Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'K. Dillon' _publ_contact_author_address ; Chemistry Department University of Durham South Road Durham DH1 3LE UNITED KINGDOM ; _publ_contact_author_email K.B.DILLON@DURHAM.AC.UK _publ_section_title ; Novel (n + 1 + 1) Cycloaddition Reactions; The Formation of Cyclic Tetraphosphonium Dications with Four linked Phosphorus Atoms and an Organic Backbone ; _publ_section_abstract ; In the presence of SnCl2, a novel cycloaddition of two moles of R_PCl2 (R_ = Et or Ph) to a diphosphane has been achieved, forming a cyclic dication with four linked phosphorus atoms and an organic backbone; two of these species have been characterised by single-crystal X-ray diffraction, and the mechanism of the reaction has been established. ; loop_ _publ_author_name 'K. Dillon' 'Alice Boyall' 'Judith A. K Howard' 'Philippa Monks' 'Amber L. Thompson' #============================================================================== data_3a _database_code_depnum_ccdc_archive 'CCDC 626260' #============================================================================== _chemical_name_systematic ; . ; _chemical_name_common . _chemical_melting_point 'not measured' _chemical_formula_moiety 'C29 H32 P4, 2(C H Cl3), Cl6 Sn' _chemical_formula_sum 'C31 H34 Cl12 P4 Sn' _chemical_formula_weight 1074.55 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' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.1214(12) _cell_length_b 18.8045(19) _cell_length_c 19.074(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.190(2) _cell_angle_gamma 90.00 _cell_volume 4341.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5025 _cell_measurement_theta_min 2.225 _cell_measurement_theta_max 27.472 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 1.499 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7562 _exptl_absorpt_correction_T_max 0.9415 _exptl_absorpt_process_details 'XPREP (SHELXTL,1997)' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 1.00 0.00 0.0500 0.00 -1.00 0.00 0.0500 0.00 0.00 1.00 0.1000 0.00 0.00 -1.00 0.1000 1.00 0.00 0.00 0.0200 -1.00 0.00 0.00 0.0200 _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 4 sets of \w scans each set at different \f and/or 2\q angles and each scan (25s exposure) covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 120(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 SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 41366 _diffrn_reflns_av_R_equivalents 0.0920 _diffrn_reflns_av_sigmaI/netI 0.0725 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.53 _reflns_number_total 9968 _reflns_number_gt 7181 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SAINT-NT V6.45A (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0130P)^2^+13.7661P] 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 9968 _refine_ls_number_parameters 435 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.0945 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _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 C1 C 0.3243(3) 0.1657(2) 0.7570(2) 0.0148(10) Uani 1 1 d . . . H1A H 0.2635 0.1671 0.7896 0.018 Uiso 1 1 calc R . . H1B H 0.2994 0.1908 0.7133 0.018 Uiso 1 1 calc R . . P1 P 0.35808(9) 0.07371(6) 0.73712(6) 0.0133(2) Uani 1 1 d . . . C111 C 0.3695(3) 0.0236(2) 0.8176(2) 0.0147(9) Uani 1 1 d . . . C112 C 0.4296(4) -0.0400(2) 0.8197(3) 0.0163(10) Uani 1 1 d . . . H112 H 0.4608 -0.0575 0.7784 0.020 Uiso 1 1 calc R . . C113 C 0.4434(4) -0.0774(3) 0.8821(3) 0.0225(11) Uani 1 1 d . . . H113 H 0.4847 -0.1203 0.8836 0.027 Uiso 1 1 calc R . . C114 C 0.3972(4) -0.0525(3) 0.9425(3) 0.0257(12) Uani 1 1 d . . . H114 H 0.4071 -0.0784 0.9851 0.031 Uiso 1 1 calc R . . C115 C 0.3362(4) 0.0106(3) 0.9404(3) 0.0264(12) Uani 1 1 d . . . H115 H 0.3048 0.0276 0.9817 0.032 Uiso 1 1 calc R . . C116 C 0.3213(4) 0.0484(2) 0.8782(3) 0.0184(10) Uani 1 1 d . . . H116 H 0.2788 0.0909 0.8767 0.022 Uiso 1 1 calc R . . C121 C 0.2588(4) 0.0365(2) 0.6740(2) 0.0146(9) Uani 1 1 d . . . C122 C 0.2922(4) -0.0216(3) 0.6348(3) 0.0215(11) Uani 1 1 d . . . H122 H 0.3664 -0.0379 0.6393 0.026 Uiso 1 1 calc R . . C123 C 0.2150(4) -0.0554(3) 0.5890(3) 0.0266(12) Uani 1 1 d . . . H123 H 0.2368 -0.0949 0.5620 0.032 Uiso 1 1 calc R . . C124 C 0.1072(4) -0.0315(3) 0.5829(3) 0.0287(12) Uani 1 1 d . . . H124 H 0.0550 -0.0551 0.5519 0.034 Uiso 1 1 calc R . . C125 C 0.0743(4) 0.0266(3) 0.6215(3) 0.0253(12) Uani 1 1 d . . . H125 H 0.0003 0.0433 0.6160 0.030 Uiso 1 1 calc R . . C126 C 0.1492(4) 0.0602(3) 0.6678(3) 0.0208(11) Uani 1 1 d . . . H126 H 0.1264 0.0991 0.6953 0.025 Uiso 1 1 calc R . . P2 P 0.52217(9) 0.07504(6) 0.69561(6) 0.0147(2) Uani 1 1 d . . . C21 C 0.4926(4) 0.1369(3) 0.6209(2) 0.0181(10) Uani 1 1 d . . . H21A H 0.4358 0.1157 0.5880 0.022 Uiso 1 1 calc R . . H21B H 0.4627 0.1820 0.6387 0.022 Uiso 1 1 calc R . . C22 C 0.5965(4) 0.1524(3) 0.5818(3) 0.0287(12) Uani 1 1 d . . . H22A H 0.5768 0.1804 0.5396 0.043 Uiso 1 1 calc R . . H22B H 0.6305 0.1076 0.5683 0.043 Uiso 1 1 calc R . . H22C H 0.6490 0.1794 0.6125 0.043 Uiso 1 1 calc R . . P3 P 0.59953(9) 0.14961(6) 0.77368(6) 0.0140(2) Uani 1 1 d . . . C31 C 0.6288(4) 0.0914(2) 0.8518(2) 0.0158(10) Uani 1 1 d . . . H31A H 0.6632 0.1198 0.8909 0.019 Uiso 1 1 calc R . . H31B H 0.5590 0.0709 0.8674 0.019 Uiso 1 1 calc R . . C32 C 0.7077(4) 0.0312(3) 0.8320(3) 0.0245(11) Uani 1 1 d . . . H32A H 0.7305 0.0040 0.8741 0.037 Uiso 1 1 calc R . . H32B H 0.7730 0.0517 0.8116 0.037 Uiso 1 1 calc R . . H32C H 0.6697 -0.0003 0.7976 0.037 Uiso 1 1 calc R . . P4 P 0.44754(9) 0.20988(6) 0.79745(6) 0.0123(2) Uani 1 1 d . . . C411 C 0.4312(4) 0.2239(2) 0.8897(2) 0.0156(10) Uani 1 1 d . . . C412 C 0.3266(4) 0.2313(3) 