# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name J.Hoeflemeyer F.Gabbai data_2 _database_code_CSD 199217 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H18 Cl2 Ga N Sn' _chemical_formula_weight 567.69 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' N N 0.0061 0.0033 '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' Ga Ga 0.2307 1.6083 '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 Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 18.926(12) _cell_length_b 9.932(6) _cell_length_c 11.510(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2164(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 2.655 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'CCD area detector' _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 10963 _diffrn_reflns_av_R_equivalents 0.1273 _diffrn_reflns_av_sigmaI/netI 0.1542 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3787 _reflns_number_gt 2373 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0050P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(3) _refine_ls_number_reflns 3787 _refine_ls_number_parameters 253 _refine_ls_number_restraints 127 _refine_ls_R_factor_all 0.1021 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1011 _refine_ls_wR_factor_gt 0.0887 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.000 _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 Sn Sn -0.04129(4) -0.58301(7) -0.63260(9) 0.01599(19) Uani 1 1 d . . . Ga Ga -0.13540(7) -0.73282(12) -0.83336(11) 0.0163(3) Uani 1 1 d . . . Cl2 Cl -0.22025(16) -0.8671(3) -0.9027(3) 0.0245(8) Uani 1 1 d . . . Cl1 Cl -0.14772(14) -0.7530(3) -0.6302(3) 0.0196(6) Uani 1 1 d . . . C1 C 0.0295(7) -0.7285(11) -0.7016(10) 0.019(2) Uani 1 1 d U . . C2 C 0.0914(6) -0.7353(10) -0.6388(13) 0.0213(19) Uani 1 1 d U . . H2A H 0.0972 -0.6790 -0.5749 0.026 Uiso 1 1 calc R . . C3 C 0.1454(7) -0.8237(10) -0.6679(10) 0.025(2) Uani 1 1 d U . . H3A H 0.1870 -0.8250 -0.6250 0.030 Uiso 1 1 calc R . . C4 C 0.1369(7) -0.9094(12) -0.7608(10) 0.023(2) Uani 1 1 d U . . H4A H 0.1726 -0.9696 -0.7800 0.027 Uiso 1 1 calc R . . C5 C 0.0698(7) -0.9935(12) -0.9231(11) 0.024(2) Uani 1 1 d U . . H5A H 0.1077 -1.0485 -0.9432 0.029 Uiso 1 1 calc R . . C6 C 0.0092(7) -0.9980(12) -0.9886(11) 0.023(2) Uani 1 1 d U . . H6A H 0.0058 -1.0546 -1.0528 0.027 Uiso 1 1 calc R . . C7 C -0.0475(7) -0.9151(11) -0.9564(9) 0.021(2) Uani 1 1 d U . . H7A H -0.0891 -0.9218 -0.9991 0.025 Uiso 1 1 calc R . . C8 C -0.0459(7) -0.8244(11) -0.8655(10) 0.019(2) Uani 1 1 d U . . C9 C 0.0193(7) -0.8190(11) -0.7976(10) 0.0174(18) Uani 1 1 d U . . C10 C 0.0760(6) -0.9067(11) -0.8251(11) 0.0209(17) Uani 1 1 d U . . C11 C -0.1008(6) -0.4260(12) -0.7105(11) 0.022(2) Uani 1 1 d U . . C12 C -0.0870(6) -0.3014(10) -0.6525(12) 0.026(2) Uani 1 1 d U . . H22A H -0.0547 -0.2995 -0.5916 0.031 Uiso 1 1 calc R . . C13 C -0.1208(7) -0.1828(12) -0.6852(11) 0.028(2) Uani 1 1 d U . . H23A H -0.1100 -0.1020 -0.6485 0.034 Uiso 1 1 calc R . . C14 C -0.1703(7) -0.1866(12) -0.7721(11) 0.028(3) Uani 1 1 d U . . H24A H -0.1942 -0.1084 -0.7931 0.034 Uiso 1 1 calc R . . C15 C -0.2372(7) -0.3055(12) -0.9216(10) 0.022(2) Uani 1 1 d U . . H25A H -0.2595 -0.2247 -0.9396 0.026 Uiso 1 1 calc R . . C16 C -0.2536(6) -0.4197(11) -0.9809(10) 0.020(2) Uani 1 1 d U . . H26A H -0.2861 -0.4180 -1.0415 0.024 Uiso 1 1 calc R . . C17 C -0.2204(6) -0.5392(11) -0.9486(10) 0.020(2) Uani 1 1 d U . . H27A H -0.2319 -0.6170 -0.9894 0.024 Uiso 1 1 calc R . . C18 C -0.1721(6) -0.5496(11) -0.8611(10) 0.018(2) Uani 1 1 d U . . C19 C -0.1520(6) -0.4300(12) -0.7991(10) 0.019(2) Uani 1 1 d U . . C20 C -0.1852(6) -0.3106(11) -0.8308(12) 0.023(3) Uani 1 1 d . . . C21 C -0.0373(7) -0.5707(14) -0.4474(10) 0.033(3) Uani 1 1 d . . . H40A H -0.0002 -0.5104 -0.4247 0.050 Uiso 1 1 calc R . . H40B H -0.0284 -0.6585 -0.4157 0.050 Uiso 1 1 calc R . . H40C H -0.0817 -0.5377 -0.4186 0.050 Uiso 1 1 calc R . . C23 C 0.1641(6) -0.2837(11) -0.7100(11) 0.0242(19) Uani 1 1 d U . . H42A H 0.1952 -0.2677 -0.6454 0.036 Uiso 1 1 calc R . . H42B H 0.1469 -0.1993 -0.7390 0.036 Uiso 1 1 calc R . . H42C H 0.1895 -0.3296 -0.7704 0.036 Uiso 1 1 calc R . . C22 C 0.1043(7) -0.3671(11) -0.6719(10) 0.0237(19) Uani 1 1 d U . . N N 0.0593(4) -0.4305(8) -0.6440(12) 0.0234(19) Uani 1 1 d U . . 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 Sn 0.0177(4) 0.0192(4) 0.0111(3) -0.0008(5) -0.0005(6) 0.0022(4) Ga 0.0168(7) 0.0167(7) 0.0155(7) 0.0006(7) -0.0009(7) -0.0007(7) Cl2 0.0243(19) 0.0221(17) 0.027(2) 0.0006(15) -0.0035(16) -0.0034(16) Cl1 0.0207(16) 0.0241(14) 0.0141(14) 0.007(2) 0.0033(19) -0.0003(13) C1 0.021(4) 0.019(4) 0.018(4) 0.009(4) 0.001(4) -0.003(4) C2 0.023(4) 0.021(4) 0.020(4) 0.005(4) 0.001(4) 0.000(4) C3 0.027(4) 0.024(4) 0.025(4) 0.003(4) -0.002(4) 0.005(4) C4 0.024(4) 0.018(4) 0.025(4) 0.003(4) 0.002(4) 0.006(4) C5 0.027(4) 0.020(4) 0.025(4) -0.001(4) 0.011(4) 0.005(4) C6 0.027(5) 0.018(4) 0.023(4) -0.003(4) 0.011(4) 0.004(4) C7 0.025(4) 0.017(4) 0.021(4) -0.001(4) 0.007(4) -0.001(4) C8 0.023(4) 0.014(4) 0.019(4) 0.003(3) 0.006(4) -0.003(4) C9 0.020(4) 0.013(3) 0.019(4) 0.006(3) 0.004(3) -0.002(3) C10 0.022(4) 0.018(3) 0.023(4) 0.004(3) 0.006(3) 0.004(3) C11 0.020(4) 0.020(4) 0.027(5) -0.001(4) 0.006(4) -0.008(4) C12 0.023(4) 0.019(4) 0.035(5) 0.000(4) 0.001(4) -0.005(4) C13 0.029(5) 0.014(4) 0.043(5) 0.002(4) -0.003(4) -0.002(4) C14 0.028(6) 0.009(5) 0.047(6) 0.004(5) -0.007(5) -0.003(5) C15 0.023(5) 0.026(5) 0.017(5) 0.010(4) 0.000(5) 0.005(5) C16 0.021(5) 0.023(4) 0.016(4) 0.009(4) -0.002(4) 0.004(4) C17 0.020(4) 0.021(4) 0.017(4) 0.006(4) -0.002(4) 0.000(4) C18 0.016(4) 0.021(4) 0.018(4) 0.005(4) 0.002(4) -0.005(4) C19 0.018(4) 0.018(4) 0.020(4) 0.003(4) 0.005(4) -0.007(4) C20 0.013(7) 0.033(7) 0.023(7) -0.001(7) -0.004(7) 0.002(6) C21 0.021(7) 0.052(8) 0.026(8) -0.008(8) -0.002(7) 0.000(9) C23 0.026(5) 0.025(4) 0.021(4) 0.000(4) -0.010(4) -0.004(3) C22 0.026(5) 0.024(4) 0.021(4) -0.001(4) -0.010(4) -0.004(3) N 0.026(5) 0.024(4) 0.020(4) -0.001(4) -0.010(4) -0.004(3) _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 Sn C1 2.125(12) . ? Sn C11 2.122(13) . ? Sn C21 2.136(11) . ? Sn N 2.436(9) . ? Sn Cl1 2.629(3) . ? Ga C8 1.958(12) . ? Ga C18 1.973(11) . ? Ga Cl2 2.235(3) . ? Ga Cl1 2.359(4) . ? C1 C2 1.379(15) . ? C1 C9 1.437(15) . ? C2 C3 1.388(14) . ? C3 C4 1.376(15) . ? C4 C10 1.369(16) . ? C5 C6 1.373(16) . ? C5 C10 1.425(16) . ? C6 C7 1.403(16) . ? C7 C8 1.381(14) . ? C8 C9 1.461(16) . ? C9 C10 1.418(15) . ? C11 C19 1.407(16) . ? C11 C12 1.431(15) . ? C12 C13 1.393(14) . ? C13 C14 1.370(16) . ? C14 C20 1.433(15) . ? C15 C16 1.359(15) . ? C15 C20 1.436(16) . ? C16 C17 1.394(15) . ? C17 C18 1.364(15) . ? C18 C19 1.437(15) . ? C19 C20 1.391(15) . ? C23 C22 1.470(15) . ? C22 N 1.108(13) . ? 