.0377(5) 0.7623(5) 0.9143(5) 0.0485(16) Uani 1 1 d . . . C104 C 0.9696(5) 0.7256(4) 0.8252(4) 0.0450(15) Uani 1 1 d . . . H104 H 0.9976 0.7309 0.7848 0.054 Uiso 1 1 calc R . . C105 C 0.8613(5) 0.6811(4) 0.7922(4) 0.0372(13) Uani 1 1 d . . . C106 C 0.8503(5) 0.7062(5) 1.0110(4) 0.0469(16) Uani 1 1 d . . . H10A H 0.9112 0.7329 1.0686 0.070 Uiso 1 1 calc R . . H10B H 0.8161 0.6395 0.9925 0.070 Uiso 1 1 calc R . . H10C H 0.7998 0.7434 1.0170 0.070 Uiso 1 1 calc R . . C107 C 1.1530(6) 0.8064(6) 0.9490(6) 0.069(2) Uani 1 1 d . . . H10D H 1.1913 0.7637 0.9637 0.104 Uiso 1 1 calc R . . H10E H 1.1748 0.8678 1.0030 0.104 Uiso 1 1 calc R . . H10F H 1.1691 0.8168 0.9034 0.104 Uiso 1 1 calc R . . C108 C 0.7973(5) 0.6422(4) 0.6919(4) 0.0423(14) Uani 1 1 d . . . H10G H 0.7564 0.6855 0.6822 0.063 Uiso 1 1 calc R . . H10H H 0.7490 0.5787 0.6675 0.063 Uiso 1 1 calc R . . H10I H 0.8455 0.6375 0.6617 0.063 Uiso 1 1 calc R . . C200 C 0.6471(4) 0.5132(4) 0.8354(4) 0.0327(12) Uani 1 1 d . . . C201 C 0.6090(5) 0.5088(4) 0.8990(4) 0.0369(13) Uani 1 1 d . . . C202 C 0.5917(5) 0.4243(5) 0.9041(5) 0.0500(17) Uani 1 1 d . . . H202 H 0.5672 0.4228 0.9475 0.060 Uiso 1 1 calc R . . C203 C 0.6079(7) 0.3432(5) 0.8501(5) 0.065(2) Uani 1 1 d . . . C204 C 0.6468(6) 0.3473(5) 0.7882(4) 0.0555(19) Uani 1 1 d . . . H204 H 0.6609 0.2923 0.7511 0.067 Uiso 1 1 calc R . . C205 C 0.6654(5) 0.4303(4) 0.7799(4) 0.0404(14) Uani 1 1 d . . . C206 C 0.5864(5) 0.5913(4) 0.9633(4) 0.0409(14) Uani 1 1 d . . . H20A H 0.5180 0.5976 0.9320 0.061 Uiso 1 1 calc R . . H20B H 0.6421 0.6504 0.9871 0.061 Uiso 1 1 calc R . . H20C H 0.5845 0.5796 1.0127 0.061 Uiso 1 1 calc R . . C207 C 0.5832(10) 0.2527(5) 0.8559(6) 0.093(3) Uani 1 1 d . . . H20D H 0.5799 0.2675 0.9137 0.139 Uiso 1 1 calc R . . H20E H 0.6387 0.2213 0.8504 0.139 Uiso 1 1 calc R . . H20F H 0.5150 0.2099 0.8074 0.139 Uiso 1 1 calc R . . C208 C 0.7077(6) 0.4285(4) 0.7114(4) 0.0485(16) Uani 1 1 d . . . H20G H 0.7166 0.3653 0.6807 0.073 Uiso 1 1 calc R . . H20H H 0.7761 0.4774 0.7414 0.073 Uiso 1 1 calc R . . H20I H 0.6577 0.4417 0.6675 0.073 Uiso 1 1 calc R . . C300 C 0.3493(5) 0.5071(4) 0.7569(4) 0.0340(13) Uani 1 1 d . . . C301 C 0.3068(5) 0.5191(4) 0.8215(4) 0.0382(14) Uani 1 1 d . . . C302 C 0.2693(5) 0.4416(4) 0.8317(4) 0.0455(15) Uani 1 1 d . . . H302 H 0.2408 0.4515 0.8752 0.055 Uiso 1 1 calc R . . C303 C 0.2718(6) 0.3498(4) 0.7805(4) 0.0498(17) Uani 1 1 d . . . C304 C 0.3158(5) 0.3392(4) 0.7184(4) 0.0457(16) Uani 1 1 d . . . H304 H 0.3197 0.2775 0.6834 0.055 Uiso 1 1 calc R . . C305 C 0.3545(5) 0.4148(4) 0.7052(4) 0.0389(14) Uani 1 1 d . . . C306 C 0.2989(5) 0.6148(4) 0.8802(4) 0.0464(15) Uani 1 1 d . . . H30A H 0.2496 0.6356 0.8432 0.070 Uiso 1 1 calc R . . H30B H 0.3689 0.6618 0.9123 0.070 Uiso 1 1 calc R . . H30C H 0.2732 0.6092 0.9235 0.070 Uiso 1 1 calc R . . C307 C 0.2319(8) 0.2670(5) 0.7926(6) 0.080(3) Uani 1 1 d . . . H30D H 0.2908 0.2430 0.8142 0.120 Uiso 1 1 calc R . . H30E H 0.1785 0.2160 0.7351 0.120 Uiso 1 1 calc R . . H30F H 0.2003 0.2875 0.8362 0.120 Uiso 1 1 calc R . . C308 C 0.3986(5) 0.3901(4) 0.6352(4) 0.0457(15) Uani 1 1 d . . . H30G H 0.4744 0.4235 0.6636 0.068 Uiso 1 1 calc R . . H30H H 0.3622 0.4098 0.5910 0.068 Uiso 1 1 calc R . . H30I H 0.3880 0.3209 0.6054 0.068 Uiso 1 1 calc R . . C400 C 0.2797(4) 0.6627(4) 0.7062(4) 0.0333(12) Uani 1 1 d . . . C401 C 0.2671(5) 0.7518(4) 0.7578(4) 0.0355(13) Uani 1 1 d . . . C402 C 0.1788(5) 0.7775(4) 0.7223(4) 0.0407(14) Uani 1 1 d . . . H402 H 0.1713 0.8373 0.7576 0.049 Uiso 1 1 calc R . . C403 C 0.1000(5) 0.7183(5) 0.6361(5) 0.0477(16) Uani 1 1 d . . . C404 C 0.1130(5) 0.6312(5) 0.5860(4) 0.0457(16) Uani 1 1 d . . . H404 H 0.0613 0.5906 0.5269 0.055 Uiso 1 1 calc R . . C405 C 0.1990(5) 0.6016(4) 0.6194(4) 0.0390(14) Uani 1 1 d . . . C406 C 0.3480(5) 0.8248(4) 0.8517(4) 0.0393(14) Uani 1 1 d . . . H40A H 0.3220 0.8800 0.8750 0.059 Uiso 1 1 calc R . . H40B H 0.4153 0.8458 0.8490 0.059 Uiso 1 1 calc R . . H40C H 0.3585 0.7952 0.8912 0.059 Uiso 1 1 calc R . . C407 C 0.0080(6) 0.7498(6) 0.5971(5) 0.062(2) Uani 1 1 d . . . H40D H 0.0293 0.7910 0.5732 0.093 Uiso 1 1 calc R . . H40E H -0.0153 0.7855 0.6438 0.093 Uiso 1 1 calc R . . H40F H -0.0503 0.6936 0.5487 0.093 Uiso 1 1 calc R . . C408 C 0.2043(5) 0.5057(4) 0.5590(4) 0.0442(15) Uani 1 1 d . . . H40G H 0.1453 0.4786 0.5002 0.066 Uiso 1 1 calc R . . H40H H 0.1997 0.4626 0.5851 0.066 Uiso 1 1 calc R . . H40I H 0.2714 0.5133 0.5523 0.066 Uiso 1 1 calc R . . C500 C 0.4815(4) 0.8586(4) 0.7184(3) 0.0304(12) Uani 1 1 d . . . C501 C 0.4887(5) 0.9493(4) 0.7812(4) 0.0320(12) Uani 1 1 d . . . C502 C 0.4101(5) 0.9923(4) 0.7629(4) 0.0346(13) Uani 1 1 d . . . H502 H 0.4177 1.0546 0.8063 0.042 Uiso 1 1 calc R . . C503 C 0.3191(5) 0.9466(5) 0.6822(4) 0.0450(15) Uani 1 1 d . . . C504 C 0.3144(5) 0.8582(5) 0.6191(4) 0.0400(14) Uani 1 1 d . . . H504 H 0.2554 0.8273 0.5628 0.048 Uiso 1 1 calc R . . C505 C 0.3916(4) 0.8126(4) 0.6339(3) 0.0332(12) Uani 1 1 d . . . C506 C 0.5828(5) 1.0069(4) 0.8713(4) 