0.9162(3) 0.0218(10) Uani 1 1 d . . . H412 H 0.2619 0.2255 0.8862 0.026 Uiso 1 1 calc R . . C413 C 0.3182(4) 0.2472(3) 0.9867(3) 0.0265(12) Uani 1 1 d . . . H413 H 0.2473 0.2524 1.0049 0.032 Uiso 1 1 calc R . . C414 C 0.4121(4) 0.2554(3) 1.0309(3) 0.0270(12) Uani 1 1 d . . . H414 H 0.4053 0.2651 1.0793 0.032 Uiso 1 1 calc R . . C415 C 0.5159(4) 0.2495(3) 1.0043(3) 0.0227(11) Uani 1 1 d . . . H415 H 0.5801 0.2559 1.0344 0.027 Uiso 1 1 calc R . . C416 C 0.5262(4) 0.2342(3) 0.9336(2) 0.0201(10) Uani 1 1 d . . . H416 H 0.5973 0.2307 0.9152 0.024 Uiso 1 1 calc R . . C421 C 0.4576(4) 0.2959(2) 0.7570(2) 0.0144(10) Uani 1 1 d . . . C422 C 0.3617(4) 0.3356(3) 0.7412(3) 0.0228(11) Uani 1 1 d . . . H422 H 0.2909 0.3160 0.7482 0.027 Uiso 1 1 calc R . . C423 C 0.3718(4) 0.4042(3) 0.7152(3) 0.0287(13) Uani 1 1 d . . . H423 H 0.3071 0.4309 0.7028 0.034 Uiso 1 1 calc R . . C424 C 0.4738(4) 0.4343(3) 0.7071(3) 0.0251(11) Uani 1 1 d . . . H424 H 0.4794 0.4818 0.6908 0.030 Uiso 1 1 calc R . . C425 C 0.5686(4) 0.3946(3) 0.7231(3) 0.0261(12) Uani 1 1 d . . . H425 H 0.6391 0.4150 0.7169 0.031 Uiso 1 1 calc R . . C426 C 0.5614(4) 0.3257(3) 0.7479(3) 0.0210(11) Uani 1 1 d . . . H426 H 0.6266 0.2989 0.7586 0.025 Uiso 1 1 calc R . . Sn1 Sn 0.45746(2) 0.261879(17) 0.273094(18) 0.01425(8) Uani 1 1 d . . . Cl1 Cl 0.35146(10) 0.16770(7) 0.21496(8) 0.0316(3) Uani 1 1 d . . . Cl2 Cl 0.31746(9) 0.26801(7) 0.36048(6) 0.0206(2) Uani 1 1 d . . . Cl3 Cl 0.56322(9) 0.35724(6) 0.33477(6) 0.0203(3) Uani 1 1 d . . . Cl4 Cl 0.59755(9) 0.25107(6) 0.18647(6) 0.0214(3) Uani 1 1 d . . . Cl5 Cl 0.36475(9) 0.35234(7) 0.20191(6) 0.0222(3) Uani 1 1 d . . . Cl6 Cl 0.56023(11) 0.17774(7) 0.34703(8) 0.0344(3) Uani 1 1 d . . . C1S C 0.2977(4) 0.0851(3) 0.4120(3) 0.0302(13) Uani 1 1 d . . . H1SA H 0.3170 0.1238 0.3788 0.036 Uiso 1 1 calc R . . Cl1S Cl 0.42078(11) 0.04972(8) 0.45181(7) 0.0332(3) Uani 1 1 d . . . Cl2S Cl 0.22478(12) 0.01804(9) 0.36450(8) 0.0431(4) Uani 1 1 d . . . Cl3S Cl 0.21591(15) 0.12118(8) 0.47680(10) 0.0525(5) Uani 1 1 d . . . C2S C 0.4468(5) 0.3492(3) 0.5012(3) 0.0453(16) Uani 1 1 d . . . H2SA H 0.4537 0.3239 0.4555 0.054 Uiso 1 1 calc R . . Cl4S Cl 0.39651(15) 0.43392(10) 0.48418(11) 0.0612(5) Uani 1 1 d . . . Cl5S Cl 0.57794(18) 0.35358(13) 0.54516(12) 0.0873(8) Uani 1 1 d . . . Cl6S Cl 0.3535(2) 0.30170(12) 0.55178(10) 0.0783(7) Uani 1 1 d . . . 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 C1 0.013(2) 0.013(2) 0.018(3) -0.0008(19) -0.0008(18) -0.0005(17) P1 0.0116(5) 0.0131(6) 0.0155(6) -0.0023(5) 0.0011(5) -0.0002(4) C111 0.009(2) 0.016(2) 0.019(2) 0.002(2) 0.0004(18) -0.0037(17) C112 0.014(2) 0.015(2) 0.019(3) -0.0014(19) 0.0002(18) -0.0006(18) C113 0.022(2) 0.018(3) 0.028(3) 0.000(2) 0.002(2) 0.000(2) C114 0.035(3) 0.019(3) 0.024(3) 0.006(2) 0.007(2) -0.002(2) C115 0.035(3) 0.027(3) 0.018(3) 0.000(2) 0.008(2) 0.001(2) C116 0.017(2) 0.016(2) 0.022(3) -0.001(2) 0.005(2) 0.0029(18) C121 0.016(2) 0.016(2) 0.011(2) 0.0008(18) -0.0015(18) -0.0040(18) C122 0.019(2) 0.020(3) 0.025(3) -0.002(2) -0.001(2) 0.004(2) C123 0.030(3) 0.025(3) 0.024(3) -0.011(2) -0.005(2) 0.001(2) C124 0.025(3) 0.028(3) 0.032(3) -0.009(2) -0.005(2) -0.009(2) C125 0.018(2) 0.028(3) 0.029(3) -0.005(2) 0.001(2) -0.003(2) C126 0.015(2) 0.023(3) 0.024(3) -0.005(2) -0.001(2) 0.0006(19) P2 0.0128(5) 0.0163(6) 0.0153(6) -0.0013(5) 0.0023(5) 0.0007(5) C21 0.018(2) 0.021(3) 0.015(2) 0.000(2) 0.0002(19) -0.0010(19) C22 0.030(3) 0.032(3) 0.025(3) 0.009(2) 0.004(2) -0.005(2) P3 0.0106(5) 0.0149(6) 0.0163(6) -0.0010(5) 0.0003(5) 0.0001(4) C31 0.015(2) 0.020(2) 0.013(2) 0.0010(19) -0.0003(18) 0.0009(18) C32 0.024(3) 0.020(3) 0.029(3) 0.002(2) -0.005(2) 0.005(2) P4 0.0110(5) 0.0125(6) 0.0135(6) -0.0021(5) 0.0011(4) -0.0004(4) C411 0.019(2) 0.013(2) 0.015(2) -0.0035(18) 0.0023(18) -0.0002(17) C412 0.021(2) 0.021(3) 0.023(3) -0.006(2) 0.000(2) -0.002(2) C413 0.022(2) 0.027(3) 0.032(3) -0.005(2) 0.010(2) 0.000(2) C414 0.033(3) 0.032(3) 0.017(3) -0.010(2) 0.009(2) -0.003(2) C415 0.024(2) 0.025(3) 0.019(3) -0.005(2) -0.003(2) -0.002(2) C416 0.012(2) 0.028(3) 0.021(3) -0.001(2) 0.0016(18) 0.000(2) C421 0.014(2) 0.012(2) 0.017(3) -0.0050(18) 0.0036(19) 0.0004(18) C422 0.016(2) 0.017(3) 0.036(3) -0.004(2) 0.001(2) 0.0016(19) C423 0.027(3) 0.021(3) 0.038(3) -0.004(2) 0.000(2) 0.009(2) C424 0.029(3) 0.016(3) 0.030(3) 0.004(2) 0.003(2) 0.000(2) C425 0.019(3) 0.025(3) 0.035(3) 0.003(2) 0.006(2) -0.004(2) C426 0.018(2) 0.020(3) 0.025(3) 0.006(2) 0.001(2) 0.0032(19) Sn1 0.01075(14) 0.01283(15) 0.01935(17) -0.00018(14) 0.00231(11) 0.00055(13) Cl1 0.0193(6) 0.0269(7) 0.0495(9) -0.0180(6) 0.0100(6) -0.0081(5) Cl2 0.0185(5) 0.0227(6) 0.0211(6) 0.0028(5) 0.0051(5) 0.0025(5) Cl3 0.0169(5) 0.0238(6) 0.0202(6) -0.0043(5) 0.0017(5) -0.0031(5) Cl4 0.0134(5) 0.0254(7) 0.0257(7) -0.0084(5) 0.0048(5) -0.0035(4) Cl5 0.0179(6) 0.0282(7) 0.0205(6) 0.0054(5) 0.0018(5) 0.0059(5) Cl6 0.0291(7) 0.0272(7) 0.0469(9) 0.0136(6) 0.0020(6) 0.0101(6) C1S 0.031(3) 0.024(3) 0.036(3) 0.004(2) 0.011(3) 0.001(2) Cl1S 0.0298(7) 0.0390(8) 0.0304(8) -0.0058(6) -0.0021(6) -0.0004(6) Cl2S 0.0266(7) 0.0588(10) 0.0430(9) -0.0065(8) -0.0057(6) -0.0009(7) Cl3S 0.0602(10) 0.0341(8) 0.0668(12) -0.0021(8) 0.0356(9) 0.0137(8) C2S 0.055(4) 0.048(4) 0.032(4) -0.006(3) -0.004(3) 0.019(3) Cl4S 0.0517(10) 0.0466(10) 0.0848(15) 0.0103(10) -0.0017(10) 0.0179(8) Cl5S 0.0785(14) 0.1062(18) 0.0719(14) -0.0505(13) -0.0439(12) 0.0589(13) Cl6S 0.133(2) 0.0655(14) 0.0373(11) 0.0107(9) 0.0146(12) 0.0070(13) _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 C1 P1 1.822(4) . ? C1 P4 1.841(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? P1 C121 1.797(5) . ? P1 C111 1.801(5) . ? P1 P2 2.1814(16) . ? C111 