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 Sn C11 132.5(4) . . ? C1 Sn C21 112.9(5) . . ? C11 Sn C21 113.5(5) . . ? C1 Sn N 84.9(4) . . ? C11 Sn N 86.3(4) . . ? C21 Sn N 89.5(5) . . ? C1 Sn Cl1 92.9(3) . . ? C11 Sn Cl1 94.0(3) . . ? C21 Sn Cl1 93.0(4) . . ? N Sn Cl1 177.1(3) . . ? C8 Ga C18 134.6(5) . . ? C8 Ga Cl2 106.1(4) . . ? C18 Ga Cl2 103.9(3) . . ? C8 Ga Cl1 103.5(3) . . ? C18 Ga Cl1 101.8(3) . . ? Cl2 Ga Cl1 103.44(12) . . ? Ga Cl1 Sn 81.89(9) . . ? C2 C1 C9 119.1(12) . . ? C2 C1 Sn 111.9(9) . . ? C9 C1 Sn 128.9(9) . . ? C1 C2 C3 122.0(13) . . ? C4 C3 C2 119.5(12) . . ? C3 C4 C10 120.4(12) . . ? C6 C5 C10 121.5(12) . . ? C5 C6 C7 118.4(12) . . ? C8 C7 C6 124.4(12) . . ? C7 C8 C9 116.6(11) . . ? C7 C8 Ga 115.2(10) . . ? C9 C8 Ga 127.8(8) . . ? C10 C9 C1 117.0(11) . . ? C10 C9 C8 119.8(11) . . ? C1 C9 C8 123.2(11) . . ? C4 C10 C9 121.9(12) . . ? C4 C10 C5 119.0(11) . . ? C9 C10 C5 119.1(12) . . ? C19 C11 C12 119.2(11) . . ? C19 C11 Sn 130.6(9) . . ? C12 C11 Sn 110.0(9) . . ? C13 C12 C11 121.4(12) . . ? C14 C13 C12 119.3(12) . . ? C13 C14 C20 120.2(12) . . ? C16 C15 C20 119.5(11) . . ? C15 C16 C17 118.3(11) . . ? C18 C17 C16 124.3(11) . . ? C17 C18 C19 118.7(11) . . ? C17 C18 Ga 115.2(9) . . ? C19 C18 Ga 126.1(9) . . ? C20 C19 C11 118.5(11) . . ? C20 C19 C18 117.1(11) . . ? C11 C19 C18 124.4(11) . . ? C19 C20 C14 121.3(12) . . ? C19 C20 C15 122.0(11) . . ? C14 C20 C15 116.6(11) . . ? N C22 C23 179.5(15) . . ? C22 N Sn 166.1(12) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.904 _refine_diff_density_min -1.020 _refine_diff_density_rms 0.179 ###END data_3 _database_code_CSD 199218 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H35 Cl3 Ga P Sn' _chemical_formula_weight 901.46 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' Ga Ga 0.2307 1.6083 '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 10.0756(5) _cell_length_b 29.5593(16) _cell_length_c 12.8883(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.2640(10) _cell_angle_gamma 90.00 _cell_volume 3832.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 1.638 _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 110(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 'CCD area detector' _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 20168 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0644 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6734 _reflns_number_gt 4839 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 i= s not relevant to the choice of reflections for refinement. R-factors base= d 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^)+(0.0500P)^2^+17.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6734 _refine_ls_number_parameters 454 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1361 _refine_ls_wR_factor_gt 0.1235 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 Sn Sn 0.55123(4) 0.120771(14) 0.33122(3) 0.02745(14) Uani 1 1 d . . . Ga Ga 0.24061(7) 0.16149(2) 0.32059(5) 0.02578(18) Uani 1 1 d . . . P P 0.23626(16) 0.10576(5) -0.12225(12) 0.0269(4) Uani 1 1 d . . . Cl3 Cl 0.67480(16) 0.08507(5) 0.19283(12) 0.0361(4) Uani 1 1 d . . . Cl1 Cl 0.37583(16) 0.16445(5) 0.47228(11) 0.0320(4) Uani 1 1 d . . . Cl2 Cl 0.05356(16) 0.19471(5) 0.36548(12) 0.0340(4) Uani 1 1 d . . . C1 C 0.4200(6) 0.06349(19) 0.3404(4) 0.0266(14) Uani 1 1 d . . . C2 C 0.4929(6) 0.0255(2) 0.3664(5) 0.0303(14) Uani 1 1 d . . . H2A H 0.5836 0.0285 0.3825 0.036 Uiso 1 1 calc R . . C3 C 0.4356(7) -0.0178(2) 0.3696(5) 0.0320(15) Uani 1 1 d . . . H3A H 0.4869 -0.0427 0.3908 0.038 Uiso 1 1 calc R . . C4 C 0.3041(6) -0.0230(2) 0.3414(5) 0.0297(14) Uani 1 1 d . . . H4A H 0.2669 -0.0517 0.3401 0.036 Uiso 1 1 calc R . . C5 C 0.0893(6) 0.0091(2) 0.2828(4) 0.0309(15) Uani 1 1 d . . . H5A H 0.0538 -0.0199 0.2779 0.037 Uiso 1 1 calc R . . C6 C 0.0094(6) 0.0451(2) 0.2596(5) 0.0293(14) Uani 1 1 d . . . H6A H -0.0792 0.0407 0.2376 0.035 Uiso 1 1 calc R . . C7 C 0.0617(6) 0.0887(2) 0.2690(4) 0.0282(14) Uani 1 1 d . . . H7A H 0.0055 0.1132 0.2556 0.034 Uiso 1 1 calc R . . C8 C 0.1937(6) 0.0968(2) 0.2975(4) 0.0283(14) Uani 1 1 d . . . C9 C 0.2780(6) 0.0602(2) 0.3173(4) 0.0262(14) Uani 1 1 d . . . C10 C 0.2243(6) 0.0145(2) 0.3141(4) 0.0269(14) Uani 1 1 d . . . C11 C 0.5610(6) 0.18609(19) 0.2591(4) 0.0251(13) Uani 1 1 d . . . C12 C 0.6920(7) 0.2002(2) 0.2554(5) 0.0320(15) Uani 1 1 d . . . H12A H 0.7594 0.1833 0.2889 0.038 Uiso 1 1 calc R . . C13 C 0.7245(7) 0.2398(2) 0.2016(5) 0.0328(15) Uani 1 1 d . . . H13A H 0.8123 0.2496 0.2026 0.039 Uiso 1 1 calc R . . C14 C 0.6290(7) 0.2637(2) 0.1488(5) 0.0319(15) Uani 1 1 d . . . H14A H 0.6525 0.2890 0.1111 0.038 Uiso 1 1 calc R . . C15 C 0.3920(7) 0.2753(2) 0.0923(5) 0.0330(15) Uani 1 1 d . . . H15A H 0.4156 0.2998 0.0518 0.040 Uiso 1 1 calc R . . C16 C 0.2629(7) 0.2640(2) 0.0953(5) 0.0338(15) Uani 1 1 d . . . H16A H 0.1988 0.2794 0.0542 0.041 Uiso 1 1 calc R . . C17 C 0.2256(7) 0.2284(2) 0.1618(5) 0.0309(14) Uani 1 1 d . . . H17A H 0.1358 0.2221 0.1668 0.037 Uiso 1 1 calc R . . C18 C 0.3184(6) 0.20301(18) 0.2192(4) 0.0259(13) Uani 1 1 d . . . C19 C 0.4557(6) 0.21276(19) 0.2113(4) 0.0277(14) Uani 1 1 d . . . C20 C 0.4926(6) 0.2510(2) 0.1492(4) 0.0278(14) Uani 1 1 d . . . C21 C 0.6993(6) 0.1164(2) 0.4541(5) 0.0348(15) Uani 1 1 d . . . H21A H 0.6662 0.1292 0.5159 0.052 Uiso 1 1 calc R . . H21B H 0.7769 0.1327 0.4357 0.052 Uiso 1 1 calc R . . H21C H 0.7219 0.0852 0.4664 0.052 Uiso 1 1 calc R . . C31 C 0.3865(6) 0.1364(2) -0.1391(4) 0.0295(14) Uani 1 1 d . . . C32 C 0.4474(7) 