0.0417(14) Uani 1 1 d . . . H50A H 0.5752 1.0706 0.9024 0.063 Uiso 1 1 calc R . . H50B H 0.6482 1.0132 0.8618 0.063 Uiso 1 1 calc R . . H50C H 0.5855 0.9740 0.9075 0.063 Uiso 1 1 calc R . . C507 C 0.2321(6) 0.9927(6) 0.6651(5) 0.066(2) Uani 1 1 d . . . H50D H 0.2443 1.0288 0.6341 0.098 Uiso 1 1 calc R . . H50E H 0.2313 1.0361 0.7222 0.098 Uiso 1 1 calc R . . H50F H 0.1639 0.9431 0.6278 0.098 Uiso 1 1 calc R . . C508 C 0.3733(5) 0.7140(4) 0.5580(4) 0.0401(14) Uani 1 1 d . . . H50G H 0.3439 0.6643 0.5701 0.060 Uiso 1 1 calc R . . H50H H 0.4406 0.7074 0.5538 0.060 Uiso 1 1 calc R . . H50I H 0.3235 0.7073 0.5013 0.060 Uiso 1 1 calc R . . C600 C 0.7221(4) 0.8628(4) 0.7730(4) 0.0319(12) Uani 1 1 d . . . C601 C 0.8078(5) 0.9168(4) 0.8580(4) 0.0373(13) Uani 1 1 d . . . C602 C 0.9016(5) 0.9648(5) 0.8638(4) 0.0437(15) Uani 1 1 d . . . H602 H 0.9579 1.0023 0.9212 0.052 Uiso 1 1 calc R . . C603 C 0.9168(5) 0.9606(5) 0.7902(5) 0.0504(16) Uani 1 1 d . . . C604 C 0.8339(5) 0.9049(5) 0.7061(5) 0.0463(15) Uani 1 1 d . . . H604 H 0.8439 0.8987 0.6542 0.056 Uiso 1 1 calc R . . C605 C 0.7370(5) 0.8585(4) 0.6972(4) 0.0403(14) Uani 1 1 d . . . C606 C 0.8046(5) 0.9235(4) 0.9437(4) 0.0430(15) Uani 1 1 d . . . H60A H 0.8116 0.8641 0.9462 0.064 Uiso 1 1 calc R . . H60B H 0.7372 0.9331 0.9457 0.064 Uiso 1 1 calc R . . H60C H 0.8631 0.9775 0.9948 0.064 Uiso 1 1 calc R . . C607 C 1.0214(6) 1.0113(6) 0.7986(6) 0.074(2) Uani 1 1 d . . . H60D H 1.0718 0.9746 0.8069 0.111 Uiso 1 1 calc R . . H60E H 1.0489 1.0753 0.8504 0.111 Uiso 1 1 calc R . . H60F H 1.0114 1.0170 0.7442 0.111 Uiso 1 1 calc R . . C608 C 0.6497(5) 0.8049(5) 0.6031(4) 0.0471(16) Uani 1 1 d . . . H60G H 0.6785 0.8059 0.5600 0.071 Uiso 1 1 calc R . . H60H H 0.5930 0.8358 0.5997 0.071 Uiso 1 1 calc R . . H60I H 0.6215 0.7385 0.5890 0.071 Uiso 1 1 calc R . . C93 C 0.6109(9) 0.1437(6) 0.5798(6) 0.076(3) Uani 1 1 d . . . H93 H 0.5831 0.1648 0.5368 0.092 Uiso 1 1 calc R . . C94 C 0.7170(11) 0.1558(7) 0.6164(7) 0.095(3) Uani 1 1 d . . . H94 H 0.7630 0.1889 0.6015 0.114 Uiso 1 1 calc R . . C95 C 0.7580(10) 0.1210(9) 0.6739(8) 0.108(4) Uani 1 1 d . . . H95 H 0.8318 0.1286 0.6971 0.129 Uiso 1 1 calc R . . C96 C 0.6947(11) 0.0753(8) 0.6992(8) 0.101(3) Uani 1 1 d . . . H96 H 0.7237 0.0524 0.7405 0.122 Uiso 1 1 calc R . . C97 C 0.5885(10) 0.0638(6) 0.6628(6) 0.083(3) Uani 1 1 d . . . H97 H 0.5429 0.0296 0.6772 0.100 Uiso 1 1 calc R . . C98 C 0.5446(9) 0.1009(6) 0.6048(6) 0.078(3) Uani 1 1 d . . . C99 C 0.4294(10) 0.0940(8) 0.5726(7) 0.103(3) Uani 1 1 d . . . H99A H 0.4205 0.1580 0.5994 0.155 Uiso 1 1 calc R . . H99B H 0.3937 0.0528 0.5900 0.155 Uiso 1 1 calc R . . H99C H 0.3984 0.0667 0.5073 0.155 Uiso 1 1 calc R . . N88 N -0.0175(11) 0.5054(9) 0.3046(9) 0.155(4) Uani 1 1 d . . . C88 C 0.0290(11) 0.6048(11) 0.3469(9) 0.113(4) Uani 1 1 d . . . C87 C 0.0676(15) 0.6826(11) 0.3822(10) 0.174(8) Uani 1 1 d . . . H87A H 0.1314 0.6986 0.4351 0.261 Uiso 1 1 calc R . . H87B H 0.0188 0.7167 0.4008 0.261 Uiso 1 1 calc R . . H87C H 0.0870 0.7016 0.3420 0.261 Uiso 1 1 calc R . . C77 C 0.1190(15) 1.1032(14) 0.5108(13) 0.136(9) Uani 0.50 1 d PDU A -1 H77A H 0.1548 1.0725 0.4727 0.204 Uiso 0.50 1 calc PR A -1 H77B H 0.1705 1.1392 0.5733 0.204 Uiso 0.50 1 calc PR A -1 H77C H 0.0873 1.1469 0.4922 0.204 Uiso 0.50 1 calc PR A -1 C76 C 0.0352(11) 1.0289(10) 0.5023(9) 0.091(4) Uani 0.50 1 d PGDU A -1 C75 C 0.0214(12) 0.9327(11) 0.4493(9) 0.108(7) Uani 0.50 1 d PGDU A -1 H75 H 0.0653 0.9145 0.4180 0.129 Uiso 0.50 1 calc PR A -1 C74 C -0.0566(13) 0.8631(9) 0.4419(9) 0.100(5) Uani 0.50 1 d PGDU A -1 H74 H -0.0659 0.7973 0.4057 0.120 Uiso 0.50 1 calc PR A -1 C73 C -0.1208(11) 0.8897(11) 0.4877(9) 0.115(8) Uani 0.50 1 d PGDU A -1 H73 H -0.1741 0.8421 0.4827 0.138 Uiso 0.50 1 calc PR A -1 C72 C -0.1070(12) 0.9859(12) 0.5408(9) 0.098(5) Uani 0.50 1 d PGDU A -1 H72 H -0.1509 1.0041 0.5720 0.118 Uiso 0.50 1 calc PR A -1 C71 C -0.0291(13) 1.0555(9) 0.5481(8) 0.099(6) Uani 0.50 1 d PGDU A -1 H71 H -0.0197 1.1213 0.5844 0.118 Uiso 0.50 1 calc PR A -1 C66 C 0.928(2) 0.457(2) 1.0035(19) 0.096(8) Uani 0.25 1 d PGU B -1 H66 H 0.8876 0.4459 1.0340 0.115 Uiso 0.25 1 calc PR B -1 C65 C 1.016(3) 0.537(2) 1.0485(14) 0.094(7) Uani 0.25 1 d PGU B -1 H65 H 1.0355 0.5801 1.1097 0.113 Uiso 0.25 1 calc PR B -1 C64 C 1.076(2) 0.5531(19) 1.0040(19) 0.101(9) Uani 0.25 1 d PGU B -1 H64 H 1.1360 0.6076 1.0347 0.122 Uiso 0.25 1 calc PR B -1 C63 C 1.048(2) 0.490(2) 0.9145(19) 0.105(8) Uani 0.25 1 d PGU B -1 H63 H 1.0887 0.5009 0.8841 0.126 Uiso 0.25 1 calc PR B -1 C62 C 0.960(2) 0.4100(19) 0.8695(13) 0.096(7) Uani 0.25 1 d PGU B -1 H62 H 0.9407 0.3667 0.8084 0.115 Uiso 0.25 1 calc PR B -1 C61 C 0.9003(19) 0.3937(17) 0.9140(19) 0.097(7) Uani 0.25 1 d PGU B -1 H61 H 0.8402 0.3392 0.8833 0.116 Uiso 0.25 1 calc PR B -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 Sn1 0.0326(2) 0.0278(2) 0.0228(2) 0.00838(17) 0.01306(17) 0.00744(17) Sn2 0.0318(2) 0.0301(2) 0.0229(2) 0.00863(17) 0.01243(17) 0.00775(17) Si1 0.0312(8) 