C112 1.401(6) . ? C111 C116 1.403(6) . ? C112 C113 1.384(7) . ? C112 H112 0.9500 . ? C113 C114 1.390(7) . ? C113 H113 0.9500 . ? C114 C115 1.397(7) . ? C114 H114 0.9500 . ? C115 C116 1.386(7) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C122 1.395(6) . ? C121 C126 1.400(6) . ? C122 C123 1.397(7) . ? C122 H122 0.9500 . ? C123 C124 1.381(7) . ? C123 H123 0.9500 . ? C124 C125 1.388(7) . ? C124 H124 0.9500 . ? C125 C126 1.385(7) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? P2 C21 1.859(5) . ? P2 P3 2.2154(17) . ? C21 C22 1.527(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? P3 C31 1.867(5) . ? P3 P4 2.2310(16) . ? C31 C32 1.543(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? P4 C421 1.799(5) . ? P4 C411 1.801(5) . ? C411 C412 1.398(6) . ? C411 C416 1.399(6) . ? C412 C413 1.387(7) . ? C412 H412 0.9500 . ? C413 C414 1.387(7) . ? C413 H413 0.9500 . ? C414 C415 1.387(7) . ? C414 H414 0.9500 . ? C415 C416 1.391(7) . ? C415 H415 0.9500 . ? C416 H416 0.9500 . ? C421 C426 1.397(6) . ? C421 C422 1.400(6) . ? C422 C423 1.391(7) . ? C422 H422 0.9500 . ? C423 C424 1.376(7) . ? C423 H423 0.9500 . ? C424 C425 1.390(7) . ? C424 H424 0.9500 . ? C425 C426 1.383(7) . ? C425 H425 0.9500 . ? C426 H426 0.9500 . ? Sn1 Cl5 2.4146(12) . ? Sn1 Cl6 2.4183(14) . ? Sn1 Cl1 2.4204(13) . ? Sn1 Cl4 2.4427(12) . ? Sn1 Cl2 2.4467(12) . ? Sn1 Cl3 2.4647(12) . ? C1S Cl2S 1.761(6) . ? C1S Cl3S 1.763(5) . ? C1S Cl1S 1.766(6) . ? C1S H1SA 1.0000 . ? C2S Cl4S 1.730(6) . ? C2S Cl5S 1.758(7) . ? C2S Cl6S 1.769(7) . ? C2S H2SA 1.0000 . ? 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 P1 C1 P4 109.2(2) . . ? P1 C1 H1A 109.8 . . ? P4 C1 H1A 109.8 . . ? P1 C1 H1B 109.8 . . ? P4 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? C121 P1 C111 112.6(2) . . ? C121 P1 C1 111.1(2) . . ? C111 P1 C1 109.1(2) . . ? C121 P1 P2 110.56(16) . . ? C111 P1 P2 106.69(15) . . ? C1 P1 P2 106.55(15) . . ? C112 C111 C116 120.1(4) . . ? C112 C111 P1 119.1(4) . . ? C116 C111 P1 120.9(3) . . ? C113 C112 C111 119.6(4) . . ? C113 C112 H112 120.2 . . ? C111 C112 H112 120.2 . . ? C112 C113 C114 120.5(5) . . ? C112 C113 H113 119.7 . . ? C114 C113 H113 119.7 . . ? C113 C114 C115 120.0(5) . . ? C113 C114 H114 120.0 . . ? C115 C114 H114 120.0 . . ? C116 C115 C114 120.2(5) . . ? C116 C115 H115 119.9 . . ? C114 C115 H115 119.9 . . ? C115 C116 C111 119.6(4) . . ? C115 C116 H116 120.2 . . ? C111 C116 H116 120.2 . . ? C122 C121 C126 120.5(4) . . ? C122 C121 P1 117.4(3) . . ? C126 C121 P1 121.9(4) . . ? C121 C122 C123 119.1(4) . . ? C121 C122 H122 120.4 . . ? C123 C122 H122 120.4 . . ? C124 C123 C122 120.2(5) . . ? C124 C123 H123 119.9 . . ? C122 C123 H123 119.9 . . ? C123 C124 C125 120.6(5) . . ? C123 C124 H124 119.7 . . ? C125 C124 H124 119.7 . . ? C126 C125 C124 120.0(5) . . ? C126 C125 H125 120.0 . . ? C124 C125 H125 120.0 . . ? C125 C126 C121 119.6(5) . . ? C125 C126 H126 120.2 . . ? C121 C126 H126 120.2 . . ? C21 P2 P1 98.31(15) . . ? C21 P2 P3 100.11(16) . . ? P1 P2 P3 97.10(6) . . ? C22 C21 P2 111.4(3) . . ? C22 C21 H21A 109.4 . . ? P2 C21 H21A 109.4 . . ? C22 C21 H21B 109.4 . . ? P2 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C31 P3 P2 102.71(16) . . ? C31 P3 P4 104.95(15) . . ? P2 P3 P4 97.74(6) . . ? C32 C31 P3 109.1(3) . . ? C32 C31 H31A 109.9 . . ? P3 C31 H31A 109.9 . . ? C32 C31 H31B 109.9 . . ? P3 C31 H31B 109.9 . . ? H31A C31 H31B 108.3 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C421 P4 C411 107.5(2) . . ? C421 P4 C1 107.4(2) . . ? C411 P4 C1 110.2(2) . . ? C421 P4 P3 107.03(15) . . ? C411 P4 P3 114.22(16) . . ? C1 P4 P3 110.22(15) . . ? C412 C411 C416 120.2(4) . . ? C412 C411 P4 121.3(4) . . ? C416 C411 P4 118.2(3) . . ? C413 C412 C411 119.3(5) . . ? C413 C412 H412 120.4 . . ? C411 C412 H412 120.4 . . ? C412 C413 C414 120.8(4) . . ? C412 C413 H413 119.6 . . ? C414 C413 H413 119.6 . . ? C415 C414 C413 119.9(5) . . ? C415 C414 H414 120.0 . . ? C413 C414 H414 120.0 . . ? C414 C415 C416 120.3(5) . . ? C414 C415 H415 119.9 . . ? C416 C415 H415 119.9 . . ? C415 C416 C411 119.5(4) . . ? C415 C416 H416 120.2 . . ? C411 C416 H416 120.2 . . ? C426 C421 C422 120.1(4) . . ? C426 C421 P4 119.8(3) . . ? C422 C421 P4 119.7(3) . . ? C423 C422 C421 118.9(4) . . ? C423 C422 H422 120.6 . . ? C421 C422 H422 120.6 . . ? C424 C423 C422 121.3(5) . . ? C424 C423 H423 119.4 . . ? C422 C423 H423 119.4 . . ? C423 C424 C425 119.4(5) . . ? C423 C424 H424 120.3 . . ? C425 C424 H424 120.3 . . ? C426 C425 C424 120.7(4) . . ? C426 C425 H425 119.6 . . ? C424 C425 H425 119.6 . . ? C425 C426 C421 119.5(4) . . ? C425 C426 H426 120.2 . . ? C421 C426 H426 120.2 . . ? Cl5 Sn1 Cl6 175.82(5) . . ? Cl5 Sn1 Cl1 92.25(5) . . ? Cl6 Sn1 Cl1 91.81(5) . . ? Cl5 Sn1 Cl4 89.86(4) . . ? Cl6 Sn1 Cl4 89.15(5) . . ? Cl1 Sn1 Cl4 90.03(4) . . ? Cl5 Sn1 Cl2 91.78(4) . . ? Cl6 Sn1 Cl2 89.31(5) . . ? Cl1 Sn1 Cl2 88.62(4) . . ? Cl4 Sn1 Cl2 177.91(4) . . ? Cl5 Sn1 Cl3 88.24(4) . . ? Cl6 Sn1 Cl3 87.72(5) . . ? Cl1 Sn1 Cl3 178.69(5) . . ? Cl4 Sn1 Cl3 91.19(4) . . ? Cl2 Sn1 Cl3 90.15(4) . . ? Cl2S C1S Cl3S 110.5(3) . . ? Cl2S C1S Cl1S 109.8(3) . . ? Cl3S C1S Cl1S 109.7(3) . . ? Cl2S C1S H1SA 108.9 . . ? Cl3S C1S H1SA 108.9 . . ? Cl1S C1S H1SA 108.9 . . ? Cl4S C2S Cl5S 110.3(4) . . ? Cl4S C2S Cl6S 109.7(3) . . ? Cl5S C2S Cl6S 110.6(4) . . ? Cl4S C2S H2SA 108.7 . . ? Cl5S C2S H2SA 108.7 . . ? Cl6S C2S H2SA 108.7 . . ? 