0.1358(2) -0.2335(5) 0.0404(17) Uani 1 1 d . . . H32A H 0.4091 0.1197 -0.2896 0.048 Uiso 1 1 calc R . . C33 C 0.5641(7) 0.1591(2) -0.2438(5) 0.0446(18) Uani 1 1 d . . . H33A H 0.6027 0.1591 -0.3076 0.054 Uiso 1 1 calc R . . C34 C 0.6254(7) 0.1825(2) -0.1617(5) 0.0400(17) Uani 1 1 d . . . H34A H 0.7055 0.1975 -0.1691 0.048 Uiso 1 1 calc R . . C35 C 0.5641(7) 0.1833(2) -0.0676(5) 0.0386(16) Uani 1 1 d . . . H35A H 0.6037 0.1990 -0.0115 0.046 Uiso 1 1 calc R . . C36 C 0.4460(7) 0.1610(2) -0.0561(5) 0.0357(16) Uani 1 1 d . . . H36A H 0.4056 0.1624 0.0069 0.043 Uiso 1 1 calc R . . C41 C 0.1708(6) 0.0882(2) -0.2492(4) 0.0272(14) Uani 1 1 d . . . C42 C 0.0746(6) 0.1135(2) -0.3036(5) 0.0307(14) Uani 1 1 d . . . H42A H 0.0361 0.1383 -0.2724 0.037 Uiso 1 1 calc R . . C43 C 0.0355(7) 0.1016(2) -0.4064(5) 0.0360(16) Uani 1 1 d . . . H43A H -0.0284 0.1187 -0.4437 0.043 Uiso 1 1 calc R . . C44 C 0.0920(6) 0.0648(2) -0.4516(5) 0.0311(14) Uani 1 1 d . . . H44A H 0.0654 0.0568 -0.5195 0.037 Uiso 1 1 calc R . . C45 C 0.1872(6) 0.0395(2) -0.3978(5) 0.0345(15) Uani 1 1 d . . . H45A H 0.2252 0.0148 -0.4297 0.041 Uiso 1 1 calc R . . C46 C 0.2266(6) 0.0504(2) -0.2970(5) 0.0332(15) Uani 1 1 d . . . H46A H 0.2900 0.0328 -0.2605 0.040 Uiso 1 1 calc R . . C51 C 0.2652(6) 0.0565(2) -0.0440(4) 0.0267(14) Uani 1 1 d . . . C52 C 0.3746(7) 0.0533(2) 0.0277(5) 0.0341(15) Uani 1 1 d . . . H52A H 0.4344 0.0772 0.0352 0.041 Uiso 1 1 calc R . . C53 C 0.3940(7) 0.0147(2) 0.0877(5) 0.0368(16) Uani 1 1 d . . . H53A H 0.4656 0.0129 0.1364 0.044 Uiso 1 1 calc R . . C54 C 0.3073(7) -0.0211(2) 0.0750(5) 0.0369(16) Uani 1 1 d . . . H54A H 0.3219 -0.0472 0.1141 0.044 Uiso 1 1 calc R . . C55 C 0.1992(7) -0.0186(2) 0.0052(5) 0.0361(16) Uani 1 1 d . . . H55A H 0.1410 -0.0430 -0.0026 0.043 Uiso 1 1 calc R . . C56 C 0.1766(4) 0.02062(12) -0.0542(3) 0.0342(15) Uani 1 1 d . . . H56A H 0.1025 0.0226 -0.1003 0.041 Uiso 1 1 calc R . . C61 C 0.1195(4) 0.14258(12) -0.0657(3) 0.0277(14) Uani 1 1 d R . . C62 C 0.1103(4) 0.18706(12) -0.0991(3) 0.0339(15) Uani 1 1 d R . . H62A H 0.1713 0.1983 -0.1441 0.041 Uiso 1 1 d R . . C63 C 0.0110(7) 0.2149(2) -0.0659(5) 0.0348(15) Uani 1 1 d . . . H63A H 0.0040 0.2446 -0.0892 0.042 Uiso 1 1 calc R . . C64 C -0.0782(7) 0.1981(2) 0.0025(5) 0.0362(16) Uani 1 1 d . . . H64A H -0.1458 0.2166 0.0245 0.043 Uiso 1 1 calc R . . C65 C -0.0678(7) 0.1545(2) 0.0381(5) 0.0377(16) Uani 1 1 d . . . H65A H -0.1275 0.1439 0.0849 0.045 Uiso 1 1 calc R . . C66 C 0.0302(7) 0.1260(2) 0.0055(5) 0.0320(15) Uani 1 1 d . . . H66A H 0.0371 0.0965 0.0300 0.038 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 Sn 0.0314(3) 0.0268(2) 0.0244(2) -0.00076(17) 0.00406(17) -0.00086(19) Ga 0.0321(4) 0.0238(4) 0.0223(3) 0.0008(3) 0.0088(3) 0.0000(3) P 0.0336(9) 0.0285(9) 0.0191(8) -0.0006(6) 0.0057(7) -0.0009(7) Cl3 0.0358(9) 0.0351(9) 0.0384(9) -0.0085(7) 0.0123(7) -0.0009(7) Cl1 0.0415(9) 0.0332(8) 0.0220(7) -0.0020(6) 0.0062(7) -0.0026(7) Cl2 0.0375(9) 0.0314(8) 0.0346(9) -0.0012(6) 0.0146(7) 0.0038(7) C1 0.035(4) 0.025(3) 0.020(3) -0.002(2) 0.005(3) -0.002(3) C2 0.030(4) 0.032(4) 0.029(3) 0.002(3) 0.002(3) -0.003(3) C3 0.043(4) 0.026(3) 0.028(3) 0.002(3) 0.006(3) 0.007(3) C4 0.041(4) 0.023(3) 0.026(3) -0.001(2) 0.007(3) -0.005(3) C5 0.038(4) 0.032(4) 0.023(3) -0.003(3) 0.009(3) -0.005(3) C6 0.027(3) 0.030(3) 0.032(3) -0.001(3) 0.013(3) -0.003(3) C7 0.034(4) 0.027(3) 0.024(3) 0.004(3) 0.006(3) 0.003(3) C8 0.037(4) 0.033(3) 0.017(3) -0.005(3) 0.009(3) -0.009(3) C9 0.038(4) 0.036(4) 0.006(3) 0.001(2) 0.005(2) -0.009(3) C10 0.034(4) 0.031(3) 0.016(3) -0.004(2) 0.009(3) -0.001(3) C11 0.031(4) 0.026(3) 0.019(3) -0.003(2) 0.008(3) -0.003(3) C12 0.037(4) 0.035(4) 0.025(3) -0.006(3) 0.010(3) 0.004(3) C13 0.036(4) 0.034(4) 0.030(3) -0.007(3) 0.014(3) -0.005(3) C14 0.046(4) 0.027(3) 0.025(3) -0.004(3) 0.017(3) -0.006(3) C15 0.048(4) 0.028(3) 0.024(3) -0.002(3) 0.009(3) 0.000(3) C16 0.047(4) 0.027(3) 0.027(3) 0.000(3) 0.007(3) 0.003(3) C17 0.034(4) 0.033(4) 0.027(3) 0.002(3) 0.010(3) 0.002(3) C18 0.040(4) 0.018(3) 0.021(3) -0.002(2) 0.009(3) -0.003(3) C19 0.045(4) 0.021(3) 0.018(3) -0.006(2) 0.016(3) 0.002(3) C20 0.041(4) 0.024(3) 0.019(3) -0.005(2) 0.015(3) 0.000(3) C21 0.036(4) 0.031(4) 0.036(4) 0.002(3) -0.013(3) 0.000(3) C31 0.037(4) 0.029(3) 0.023(3) 0.002(3) 0.008(3) 0.000(3) C32 0.047(4) 0.047(4) 0.028(4) -0.009(3) 0.011(3) -0.012(3) C33 0.046(4) 0.059(5) 0.030(4) -0.006(3) 0.014(3) -0.018(4) C34 0.045(4) 0.038(4) 0.038(4) 0.001(3) 0.015(3) -0.010(3) C35 0.040(4) 0.039(4) 0.037(4) -0.012(3) 0.007(3) -0.012(3) C36 0.037(4) 0.041(4) 0.030(4) -0.004(3) 0.006(3) -0.002(3) C41 0.034(4) 0.029(3) 0.019(3) 0.001(2) 0.008(3) -0.003(3) C42 0.034(4) 0.027(3) 0.032(3) -0.005(3) 0.006(3) -0.004(3) C43 0.050(4) 0.028(3) 0.029(3) 0.006(3) -0.008(3) -0.005(3) C44 0.039(4) 0.032(4) 0.022(3) -0.001(3) 0.003(3) -0.003(3) C45 0.035(4) 0.045(4) 0.025(3) -0.008(3) 0.009(3) 0.003(3) C46 0.033(4) 0.041(4) 0.026(3) 0.002(3) 0.005(3) 0.007(3) C51 0.034(4) 0.028(3) 0.018(3) -0.002(2) 0.006(3) 0.000(3) C52 0.040(4) 0.036(4) 0.027(3) -0.004(3) 0.006(3) -0.003(3) C53 0.053(4) 0.035(4) 0.023(3) -0.002(3) 0.007(3) 0.006(3) C54 0.060(5) 0.026(3) 0.026(3) 0.000(3) 0.010(3) 0.007(3) C55 0.053(5) 0.028(4) 0.029(4) -0.001(3) 0.014(3) -0.004(3) C56 0.041(4) 0.035(4) 0.027(3) -0.001(3) 0.007(3) 0.000(3) C61 0.030(4) 0.031(3) 0.022(3) 0.003(3) 0.004(3) 0.003(3) C62 0.040(4) 0.038(4) 0.024(3) 0.004(3) 0.008(3) -0.003(3) C63 0.046(4) 0.036(4) 0.023(3) 0.000(3) 0.007(3) 0.006(3) C64 0.038(4) 0.042(4) 0.030(3) -0.003(3) 0.010(3) 0.009(3) C65 0.037(4) 0.048(4) 0.029(4) -0.001(3) 0.011(3) 0.001(3) C66 0.048(4) 0.027(3) 0.021(3) 0.003(3) 0.002(3) 0.001(3) _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 Sn C21 2.117(6) . ? Sn C11 2.147(6) . ? Sn C1 2.156(6) . ? Sn Cl3 2.4694(15) . ? Sn Cl1 2.9088(15) . ? Ga C18 1.986(6) . ? Ga C8 1.987(6) . ? Ga Cl2 2.2305(17) . ? Ga Cl1 2.3201(16) . ? P C51 1.786(6) . ? P C31 1.788(6) . ? P C61 1.788(4) . ? P C41 1.805(6) . ? C1 C2 1.374(8) . ? C1 C9 1.448(8) . ? C2 C3 1.404(8) . ? C3 C4 1.362(9) . ? C4 C10 1.402(9) . ? C5 C6 1.356(9) . ? C5 C10 1.405(9) . ? C6 C7 1.395(8) . ? C7 C8 1.380(9) . ? C8 C9 1.392(9) . ? C9 C10 1.454(8) . ? C11 C12 1.389(9) . ? C11 C19 1.432(9) . ? C12 C13 1.408(9) . ? C13 C14 1.345(9) . ? C14 C20 1.425(9) . ? C15 C16 1.345(9) . ? C15 C20 1.414(9) . ? C16 C17 1.422(8) . ? C17 C18 1.381(9) . ? C18 C19 1.423(9) . ? C19 C20 1.444(8) . ? C31 C32 1.394(8) . ? C31 C36 1.401(9) . ? C32 C33 1.376(9) . ? C33 C34 1.381(9) . ? C34 C35 1.392(9) . ? C35 C36 1.374(9) . ? C41 C42 1.384(9) . ? C41 C46 1.409(8) . ? C42 C43 1.405(9) . ? C43 C44 1.375(9) . ? C44 C45 1.372(9) . ? C45 C46 1.375(8) . ? C51 C56 1.387(7) . ? C51 C52 1.401(9) . ? C52 C53 1.387(9) . ? C53 C54 1.375(9) . ? C54 C55 1.375(10) . ? C55 C56 1.401(7) . ? C61 C62 1.3848 . ? C61 C66 1.409(7) . ? C62 C63 1.383(7) . ? C63 C64 1.386(9) . ? C64 C65 1.371(9) . ? C65 C66 1.380(9) . ? 