0.0324(8) 0.0304(8) 0.0151(7) 0.0159(6) 0.0107(7) Si2 0.0298(8) 0.0277(8) 0.0280(7) 0.0095(6) 0.0125(6) 0.0057(6) Si3 0.0284(8) 0.0285(8) 0.0264(7) 0.0112(6) 0.0101(6) 0.0064(6) C1 0.021(2) 0.014(2) 0.0092(18) 0.0011(16) 0.0067(18) 0.0047(19) C2 0.052(4) 0.042(3) 0.018(3) 0.003(2) 0.016(3) 0.010(3) C100 0.034(3) 0.036(3) 0.038(3) 0.015(3) 0.022(3) 0.015(3) C101 0.037(3) 0.041(3) 0.034(3) 0.015(3) 0.016(3) 0.014(3) C102 0.035(3) 0.044(4) 0.039(3) 0.011(3) 0.010(3) 0.008(3) C103 0.038(4) 0.041(4) 0.061(4) 0.015(3) 0.024(3) 0.012(3) C104 0.045(4) 0.042(4) 0.057(4) 0.017(3) 0.039(3) 0.012(3) C105 0.045(4) 0.028(3) 0.044(3) 0.014(3) 0.026(3) 0.014(3) C106 0.039(3) 0.061(4) 0.034(3) 0.021(3) 0.008(3) 0.011(3) C107 0.043(4) 0.068(5) 0.079(5) 0.018(4) 0.030(4) 0.002(4) C108 0.047(4) 0.044(4) 0.049(4) 0.026(3) 0.030(3) 0.013(3) C200 0.033(3) 0.036(3) 0.036(3) 0.020(3) 0.018(3) 0.012(3) C201 0.038(3) 0.041(3) 0.031(3) 0.018(3) 0.012(3) 0.008(3) C202 0.059(4) 0.048(4) 0.054(4) 0.031(3) 0.027(3) 0.011(3) C203 0.097(6) 0.047(4) 0.058(4) 0.030(4) 0.036(4) 0.015(4) C204 0.088(6) 0.040(4) 0.048(4) 0.022(3) 0.037(4) 0.022(4) C205 0.049(4) 0.033(3) 0.043(3) 0.021(3) 0.020(3) 0.010(3) C206 0.048(4) 0.050(4) 0.036(3) 0.024(3) 0.024(3) 0.018(3) C207 0.173(11) 0.041(4) 0.084(6) 0.034(4) 0.074(7) 0.015(6) C208 0.072(5) 0.036(3) 0.055(4) 0.021(3) 0.046(4) 0.021(3) C300 0.038(3) 0.024(3) 0.031(3) 0.009(2) 0.011(3) 0.005(2) C301 0.038(3) 0.041(3) 0.033(3) 0.016(3) 0.016(3) 0.010(3) C302 0.061(4) 0.040(4) 0.035(3) 0.016(3) 0.024(3) 0.006(3) C303 0.068(5) 0.034(3) 0.037(3) 0.014(3) 0.017(3) 0.002(3) C304 0.058(4) 0.028(3) 0.035(3) 0.008(3) 0.013(3) 0.002(3) C305 0.042(3) 0.031(3) 0.031(3) 0.006(2) 0.013(3) 0.004(3) C306 0.057(4) 0.045(4) 0.046(4) 0.019(3) 0.034(3) 0.011(3) C307 0.136(8) 0.044(4) 0.067(5) 0.029(4) 0.054(6) 0.005(5) C308 0.058(4) 0.037(3) 0.035(3) 0.007(3) 0.024(3) 0.016(3) C400 0.029(3) 0.037(3) 0.033(3) 0.016(3) 0.015(2) 0.006(3) C401 0.036(3) 0.036(3) 0.036(3) 0.016(3) 0.020(3) 0.005(3) C402 0.040(3) 0.039(3) 0.051(4) 0.022(3) 0.025(3) 0.017(3) C403 0.038(4) 0.050(4) 0.059(4) 0.028(3) 0.020(3) 0.012(3) C404 0.030(3) 0.056(4) 0.044(3) 0.027(3) 0.005(3) 0.005(3) C405 0.033(3) 0.041(3) 0.041(3) 0.019(3) 0.014(3) 0.008(3) C406 0.048(4) 0.032(3) 0.040(3) 0.012(3) 0.026(3) 0.012(3) C407 0.045(4) 0.060(5) 0.073(5) 0.031(4) 0.014(4) 0.023(4) C408 0.040(3) 0.041(4) 0.038(3) 0.012(3) 0.010(3) 0.008(3) C500 0.034(3) 0.028(3) 0.031(3) 0.017(2) 0.012(2) 0.009(2) C501 0.043(3) 0.029(3) 0.032(3) 0.017(2) 0.020(3) 0.009(3) C502 0.041(3) 0.033(3) 0.032(3) 0.014(2) 0.018(3) 0.015(3) C503 0.045(4) 0.046(4) 0.048(4) 0.029(3) 0.015(3) 0.015(3) C504 0.031(3) 0.055(4) 0.039(3) 0.032(3) 0.011(3) 0.010(3) C505 0.036(3) 0.039(3) 0.028(3) 0.020(2) 0.013(2) 0.007(3) C506 0.043(4) 0.033(3) 0.042(3) 0.011(3) 0.017(3) 0.015(3) C507 0.051(4) 0.061(5) 0.075(5) 0.031(4) 0.011(4) 0.026(4) C508 0.040(3) 0.037(3) 0.026(3) 0.010(2) 0.002(3) 0.002(3) C600 0.032(3) 0.028(3) 0.033(3) 0.012(2) 0.013(2) 0.007(2) C601 0.032(3) 0.039(3) 0.038(3) 0.014(3) 0.015(3) 0.014(3) C602 0.036(3) 0.044(4) 0.052(4) 0.021(3) 0.021(3) 0.014(3) C603 0.043(4) 0.045(4) 0.061(4) 0.020(3) 0.026(3) 0.010(3) C604 0.036(3) 0.051(4) 0.054(4) 0.025(3) 0.020(3) 0.009(3) C605 0.044(4) 0.035(3) 0.039(3) 0.013(3) 0.020(3) 0.012(3) C606 0.034(3) 0.042(4) 0.039(3) 0.014(3) 0.006(3) 0.005(3) C607 0.051(5) 0.068(5) 0.091(6) 0.031(5) 0.033(4) -0.008(4) C608 0.055(4) 0.052(4) 0.036(3) 0.021(3) 0.022(3) 0.011(3) C93 0.114(8) 0.053(5) 0.071(6) 0.029(4) 0.052(6) 0.015(5) C94 0.134(10) 0.067(6) 0.096(7) 0.039(6) 0.067(8) 0.016(7) C95 0.109(9) 0.112(9) 0.123(9) 0.053(8) 0.066(8) 0.057(8) C96 0.133(11) 0.089(8) 0.110(8) 0.054(7) 0.062(8) 0.063(8) C97 0.146(10) 0.051(5) 0.086(6) 0.036(5) 0.079(7) 0.039(6) C98 0.114(8) 0.042(4) 0.082(6) 0.021(4) 0.056(6) 0.021(5) C99 0.128(10) 0.088(7) 0.114(8) 0.048(7) 0.064(8) 0.050(7) N88 0.165(11) 0.112(9) 0.171(11) 0.069(8) 0.050(9) 0.027(8) C88 0.119(10) 0.095(9) 0.112(9) 0.045(8) 0.044(8) 0.011(8) C87 0.23(2) 0.115(12) 0.132(12) 0.023(10) 0.095(13) -0.024(13) C77 0.124(18) 0.194(15) 0.13(2) 0.130(16) 0.030(15) 0.036(14) C76 0.094(10) 0.139(9) 0.064(9) 0.072(8) 0.023(7) 0.050(8) C75 0.100(12) 0.150(11) 0.075(12) 0.054(10) 0.029(9) 0.060(9) C74 0.121(13) 0.123(10) 0.072(9) 0.055(9) 0.033(9) 0.068(8) C73 0.113(14) 0.137(11) 0.079(13) 0.039(11) 0.034(10) 0.043(11) C72 0.104(11) 0.139(12) 0.058(9) 0.046(9) 0.034(8) 0.052(9) C71 0.098(12) 0.136(11) 0.065(11) 0.052(10) 0.022(8) 0.053(9) C66 0.094(13) 0.103(13) 0.113(11) 0.072(11) 0.037(10) 0.042(10) C65 0.097(10) 0.096(10) 0.102(10) 0.061(7) 0.030(7) 0.044(7) C64 0.084(14) 0.107(15) 0.125(14) 0.067(12) 0.036(11) 0.040(11) C63 0.085(14) 0.129(17) 0.128(14) 0.071(13) 0.051(12) 0.055(11) C62 0.077(13) 0.119(15) 0.105(12) 0.061(11) 0.029(10) 0.062(10) C61 0.092(10) 0.096(10) 0.109(10) 0.067(7) 0.023(7) 0.036(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 Sn1 C1 2.138(4) . ? Sn1 Si3 2.6042(18) . ? Sn1 Si2 