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 P4 C1 P1 C121 -161.6(2) . . . . ? P4 C1 P1 C111 73.7(3) . . . . ? P4 C1 P1 P2 -41.1(3) . . . . ? C121 P1 C111 C112 77.6(4) . . . . ? C1 P1 C111 C112 -158.6(3) . . . . ? P2 P1 C111 C112 -43.9(4) . . . . ? C121 P1 C111 C116 -103.9(4) . . . . ? C1 P1 C111 C116 19.9(4) . . . . ? P2 P1 C111 C116 134.6(3) . . . . ? C116 C111 C112 C113 -1.5(7) . . . . ? P1 C111 C112 C113 177.0(4) . . . . ? C111 C112 C113 C114 0.6(7) . . . . ? C112 C113 C114 C115 0.1(8) . . . . ? C113 C114 C115 C116 0.2(8) . . . . ? C114 C115 C116 C111 -1.1(8) . . . . ? C112 C111 C116 C115 1.8(7) . . . . ? P1 C111 C116 C115 -176.7(4) . . . . ? C111 P1 C121 C122 -80.1(4) . . . . ? C1 P1 C121 C122 157.2(4) . . . . ? P2 P1 C121 C122 39.1(4) . . . . ? C111 P1 C121 C126 94.5(4) . . . . ? C1 P1 C121 C126 -28.1(5) . . . . ? P2 P1 C121 C126 -146.2(4) . . . . ? C126 C121 C122 C123 0.5(7) . . . . ? P1 C121 C122 C123 175.2(4) . . . . ? C121 C122 C123 C124 -0.1(8) . . . . ? C122 C123 C124 C125 0.6(8) . . . . ? C123 C124 C125 C126 -1.5(8) . . . . ? C124 C125 C126 C121 1.8(8) . . . . ? C122 C121 C126 C125 -1.3(7) . . . . ? P1 C121 C126 C125 -175.9(4) . . . . ? C121 P1 P2 C21 63.5(2) . . . . ? C111 P1 P2 C21 -173.8(2) . . . . ? C1 P1 P2 C21 -57.4(2) . . . . ? C121 P1 P2 P3 164.81(17) . . . . ? C111 P1 P2 P3 -72.41(17) . . . . ? C1 P1 P2 P3 44.01(17) . . . . ? P1 P2 C21 C22 177.0(3) . . . . ? P3 P2 C21 C22 78.2(4) . . . . ? C21 P2 P3 C31 178.7(2) . . . . ? P1 P2 P3 C31 78.87(15) . . . . ? C21 P2 P3 P4 71.35(15) . . . . ? P1 P2 P3 P4 -28.45(7) . . . . ? P2 P3 C31 C32 60.3(3) . . . . ? P4 P3 C31 C32 162.0(3) . . . . ? P1 C1 P4 C421 135.6(2) . . . . ? P1 C1 P4 C411 -107.6(3) . . . . ? P1 C1 P4 P3 19.4(3) . . . . ? C31 P3 P4 C421 147.5(2) . . . . ? P2 P3 P4 C421 -107.05(16) . . . . ? C31 P3 P4 C411 28.7(2) . . . . ? P2 P3 P4 C411 134.09(17) . . . . ? C31 P3 P4 C1 -96.0(2) . . . . ? P2 P3 P4 C1 9.44(17) . . . . ? C421 P4 C411 C412 89.6(4) . . . . ? C1 P4 C411 C412 -27.1(5) . . . . ? P3 P4 C411 C412 -151.8(3) . . . . ? C421 P4 C411 C416 -84.4(4) . . . . ? C1 P4 C411 C416 158.9(4) . . . . ? P3 P4 C411 C416 34.2(4) . . . . ? C416 C411 C412 C413 -1.5(7) . . . . ? P4 C411 C412 C413 -175.4(4) . . . . ? C411 C412 C413 C414 -0.3(8) . . . . ? C412 C413 C414 C415 1.6(8) . . . . ? C413 C414 C415 C416 -1.0(8) . . . . ? C414 C415 C416 C411 -0.8(8) . . . . ? C412 C411 C416 C415 2.1(7) . . . . ? P4 C411 C416 C415 176.1(4) . . . . ? C411 P4 C421 C426 94.3(4) . . . . ? C1 P4 C421 C426 -147.2(4) . . . . ? P3 P4 C421 C426 -28.8(4) . . . . ? C411 P4 C421 C422 -79.4(4) . . . . ? C1 P4 C421 C422 39.2(4) . . . . ? P3 P4 C421 C422 157.5(4) . . . . ? C426 C421 C422 C423 1.3(7) . . . . ? P4 C421 C422 C423 174.9(4) . . . . ? C421 C422 C423 C424 -2.3(8) . . . . ? C422 C423 C424 C425 2.1(8) . . . . ? C423 C424 C425 C426 -0.9(8) . . . . ? C424 C425 C426 C421 0.0(8) . . . . ? C422 C421 C426 C425 -0.1(7) . . . . ? P4 C421 C426 C425 -173.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.995 _refine_diff_density_min -1.021 _refine_diff_density_rms 0.124 #============================================================================== data_3c _database_code_depnum_ccdc_archive 'CCDC 626261' #============================================================================== _chemical_name_systematic ; . ; _chemical_name_common . _chemical_melting_point 'not measured' _chemical_formula_moiety 'C40 H38 P4, Sn1 Cl5, 0.5(Sn1 Cl6), 4(C H Cl3)' _chemical_formula_sum 'C44 H42 Cl20 P4 Sn1.50' _chemical_formula_weight 1581.69 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4942(4) _cell_length_b 14.1464(5) _cell_length_c 17.8670(6) _cell_angle_alpha 100.565(1) _cell_angle_beta 93.135(1) _cell_angle_gamma 111.495(1) _cell_volume 3091.88(18) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5325 _cell_measurement_theta_min 2.167 _cell_measurement_theta_max 27.319 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1562 _exptl_absorpt_coefficient_mu 1.610 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6581 _exptl_absorpt_correction_T_max 0.9363 _exptl_absorpt_process_details 'XPREP (SHELXTL,1997)' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 0.00 0.0200 -1.00 0.00 0.00 0.0200 0.00 1.00 0.00 0.2000 0.00 -1.00 0.00 0.2000 0.00 0.00 1.00 0.0400 0.00 0.00 -1.00 0.0400 _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 4 sets of \w scans each set at different \f and/or 2\q angles and each scan covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 120(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 SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 30280 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.1169 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.49 _reflns_number_total 14021 _reflns_number_gt 8000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SAINT-NT V6.45A (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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. The large peak of residual density (5 e/\%A^3^) is close to Sn2 and is caused by a small amount of disorder (less than 10%) in the SnCl~5~^-^ counter ion; efforts to model this were unsuccessful. ; _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^)+(0.0976P)^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 14021 _refine_ls_number_parameters 628 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1152 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1764 _refine_ls_wR_factor_gt 0.1583 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.916 _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 0.80261(13) 0.05985(12) 0.17197(9) 0.0151(3) Uani 1 1 d . . . C11 C 0.9460(5) 0.1219(5) 0.2064(3) 0.0144(12) Uani 1 1 d . . . C12 C 0.9935(5) 0.0715(5) 0.2482(4) 0.0189(13) Uani 1 1 d . . . H12A H 0.9502 0.0091 0.2621 0.023 Uiso 1 1 calc R . . C13 C 1.1035(5) 0.1124(5) 0.2691(4) 0.0212(14) Uani 1 1 d . . . H13A H 1.1351 0.0788 0.2986 0.025 Uiso 1 1 calc R . . C14 C 1.1678(5) 0.2011(5) 0.2478(4) 0.0216(14) Uani 1 1 d . . . H14A