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 C21 Sn C11 109.3(2) . . ? C21 Sn C1 108.6(2) . . ? C11 Sn C1 140.6(2) . . ? C21 Sn Cl3 98.70(19) . . ? C11 Sn Cl3 91.98(15) . . ? C1 Sn Cl3 92.28(16) . . ? C21 Sn Cl1 89.26(19) . . ? C11 Sn Cl1 85.16(15) . . ? C1 Sn Cl1 85.31(16) . . ? Cl3 Sn Cl1 172.04(5) . . ? C18 Ga C8 126.5(2) . . ? C18 Ga Cl2 105.63(18) . . ? C8 Ga Cl2 105.37(19) . . ? C18 Ga Cl1 107.24(18) . . ? C8 Ga Cl1 106.61(18) . . ? Cl2 Ga Cl1 103.25(6) . . ? C51 P C31 111.7(3) . . ? C51 P C61 110.9(2) . . ? C31 P C61 108.8(2) . . ? C51 P C41 108.5(3) . . ? C31 P C41 107.7(3) . . ? C61 P C41 109.3(2) . . ? Ga Cl1 Sn 78.76(4) . . ? C2 C1 C9 120.2(5) . . ? C2 C1 Sn 109.6(4) . . ? C9 C1 Sn 130.1(4) . . ? C1 C2 C3 122.5(6) . . ? C4 C3 C2 119.3(6) . . ? C3 C4 C10 120.9(6) . . ? C6 C5 C10 121.8(6) . . ? C5 C6 C7 119.2(6) . . ? C8 C7 C6 122.6(6) . . ? C7 C8 C9 118.8(6) . . ? C7 C8 Ga 115.2(5) . . ? C9 C8 Ga 125.7(5) . . ? C8 C9 C1 124.8(5) . . ? C8 C9 C10 119.7(6) . . ? C1 C9 C10 115.5(5) . . ? C4 C10 C5 121.0(6) . . ? C4 C10 C9 121.3(6) . . ? C5 C10 C9 117.8(6) . . ? C12 C11 C19 120.1(5) . . ? C12 C11 Sn 110.7(4) . . ? C19 C11 Sn 129.1(4) . . ? C11 C12 C13 121.0(6) . . ? C14 C13 C12 120.3(6) . . ? C13 C14 C20 121.5(6) . . ? C16 C15 C20 121.6(6) . . ? C15 C16 C17 119.4(6) . . ? C18 C17 C16 122.1(6) . . ? C17 C18 C19 118.9(5) . . ? C17 C18 Ga 114.1(4) . . ? C19 C18 Ga 126.4(4) . . ? C18 C19 C11 123.9(5) . . ? C18 C19 C20 118.6(6) . . ? C11 C19 C20 117.5(6) . . ? C15 C20 C14 121.8(6) . . ? C15 C20 C19 119.1(6) . . ? C14 C20 C19 119.1(6) . . ? C32 C31 C36 118.9(6) . . ? C32 C31 P 121.2(5) . . ? C36 C31 P 120.0(5) . . ? C33 C32 C31 119.9(6) . . ? C32 C33 C34 121.7(6) . . ? C33 C34 C35 118.3(6) . . ? C36 C35 C34 121.0(6) . . ? C35 C36 C31 120.2(6) . . ? C42 C41 C46 119.6(5) . . ? C42 C41 P 120.8(5) . . ? C46 C41 P 119.4(5) . . ? C41 C42 C43 119.5(6) . . ? C44 C43 C42 119.9(6) . . ? C45 C44 C43 120.7(6) . . ? C44 C45 C46 120.4(6) . . ? C45 C46 C41 119.9(6) . . ? C56 C51 C52 119.2(5) . . ? C56 C51 P 119.1(4) . . ? C52 C51 P 121.7(5) . . ? C53 C52 C51 120.3(6) . . ? C54 C53 C52 119.9(7) . . ? C53 C54 C55 120.8(6) . . ? C54 C55 C56 120.0(6) . . ? C51 C56 C55 119.9(5) . . ? C62 C61 C66 119.9(3) . . ? C62 C61 P 119.04(12) . . ? C66 C61 P 120.9(3) . . ? C63 C62 C61 120.4(3) . . ? C62 C63 C64 119.4(6) . . ? C65 C64 C63 120.7(6) . . ? C64 C65 C66 120.9(6) . . ? C65 C66 C61 118.8(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.813 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.154 ###END data_4 _database_code_CSD 199219 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H35 Br Cl2 Ga P Sn' _chemical_formula_weight 945.92 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 10.1349(12) _cell_length_b 29.554(4) _cell_length_c 12.9071(16) _cell_angle_alpha 90.00 _cell_angle_beta 93.519(2) _cell_angle_gamma 90.00 _cell_volume 3858.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 2.593 _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 110(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 'CCD area detector' _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 20170 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0876 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6797 _reflns_number_gt 4245 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0350P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6797 _refine_ls_number_parameters 460 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1057 _refine_ls_wR_factor_gt 0.0975 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 Sn Sn 0.55038(4) 0.120682(15) 0.33179(3) 0.02934(14) Uani 1 1 d . . . Ga Ga 0.24047(6) 0.16105(2) 0.32088(5) 0.02718(19) Uani 1 1 d . . . Br1 Br 0.3837(7) 0.1630(3) 0.4797(6) 0.034(3) Uiso 0.267(3) 1 d P A 1 Br2 Br 0.0405(5) 0.19469(19) 0.3567(4) 0.0293(19) Uiso 0.226(3) 1 d P A 2 Br3 Br 0.6743(2) 0.08456(8) 0.18285(18) 0.0309(8) Uiso 0.507(2) 1 d P A 3 Cl1 Cl 0.3706(6) 0.1657(2) 0.4783(5) 0.0271(19) Uiso 0.733(3) 1 d P A 1 Cl2 Cl 0.0547(4) 0.19497(13) 0.3712(3) 0.0277(13) Uiso 0.774(3) 1 d P A 2 Cl3 Cl 0.6836(6) 0.0815(2) 0.1999(4) 0.0283(19) Uiso 0.493(2) 1 d P A 3 P P 0.73586(16) 0.39446(6) 0.37816(12) 0.0283(4) Uani 1 1 d . . . C1 C 0.4211(6) 0.0633(2) 0.3411(4) 0.0272(15) Uani 1 1 d . A . C2 C 0.4944(6) 0.0253(2) 0.3668(4) 0.0296(15) Uani 1 1 d . . . H2A H 0.5847 0.0285 0.3827 0.036 Uiso 1 1 calc R A . C3 C 0.4379(6) -0.0182(2) 0.3698(5) 0.0349(16) Uani 1 1 d . A . H3A H 0.4898 -0.0429 0.3902 0.042 Uiso 1 1 calc R . . C4 C 0.3069(6) -0.0238(2) 0.3427(4) 0.0288(15) Uani 1 1 d . . . H4A H 0.2700 -0.0527 0.3427 0.035 Uiso 1 1 calc R A . C5 C 0.0916(6) 0.0075(2) 0.2848(4) 0.0321(16) Uani 1 1 d . . . H5A H 0.0560 -0.0215 0.2819 0.038 Uiso 1 1 calc R A . C6 C 0.0138(6) 0.0439(2) 0.2604(5) 0.0307(15) Uani 1 1 d . A . H6A H -0.0741 0.0394 0.2377 0.037 Uiso 1 1 calc R . . C7 C 0.0640(6) 0.0878(2) 0.2691(4) 0.0294(15) Uani 1 1 d . . . H7A H 0.0072 0.1121 0.2549 0.035 Uiso 1 1 calc R A . C8 C 0.1958(6) 0.0965(2) 0.2982(4) 0.0267(15) Uani 1 1 d . A . C9 C 0.2806(6) 0.0594(2) 0.3176(4) 0.0275(15) Uani 1 1 d . . . C10 C 0.2269(6) 0.0139(2) 0.3145(4) 0.0257(15) Uani 1 1 d . A . C11 C 0.5595(6) 0.1859(2) 0.2603(4) 0.0249(14) Uani 1 1 d . A . C12 C 0.6900(6) 0.2004(2) 0.2553(4) 0.0321(16) Uani 1 1 d . . . H12A H 0.7579 0.1837 0.2885 0.039 Uiso 1 1 calc R A . C13 