2.6160(17) . ? Sn1 Si1 2.6247(18) . ? Sn1 Sn2 3.1865(15) . ? Sn2 C2 2.171(5) . ? Sn2 Si1 2.6093(17) . ? Sn2 Si2 2.627(2) . ? Sn2 Si3 2.6277(16) . ? Si1 C200 1.900(6) . ? Si1 C100 1.902(6) . ? Si2 C300 1.907(6) . ? Si2 C400 1.922(6) . ? Si3 C500 1.911(5) . ? Si3 C600 1.911(6) . ? C1 C1 1.160(9) 2_666 ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C100 C105 1.404(8) . ? C100 C101 1.425(8) . ? C101 C102 1.397(8) . ? C101 C106 1.495(8) . ? C102 C103 1.393(9) . ? C102 H102 0.9500 . ? C103 C104 1.387(9) . ? C103 C107 1.483(9) . ? C104 C105 1.402(8) . ? C104 H104 0.9500 . ? C105 C108 1.529(8) . ? C106 H10A 0.9800 . ? C106 H10B 0.9800 . ? C106 H10C 0.9800 . ? C107 H10D 0.9800 . ? C107 H10E 0.9800 . ? C107 H10F 0.9800 . ? C108 H10G 0.9800 . ? C108 H10H 0.9800 . ? C108 H10I 0.9800 . ? C200 C205 1.410(8) . ? C200 C201 1.422(8) . ? C201 C202 1.383(8) . ? C201 C206 1.505(8) . ? C202 C203 1.364(10) . ? C202 H202 0.9500 . ? C203 C204 1.399(10) . ? C203 C207 1.495(10) . ? C204 C205 1.394(8) . ? C204 H204 0.9500 . ? C205 C208 1.511(8) . ? C206 H20A 0.9800 . ? C206 H20B 0.9800 . ? C206 H20C 0.9800 . ? C207 H20D 0.9800 . ? C207 H20E 0.9800 . ? C207 H20F 0.9800 . ? C208 H20G 0.9800 . ? C208 H20H 0.9800 . ? C208 H20I 0.9800 . ? C300 C305 1.413(8) . ? C300 C301 1.417(8) . ? C301 C302 1.385(8) . ? C301 C306 1.506(8) . ? C302 C303 1.391(9) . ? C302 H302 0.9500 . ? C303 C304 1.395(9) . ? C303 C307 1.493(9) . ? C304 C305 1.398(8) . ? C304 H304 0.9500 . ? C305 C308 1.501(8) . ? C306 H30A 0.9800 . ? C306 H30B 0.9800 . ? C306 H30C 0.9800 . ? C307 H30D 0.9800 . ? C307 H30E 0.9800 . ? C307 H30F 0.9800 . ? C308 H30G 0.9800 . ? C308 H30H 0.9800 . ? C308 H30I 0.9800 . ? C400 C401 1.418(8) . ? C400 C405 1.421(8) . ? C401 C402 1.383(8) . ? C401 C406 1.529(8) . ? C402 C403 1.401(9) . ? C402 H402 0.9500 . ? C403 C404 1.388(9) . ? C403 C407 1.501(9) . ? C404 C405 1.386(8) . ? C404 H404 0.9500 . ? C405 C408 1.504(8) . ? C406 H40A 0.9800 . ? C406 H40B 0.9800 . ? C406 H40C 0.9800 . ? C407 H40D 0.9800 . ? C407 H40E 0.9800 . ? C407 H40F 0.9800 . ? C408 H40G 0.9800 . ? C408 H40H 0.9800 . ? C408 H40I 0.9800 . ? C500 C501 1.395(8) . ? C500 C505 1.436(7) . ? C501 C502 1.382(8) . ? C501 C506 1.522(8) . ? C502 C503 1.405(8) . ? C502 H502 0.9500 . ? C503 C504 1.383(9) . ? C503 C507 1.506(9) . ? C504 C505 1.386(8) . ? C504 H504 0.9500 . ? C505 C508 1.529(8) . ? C506 H50A 0.9800 . ? C506 H50B 0.9800 . ? C506 H50C 0.9800 . ? C507 H50D 0.9800 . ? C507 H50E 0.9800 . ? C507 H50F 0.9800 . ? C508 H50G 0.9800 . ? C508 H50H 0.9800 . ? C508 H50I 0.9800 . ? C600 C605 1.410(8) . ? C600 C601 1.418(8) . ? C601 C602 1.382(8) . ? C601 C606 1.507(8) . ? C602 C603 1.377(9) . ? C602 H602 0.9500 . ? C603 C604 1.395(9) . ? C603 C607 1.509(9) . ? C604 C605 1.386(9) . ? C604 H604 0.9500 . ? C605 C608 1.523(8) . ? C606 H60A 0.9800 . ? C606 H60B 0.9800 . ? C606 H60C 0.9800 . ? C607 H60D 0.9800 . ? C607 H60E 0.9800 . ? C607 H60F 0.9800 . ? C608 H60G 0.9800 . ? C608 H60H 0.9800 . ? C608 H60I 0.9800 . ? C93 C94 1.364(14) . ? C93 C98 1.371(12) . ? C93 H93 0.9500 . ? C94 C95 1.359(14) . ? C94 H94 0.9500 . ? C95 C96 1.371(16) . ? C95 H95 0.9500 . ? C96 C97 1.368(15) . ? C96 H96 0.9500 . ? C97 C98 1.405(13) . ? C97 H97 0.9500 . ? C98 C99 1.496(14) . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? N88 C88 1.406(16) . ? C88 C87 1.104(15) . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C77 C76 1.483(10) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C76 C75 1.3900 . ? C76 C71 1.3900 . ? C75 C74 1.3900 . ? C75 H75 0.9500 . ? C74 C73 1.3900 . ? C74 H74 0.9500 . ? C73 C72 1.3900 . ? C73 H73 0.9500 . ? C72 C71 1.3900 . ? C72 H72 0.9500 . ? C71 H71 0.9500 . ? C66 C65 1.3900 . ? C66 C61 1.3900 . ? C66 H66 0.9500 . ? C65 C64 1.3900 . ? C65 H65 0.9500 . ? C64 C63 1.3900 . ? C64 H64 0.9500 . ? C63 C62 1.3900 . ? C63 H63 0.9500 . ? C62 C61 1.3900 . ? C62 H62 0.9500 . ? C61 H61 0.9500 . ? 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 C1 Sn1 Si3 125.35(13) . . ? C1 Sn1 Si2 128.55(14) . . ? Si3 Sn1 Si2 86.63(6) . . ? C1 Sn1 Si1 128.26(13) . . ? Si3 Sn1 Si1 87.71(6) . . ? Si2 Sn1 Si1 86.51(5) . . ? C1 Sn1 Sn2 178.11(13) . . ? Si3 Sn1 Sn2 52.81(4) . . ? Si2 Sn1 Sn2 52.74(5) . . ? Si1 Sn1 Sn2 52.28(4) . . ? C2 Sn2 Si1 127.57(18) . . ? C2 Sn2 Si2 127.65(18) . . ? Si1 Sn2 Si2 86.59(6) . . ? C2 Sn2 Si3 127.51(18) . . ? Si1 Sn2 Si3 87.54(5) . . ? Si2 Sn2 Si3 85.92(5) . . ? C2 Sn2 Sn1 179.63(18) . . ? Si1 Sn2 Sn1 52.72(4) . . ? Si2 Sn2 Sn1 52.41(5) . . ? Si3 Sn2 Sn1 52.14(4) . . ? C200 Si1 C100 111.2(3) . . ? C200 Si1 Sn2 116.91(18) . . ? C100 Si1 Sn2 115.34(18) . . ? C200 Si1 Sn1 115.65(19) . . ? C100 Si1 Sn1 118.56(18) . . ? Sn2 Si1 Sn1 75.01(5) . . ? C300 Si2 C400 109.4(3) . . ? C300 Si2 Sn1 117.24(19) . . ? C400 Si2 Sn1 116.88(17) . . ? C300 Si2 Sn2 118.61(18) . . ? C400 Si2 Sn2 116.57(18) . . ? Sn1 Si2 Sn2 74.85(5) . . ? C500 Si3 C600 111.7(2) . . ? C500 Si3 Sn1 117.88(18) . . ? C600 Si3 Sn1 116.16(18) . . ? C500 Si3 Sn2 114.63(18) . . ? C600 Si3 Sn2 