H 1.2435 0.2278 0.2616 0.026 Uiso 1 1 calc R . . C15 C 1.1217(5) 0.2518(5) 0.2058(4) 0.0203(14) Uani 1 1 d . . . H15A H 1.1662 0.3121 0.1898 0.024 Uiso 1 1 calc R . . C16 C 1.0107(5) 0.2146(5) 0.1872(3) 0.0162(13) Uani 1 1 d . . . C111 C 0.7476(5) -0.0640(5) 0.1976(4) 0.0198(14) Uani 1 1 d . . . C112 C 0.7531(5) -0.0688(5) 0.2760(4) 0.0220(14) Uani 1 1 d . . . H11A H 0.7898 -0.0074 0.3145 0.026 Uiso 1 1 calc R . . C113 C 0.7047(6) -0.1637(6) 0.2960(4) 0.0290(17) Uani 1 1 d . . . H11B H 0.7091 -0.1674 0.3486 0.035 Uiso 1 1 calc R . . C114 C 0.6501(6) -0.2529(6) 0.2405(5) 0.0326(18) Uani 1 1 d . . . H11C H 0.6158 -0.3174 0.2548 0.039 Uiso 1 1 calc R . . C115 C 0.6456(6) -0.2480(6) 0.1646(5) 0.0315(17) Uani 1 1 d . . . H11D H 0.6096 -0.3101 0.1265 0.038 Uiso 1 1 calc R . . C116 C 0.6925(5) -0.1537(5) 0.1418(4) 0.0231(15) Uani 1 1 d . . . H11E H 0.6869 -0.1512 0.0890 0.028 Uiso 1 1 calc R . . C121 C 0.7860(6) 0.0398(5) 0.0689(4) 0.0213(14) Uani 1 1 d . . . C122 C 0.8409(6) -0.0134(6) 0.0283(4) 0.0309(17) Uani 1 1 d . . . H12B H 0.8856 -0.0390 0.0543 0.037 Uiso 1 1 calc R . . C123 C 0.8293(7) -0.0287(6) -0.0523(5) 0.041(2) Uani 1 1 d . . . H12C H 0.8647 -0.0665 -0.0817 0.049 Uiso 1 1 calc R . . C124 C 0.7659(7) 0.0118(8) -0.0880(5) 0.050(3) Uani 1 1 d . . . H12D H 0.7576 0.0007 -0.1424 0.060 Uiso 1 1 calc R . . C125 C 0.7153(6) 0.0665(7) -0.0481(4) 0.041(2) Uani 1 1 d . . . H12E H 0.6744 0.0957 -0.0741 0.049 Uiso 1 1 calc R . . C126 C 0.7231(6) 0.0801(6) 0.0312(4) 0.0318(18) Uani 1 1 d . . . H12F H 0.6857 0.1167 0.0596 0.038 Uiso 1 1 calc R . . P2 P 0.71482(14) 0.16028(13) 0.21729(10) 0.0184(4) Uani 1 1 d . . . C21 C 0.5987(5) 0.0657(5) 0.2500(4) 0.0233(15) Uani 1 1 d . . . H21A H 0.6238 0.0233 0.2786 0.028 Uiso 1 1 calc R . . H21B H 0.5648 0.1037 0.2851 0.028 Uiso 1 1 calc R . . C22 C 0.5158(6) -0.0058(6) 0.1811(5) 0.0320(17) Uani 1 1 d . . . H22A H 0.4550 -0.0552 0.1993 0.048 Uiso 1 1 calc R . . H22B H 0.5492 -0.0440 0.1467 0.048 Uiso 1 1 calc R . . H22C H 0.4902 0.0362 0.1532 0.048 Uiso 1 1 calc R . . P3 P 0.82729(13) 0.22518(12) 0.32633(9) 0.0156(3) Uani 1 1 d . . . C31 C 0.7473(5) 0.2718(5) 0.3940(4) 0.0215(14) Uani 1 1 d . . . H31A H 0.7141 0.3128 0.3702 0.026 Uiso 1 1 calc R . . H31B H 0.6891 0.2115 0.4057 0.026 Uiso 1 1 calc R . . C32 C 0.8201(6) 0.3395(6) 0.4683(4) 0.0282(16) Uani 1 1 d . . . H32A H 0.7775 0.3642 0.5038 0.042 Uiso 1 1 calc R . . H32B H 0.8772 0.3994 0.4565 0.042 Uiso 1 1 calc R . . H32C H 0.8521 0.2984 0.4920 0.042 Uiso 1 1 calc R . . P4 P 0.92755(13) 0.36886(12) 0.29072(9) 0.0145(3) Uani 1 1 d . . . C41 C 0.9257(5) 0.3475(5) 0.1869(3) 0.0181(13) Uani 1 1 d . . . C42 C 0.8881(6) 0.4070(5) 0.1472(4) 0.0230(15) Uani 1 1 d . . . H42A H 0.8609 0.4546 0.1741 0.028 Uiso 1 1 calc R . . C43 C 0.8902(6) 0.3966(6) 0.0686(4) 0.0291(17) Uani 1 1 d . . . H43A H 0.8637 0.4364 0.0419 0.035 Uiso 1 1 calc R . . C44 C 0.9307(6) 0.3285(5) 0.0294(4) 0.0277(16) Uani 1 1 d . . . H44A H 0.9313 0.3207 -0.0245 0.033 Uiso 1 1 calc R . . C45 C 0.9704(6) 0.2716(5) 0.0685(4) 0.0223(14) Uani 1 1 d . . . H45A H 1.0013 0.2274 0.0413 0.027 Uiso 1 1 calc R . . C46 C 0.9662(5) 0.2775(5) 0.1472(4) 0.0172(13) Uani 1 1 d . . . C411 C 1.0619(5) 0.4037(5) 0.3360(3) 0.0135(12) Uani 1 1 d . . . C412 C 1.0834(5) 0.3526(5) 0.3907(4) 0.0184(13) Uani 1 1 d . . . H41A H 1.0263 0.2992 0.4055 0.022 Uiso 1 1 calc R . . C413 C 1.1885(5) 0.3801(5) 0.4236(4) 0.0228(15) Uani 1 1 d . . . H41B H 1.2027 0.3454 0.4611 0.027 Uiso 1 1 calc R . . C414 C 1.2710(6) 0.4554(5) 0.4031(4) 0.0257(15) Uani 1 1 d . . . H41C H 1.3426 0.4730 0.4257 0.031 Uiso 1 1 calc R . . C415 C 1.2502(5) 0.5077(5) 0.3479(4) 0.0258(16) Uani 1 1 d . . . H41D H 1.3078 0.5608 0.3333 0.031 Uiso 1 1 calc R . . C416 C 1.1468(5) 0.4818(5) 0.3152(4) 0.0191(14) Uani 1 1 d . . . H41E H 1.1330 0.5174 0.2782 0.023 Uiso 1 1 calc R . . C421 C 0.8835(5) 0.4737(5) 0.3212(3) 0.0164(13) Uani 1 1 d . . . C422 C 0.9536(5) 0.5666(5) 0.3693(4) 0.0195(14) Uani 1 1 d . . . H42B H 1.0245 0.5746 0.3870 0.023 Uiso 1 1 calc R . . C423 C 0.9186(6) 0.6469(5) 0.3911(4) 0.0217(14) Uani 1 1 d . . . H42C H 0.9661 0.7110 0.4230 0.026 Uiso 1 1 calc R . . C424 C 0.8145(6) 0.6341(5) 0.3664(4) 0.0259(16) Uani 1 1 d . . . H42D H 0.7910 0.6895 0.3817 0.031 Uiso 1 1 calc R . . C425 C 0.7451(6) 0.5423(5) 0.3201(4) 0.0258(16) Uani 1 1 d . . . H42E H 0.6739 0.5344 0.3034 0.031 Uiso 1 1 calc R . . C426 C 0.7785(6) 0.4608(5) 0.2976(4) 0.0223(15) Uani 1 1 d . . . H42F H 0.7300 0.3967 0.2664 0.027 Uiso 1 1 calc R . . Sn1 Sn 1.0000 1.0000 0.5000 0.01252(14) Uani 1 2 d S . . Cl1 Cl 0.99120(13) 0.90669(12) 0.36961(9) 0.0188(3) Uani 1 1 d . . . Cl2 Cl 0.82741(13) 0.86920(12) 0.51203(9) 0.0214(3) Uani 1 1 d . . . Cl3 Cl 0.90973(13) 1.10253(12) 0.45449(9) 0.0201(3) Uani 1 1 d . . . Sn2 Sn 0.46055(4) 0.32364(4) 0.13353(3) 0.03109(15) Uani 1 1 d . . . Cl4 Cl 0.4624(2) 0.2306(2) 0.22882(13) 0.0510(6) Uani 1 1 d . . . Cl5 Cl 0.30860(17) 0.30536(17) 0.05455(12) 0.0411(5) Uani 1 1 d . . . Cl6 Cl 0.62272(19) 0.45020(18) 0.12045(14) 0.0524(6) Uani 1 1 d . . . Cl7 Cl 0.48838(17) 0.19063(16) 0.04379(11) 0.0386(5) Uani 1 1 d . . . Cl8 Cl 0.42873(18) 0.44962(17) 0.23042(12) 0.0451(5) Uani 1 1 d . . . C1S C 0.7331(6) 0.0634(6) 0.5955(5) 0.038(2) Uani 1 1 d . . . H1SA H 0.7968 0.0484 0.5799 0.045 Uiso 1 1 calc R . . Cl11 Cl 0.6863(3) 0.0008(3) 0.6696(3) 0.1212(18) Uani 1 1 d . . . Cl12 Cl 0.77219(18) 0.19911(17) 0.62509(13) 0.0472(5) Uani 1 1 d . . . Cl13 Cl 0.6341(2) 0.0176(2) 0.5161(2) 0.0826(11) Uani 1 1 d . . . C2S C 0.5518(6) 0.7262(7) 0.4920(5) 0.038(2) Uani 1 1 d . . . H2SA H 0.6207 0.7886 0.5003 0.046 Uiso 1 1 calc R . . Cl21 Cl 0.56658(18) 0.62301(18) 0.42838(15) 0.0546(6) Uani 1 1 d . . . Cl22 Cl 0.44903(17) 0.75754(17) 0.45416(16) 0.0521(6) Uani 1 1 d . . . Cl23 Cl 0.5261(2) 0.6927(3) 0.58014(16) 0.0709(8) Uani 1 1 d . . . C3S C 0.9421(10) 0.7356(7) 0.1798(6) 0.067(4) Uani 1 1 d . . . H3SA H 0.9142 0.7538 0.2289 0.080 Uiso 1 1 calc R . . Cl31 Cl 1.0432(3) 0.6869(3) 0.19781(18) 0.0928(12) Uani 1 1 d . . . Cl32 Cl 0.8412(2) 0.6438(2) 0.1160(3) 0.136(2) Uani 1 1 d . . . Cl33 Cl 0.9995(3) 0.84776(18) 0.14280(18) 0.0730(9) Uani 1 1 d . . . C4S C 0.6823(7) 0.3945(8) -0.1424(5) 0.047(2) Uani 1 1 d . . . H4SA H 0.6374 0.4343 -0.1535 0.056 Uiso 1 1 calc R . . Cl41 Cl 0.6318(2) 0.3313(3) -0.06980(15) 0.0756(9) Uani 1 1 d . . . Cl42 Cl 0.8138(2) 0.48281(18) -0.11307(13) 0.0505(6) Uani 1 1 d . . . Cl43 Cl 0.6693(3) 0.30204(18) -0.22520(14) 0.0642(7) Uani 1 1 d . . . 