C 0.7204(6) 0.2396(2) 0.2013(4) 0.0331(16) Uani 1 1 d . A . H13A H 0.8075 0.2495 0.2018 0.040 Uiso 1 1 calc R . . C14 C 0.6239(6) 0.2635(2) 0.1481(4) 0.0307(15) Uani 1 1 d . . . H14A H 0.6464 0.2886 0.1094 0.037 Uiso 1 1 calc R A . C15 C 0.3914(6) 0.2751(2) 0.0941(5) 0.0337(16) Uani 1 1 d . . . H15A H 0.4149 0.2992 0.0529 0.040 Uiso 1 1 calc R A . C16 C 0.2615(7) 0.2639(2) 0.0984(5) 0.0360(17) Uani 1 1 d . A . H16A H 0.1974 0.2797 0.0583 0.043 Uiso 1 1 calc R . . C17 C 0.2241(6) 0.2284(2) 0.1637(5) 0.0347(16) Uani 1 1 d . . . H17A H 0.1348 0.2221 0.1684 0.042 Uiso 1 1 calc R A . C18 C 0.3167(6) 0.2027(2) 0.2210(4) 0.0272(15) Uani 1 1 d . A . C19 C 0.4533(6) 0.2126(2) 0.2106(4) 0.0265(15) Uani 1 1 d . . . C20 C 0.4901(6) 0.2508(2) 0.1506(4) 0.0278(15) Uani 1 1 d . A . C21 C 0.7008(6) 0.1169(2) 0.4541(4) 0.0355(16) Uani 1 1 d . A . H21A H 0.7782 0.1030 0.4288 0.053 Uiso 1 1 calc R . . H21B H 0.6698 0.0992 0.5100 0.053 Uiso 1 1 calc R . . H21C H 0.7223 0.1469 0.4786 0.053 Uiso 1 1 calc R . . C31 C 0.6209(6) 0.3573(2) 0.4351(4) 0.0282(15) Uani 1 1 d . . . C32 C 0.5342(6) 0.3732(2) 0.5054(4) 0.0332(16) Uani 1 1 d . . . H32A H 0.5413 0.4026 0.5304 0.040 Uiso 1 1 calc R . . C33 C 0.4367(6) 0.3447(2) 0.5381(5) 0.0383(17) Uani 1 1 d . . . H33A H 0.3774 0.3553 0.5846 0.046 Uiso 1 1 calc R . . C34 C 0.4261(6) 0.3008(2) 0.5029(5) 0.0358(17) Uani 1 1 d . . . H34A H 0.3600 0.2822 0.5257 0.043 Uiso 1 1 calc R . . C35 C 0.5135(6) 0.2845(2) 0.4337(5) 0.0364(17) Uani 1 1 d . . . H35A H 0.5074 0.2547 0.4103 0.044 Uiso 1 1 calc R . . C36 C 0.6104(6) 0.3131(2) 0.3999(4) 0.0343(17) Uani 1 1 d . . . H36A H 0.6692 0.3024 0.3530 0.041 Uiso 1 1 calc R . . C41 C 0.7632(6) 0.4443(2) 0.4560(4) 0.0256(14) Uani 1 1 d . . . C42 C 0.6723(6) 0.4795(2) 0.4462(5) 0.0335(16) Uani 1 1 d . . . H42A H 0.5982 0.4770 0.4004 0.040 Uiso 1 1 calc R . . C43 C 0.6932(7) 0.5186(2) 0.5057(5) 0.0381(17) Uani 1 1 d . . . H43A H 0.6343 0.5427 0.4986 0.046 Uiso 1 1 calc R . . C44 C 0.8010(7) 0.5212(2) 0.5745(5) 0.0374(17) Uani 1 1 d . . . H44A H 0.8138 0.5474 0.6139 0.045 Uiso 1 1 calc R . . C45 C 0.8909(7) 0.4866(2) 0.5875(5) 0.0377(17) Uani 1 1 d . . . H45A H 0.9626 0.4890 0.6357 0.045 Uiso 1 1 calc R . . C46 C 0.8720(6) 0.4477(2) 0.5262(5) 0.0356(16) Uani 1 1 d . . . H46A H 0.9326 0.4241 0.5327 0.043 Uiso 1 1 calc R . . C51 C 0.6706(6) 0.4121(2) 0.2515(4) 0.0289(15) Uani 1 1 d . . . C52 C 0.7255(6) 0.4501(2) 0.2047(4) 0.0313(16) Uani 1 1 d . . . H52A H 0.7879 0.4678 0.2417 0.038 Uiso 1 1 calc R . . C53 C 0.6859(6) 0.4609(2) 0.1035(5) 0.0336(16) Uani 1 1 d . . . H53A H 0.7226 0.4857 0.0716 0.040 Uiso 1 1 calc R . . C54 C 0.5916(6) 0.4347(2) 0.0495(5) 0.0326(16) Uani 1 1 d . . . H54A H 0.5648 0.4423 -0.0185 0.039 Uiso 1 1 calc R . . C55 C 0.5376(6) 0.3980(2) 0.0948(5) 0.0362(17) Uani 1 1 d . . . H55A H 0.4741 0.3808 0.0575 0.043 Uiso 1 1 calc R . . C56 C 0.5764(6) 0.3860(2) 0.1959(5) 0.0334(16) Uani 1 1 d . . . H56A H 0.5399 0.3608 0.2262 0.040 Uiso 1 1 calc R . . C61 C 0.8868(6) 0.3642(2) 0.3622(4) 0.0304(15) Uani 1 1 d . . . C62 C 0.9458(6) 0.3404(2) 0.4463(5) 0.0335(16) Uani 1 1 d . . . H62A H 0.9055 0.3394 0.5091 0.040 Uiso 1 1 calc R . . C63 C 1.0643(6) 0.3184(2) 0.4355(5) 0.0397(18) Uani 1 1 d . . . H63A H 1.1039 0.3027 0.4916 0.048 Uiso 1 1 calc R . . C64 C 1.1248(6) 0.3192(2) 0.3424(5) 0.0424(18) Uani 1 1 d . . . H64A H 1.2051 0.3046 0.3357 0.051 Uiso 1 1 calc R . . C65 C 1.0636(7) 0.3423(3) 0.2591(5) 0.047(2) Uani 1 1 d . . . H65A H 1.1024 0.3425 0.1957 0.057 Uiso 1 1 calc R . . C66 C 0.9467(6) 0.3647(2) 0.2691(5) 0.0431(19) Uani 1 1 d . . . H66A H 0.9076 0.3804 0.2128 0.052 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 Sn 0.0306(3) 0.0271(3) 0.0300(3) 0.0001(2) -0.00052(19) -0.0015(2) Ga 0.0296(4) 0.0239(4) 0.0284(4) 0.0011(3) 0.0042(3) 0.0001(3) P 0.0317(9) 0.0286(11) 0.0246(9) 0.0004(7) 0.0018(7) 0.0019(8) C1 0.034(4) 0.028(4) 0.020(3) 0.003(3) 0.009(3) -0.005(3) C2 0.024(3) 0.034(4) 0.031(4) 0.002(3) 0.003(3) -0.002(3) C3 0.043(4) 0.027(4) 0.034(4) 0.001(3) 0.001(3) 0.002(3) C4 0.038(4) 0.019(4) 0.030(4) -0.002(3) 0.004(3) 0.001(3) C5 0.040(4) 0.030(4) 0.027(4) -0.004(3) 0.005(3) -0.007(3) C6 0.026(4) 0.026(4) 0.040(4) 0.002(3) 0.007(3) -0.001(3) C7 0.038(4) 0.028(4) 0.022(3) 0.002(3) 0.003(3) 0.004(3) C8 0.033(4) 0.031(4) 0.017(3) -0.007(3) 0.006(3) -0.011(3) C9 0.041(4) 0.034(4) 0.008(3) 0.001(3) 0.003(3) -0.014(3) C10 0.028(4) 0.029(4) 0.020(3) -0.006(3) 0.003(3) 0.001(3) C11 0.026(3) 0.025(4) 0.025(3) -0.004(3) 0.007(3) -0.001(3) C12 0.034(4) 0.033(4) 0.031(4) -0.006(3) 0.007(3) 0.001(3) C13 0.042(4) 0.027(4) 0.032(4) -0.002(3) 0.017(3) -0.005(3) C14 0.046(4) 0.020(4) 0.027(4) -0.004(3) 0.009(3) -0.009(3) C15 0.044(4) 0.026(4) 0.032(4) 0.000(3) 0.010(3) -0.007(3) C16 0.046(4) 0.029(4) 0.034(4) 0.002(3) 0.006(3) 0.003(3) C17 0.039(4) 0.027(4) 0.038(4) 0.004(3) 0.004(3) -0.005(3) C18 0.038(4) 0.021(4) 0.022(3) -0.005(3) -0.001(3) -0.002(3) C19 0.038(4) 0.023(4) 0.020(3) -0.004(3) 0.010(3) 0.005(3) C20 0.034(4) 0.026(4) 0.024(3) -0.008(3) 0.006(3) -0.002(3) C21 0.038(4) 0.024(4) 0.042(4) 0.001(3) -0.018(3) -0.003(3) C31 0.027(3) 0.027(4) 0.031(4) 0.002(3) -0.001(3) 0.004(3) C32 0.049(4) 0.022(4) 0.029(4) 0.000(3) -0.002(3) -0.003(3) C33 0.043(4) 0.041(5) 0.031(4) -0.003(3) 0.006(3) 0.004(4) C34 0.037(4) 0.040(5) 0.031(4) 0.006(3) 0.006(3) -0.007(3) C35 0.049(4) 0.033(4) 0.027(4) -0.002(3) -0.003(3) -0.006(4) C36 0.042(4) 0.036(5) 0.025(4) -0.007(3) 0.009(3) 0.001(3) C41 0.028(3) 0.026(4) 0.023(3) 0.003(3) 0.000(3) 0.003(3) C42 0.039(4) 0.031(4) 0.030(4) 0.000(3) -0.002(3) 0.000(3) C43 0.055(5) 0.030(4) 0.031(4) 0.004(3) 0.013(3) 0.009(4) C44 0.053(5) 0.034(5) 0.025(4) -0.006(3) 0.005(3) -0.008(4) C45 0.053(5) 0.036(5) 0.024(4) -0.003(3) 0.002(3) -0.005(4) C46 0.045(4) 0.030(4) 0.032(4) 0.008(3) 0.002(3) 0.003(3) C51 0.030(4) 0.027(4) 0.030(4) -0.004(3) 0.003(3) 0.005(3) C52 0.023(3) 0.039(5) 0.031(4) -0.001(3) -0.008(3) -0.005(3) C53 0.031(4) 0.040(5) 0.030(4) 0.006(3) 0.004(3) -0.004(3) C54 0.036(4) 0.037(5) 0.024(4) 0.003(3) -0.002(3) 0.010(3) C55 0.046(4) 0.031(4) 0.030(4) -0.006(3) -0.010(3) 0.002(3) C56 0.033(4) 0.030(4) 0.037(4) 0.007(3) 