117.13(18) . . ? Sn1 Si3 Sn2 75.04(5) . . ? C1 C1 Sn1 178.2(6) 2_666 . ? Sn2 C2 H2A 109.5 . . ? Sn2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sn2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C105 C100 C101 117.7(5) . . ? C105 C100 Si1 125.3(4) . . ? C101 C100 Si1 117.0(4) . . ? C102 C101 C100 120.5(5) . . ? C102 C101 C106 116.5(5) . . ? C100 C101 C106 123.1(5) . . ? C103 C102 C101 121.8(6) . . ? C103 C102 H102 119.1 . . ? C101 C102 H102 119.1 . . ? C104 C103 C102 117.3(6) . . ? C104 C103 C107 123.2(7) . . ? C102 C103 C107 119.5(6) . . ? C103 C104 C105 122.9(6) . . ? C103 C104 H104 118.5 . . ? C105 C104 H104 118.5 . . ? C104 C105 C100 119.8(5) . . ? C104 C105 C108 116.6(5) . . ? C100 C105 C108 123.6(5) . . ? C101 C106 H10A 109.5 . . ? C101 C106 H10B 109.5 . . ? H10A C106 H10B 109.5 . . ? C101 C106 H10C 109.5 . . ? H10A C106 H10C 109.5 . . ? H10B C106 H10C 109.5 . . ? C103 C107 H10D 109.5 . . ? C103 C107 H10E 109.5 . . ? H10D C107 H10E 109.5 . . ? C103 C107 H10F 109.5 . . ? H10D C107 H10F 109.5 . . ? H10E C107 H10F 109.5 . . ? C105 C108 H10G 109.5 . . ? C105 C108 H10H 109.5 . . ? H10G C108 H10H 109.5 . . ? C105 C108 H10I 109.5 . . ? H10G C108 H10I 109.5 . . ? H10H C108 H10I 109.5 . . ? C205 C200 C201 117.9(5) . . ? C205 C200 Si1 118.1(4) . . ? C201 C200 Si1 124.0(4) . . ? C202 C201 C200 119.2(6) . . ? C202 C201 C206 116.6(5) . . ? C200 C201 C206 124.2(5) . . ? C203 C202 C201 123.6(6) . . ? C203 C202 H202 118.2 . . ? C201 C202 H202 118.2 . . ? C202 C203 C204 117.7(6) . . ? C202 C203 C207 121.2(7) . . ? C204 C203 C207 121.1(7) . . ? C205 C204 C203 121.3(6) . . ? C205 C204 H204 119.3 . . ? C203 C204 H204 119.3 . . ? C204 C205 C200 120.3(6) . . ? C204 C205 C208 117.9(6) . . ? C200 C205 C208 121.8(5) . . ? C201 C206 H20A 109.5 . . ? C201 C206 H20B 109.5 . . ? H20A C206 H20B 109.5 . . ? C201 C206 H20C 109.5 . . ? H20A C206 H20C 109.5 . . ? H20B C206 H20C 109.5 . . ? C203 C207 H20D 109.5 . . ? C203 C207 H20E 109.5 . . ? H20D C207 H20E 109.5 . . ? C203 C207 H20F 109.5 . . ? H20D C207 H20F 109.5 . . ? H20E C207 H20F 109.5 . . ? C205 C208 H20G 109.5 . . ? C205 C208 H20H 109.5 . . ? H20G C208 H20H 109.5 . . ? C205 C208 H20I 109.5 . . ? H20G C208 H20I 109.5 . . ? H20H C208 H20I 109.5 . . ? C305 C300 C301 118.1(5) . . ? C305 C300 Si2 124.5(4) . . ? C301 C300 Si2 117.4(4) . . ? C302 C301 C300 120.5(6) . . ? C302 C301 C306 117.5(5) . . ? C300 C301 C306 122.0(5) . . ? C301 C302 C303 122.5(6) . . ? C301 C302 H302 118.8 . . ? C303 C302 H302 118.8 . . ? C302 C303 C304 116.6(6) . . ? C302 C303 C307 122.0(6) . . ? C304 C303 C307 121.4(6) . . ? C303 C304 C305 123.3(6) . . ? C303 C304 H304 118.4 . . ? C305 C304 H304 118.4 . . ? C304 C305 C300 119.1(6) . . ? C304 C305 C308 116.0(5) . . ? C300 C305 C308 124.9(5) . . ? C301 C306 H30A 109.5 . . ? C301 C306 H30B 109.5 . . ? H30A C306 H30B 109.5 . . ? C301 C306 H30C 109.5 . . ? H30A C306 H30C 109.5 . . ? H30B C306 H30C 109.5 . . ? C303 C307 H30D 109.5 . . ? C303 C307 H30E 109.5 . . ? H30D C307 H30E 109.5 . . ? C303 C307 H30F 109.5 . . ? H30D C307 H30F 109.5 . . ? H30E C307 H30F 109.5 . . ? C305 C308 H30G 109.5 . . ? C305 C308 H30H 109.5 . . ? H30G C308 H30H 109.5 . . ? C305 C308 H30I 109.5 . . ? H30G C308 H30I 109.5 . . ? H30H C308 H30I 109.5 . . ? C401 C400 C405 118.1(5) . . ? C401 C400 Si2 124.3(4) . . ? C405 C400 Si2 117.6(4) . . ? C402 C401 C400 119.7(5) . . ? C402 C401 C406 116.6(5) . . ? C400 C401 C406 123.7(5) . . ? C401 C402 C403 122.4(6) . . ? C401 C402 H402 118.8 . . ? C403 C402 H402 118.8 . . ? C404 C403 C402 117.5(6) . . ? C404 C403 C407 120.9(6) . . ? C402 C403 C407 121.4(6) . . ? C405 C404 C403 122.2(6) . . ? C405 C404 H404 118.9 . . ? C403 C404 H404 118.9 . . ? C404 C405 C400 120.0(6) . . ? C404 C405 C408 117.3(5) . . ? C400 C405 C408 122.6(5) . . ? C401 C406 H40A 109.5 . . ? C401 C406 H40B 109.5 . . ? H40A C406 H40B 109.5 . . ? C401 C406 H40C 109.5 . . ? H40A C406 H40C 109.5 . . ? H40B C406 H40C 109.5 . . ? C403 C407 H40D 109.5 . . ? C403 C407 H40E 109.5 . . ? H40D C407 H40E 109.5 . . ? C403 C407 H40F 109.5 . . ? H40D C407 H40F 109.5 . . ? H40E C407 H40F 109.5 . . ? C405 C408 H40G 109.5 . . ? C405 C408 H40H 109.5 . . ? H40G C408 H40H 109.5 . . ? C405 C408 H40I 109.5 . . ? H40G C408 H40I 109.5 . . ? H40H C408 H40I 109.5 . . ? C501 C500 C505 118.1(5) . . ? C501 C500 Si3 117.9(4) . . ? C505 C500 Si3 123.7(4) . . ? C502 C501 C500 120.7(5) . . ? C502 C501 C506 116.6(5) . . ? C500 C501 C506 122.8(5) . . ? C501 C502 C503 122.1(5) . . ? C501 C502 H502 119.0 . . ? C503 C502 H502 119.0 . . ? C504 C503 C502 116.8(5) . . ? C504 C503 C507 121.8(6) . . ? C502 C503 C507 121.4(6) . . ? C503 C504 C505 123.1(6) . . ? C503 C504 H504 118.4 . . ? C505 C504 H504 118.4 . . ? C504 C505 C500 119.0(5) . . ? C504 C505 C508 116.7(5) . . ? C500 C505 C508 124.3(5) . . ? C501 C506 H50A 109.5 . . ? C501 C506 H50B 109.5 . . ? H50A C506 H50B 109.5 . . ? C501 C506 H50C 109.5 . . ? H50A C506 H50C 109.5 . . ? H50B C506 H50C 109.5 . . ? C503 C507 H50D 109.5 . . ? C503 C507 H50E 109.5 . . ? H50D C507 H50E 109.5 . . ? C503 C507 H50F 109.5 . . ? H50D C507 H50F 109.5 . . ? H50E C507 H50F 109.5 . . ? C505 C508 H50G 109.5 . . ? C505 C508 H50H 109.5 . . ? H50G C508 H50H 109.5 . . ? C505 C508 H50I 109.5 . . ? H50G C508 H50I 109.5 . . ? H50H C508 H50I 109.5 . . ? C605 C600 C601 118.3(5) . . ? C605 C600 Si3 117.3(4) . . ? C601 C600 Si3 124.4(4) . . ? C602 C601 C600 119.1(5) . . ? C602 C601 C606 117.0(5) . . ? C600 C601 C606 123.9(5) . . ? C603 C602 C601 122.9(6) . . ? C603 C602 H602 118.6 . . ? C601 C602 H602 118.6 . . ? C602 C603 C604 118.2(6) . . ? C602 C603 C607 121.5(7) . . ? C604 C603 C607 120.3(7) . . ? C605 C604 C603 121.0(6) . . ? C605 C604 H604 119.5 . . ? C603 C604 H604 119.5 . . ? C604 C605 C600 120.5(6) . . ? C604 C605 C608 116.7(6) . . ? C600 C605 C608 122.8(5) . . ? C601 C606 H60A 109.5 . . ? C601 C606 H60B 109.5 . . ? H60A C606 H60B 109.5 . . ? C601 C606 H60C 109.5 . . ? H60A C606 H60C 109.5 . . ? H60B C606 H60C 109.5 . . ? C603 C607 H60D 109.5 . . ? C603 C607 H60E 109.5 . . ? H60D C607 H60E 109.5 . . ? C603 C607 H60F 109.5 . . ? H60D C607 H60F 109.5 . . ? H60E C607 H60F 109.5 . . ? C605 C608 H60G 109.5 . . ? C605 C608 H60H 109.5 . . ? H60G C608 H60H 109.5 . . ? C605 C608 H60I 109.5 . . ? H60G C608 H60I 109.5 . . ? H60H C608 H60I 109.5 . . ? C94 C93 C98 120.0(9) . . ? C94 C93 H93 120.0 . . ? C98 C93 H93 120.0 . . ? C95 C94 C93 121.0(10) . . ? C95 C94 H94 119.5 . . ? C93 C94 H94 119.5 . . ? C94 C95 C96 121.3(12) . . ? C94 C95 H95 119.4 . . ? C96 C95 H95 119.4 . . ? C97 C96 C95 117.6(11) . . ? C97 C96 H96 121.2 . . ? C95 C96 H96 121.2 . . ? C96 C97 C98 122.2(10) . . ? C96 C97 H97 118.9 . . ? C98 C97 H97 118.9 . . ? C93 C98 C97 117.7(10) . . ? C93 C98 C99 121.8(9) . . ? C97 C98 C99 120.5(9) . . ? C98 C99 H99A 109.5 . . ? C98 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? C98 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? C87 C88 N88 177.9(19) . . ? C88 C87 H87A 109.5 . . ? C88 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C88 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C75 C76 C71 120.0 . . ? C75 C76 C77 120.0(4) . . ? C71 C76 C77 120.0(4) . . ? C76 C75 C74 120.0 . . ? C76 C75 H75 120.0 . . ? C74 C75 H75 120.0 . . ? C75 C74 C73 120.0 . . ? C75 C74 H74 120.0 . . ? C73 C74 H74 120.0 . . ? C72 C73 C74 120.0 . . ? C72 C73 H73 120.0 . . ? C74 C73 H73 120.0 . . ? C73 C72 C71 120.0 . . ? C73 C72 H72 120.0 . . ? C71 C72 H72 120.0 . . ? C72 C71 C76 120.0 . . ? C72 C71 H71 120.0 . . ? C76 C71 H71 120.0 . . ? C65 C66 C61 120.0 . . ? C65 C66 H66 120.0 . . ? C61 C66 H66 120.0 . . ? C64 C65 C66 120.0 . . ? C64 C65 H65 120.0 . . ? C66 C65 H65 120.0 . . ? C63 C64 C65 120.00(7) . . ? C63 C64 H64 120.0 . . ? C65 C64 H64 120.0 . . ? C64 C63 C62 120.0 . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C61 C62 C63 120.0 . . ? C61 C62 H62 120.0 . . ? C63 C62 H62 120.0 . . ? C62 C61 C66 120.0 . . ? C62 C61 H61 120.0 . . ? C66 C61 H61 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Si3 Sn1 Sn2 Si1 -121.56(7) . . . . ? Si2 Sn1 Sn2 Si1 119.46(6) . . . . ? Si3 Sn1 Sn2 Si2 118.98(6) . . . . ? Si1 Sn1 Sn2 Si2 -119.46(6) . . . . ? Si2 Sn1 Sn2 Si3 -118.98(6) . . . . ? Si1 Sn1 Sn2 Si3 121.56(6) . . . . ? C2 Sn2 Si1 C200 68.8(3) . . . . ? Si2 Sn2 Si1 C200 -67.8(2) . . . . ? Si3 Sn2 Si1 C200 -153.8(2) . . . . ? Sn1 Sn2 Si1 C200 -111.5(2) . . . . ? C2 Sn2 Si1 C100 -64.8(3) . . . . ? Si2 Sn2 Si1 C100 158.6(2) . . . . ? Si3 Sn2 Si1 C100 72.6(2) . . . . ? Sn1 Sn2 Si1 C100 114.9(2) . . . . ? C2 Sn2 Si1 Sn1 -179.7(2) . . . . ? Si2 Sn2 Si1 Sn1 43.72(5) . . . . ? Si3 Sn2 Si1 Sn1 -42.33(5) . . . . ? C1 Sn1 Si1 C200 -69.3(3) . . . . ? Si3 Sn1 Si1 C200 155.8(2) . . . . ? Si2 Sn1 Si1 C200 69.1(2) . . . . ? Sn2 Sn1 Si1 C200 113.0(2) . . . . ? C1 Sn1 Si1 C100 66.7(3) . . . . ? Si3 Sn1 Si1 C100 -68.2(2) . . . . ? Si2 Sn1 Si1 C100 -155.0(2) . . . . ? Sn2 Sn1 Si1 C100 -111.0(2) . . . . ? C1 Sn1 Si1 Sn2 177.70(16) . . . . ? Si3 Sn1 Si1 Sn2 42.80(5) . . . . ? Si2 Sn1 Si1 Sn2 -43.97(5) . . . . ? C1 Sn1 Si2 C300 67.0(3) . . . . ? Si3 Sn1 Si2 C300 -159.0(2) . . . . ? Si1 Sn1 Si2 C300 -71.1(2) . . . . ? Sn2 Sn1 Si2 C300 -114.8(2) . . . . ? C1 Sn1 Si2 C400 -65.8(3) . . . . ? Si3 Sn1 Si2 C400 68.2(2) . . . . ? Si1 Sn1 Si2 C400 156.1(2) . . . . ? Sn2 Sn1 Si2 C400 112.5(2) . . . . ? C1 Sn1 Si2 Sn2 -178.24(15) . . . . ? Si3 Sn1 Si2 Sn2 -44.28(5) . . . . ? Si1 Sn1 Si2 Sn2 43.63(5) . . . . ? C2 Sn2 Si2 C300 -67.3(3) . . . . ? Si1 Sn2 Si2 C300 69.2(2) . . . . ? Si3 Sn2 Si2 C300 156.9(2) . . . . ? Sn1 Sn2 Si2 C300 113.1(2) . . . . ? C2 Sn2 Si2 C400 66.7(3) . . . . ? Si1 Sn2 Si2 C400 -156.80(19) . . . . ? Si3 Sn2 Si2 C400 -69.03(19) . . . . ? Sn1 Sn2 Si2 C400 -112.9(2) . . . . ? C2 Sn2 Si2 Sn1 179.5(2) . . . . ? Si1 Sn2 Si2 Sn1 -43.95(4) . . . . ? Si3 Sn2 Si2 Sn1 43.82(4) . . . . ? C1 Sn1 Si3 C500 70.3(3) . . . . ? Si2 Sn1 Si3 C500 -66.1(2) . . . . ? Si1 Sn1 Si3 C500 -152.7(2) . . . . ? Sn2 Sn1 Si3 C500 -110.3(2) . . . . ? C1 Sn1 Si3 C600 -66.2(2) . . . . ? Si2 Sn1 Si3 C600 157.46(19) . . . . ? Si1 