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 0.0190(8) 0.0118(8) 0.0138(8) 0.0015(6) -0.0024(6) 0.0061(7) C11 0.020(3) 0.016(3) 0.009(3) 0.000(2) -0.001(2) 0.010(3) C12 0.020(3) 0.017(3) 0.020(3) 0.004(3) 0.004(3) 0.007(3) C13 0.019(3) 0.023(4) 0.025(4) 0.006(3) -0.001(3) 0.013(3) C14 0.019(3) 0.023(4) 0.024(4) 0.005(3) 0.003(3) 0.010(3) C15 0.016(3) 0.015(3) 0.028(4) 0.002(3) 0.006(3) 0.005(3) C16 0.023(3) 0.017(3) 0.012(3) 0.001(2) 0.006(3) 0.012(3) C111 0.017(3) 0.018(3) 0.027(4) 0.006(3) 0.001(3) 0.010(3) C112 0.018(3) 0.027(4) 0.023(4) 0.007(3) 0.000(3) 0.010(3) C113 0.026(4) 0.036(4) 0.036(4) 0.020(4) 0.003(3) 0.019(3) C114 0.024(4) 0.020(4) 0.052(5) 0.017(4) 0.001(4) 0.002(3) C115 0.026(4) 0.016(4) 0.048(5) 0.003(3) -0.004(3) 0.007(3) C116 0.026(4) 0.016(3) 0.027(4) 0.002(3) 0.001(3) 0.010(3) C121 0.026(4) 0.014(3) 0.015(3) 0.002(3) 0.000(3) 0.000(3) C122 0.034(4) 0.023(4) 0.025(4) 0.000(3) 0.006(3) 0.003(3) C123 0.040(5) 0.038(5) 0.027(4) -0.001(4) 0.012(4) -0.002(4) C124 0.039(5) 0.066(6) 0.017(4) 0.010(4) -0.001(4) -0.011(5) C125 0.029(4) 0.055(6) 0.021(4) 0.013(4) -0.010(3) -0.005(4) C126 0.029(4) 0.035(4) 0.022(4) 0.010(3) -0.008(3) 0.002(3) P2 0.0184(9) 0.0159(8) 0.0209(9) 0.0008(7) -0.0052(7) 0.0092(7) C21 0.009(3) 0.024(4) 0.033(4) 0.007(3) 0.000(3) 0.004(3) C22 0.020(4) 0.022(4) 0.042(5) -0.002(3) -0.007(3) 0.001(3) P3 0.0174(8) 0.0133(8) 0.0152(8) 0.0005(6) -0.0018(6) 0.0065(7) C31 0.018(3) 0.020(3) 0.024(4) 0.000(3) 0.006(3) 0.007(3) C32 0.035(4) 0.026(4) 0.022(4) -0.001(3) 0.008(3) 0.011(3) P4 0.0177(8) 0.0118(8) 0.0145(8) 0.0007(6) -0.0018(6) 0.0078(7) C41 0.024(3) 0.020(3) 0.011(3) 0.001(3) 0.000(3) 0.010(3) C42 0.036(4) 0.017(3) 0.018(3) 0.001(3) -0.007(3) 0.015(3) C43 0.041(4) 0.027(4) 0.023(4) 0.010(3) -0.004(3) 0.016(3) C44 0.040(4) 0.027(4) 0.015(3) 0.006(3) -0.002(3) 0.012(3) C45 0.032(4) 0.017(3) 0.019(3) 0.003(3) 0.003(3) 0.011(3) C46 0.014(3) 0.014(3) 0.022(3) 0.005(3) 0.003(3) 0.004(3) C411 0.019(3) 0.011(3) 0.011(3) -0.002(2) 0.002(2) 0.008(3) C412 0.018(3) 0.017(3) 0.021(3) 0.003(3) 0.001(3) 0.009(3) C413 0.022(4) 0.023(4) 0.024(4) 0.006(3) -0.002(3) 0.010(3) C414 0.016(3) 0.023(4) 0.034(4) 0.002(3) -0.003(3) 0.006(3) C415 0.017(3) 0.016(3) 0.039(4) 0.004(3) 0.004(3) 0.002(3) C416 0.022(3) 0.014(3) 0.021(3) 0.006(3) 0.006(3) 0.006(3) C421 0.027(4) 0.011(3) 0.014(3) -0.001(2) -0.001(3) 0.013(3) C422 0.019(3) 0.014(3) 0.023(4) 0.003(3) -0.001(3) 0.006(3) C423 0.032(4) 0.012(3) 0.021(3) 0.001(3) 0.002(3) 0.010(3) C424 0.037(4) 0.019(4) 0.028(4) 0.003(3) 0.007(3) 0.018(3) C425 0.022(4) 0.026(4) 0.031(4) 0.001(3) -0.001(3) 0.015(3) C426 0.027(4) 0.014(3) 0.025(4) -0.002(3) -0.005(3) 0.011(3) Sn1 0.0133(3) 0.0101(3) 0.0153(3) 0.0042(2) -0.0009(2) 0.0055(2) Cl1 0.0244(8) 0.0177(8) 0.0164(7) 0.0035(6) -0.0003(6) 0.0110(7) Cl2 0.0179(8) 0.0160(8) 0.0284(9) 0.0052(7) 0.0037(7) 0.0039(6) Cl3 0.0251(8) 0.0163(8) 0.0215(8) 0.0043(6) -0.0046(6) 0.0119(7) Sn2 0.0304(3) 0.0309(3) 0.0331(3) 0.0032(2) 0.0013(2) 0.0153(2) Cl4 0.0721(16) 0.0669(16) 0.0384(12) 0.0179(11) 0.0134(11) 0.0506(14) Cl5 0.0393(11) 0.0481(12) 0.0371(11) 0.0013(9) -0.0069(9) 0.0236(10) Cl6 0.0449(13) 0.0447(13) 0.0535(14) 0.0071(11) 0.0081(11) 0.0027(11) Cl7 0.0433(12) 0.0384(11) 0.0362(11) 0.0065(9) 0.0090(9) 0.0185(10) Cl8 0.0514(13) 0.0453(12) 0.0404(12) -0.0054(10) 0.0016(10) 0.0283(11) C1S 0.028(4) 0.030(4) 0.062(6) 0.019(4) 0.009(4) 0.014(4) Cl11 0.110(3) 0.164(4) 0.193(4) 0.146(4) 0.117(3) 0.107(3) Cl12 0.0451(13) 0.0385(12) 0.0537(14) -0.0046(10) 0.0008(10) 0.0189(10) Cl13 0.0370(13) 0.0481(15) 0.142(3) -0.0264(16) -0.0366(16) 0.0216(12) C2S 0.023(4) 0.038(5) 0.043(5) -0.009(4) 0.002(4) 0.008(4) Cl21 0.0352(12) 0.0406(12) 0.0769(17) -0.0079(12) 0.0200(11) 0.0099(10) Cl22 0.0292(11) 0.0352(12) 0.0839(18) 0.0059(11) -0.0109(11) 0.0092(9) Cl23 0.0711(19) 0.102(2) 0.0543(16) 0.0211(16) 0.0148(14) 0.0465(18) C3S 0.125(10) 0.037(5) 0.056(6) 0.016(5) 0.063(7) 0.041(6) Cl31 0.108(3) 0.087(2) 0.0605(18) 0.0301(17) -0.0334(18) 0.011(2) Cl32 0.0372(16) 0.0422(16) 0.323(7) 0.024(3) 0.004(3) 0.0179(13) Cl33 0.105(2) 0.0268(12) 0.085(2) 0.0165(13) 0.0424(18) 0.0165(13) C4S 0.043(5) 0.071(7) 0.036(5) 0.016(5) 0.012(4) 0.029(5) Cl41 0.0476(15) 0.130(3) 0.0437(14) 0.0386(16) 0.0135(12) 0.0174(16) Cl42 0.0611(15) 0.0460(13) 0.0397(12) 0.0133(10) 0.0051(11) 0.0137(11) Cl43 0.096(2) 0.0369(13) 0.0450(14) 0.0047(11) 0.0151(14) 0.0107(13) _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 C111 1.791(7) . ? P1 C121 1.799(7) . ? P1 C11 1.822(6) . ? P1 P2 2.235(2) . ? C11 C12 1.397(8) . ? C11 C16 1.400(9) . ? C12 C13 1.382(9) . ? C12 H12A 0.9500 . ? C13 C14 1.374(9) . ? C13 H13A 0.9500 . ? C14 C15 1.392(9) . ? C14 H14A 0.9500 . ? C15 C16 1.390(9) . ? C15 H15A 0.9500 . ? C16 C46 1.497(9) . ? C111 C116 1.387(9) . ? C111 C112 1.413(9) . ? C112 C113 1.385(10) . ? C112 H11A 0.9500 . ? C113 C114 1.378(11) . ? C113 H11B 0.9500 . ? C114 C115 1.370(11) . ? C114 H11C 0.9500 . ? C115 C116 1.397(10) . ? C115 H11D 0.9500 . ? C116 H11E 0.9500 . ? C121 C122 1.382(10) . ? C121 C126 1.390(10) . ? C122 C123 1.408(10) . ? C122 H12B 0.9500 . ? C123 C124 1.378(13) . ? C123 H12C 0.9500 . ? C124 C125 1.346(14) . ? C124 H12D 0.9500 . ? C125 C126 1.387(10) . ? C125 H12E 0.9500 . ? C126 H12F 0.9500 . ? P2 C21 1.854(7) . ? P2 P3 2.223(2) . ? C21 C22 1.534(9) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? P3 C31 1.853(7) . ? P3 P4 2.218(2) . ? C31 C32 1.531(9) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? P4 C411 1.795(6) . ? P4 C421 1.799(6) . ? P4 C41 1.822(6) . ? C41 C42 1.400(9) . ? C41 C46 1.401(9) . ? C42 C43 1.386(9) . ? C42 H42A 0.9500 . ? C43 C44 1.377(10) . ? C43 H43A 0.9500 . ? C44 C45 1.379(9) . ? C44 H44A 0.9500 . ? C45 C46 1.399(9) . ? C45 H45A 0.9500 . ? C411 C416 1.392(9) . ? C411 C412 1.395(8) . ? C412 C413 1.388(9) . ? C412 H41A 0.9500 . ? C413 C414 1.351(10) . ? C413 H41B 0.9500 . ? C414 C415 1.410(10) . ? C414 H41C 0.9500 . ? C415 C416 1.371(9) . ? C415 H41D 0.9500 . ? C416 H41E 0.9500 . ? C421 C426 1.391(9) . ? C421 C422 1.395(9) . ? C422 C423 1.385(9) . ? C422 H42B 0.9500 . ? C423 C424 1.384(10) . ? C423 H42C 0.9500 . ? C424 C425 1.371(10) . ? C424 H42D 0.9500 . ? C425 C426 1.387(9) . ? C425 H42E 0.9500 . ? C426 H42F 0.9500 . ? Sn1 Cl3 2.4224(14) . ? Sn1 Cl3 2.4224(14) 2_776 ? Sn1 Cl1 2.4312(15) . ? Sn1 Cl1 2.4312(15) 2_776 ? Sn1 Cl2 2.4365(16) 2_776 ? Sn1 Cl2 2.4365(16) . ? Sn2 Cl6 2.321(2) . ? Sn2 Cl5 2.329(2) . ? Sn2 Cl4 2.339(2) . ? Sn2 Cl7 2.394(2) . ? Sn2 Cl8 2.422(2) . ? C1S Cl13 1.742(9) . ? C1S Cl11 1.746(9) . ? C1S Cl12 1.761(8) . ? C1S H1SA 1.0000 . ? C2S Cl23 1.742(9) . ? C2S Cl22 1.743(9) . ? C2S Cl21 1.758(8) . ? C2S H2SA 1.0000 . ? C3S Cl32 1.684(13) . ? C3S Cl33 1.759(9) . ? C3S Cl31 1.778(12) . ? C3S H3SA 1.0000 . ? C4S Cl42 1.737(10) . ? C4S Cl43 1.738(9) . ? C4S Cl41 1.739(9) . ? C4S H4SA 1.0000 . ? 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 C111 P1 C121 108.8(3) . . ? C111 P1 C11 109.9(3) . . ? C121 P1 C11 108.0(3) . . ? C111 P1 P2 110.6(2) . . ? C121 P1 P2 107.7(2) . . ? C11 P1 P2 111.8(2) . . ? C12 C11 C16 119.3(6) . . ? C12 C11 P1 119.0(5) . . ? C16 C11 P1 121.5(4) . . ? C13 C12 C11 120.1(6) . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C14 C13 C12 120.8(6) . . ? C14 C13 H13A 119.6 . . ? C12 C13 H13A 119.6 . . ? C13 C14 C15 119.8(6) . . ? C13 C14 H14A 120.1 . . ? C15 C14 H14A 120.1 . . ? C16 C15 C14 120.3(6) . . ? C16 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? C15 C16 C11 119.6(6) . . ? C15 C16 C46 117.4(6) . . ? C11 C16 C46 123.1(6) . . ? C116 C111 C112 119.8(6) . . ? C116 C111 P1 120.5(5) . . ? C112 C111 P1 119.5(5) . . ? C113 C112 C111 119.4(7) . . ? C113 C112 H11A 120.3 . . ? C111 C112 H11A 120.3 . . ? C114 C113 C112 120.7(7) . . ? C114 C113 H11B 119.7 . . ? C112 C113 H11B 119.7 . . ? C115 C114 C113 119.7(7) . . ? C115 C114 H11C 120.2 . . ? C113 C114 H11C 120.2 . . ? C114 C115 C116 121.6(7) . . ? C114 C115 H11D 119.2 . . ? C116 C115 H11D 119.2 . . ? C111 C116 C115 118.8(7) . . ? C111 C116 H11E 120.6 . . ? C115 C116 H11E 120.6 . . ? C122 C121 C126 120.8(7) . . ? C122 C121 P1 118.1(5) . . ? C126 C121 P1 121.1(6) . . ? C121 C122 C123 118.6(8) . . ? C121 C122 H12B 120.7 . . ? C123 C122 H12B 120.7 . . ? C124 C123 C122 119.2(8) . . ? C124 C123 H12C 120.4 . . ? C122 C123 H12C 120.4 . . ? C125 C124 C123 122.0(8) . . ? C125 C124 H12D 119.0 . . ? C123 C124 H12D 119.0 . . ? C124 C125 C126 119.8(8) . . ? C124 C125 H12E 120.1 . . ? C126 C125 H12E 120.1 . . ? C125 C126 C121 119.5(8) . . ? C125 C126 H12F 120.2 . . ? C121 C126 H12F 120.2 . . ? C21 P2 P3 99.8(2) . . ? C21 P2 P1 101.4(2) . . ? P3 P2 P1 91.24(8) . . ? C22 C21 P2 110.5(5) . . ? C22 C21 H21A 109.6 . . ? P2 C21 H21A 109.6 . . ? C22 C21 H21B 109.6 . . ? P2 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C31 P3 P4 102.8(2) . . ? C31 P3 P2 102.5(2) . . ? P4 P3 P2 94.47(9) . . ? C32 C31 P3 109.8(5) . . ? C32 C31 H31A 109.7 . . ? P3 C31 H31A 109.7 . . ? C32 C31 H31B 109.7 . . ? P3 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C411 P4 C421 109.6(3) . . ? C411 P4 C41 109.5(3) . . ? C421 P4 C41 108.1(3) . . ? C411 P4 P3 106.1(2) . . ? C421 P4 P3 111.8(2) . . ? C41 P4 P3 111.7(2) . . ? C42 C41 C46 119.9(6) . . ? C42 C41 P4 118.6(5) . . ? C46 C41 P4 121.4(5) . . ? C43 C42 C41 120.3(6) . . ? C43 C42 H42A 119.8 . . ? C41 C42 H42A 119.8 . . ? C44 C43 C42 120.1(6) . . ? C44 C43 H43A 120.0 . . ? C42 C43 H43A 120.0 . . ? C43 C44 C45 119.9(6) . . ? C43 C44 H44A 120.0 . . ? C45 C44 H44A 120.0 . . ? C44 C45 C46 121.5(6) . . ? C44 C45 H45A 119.2 . . ? C46 C45 H45A 119.2 . . ? C45 C46 C41 118.2(6) . . ? C45 C46 C16 119.6(6) . . ? C41 C46 C16 122.1(6) . . ? C416 C411 C412 119.1(6) . . ? C416 C411 P4 119.7(5) . . ? C412 C411 P4 121.2(5) . . ? C413 C412 C411 119.7(6) . . ? C413 C412 H41A 120.1 . . ? C411 C412 H41A 120.1 . . ? C414 C413 C412 121.1(6) . . ? C414 C413 H41B 119.4 . . ? C412 C413 H41B 119.4 . . ? C413 C414 C415 119.6(6) . . ? C413 C414 H41C 120.2 . . ? C415 C414 H41C 120.2 . . ? C416 C415 C414 120.0(6) . . ? C416 C415 H41D 120.0 . . ? C414 C415 H41D 120.0 . . ? C415 C416 C411 120.4(6) . . ? C415 C416 H41E 119.8 . . ? C411 C416 H41E 119.8 . . ? C426 C421 C422 120.3(6) . . ? C426 C421 P4 119.5(5) . . ? C422 C421 P4 120.2(5) . . ? C423 C422 C421 119.2(6) . . ? C423 C422 H42B 120.4 . . ? C421 C422 H42B 120.4 . . ? C424 C423 C422 120.2(6) . . ? C424 C423 H42C 119.9 . . ? C422 C423 H42C 119.9 . . ? C425 C424 C423 120.6(6) . . ? C425 C424 H42D 119.7 . . ? C423 C424 H42D 119.7 . . ? C424 C425 C426 120.2(6) . . ? C424 C425 H42E 119.9 . . ? C426 C425 H42E 119.9 . . ? C425 C426 C421 119.5(6) . . ? C425 C426 H42F 120.2 . . ? C421 C426 H42F 120.2 . . ? Cl3 Sn1 Cl3 180.00(7) . 