0.004(3) 0.005(3) C61 0.037(4) 0.030(4) 0.024(4) -0.003(3) 0.003(3) -0.003(3) C62 0.037(4) 0.030(4) 0.034(4) 0.005(3) 0.007(3) 0.004(3) C63 0.042(4) 0.035(5) 0.041(4) 0.007(3) -0.002(3) 0.010(4) C64 0.036(4) 0.044(5) 0.047(5) 0.005(4) 0.007(4) 0.010(4) C65 0.045(4) 0.066(6) 0.031(4) 0.000(4) 0.011(3) 0.015(4) C66 0.044(4) 0.048(5) 0.037(4) 0.010(3) 0.004(3) 0.014(4) _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 Sn C21 2.129(5) . ? Sn C11 2.142(6) . ? Sn C1 2.152(6) . ? Sn Cl3 2.519(6) . ? Sn Br3 2.590(2) . ? Sn Br1 2.908(7) . ? Sn Cl1 3.015(6) . ? Ga C18 1.974(6) . ? Ga C8 1.977(6) . ? Ga Cl2 2.263(4) . ? Ga Br2 2.329(6) . ? Ga Cl1 2.358(6) . ? Ga Br1 2.439(7) . ? P C61 1.795(6) . ? P C31 1.791(6) . ? P C41 1.795(6) . ? P C51 1.802(6) . ? C1 C2 1.375(8) . ? C1 C9 1.442(8) . ? C2 C3 1.409(8) . ? C3 C4 1.362(8) . ? C4 C10 1.414(8) . ? C5 C6 1.358(8) . ? C5 C10 1.414(8) . ? C6 C7 1.397(8) . ? C7 C8 1.390(8) . ? C8 C9 1.408(8) . ? C9 C10 1.449(8) . ? C11 C12 1.395(8) . ? C11 C19 1.452(8) . ? C12 C13 1.397(8) . ? C13 C14 1.357(8) . ? C14 C20 1.410(8) . ? C15 C16 1.361(8) . ? C15 C20 1.400(8) . ? C16 C17 1.412(8) . ? C17 C18 1.385(8) . ? C18 C19 1.429(8) . ? C19 C20 1.431(8) . ? C31 C32 1.383(8) . ? C31 C36 1.387(8) . ? C32 C33 1.384(8) . ? C33 C34 1.374(9) . ? C34 C35 1.384(8) . ? C35 C36 1.386(8) . ? C41 C42 1.389(8) . ? C41 C46 1.388(8) . ? C42 C43 1.398(9) . ? C43 C44 1.366(8) . ? C44 C45 1.373(9) . ? C45 C46 1.402(9) . ? C51 C56 1.392(8) . ? C51 C52 1.407(8) . ? C52 C53 1.380(8) . ? C53 C54 1.383(8) . ? C54 C55 1.364(9) . ? C55 C56 1.385(8) . ? C61 C66 1.380(8) . ? C61 C62 1.397(8) . ? C62 C63 1.380(8) . ? C63 C64 1.383(8) . ? C64 C65 1.386(9) . ? C65 C66 1.370(8) . ? 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 C21 Sn C11 108.6(2) . . ? C21 Sn C1 109.2(2) . . ? C11 Sn C1 140.9(2) . . ? C21 Sn Cl3 95.0(2) . . ? C11 Sn Cl3 94.79(19) . . ? C1 Sn Cl3 91.7(2) . . ? C21 Sn Br3 99.85(18) . . ? C11 Sn Br3 90.90(15) . . ? C1 Sn Br3 92.36(16) . . ? Cl3 Sn Br3 5.39(16) . . ? C21 Sn Br1 87.4(2) . . ? C11 Sn Br1 86.5(2) . . ? C1 Sn Br1 85.5(2) . . ? Cl3 Sn Br1 176.8(2) . . ? Br3 Sn Br1 172.78(15) . . ? C21 Sn Cl1 89.5(2) . . ? C11 Sn Cl1 85.21(18) . . ? C1 Sn Cl1 85.37(19) . . ? Cl3 Sn Cl1 175.23(17) . . ? Br3 Sn Cl1 170.63(12) . . ? Br1 Sn Cl1 2.2(2) . . ? C18 Ga C8 126.9(2) . . ? C18 Ga Cl2 106.1(2) . . ? C8 Ga Cl2 106.4(2) . . ? C18 Ga Br2 104.1(2) . . ? C8 Ga Br2 104.3(2) . . ? Cl2 Ga Br2 5.5(2) . . ? C18 Ga Cl1 107.8(2) . . ? C8 Ga Cl1 107.1(2) . . ? Cl2 Ga Cl1 99.09(17) . . ? Br2 Ga Cl1 104.58(19) . . ? C18 Ga Br1 107.3(2) . . ? C8 Ga Br1 105.4(3) . . ? Cl2 Ga Br1 102.18(19) . . ? Br2 Ga Br1 107.7(2) . . ? Cl1 Ga Br1 3.2(3) . . ? Ga Br1 Sn 77.2(2) . . ? Ga Cl1 Sn 76.20(16) . . ? C61 P C31 108.8(3) . . ? C61 P C41 111.7(3) . . ? C31 P C41 110.8(3) . . ? C61 P C51 107.9(3) . . ? C31 P C51 109.7(3) . . ? C41 P C51 107.8(3) . . ? C2 C1 C9 119.8(6) . . ? C2 C1 Sn 109.5(4) . . ? C9 C1 Sn 130.4(5) . . ? C1 C2 C3 122.4(6) . . ? C4 C3 C2 119.8(6) . . ? C3 C4 C10 120.2(6) . . ? C6 C5 C10 119.7(6) . . ? C5 C6 C7 120.9(6) . . ? C8 C7 C6 122.2(6) . . ? C7 C8 C9 118.0(6) . . ? C7 C8 Ga 115.2(5) . . ? C9 C8 Ga 126.5(4) . . ? C8 C9 C1 124.0(6) . . ? C8 C9 C10 119.6(5) . . ? C1 C9 C10 116.4(6) . . ? C4 C10 C5 119.7(6) . . ? C4 C10 C9 121.1(6) . . ? C5 C10 C9 119.2(6) . . ? C12 C11 C19 119.5(6) . . ? C12 C11 Sn 111.2(4) . . ? C19 C11 Sn 128.9(4) . . ? C11 C12 C13 121.1(6) . . ? C14 C13 C12 120.6(6) . . ? C13 C14 C20 121.0(6) . . ? C16 C15 C20 121.1(6) . . ? C15 C16 C17 120.0(6) . . ? C18 C17 C16 121.9(6) . . ? C17 C18 C19 117.8(6) . . ? C17 C18 Ga 114.3(4) . . ? C19 C18 Ga 127.5(4) . . ? C18 C19 C20 119.8(6) . . ? C18 C19 C11 123.0(5) . . ? C20 C19 C11 117.2(5) . . ? C15 C20 C14 120.6(6) . . ? C15 C20 C19 119.0(6) . . ? C14 C20 C19 120.3(6) . . ? C32 C31 C36 119.7(6) . . ? C32 C31 P 121.1(5) . . ? C36 C31 P 118.8(5) . . ? C31 C32 C33 119.2(6) . . ? C34 C33 C32 121.0(6) . . ? C33 C34 C35 120.2(6) . . ? C36 C35 C34 118.9(6) . . ? C35 C36 C31 120.9(6) . . ? C42 C41 C46 120.0(6) . . ? C42 C41 P 119.0(5) . . ? C46 C41 P 121.0(5) . . ? C41 C42 C43 119.5(6) . . ? C44 C43 C42 119.4(6) . . ? C43 C44 C45 122.4(6) . . ? C44 C45 C46 118.4(6) . . ? C41 C46 C45 120.2(6) . . ? C56 C51 C52 119.8(6) . . ? C56 C51 P 120.7(5) . . ? C52 C51 P 119.2(5) . . ? C53 C52 C51 119.4(6) . . ? C52 C53 C54 120.0(6) . . ? C55 C54 C53 120.8(6) . . ? C54 C55 C56 120.6(6) . . ? C55 C56 C51 119.4(6) . . ? C66 C61 C62 119.5(6) . . ? C66 C61 P 121.2(5) . . ? C62 C61 P 119.3(4) . . ? C63 C62 C61 119.5(6) . . ? C62 C63 C64 121.0(6) . . ? C63 C64 C65 118.8(6) . . ? C66 C65 C64 120.9(6) . . ? C65 C66 C61 120.4(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.142 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.131 ###END data_5 _database_code_CSD 199220 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H35 Cl2 Ga I P Sn' _chemical_formula_weight 992.91 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 10.2589(7) _cell_length_b 29.596(2) _cell_length_c 12.9930(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.6600(10) _cell_angle_gamma 90.00 _cell_volume 3936.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 2.311 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25839 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6907 _reflns_number_gt 6552 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0468P)^2^+17.3551P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6907 _refine_ls_number_parameters 458 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _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 Sn Sn 0.54767(3) 0.121235(11) 0.33513(3) 0.02913(11) Uani 1 1 d . . . Ga Ga 0.23972(5) 0.160512(17) 0.32176(4) 0.02542(14) Uani 1 1 d . . . I1 I 0.3777(3) 0.16415(9) 0.4999(2) 0.0405(8) Uiso 0.204(2) 1 d P A 1 I2 I 0.0349(4) 0.19788(14) 0.3586(3) 0.0463(12) Uiso 0.162(2) 1 d P A 2 I3 I 0.67973(7) 0.08221(3) 0.17945(5) 0.0327(2) Uiso 0.6346(18) 1 d P A 3 Cl1 Cl 0.3727(2) 0.16481(8) 0.4730(2) 0.0378(5) Uiso 0.796(2) 1 d P A 1 Cl2 Cl 0.0540(3) 0.19244(9) 0.3684(2) 0.0378(5) Uiso 0.838(2) 1 d P A 2 Cl3 Cl 0.6897(5) 0.08136(18) 0.2025(4) 