Sn1 Si3 C600 70.82(19) . . . . ? Sn2 Sn1 Si3 C600 113.2(2) . . . . ? C1 Sn1 Si3 Sn2 -179.42(15) . . . . ? Si2 Sn1 Si3 Sn2 44.22(5) . . . . ? Si1 Sn1 Si3 Sn2 -42.42(4) . . . . ? C2 Sn2 Si3 C500 -65.6(3) . . . . ? Si1 Sn2 Si3 C500 156.94(19) . . . . ? Si2 Sn2 Si3 C500 70.18(19) . . . . ? Sn1 Sn2 Si3 C500 114.2(2) . . . . ? C2 Sn2 Si3 C600 68.1(3) . . . . ? Si1 Sn2 Si3 C600 -69.3(2) . . . . ? Si2 Sn2 Si3 C600 -156.1(2) . . . . ? Sn1 Sn2 Si3 C600 -112.1(2) . . . . ? C2 Sn2 Si3 Sn1 -179.8(2) . . . . ? Si1 Sn2 Si3 Sn1 42.73(5) . . . . ? Si2 Sn2 Si3 Sn1 -44.02(5) . . . . ? C200 Si1 C100 C105 117.6(5) . . . . ? Sn2 Si1 C100 C105 -106.3(5) . . . . ? Sn1 Si1 C100 C105 -20.2(6) . . . . ? C200 Si1 C100 C101 -63.7(5) . . . . ? Sn2 Si1 C100 C101 72.5(5) . . . . ? Sn1 Si1 C100 C101 158.6(4) . . . . ? C105 C100 C101 C102 2.5(8) . . . . ? Si1 C100 C101 C102 -176.4(5) . . . . ? C105 C100 C101 C106 -179.2(5) . . . . ? Si1 C100 C101 C106 2.0(8) . . . . ? C100 C101 C102 C103 -1.4(9) . . . . ? C106 C101 C102 C103 -179.9(6) . . . . ? C101 C102 C103 C104 0.3(10) . . . . ? C101 C102 C103 C107 -177.8(6) . . . . ? C102 C103 C104 C105 -0.3(9) . . . . ? C107 C103 C104 C105 177.7(6) . . . . ? C103 C104 C105 C100 1.5(9) . . . . ? C103 C104 C105 C108 -178.6(6) . . . . ? C101 C100 C105 C104 -2.5(8) . . . . ? Si1 C100 C105 C104 176.2(4) . . . . ? C101 C100 C105 C108 177.6(5) . . . . ? Si1 C100 C105 C108 -3.7(8) . . . . ? C100 Si1 C200 C205 -67.1(5) . . . . ? Sn2 Si1 C200 C205 157.5(4) . . . . ? Sn1 Si1 C200 C205 72.0(5) . . . . ? C100 Si1 C200 C201 114.7(5) . . . . ? Sn2 Si1 C200 C201 -20.7(5) . . . . ? Sn1 Si1 C200 C201 -106.3(5) . . . . ? C205 C200 C201 C202 0.1(9) . . . . ? Si1 C200 C201 C202 178.4(5) . . . . ? C205 C200 C201 C206 179.5(6) . . . . ? Si1 C200 C201 C206 -2.2(8) . . . . ? C200 C201 C202 C203 -0.9(10) . . . . ? C206 C201 C202 C203 179.6(7) . . . . ? C201 C202 C203 C204 1.8(12) . . . . ? C201 C202 C203 C207 -177.2(8) . . . . ? C202 C203 C204 C205 -2.0(12) . . . . ? C207 C203 C204 C205 177.1(8) . . . . ? C203 C204 C205 C200 1.2(11) . . . . ? C203 C204 C205 C208 179.9(7) . . . . ? C201 C200 C205 C204 -0.3(9) . . . . ? Si1 C200 C205 C204 -178.6(5) . . . . ? C201 C200 C205 C208 -178.9(6) . . . . ? Si1 C200 C205 C208 2.7(8) . . . . ? C400 Si2 C300 C305 116.1(5) . . . . ? Sn1 Si2 C300 C305 -20.0(6) . . . . ? Sn2 Si2 C300 C305 -106.9(5) . . . . ? C400 Si2 C300 C301 -64.8(5) . . . . ? Sn1 Si2 C300 C301 159.2(4) . . . . ? Sn2 Si2 C300 C301 72.3(5) . . . . ? C305 C300 C301 C302 -1.4(9) . . . . ? Si2 C300 C301 C302 179.4(5) . . . . ? C305 C300 C301 C306 179.4(6) . . . . ? Si2 C300 C301 C306 0.2(8) . . . . ? C300 C301 C302 C303 0.3(10) . . . . ? C306 C301 C302 C303 179.5(6) . . . . ? C301 C302 C303 C304 1.0(10) . . . . ? C301 C302 C303 C307 179.5(7) . . . . ? C302 C303 C304 C305 -1.2(10) . . . . ? C307 C303 C304 C305 -179.8(7) . . . . ? C303 C304 C305 C300 0.1(10) . . . . ? C303 C304 C305 C308 -179.7(6) . . . . ? C301 C300 C305 C304 1.2(9) . . . . ? Si2 C300 C305 C304 -179.6(5) . . . . ? C301 C300 C305 C308 -179.1(6) . . . . ? Si2 C300 C305 C308 0.1(9) . . . . ? C300 Si2 C400 C401 114.6(5) . . . . ? Sn1 Si2 C400 C401 -109.1(4) . . . . ? Sn2 Si2 C400 C401 -23.4(5) . . . . ? C300 Si2 C400 C405 -63.9(5) . . . . ? Sn1 Si2 C400 C405 72.3(5) . . . . ? Sn2 Si2 C400 C405 158.1(4) . . . . ? C405 C400 C401 C402 -1.2(8) . . . . ? Si2 C400 C401 C402 -179.7(4) . . . . ? C405 C400 C401 C406 -179.5(5) . . . . ? Si2 C400 C401 C406 1.9(8) . . . . ? C400 C401 C402 C403 -0.1(9) . . . . ? C406 C401 C402 C403 178.4(5) . . . . ? C401 C402 C403 C404 0.0(9) . . . . ? C401 C402 C403 C407 -176.6(6) . . . . ? C402 C403 C404 C405 1.4(10) . . . . ? C407 C403 C404 C405 178.0(6) . . . . ? C403 C404 C405 C400 -2.7(9) . . . . ? C403 C404 C405 C408 179.8(6) . . . . ? C401 C400 C405 C404 2.5(8) . . . . ? Si2 C400 C405 C404 -178.8(5) . . . . ? C401 C400 C405 C408 179.9(5) . . . . ? Si2 C400 C405 C408 -1.5(8) . . . . ? C600 Si3 C500 C501 -68.2(5) . . . . ? Sn1 Si3 C500 C501 153.5(4) . . . . ? Sn2 Si3 C500 C501 68.0(4) . . . . ? C600 Si3 C500 C505 117.8(5) . . . . ? Sn1 Si3 C500 C505 -20.5(5) . . . . ? Sn2 Si3 C500 C505 -106.0(4) . . . . ? C505 C500 C501 C502 1.4(8) . . . . ? Si3 C500 C501 C502 -173.0(4) . . . . ? C505 C500 C501 C506 -177.1(5) . . . . ? Si3 C500 C501 C506 8.5(7) . . . . ? C500 C501 C502 C503 1.5(8) . . . . ? C506 C501 C502 C503 -179.9(5) . . . . ? C501 C502 C503 C504 -3.7(9) . . . . ? C501 C502 C503 C507 177.3(6) . . . . ? C502 C503 C504 C505 3.1(9) . . . . ? C507 C503 C504 C505 -178.0(6) . . . . ? C503 C504 C505 C500 -0.3(9) . . . . ? C503 C504 C505 C508 178.6(6) . . . . ? C501 C500 C505 C504 -2.0(8) . . . . ? Si3 C500 C505 C504 172.0(4) . . . . ? C501 C500 C505 C508 179.2(5) . . . . ? Si3 C500 C505 C508 -6.8(8) . . . . ? C500 Si3 C600 C605 -67.9(5) . . . . ? Sn1 Si3 C600 C605 71.1(5) . . . . ? Sn2 Si3 C600 C605 157.0(4) . . . . ? C500 Si3 C600 C601 109.8(5) . . . . ? Sn1 Si3 C600 C601 -111.1(5) . . . . ? Sn2 Si3 C600 C601 -25.2(5) . . . . ? C605 C600 C601 C602 1.4(8) . . . . ? Si3 C600 C601 C602 -176.4(4) . . . . ? C605 C600 C601 C606 -176.8(6) . . . . ? Si3 C600 C601 C606 5.5(8) . . . . ? C600 C601 C602 C603 -1.7(9) . . . . ? C606 C601 C602 C603 176.6(6) . . . . ? C601 C602 C603 C604 -0.4(10) . . . . ? C601 C602 C603 C607 -178.0(6) . . . . ? C602 C603 C604 C605 2.9(10) . . . . ? C607 C603 C604 C605 -179.5(6) . . . . ? C603 C604 C605 C600 -3.2(10) . . . . ? C603 C604 C605 C608 176.1(6) . . . . ? C601 C600 C605 C604 1.0(8) . . . . ? Si3 C600 C605 C604 178.9(5) . . . . ? C601 C600 C605 C608 -178.3(6) . . . . ? Si3 C600 C605 C608 -0.4(8) . . . . ? C98 C93 C94 C95 3.9(15) . . . . ? C93 C94 C95 C96 -2.0(17) . . . . ? C94 C95 C96 C97 1.5(17) . . . . ? C95 C96 C97 C98 -3.0(15) . . . . ? C94 C93 C98 C97 -5.1(13) . . . . ? C94 C93 C98 C99 174.5(9) . . . . ? C96 C97 C98 C93 4.8(13) . . . . ? C96 C97 C98 C99 -174.8(9) . . . . ? C71 C76 C75 C74 0.0 . . . . ? C77 C76 C75 C74 179.4(8) . . . . ? C76 C75 C74 C73 0.0 . . . . ? C75 C74 C73 C72 0.0 . . . . ? C74 C73 C72 C71 0.0 . . . . ? C73 C72 C71 C76 0.0 . . . . ? C75 C76 C71 C72 0.0 . . . . ? C77 C76 C71 C72 -179.4(8) . . . . ? C61 C66 C65 C64 0.0 . . . . ? C66 C65 C64 C63 0.0 . . . . ? C65 C64 C63 C62 0.0 . . . . ? C64 C63 C62 C61 0.0 . . . . ? C63 C62 C61 C66 0.0 . . . . ? C65 C66 C61 C62 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.942 _refine_diff_density_min -1.175 _refine_diff_density_rms 0.131 data_vic1148 _database_code_depnum_ccdc_archive 'CCDC 879400' #TrackingRef '- [P2Me5][Cl].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H15 P2, Cl' _chemical_formula_sum 'C5 H15 Cl P2' _chemical_formula_weight 172.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P m n 21' _symmetry_space_group_name_Hall 'P 2ac -2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y, z+1/2' '-x, y, z' _cell_length_a 9.4581(6) _cell_length_b 6.5601(4) _cell_length_c 7.3060(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 453.31(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3338 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 27.39 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 184 _exptl_absorpt_coefficient_mu 0.690 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7760 _exptl_absorpt_correction_T_max 0.9317 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3886 _diffrn_reflns_av_R_equivalents 0.0167 _diffrn_reflns_av_sigmaI/netI 0.0146 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.51 _reflns_number_total 1106 _reflns_number_gt 1083 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0265P)^2^+0.0418P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.19(8) _refine_ls_number_reflns 1106 _refine_ls_number_parameters 48 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0183 _refine_ls_R_factor_gt 0.0177 _refine_ls_wR_factor_ref 0.0465 _refine_ls_wR_factor_gt 0.0461 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.0000 0.32712(7) -0.07922(5) 0.02115(11) Uani 1 2 d S . . P2 P 0.0000 0.10327(7) 0.14071(6) 0.02593(12) Uani 1 2 d S . . C1 C 0.0000 0.5875(3) -0.0060(3) 0.0315(4) Uani 1 2 d S . . H1A H -0.0272 0.6755 -0.1085 0.038 Uiso 0.50 1 calc PR . . H1B H 0.0949 0.6250 0.0363 0.038 Uiso 0.50 1 calc PR . . H1C H -0.0676 0.6047 0.0945 0.038 Uiso 0.50 1 calc PR . . C2 C 0.15109(17) 0.2839(2) -0.22048(18) 0.0321(3) Uani 1 1 d . . . H2A H 0.1551 0.3881 -0.3165 0.039 Uiso 1 1 calc R . . H2B H 0.1442 0.1487 -0.2768 0.039 Uiso 1 1 calc R . . H2C H 0.2370 0.2911 -0.1457 0.039 Uiso 1 1 calc R . . C3 C 0.14922(17) 0.2046(2) 0.27243(18) 0.0315(3) Uani 1 1 d . . . H3A H 0.1647 0.1196 0.3809 0.038 Uiso 1 1 calc R . . H3B H 0.1283 0.3446 0.3106 0.038 Uiso 1 1 calc R . . H3C H 0.2345 0.2037 0.1962 0.038 Uiso 1 1 calc R . . Cl Cl 0.5000 0.25690(8) 0.01496(7) 0.03395(13) Uani 1 2 d S . . 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 P1 0.0253(2) 0.0196(2) 0.0185(2) -0.00052(17) 0.000 0.000 P2 0.0377(3) 0.0181(2) 0.0219(2) 0.00005(18) 0.000 0.000 C1 0.0477(11) 0.0193(9) 0.0275(9) -0.0003(7) 0.000 0.000 C2 0.0299(7) 0.0385(8) 0.0280(7) 0.0030(6) 0.0062(5) 0.0056(6) C3 0.0317(8) 0.0354(8) 0.0275(7) 0.0038(6) -0.0033(5) 0.0035(6) Cl 0.0273(2) 0.0428(3) 0.0318(2) -0.0115(2) 0.000 0.000 _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 P1 C2 1.7855(15) 4 ? P1 C2 1.7855(15) . ? P1 C1 1.790(2) . ? P1 P2 2.1767(6) . ? P2 C3 1.8329(15) 4 ? P2 C3 1.8329(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 P1 C2 106.33(10) 4 . ? C2 P1 C1 108.93(6) 4 . ? C2 P1 C1 108.93(6) . . ? C2 P1 P2 108.63(5) 4 . ? C2 P1 P2 108.63(5) . . ? C1 P1 P2 115.03(7) . . ? C3 P2 C3 100.71(9) 4 . ? C3 P2 P1 98.22(4) 4 . ? C3 P2 P1 98.22(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 P1 P2 C3 -71.29(7) 4 . . 4 ? C2 P1 P2 C3 173.44(8) . . . 4 ? C1 P1 P2 C3 51.08(5) . . . 4 ? C2 P1 P2 C3 -173.44(8) 4 . . . ? C2 P1 P2 C3 71.29(7) . . . . ? C1 P1 P2 C3 -51.08(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.239 _refine_diff_density_min -0.189 _refine_diff_density_rms 0.038