2_776 ? Cl3 Sn1 Cl1 91.36(5) . . ? Cl3 Sn1 Cl1 88.64(5) 2_776 . ? Cl3 Sn1 Cl1 88.64(5) . 2_776 ? Cl3 Sn1 Cl1 91.36(5) 2_776 2_776 ? Cl1 Sn1 Cl1 180.000(1) . 2_776 ? Cl3 Sn1 Cl2 89.69(5) . 2_776 ? Cl3 Sn1 Cl2 90.31(5) 2_776 2_776 ? Cl1 Sn1 Cl2 89.79(5) . 2_776 ? Cl1 Sn1 Cl2 90.21(5) 2_776 2_776 ? Cl3 Sn1 Cl2 90.31(5) . . ? Cl3 Sn1 Cl2 89.69(5) 2_776 . ? Cl1 Sn1 Cl2 90.21(5) . . ? Cl1 Sn1 Cl2 89.79(5) 2_776 . ? Cl2 Sn1 Cl2 180.000(1) 2_776 . ? Cl6 Sn2 Cl5 117.23(9) . . ? Cl6 Sn2 Cl4 117.16(10) . . ? Cl5 Sn2 Cl4 125.55(9) . . ? Cl6 Sn2 Cl7 92.76(8) . . ? Cl5 Sn2 Cl7 91.16(7) . . ? Cl4 Sn2 Cl7 88.75(7) . . ? Cl6 Sn2 Cl8 90.05(9) . . ? Cl5 Sn2 Cl8 90.21(8) . . ? Cl4 Sn2 Cl8 87.30(8) . . ? Cl7 Sn2 Cl8 175.89(8) . . ? Cl13 C1S Cl11 110.6(5) . . ? Cl13 C1S Cl12 108.9(4) . . ? Cl11 C1S Cl12 111.3(5) . . ? Cl13 C1S H1SA 108.7 . . ? Cl11 C1S H1SA 108.7 . . ? Cl12 C1S H1SA 108.7 . . ? Cl23 C2S Cl22 110.4(4) . . ? Cl23 C2S Cl21 109.8(5) . . ? Cl22 C2S Cl21 110.9(5) . . ? Cl23 C2S H2SA 108.6 . . ? Cl22 C2S H2SA 108.6 . . ? Cl21 C2S H2SA 108.6 . . ? Cl32 C3S Cl33 110.3(6) . . ? Cl32 C3S Cl31 109.2(5) . . ? Cl33 C3S Cl31 108.4(6) . . ? Cl32 C3S H3SA 109.7 . . ? Cl33 C3S H3SA 109.6 . . ? Cl31 C3S H3SA 109.7 . . ? Cl42 C4S Cl43 113.0(5) . . ? Cl42 C4S Cl41 110.7(5) . . ? Cl43 C4S Cl41 109.1(6) . . ? Cl42 C4S H4SA 108.0 . . ? Cl43 C4S H4SA 108.0 . . ? Cl41 C4S H4SA 108.0 . . ? 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 C111 P1 C11 C12 -1.8(6) . . . . ? C121 P1 C11 C12 -120.4(5) . . . . ? P2 P1 C11 C12 121.3(5) . . . . ? C111 P1 C11 C16 173.3(5) . . . . ? C121 P1 C11 C16 54.8(6) . . . . ? P2 P1 C11 C16 -63.5(5) . . . . ? C16 C11 C12 C13 -0.9(9) . . . . ? P1 C11 C12 C13 174.3(5) . . . . ? C11 C12 C13 C14 -1.7(10) . . . . ? C12 C13 C14 C15 1.3(10) . . . . ? C13 C14 C15 C16 1.7(10) . . . . ? C14 C15 C16 C11 -4.3(9) . . . . ? C14 C15 C16 C46 175.5(6) . . . . ? C12 C11 C16 C15 3.9(9) . . . . ? P1 C11 C16 C15 -171.3(5) . . . . ? C12 C11 C16 C46 -175.9(6) . . . . ? P1 C11 C16 C46 9.0(8) . . . . ? C121 P1 C111 C116 -6.3(6) . . . . ? C11 P1 C111 C116 -124.4(5) . . . . ? P2 P1 C111 C116 111.8(5) . . . . ? C121 P1 C111 C112 178.7(5) . . . . ? C11 P1 C111 C112 60.6(6) . . . . ? P2 P1 C111 C112 -63.2(5) . . . . ? C116 C111 C112 C113 0.9(10) . . . . ? P1 C111 C112 C113 176.0(5) . . . . ? C111 C112 C113 C114 -0.9(10) . . . . ? C112 C113 C114 C115 1.3(11) . . . . ? C113 C114 C115 C116 -1.8(11) . . . . ? C112 C111 C116 C115 -1.4(10) . . . . ? P1 C111 C116 C115 -176.4(5) . . . . ? C114 C115 C116 C111 1.9(11) . . . . ? C111 P1 C121 C122 -65.3(6) . . . . ? C11 P1 C121 C122 54.0(6) . . . . ? P2 P1 C121 C122 174.8(5) . . . . ? C111 P1 C121 C126 117.2(6) . . . . ? C11 P1 C121 C126 -123.6(6) . . . . ? P2 P1 C121 C126 -2.7(6) . . . . ? C126 C121 C122 C123 -1.9(11) . . . . ? P1 C121 C122 C123 -179.5(5) . . . . ? C121 C122 C123 C124 1.6(11) . . . . ? C122 C123 C124 C125 0.6(13) . . . . ? C123 C124 C125 C126 -2.4(13) . . . . ? C124 C125 C126 C121 2.1(12) . . . . ? C122 C121 C126 C125 0.1(11) . . . . ? P1 C121 C126 C125 177.6(6) . . . . ? C111 P1 P2 C21 -10.2(3) . . . . ? C121 P1 P2 C21 108.5(3) . . . . ? C11 P1 P2 C21 -133.0(3) . . . . ? C111 P1 P2 P3 90.0(2) . . . . ? C121 P1 P2 P3 -151.2(2) . . . . ? C11 P1 P2 P3 -32.8(2) . . . . ? P3 P2 C21 C22 -169.3(4) . . . . ? P1 P2 C21 C22 -76.0(5) . . . . ? C21 P2 P3 C31 -55.8(3) . . . . ? P1 P2 P3 C31 -157.6(2) . . . . ? C21 P2 P3 P4 -160.0(2) . . . . ? P1 P2 P3 P4 98.17(9) . . . . ? P4 P3 C31 C32 -70.6(5) . . . . ? P2 P3 C31 C32 -168.3(4) . . . . ? C31 P3 P4 C411 108.2(3) . . . . ? P2 P3 P4 C411 -147.9(2) . . . . ? C31 P3 P4 C421 -11.2(3) . . . . ? P2 P3 P4 C421 92.7(2) . . . . ? C31 P3 P4 C41 -132.6(3) . . . . ? P2 P3 P4 C41 -28.6(2) . . . . ? C411 P4 C41 C42 -122.3(6) . . . . ? C421 P4 C41 C42 -3.0(6) . . . . ? P3 P4 C41 C42 120.4(5) . . . . ? C411 P4 C41 C46 54.2(6) . . . . ? C421 P4 C41 C46 173.5(5) . . . . ? P3 P4 C41 C46 -63.0(6) . . . . ? C46 C41 C42 C43 0.3(10) . . . . ? P4 C41 C42 C43 176.9(6) . . . . ? C41 C42 C43 C44 -0.8(11) . . . . ? C42 C43 C44 C45 -0.8(11) . . . . ? C43 C44 C45 C46 3.0(11) . . . . ? C44 C45 C46 C41 -3.5(10) . . . . ? C44 C45 C46 C16 -179.8(6) . . . . ? C42 C41 C46 C45 1.8(10) . . . . ? P4 C41 C46 C45 -174.7(5) . . . . ? C42 C41 C46 C16 178.0(6) . . . . ? P4 C41 C46 C16 1.5(9) . . . . ? C15 C16 C46 C45 78.3(8) . . . . ? C11 C16 C46 C45 -101.9(7) . . . . ? C15 C16 C46 C41 -97.9(7) . . . . ? C11 C16 C46 C41 81.9(8) . . . . ? C421 P4 C411 C416 -69.0(5) . . . . ? C41 P4 C411 C416 49.4(6) . . . . ? P3 P4 C411 C416 170.1(4) . . . . ? C421 P4 C411 C412 112.2(5) . . . . ? C41 P4 C411 C412 -129.4(5) . . . . ? P3 P4 C411 C412 -8.7(5) . . . . ? C416 C411 C412 C413 0.0(9) . . . . ? P4 C411 C412 C413 178.8(5) . . . . ? C411 C412 C413 C414 -0.4(10) . . . . ? C412 C413 C414 C415 0.5(11) . . . . ? C413 C414 C415 C416 -0.2(11) . . . . ? C414 C415 C416 C411 -0.3(10) . . . . ? C412 C411 C416 C415 0.4(9) . . . . ? P4 C411 C416 C415 -178.4(5) . . . . ? C411 P4 C421 C426 -175.3(5) . . . . ? C41 P4 C421 C426 65.5(6) . . . . ? P3 P4 C421 C426 -57.9(6) . . . . ? C411 P4 C421 C422 3.4(6) . . . . ? C41 P4 C421 C422 -115.9(6) . . . . ? P3 P4 C421 C422 120.8(5) . . . . ? C426 C421 C422 C423 -2.3(10) . . . . ? P4 C421 C422 C423 179.0(5) . . . . ? C421 C422 C423 C424 1.2(10) . . . . ? C422 C423 C424 C425 -0.2(11) . . . . ? C423 C424 C425 C426 0.1(11) . . . . ? C424 C425 C426 C421 -1.2(11) . . . . ? C422 C421 C426 C425 2.3(10) . . . . ? P4 C421 C426 C425 -179.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 5.294 _refine_diff_density_min -2.108 _refine_diff_density_rms 0.167