0.0378(5) Uiso 0.3654(18) 1 d P A 3 P P 0.73327(13) 0.39396(4) 0.37744(9) 0.0260(3) Uani 1 1 d . . . C1 C 0.4220(5) 0.06319(16) 0.3440(4) 0.0285(10) Uani 1 1 d . A . C2 C 0.4964(5) 0.02550(17) 0.3695(4) 0.0349(12) Uani 1 1 d . . . H2A H 0.5855 0.0290 0.3856 0.042 Uiso 1 1 calc R A . C3 C 0.4413(6) -0.01846(18) 0.3719(4) 0.0363(12) Uani 1 1 d . A . H3A H 0.4929 -0.0431 0.3925 0.044 Uiso 1 1 calc R . . C4 C 0.3122(6) -0.02423(17) 0.3437(4) 0.0346(12) Uani 1 1 d . . . H4A H 0.2767 -0.0532 0.3419 0.042 Uiso 1 1 calc R A . C5 C 0.0982(6) 0.00646(18) 0.2861(4) 0.0342(12) Uani 1 1 d . . . H5A H 0.0647 -0.0227 0.2823 0.041 Uiso 1 1 calc R A . C6 C 0.0183(6) 0.04230(18) 0.2618(4) 0.0362(12) Uani 1 1 d . A . H6A H -0.0688 0.0376 0.2403 0.043 Uiso 1 1 calc R . . C7 C 0.0688(5) 0.08656(18) 0.2696(4) 0.0319(11) Uani 1 1 d . . . H7A H 0.0128 0.1106 0.2539 0.038 Uiso 1 1 calc R A . C8 C 0.1976(5) 0.09575(17) 0.2996(3) 0.0276(10) Uani 1 1 d . A . C9 C 0.2845(5) 0.05831(16) 0.3200(3) 0.0262(10) Uani 1 1 d . . . C10 C 0.2313(5) 0.01335(17) 0.3170(4) 0.0289(11) Uani 1 1 d . A . C11 C 0.5543(5) 0.18655(16) 0.2616(4) 0.0283(10) Uani 1 1 d . A . C12 C 0.6821(5) 0.20046(17) 0.2573(4) 0.0314(11) Uani 1 1 d . . . H12A H 0.7483 0.1839 0.2920 0.038 Uiso 1 1 calc R A . C13 C 0.7144(5) 0.23946(17) 0.2011(4) 0.0336(12) Uani 1 1 d . A . H13A H 0.8008 0.2490 0.2011 0.040 Uiso 1 1 calc R . . C14 C 0.6190(5) 0.26288(16) 0.1474(4) 0.0321(11) Uani 1 1 d . . . H14A H 0.6409 0.2875 0.1076 0.039 Uiso 1 1 calc R A . C15 C 0.3874(6) 0.27440(17) 0.0934(4) 0.0346(12) Uani 1 1 d . . . H15A H 0.4101 0.2981 0.0511 0.041 Uiso 1 1 calc R A . C16 C 0.2590(6) 0.26315(18) 0.0994(4) 0.0377(12) Uani 1 1 d . A . H16A H 0.1949 0.2787 0.0598 0.045 Uiso 1 1 calc R . . C17 C 0.2235(5) 0.22808(17) 0.1653(4) 0.0333(11) Uani 1 1 d . . . H17A H 0.1354 0.2217 0.1704 0.040 Uiso 1 1 calc R A . C18 C 0.3148(5) 0.20279(15) 0.2226(4) 0.0274(10) Uani 1 1 d . A . C19 C 0.4496(5) 0.21224(15) 0.2127(4) 0.0263(10) Uani 1 1 d . . . C20 C 0.4866(5) 0.25019(16) 0.1513(4) 0.0310(11) Uani 1 1 d . A . C21 C 0.6971(6) 0.11819(18) 0.4576(5) 0.0414(14) Uani 1 1 d . A . H21A H 0.7739 0.1044 0.4329 0.062 Uiso 1 1 calc R . . H21B H 0.6668 0.1006 0.5133 0.062 Uiso 1 1 calc R . . H21C H 0.7176 0.1482 0.4815 0.062 Uiso 1 1 calc R . . C31 C 0.6194(5) 0.35675(17) 0.4342(4) 0.0278(10) Uani 1 1 d . . . C32 C 0.5358(5) 0.37240(17) 0.5063(4) 0.0335(11) Uani 1 1 d . . . H32A H 0.5439 0.4017 0.5317 0.040 Uiso 1 1 calc R . . C33 C 0.4400(6) 0.34374(19) 0.5401(4) 0.0400(13) Uani 1 1 d . . . H33A H 0.3840 0.3540 0.5885 0.048 Uiso 1 1 calc R . . C34 C 0.4272(5) 0.30012(19) 0.5023(4) 0.0363(12) Uani 1 1 d . . . H34A H 0.3609 0.2816 0.5236 0.044 Uiso 1 1 calc R . . C35 C 0.5131(6) 0.28414(18) 0.4329(4) 0.0356(12) Uani 1 1 d . . . H35A H 0.5057 0.2546 0.4087 0.043 Uiso 1 1 calc R . . C36 C 0.6107(5) 0.31220(17) 0.3991(4) 0.0331(11) Uani 1 1 d . . . H36A H 0.6696 0.3013 0.3535 0.040 Uiso 1 1 calc R . . C41 C 0.7589(5) 0.44375(17) 0.4550(4) 0.0293(11) Uani 1 1 d . . . C42 C 0.6672(6) 0.47812(18) 0.4473(4) 0.0401(13) Uani 1 1 d . . . H42A H 0.5934 0.4750 0.4024 0.048 Uiso 1 1 calc R . . C43 C 0.6843(7) 0.5172(2) 0.5062(5) 0.0472(15) Uani 1 1 d . . . H43A H 0.6236 0.5405 0.4994 0.057 Uiso 1 1 calc R . . C44 C 0.7915(7) 0.52112(19) 0.5743(4) 0.0440(14) Uani 1 1 d . . . H44A H 0.8030 0.5472 0.6138 0.053 Uiso 1 1 calc R . . C45 C 0.8824(6) 0.4868(2) 0.5847(4) 0.0430(14) Uani 1 1 d . . . H45A H 0.9540 0.4897 0.6319 0.052 Uiso 1 1 calc R . . C46 C 0.8673(6) 0.44815(19) 0.5251(4) 0.0373(12) Uani 1 1 d . . . H46A H 0.9291 0.4252 0.5317 0.045 Uiso 1 1 calc R . . C51 C 0.6688(5) 0.41131(16) 0.2510(4) 0.0266(10) Uani 1 1 d . . . C52 C 0.7231(5) 0.44936(18) 0.2049(4) 0.0322(11) Uani 1 1 d . . . H52A H 0.7852 0.4669 0.2416 0.039 Uiso 1 1 calc R . . C53 C 0.6831(5) 0.46043(19) 0.1045(4) 0.0360(12) Uani 1 1 d . . . H53A H 0.7187 0.4856 0.0738 0.043 Uiso 1 1 calc R . . C54 C 0.5905(5) 0.43452(18) 0.0490(4) 0.0348(12) Uani 1 1 d . . . H54A H 0.5647 0.4422 -0.0186 0.042 Uiso 1 1 calc R . . C55 C 0.5367(5) 0.39722(18) 0.0943(4) 0.0353(12) Uani 1 1 d . . . H55A H 0.4744 0.3799 0.0570 0.042 Uiso 1 1 calc R . . C56 C 0.5754(5) 0.38539(17) 0.1955(4) 0.0314(11) Uani 1 1 d . . . H56A H 0.5391 0.3603 0.2258 0.038 Uiso 1 1 calc R . . C61 C 0.8835(5) 0.36426(17) 0.3632(4) 0.0305(11) Uani 1 1 d . . . C62 C 0.9425(5) 0.34055(19) 0.4471(4) 0.0362(12) Uani 1 1 d . . . H62A H 0.9026 0.3394 0.5093 0.043 Uiso 1 1 calc R . . C63 C 1.0609(6) 0.3187(2) 0.4371(5) 0.0441(14) Uani 1 1 d . . . H63A H 1.1011 0.3035 0.4932 0.053 Uiso 1 1 calc R . . C64 C 1.1194(6) 0.3195(2) 0.3439(5) 0.0476(15) Uani 1 1 d . . . H64A H 1.1985 0.3048 0.3373 0.057 Uiso 1 1 calc R . . C65 C 1.0595(7) 0.3422(2) 0.2610(5) 0.0568(19) Uani 1 1 d . . . H65A H 1.0983 0.3424 0.1982 0.068 Uiso 1 1 calc R . . C66 C 0.9428(6) 0.3646(2) 0.2701(4) 0.0452(15) Uani 1 1 d . . . H66A H 0.9038 0.3800 0.2138 0.054 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 Sn 0.0350(2) 0.02282(18) 0.0289(2) 0.00254(13) -0.00389(14) -0.00393(13) Ga 0.0323(3) 0.0211(3) 0.0231(3) 0.0008(2) 0.0030(2) -0.0029(2) P 0.0335(7) 0.0240(6) 0.0204(6) 0.0019(5) 0.0011(5) 0.0005(5) C1 0.037(3) 0.023(2) 0.025(2) 0.0004(19) 0.002(2) -0.003(2) C2 0.038(3) 0.027(3) 0.039(3) 0.001(2) -0.003(2) -0.002(2) C3 0.050(3) 0.025(3) 0.033(3) 0.003(2) 0.004(2) 0.004(2) C4 0.057(3) 0.023(2) 0.025(3) 0.002(2) 0.005(2) -0.003(2) C5 0.051(3) 0.029(3) 0.023(3) -0.003(2) 0.002(2) -0.013(2) C6 0.040(3) 0.034(3) 0.034(3) 0.005(2) -0.001(2) -0.012(2) C7 0.039(3) 0.032(3) 0.024(2) 0.003(2) -0.003(2) -0.003(2) C8 0.038(3) 0.028(2) 0.018(2) 0.0030(19) 0.004(2) -0.005(2) C9 0.041(3) 0.023(2) 0.015(2) 0.0005(18) 0.0032(19) -0.003(2) C10 0.042(3) 0.027(2) 0.018(2) -0.0007(19) 0.005(2) -0.005(2) C11 0.040(3) 0.024(2) 0.021(2) -0.0019(19) 0.005(2) -0.002(2) C12 0.036(3) 0.027(3) 0.032(3) -0.005(2) 0.005(2) 0.000(2) C13 0.041(3) 0.027(3) 0.036(3) -0.008(2) 0.017(2) -0.010(2) C14 0.049(3) 0.021(2) 0.028(3) -0.001(2) 0.012(2) -0.004(2) C15 0.054(3) 0.022(2) 0.028(3) 0.005(2) 0.007(2) -0.005(2) C16 0.054(3) 0.026(3) 0.033(3) 0.006(2) 0.001(2) 0.000(2) C17 0.041(3) 0.028(3) 0.031(3) 0.003(2) 0.000(2) -0.005(2) C18 0.039(3) 0.019(2) 0.025(2) -0.0032(19) 0.003(2) -0.0039(19) C19 0.043(3) 0.018(2) 0.019(2) -0.0044(18) 0.007(2) -0.004(2) C20 0.045(3) 0.022(2) 0.026(3) -0.006(2) 0.007(2) -0.004(2) C21 0.051(3) 0.029(3) 0.042(3) 0.006(2) -0.022(3) -0.008(2) C31 0.034(3) 0.028(2) 0.021(2) 0.0004(19) 0.000(2) -0.001(2) C32 0.044(3) 0.027(3) 0.029(3) -0.003(2) 0.004(2) 0.001(2) C33 0.049(3) 0.037(3) 0.036(3) 0.002(2) 0.016(3) 0.000(2) C34 0.035(3) 0.041(3) 0.033(3) 0.006(2) -0.001(2) -0.008(2) C35 0.052(3) 0.029(3) 0.026(3) 0.000(2) 0.002(2) -0.008(2) C36 0.045(3) 0.031(3) 0.024(2) -0.002(2) 0.005(2) 0.000(2) C41 0.039(3) 0.027(2) 0.022(2) 0.0014(19) 0.005(2) -0.003(2) C42 0.051(3) 0.033(3) 0.035(3) -0.003(2) -0.004(3) 0.003(2) C43 0.068(4) 0.031(3) 0.042(3) -0.004(3) 0.004(3) 0.004(3) C44 0.077(4) 0.028(3) 0.027(3) -0.002(2) 0.007(3) -0.011(3) C45 0.059(4) 0.042(3) 0.027(3) -0.001(2) -0.001(3) -0.011(3) C46 0.045(3) 0.039(3) 0.027(3) 0.002(2) -0.001(2) 0.001(2) C51 0.033(3) 0.025(2) 0.022(2) -0.0020(19) 0.000(2) 0.0060(19) C52 0.033(3) 0.035(3) 0.028(3) 0.002(2) -0.002(2) -0.003(2) C53 0.037(3) 0.042(3) 0.029(3) 0.006(2) 0.002(2) -0.004(2) C54 0.045(3) 0.037(3) 0.022(2) 0.002(2) -0.001(2) 0.009(2) C55 0.045(3) 0.030(3) 0.029(3) -0.003(2) -0.011(2) 0.000(2) C56 0.039(3) 0.024(2) 0.030(3) 0.001(2) 0.000(2) 0.004(2) C61 0.035(3) 0.027(3) 0.030(3) 0.003(2) 0.003(2) 0.002(2) C62 0.037(3) 0.043(3) 0.029(3) 0.009(2) 0.003(2) 0.006(2) C63 0.049(3) 0.044(3) 0.040(3) 0.018(3) 0.004(3) 0.012(3) C64 0.046(3) 0.047(4) 0.051(4) 0.012(3) 0.010(3) 0.018(3) C65 0.060(4) 0.074(5) 0.038(3) 0.016(3) 0.019(3) 0.030(4) C66 0.055(4) 0.049(3) 0.032(3) 0.013(3) 0.010(3) 0.021(3) _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 Sn C21 2.140(5) . ? Sn C1 2.155(5) . ? Sn C11 2.159(5) . ? Sn Cl3 2.609(5) . ? Sn I3 2.7589(8) . ? Sn Cl1 2.916(2) . ? Sn I1 3.116(3) . ? Ga C8 1.982(5) . ? Ga C18 1.986(5) . ? Ga Cl2 2.245(3) . ? Ga Cl1 2.323(3) . ? Ga I2 2.448(4) . ? Ga I1 2.637(3) . ? P C61 1.794(5) . ? P C41 1.795(5) . ? P C31 1.798(5) . ? P C51 1.806(5) . ? C1 C2 1.380(7) . ? C1 C9 1.433(7) . ? C2 C3 1.420(7) . ? C3 C4 1.362(8) . ? C4 C10 1.417(7) . ? C5 C6 1.365(8) . ? C5 C10 1.414(7) . ? C6 C7 1.410(7) . ? C7 C8 1.380(7) . ? C8 C9 1.436(7) . ? C9 C10 1.438(7) . ? C11 C12 1.378(7) . ? C11 C19 1.432(7) . ? C12 C13 1.416(7) . ? C13 C14 1.356(8) . ? C14 C20 1.413(8) . ? C15 C16 1.366(8) . ? C15 C20 1.421(8) . ? C16 C17 1.408(7) . ? C17 C18 1.379(7) . ? C18 C19 1.425(7) . ? C19 C20 1.443(7) . ? C31 C32 1.389(7) . ? C31 C36 1.396(7) . ? C32 C33 1.390(8) . ? C33 C34 1.384(8) . ? C34 C35 1.385(8) . ? C35 C36 1.394(7) . ? C41 C42 1.385(8) . ? C41 C46 1.398(8) . ? C42 C43 1.392(8) . ? C43 C44 1.372(9) . ? C44 C45 1.379(9) . ? C45 C46 1.385(8) . ? C51 C56 1.392(7) . ? C51 C52 1.407(7) . ? C52 C53 1.381(7) . ? C53 C54 1.387(8) . ? C54 C55 1.383(8) . ? C55 C56 1.395(7) . ? C61 C66 1.389(8) . ? C61 C62 1.401(7) . ? C62 C63 1.390(8) . ? C63 C64 1.385(8) . ? C64 C65 1.381(9) . ? C65 C66 1.380(8) . ? 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 C21 Sn C1 109.2(2) . . ? C21 Sn C11 109.0(2) . . ? C1 Sn C11 140.64(19) . . ? C21 Sn Cl3 93.9(2) . . ? C1 Sn Cl3 92.05(18) . . ? C11 Sn Cl3 94.48(18) . . ? C21 Sn I3 99.53(18) . . ? C1 Sn I3 91.65(13) . . ? C11 Sn I3 91.13(13) . . ? Cl3 Sn I3 5.82(13) . . ? C21 Sn Cl1 90.10(19) . . ? C1 Sn Cl1 85.76(14) . . ? C11 Sn Cl1 85.05(14) . . ? Cl3 Sn Cl1 175.87(13) . . ? I3 Sn Cl1 170.34(6) . . ? C21 Sn I1 84.95(19) . . ? C1 Sn I1 85.73(14) . . ? C11 Sn I1 88.50(14) . . ? Cl3 Sn I1 177.02(13) . . ? I3 Sn I1 175.36(5) . . ? Cl1 Sn I1 5.47(7) . . ? C8 Ga C18 127.23(19) . . ? C8 Ga Cl2 105.38(16) . . ? C18 Ga Cl2 106.31(16) . . ? C8 Ga Cl1 106.66(15) . . ? C18 Ga Cl1 106.45(16) . . ? Cl2 Ga Cl1 102.22(9) . . ? C8 Ga I2 106.45(18) . . ? C18 Ga I2 102.42(17) . . ? Cl2 Ga I2 4.63(14) . . ? Cl1 Ga I2 105.98(11) . . ? C8 Ga I1 105.48(15) . . ? C18 Ga I1 109.57(16) . . ? Cl2 Ga I1 99.41(9) . . ? Cl1 Ga I1 3.60(10) . . ? I2 Ga I1 103.28(11) . . ? Ga I1 Sn 70.93(6) . . ? Ga Cl1 Sn 78.91(8) . . ? C61 P C41 111.4(2) . . ? C61 P C31 109.1(2) . . ? C41 P C31 110.4(2) . . ? C61 P C51 108.2(2) . . ? C41 P C51 108.0(2) . . ? C31 P C51 109.7(2) . . ? C2 C1 C9 119.5(4) . . ? C2 C1 Sn 109.5(4) . . ? C9 C1 Sn 130.7(4) . . ? C1 C2 C3 122.1(5) . . ? C4 C3 C2 119.4(5) . . ? C3 C4 C10 120.7(5) . . ? C6 C5 C10 120.6(5) . . ? C5 C6 C7 119.5(5) . . ? C8 C7 C6 123.0(5) . . ? C7 C8 C9 118.1(5) . . ? C7 C8 Ga 115.3(4) . . ? C9 C8 Ga 126.3(4) . . ? C1 C9 C8 123.6(4) . . ? C1 C9 C10 117.8(4) . . ? C8 C9 C10 118.6(5) . . ? C5 C10 C4 119.7(5) . . ? C5 C10 C9 119.9(5) . . ? C4 C10 C9 120.3(5) . . ? C12 C11 C19 120.8(5) . . ? C12 C11 Sn 110.0(4) . . ? C19 C11 Sn 128.9(4) . . ? C11 C12 C13 121.3(5) . . ? C14 C13 C12 119.8(5) . . ? C13 C14 C20 120.6(5) . . ? C16 C15 C20 120.5(5) . . ? C15 C16 C17 120.1(5) . . ? C18 C17 C16 122.4(5) . . ? C17 C18 C19 118.3(4) . . ? C17 C18 Ga 114.5(4) . . ? C19 C18 Ga 126.9(4) . . ? C18 C19 C11 124.1(4) . . ? C18 C19 C20 119.6(5) . . ? C11 C19 C20 116.3(5) . . ? C14 C20 C15 120.3(5) . . ? C14 C20 C19 121.0(5) . . ? C15 C20 C19 118.7(5) . . ? C32 C31 C36 120.4(5) . . ? C32 C31 P 121.2(4) . . ? C36 C31 P 118.3(4) . . ? C31 C32 C33 119.2(5) . . ? C34 C33 C32 120.7(5) . . ? C33 C34 C35 120.0(5) . . ? C34 C35 C36 120.2(5) . . ? C35 C36 C31 119.4(5) . . ? C42 C41 C46 119.1(5) . . ? C42 C41 P 119.2(4) . . ? C46 C41 P 121.6(4) . . ? C41 C42 C43 120.6(6) . . ? C44 C43 C42 119.5(6) . . ? C43 C44 C45 120.7(5) . . ? C44 C45 C46 120.2(6) . . ? C45 C46 C41 119.8(5) . . ? C56 C51 C52 119.9(5) . . ? C56 C51 P 121.0(4) . . ? C52 C51 P 118.9(4) . . ? C53 C52 C51 119.4(5) . . ? C52 C53 C54 120.8(5) . . ? C55 C54 C53 119.9(5) . . ? C54 C55 C56 120.3(5) . . ? C51 C56 C55 119.7(5) . . ? C66 C61 C62 119.3(5) . . ? C66 C61 P 120.9(4) . . ? C62 C61 P 119.8(4) . . ? C63 C62 C61 119.9(5) . . ? C64 C63 C62 120.2(5) . . ? C65 C64 C63 119.7(5) . . ? C66 C65 C64 120.8(6) . . ? C65 C66 C61 120.1(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.770 _refine_diff_density_min -1.549 _refine_diff_density_rms 0.102