Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Fischer, Roland A.' 'Cheng, Q. M.' 'Merz, K.' 'Stark, O.' 'Winter, Manuela' _publ_contact_author_name 'Prof Roland A Fischer' _publ_contact_author_address ; Lehrstuhl fur Anorganische Chemie II Ruhr-Universitat Bochum Organometallics & Materials Chemist Universitatstrasse 150 Bochum 44780 GERMANY ; _publ_contact_author_email 'ROLAND.FISCHER@RUHR-UNI-BOCHUM.DE' _publ_section_title ; Lew base properties of tris(trimethylstannyl)amine: Unusually short M-N bonds of the adduct compounds [X3M.N(SnMe3)3] (X = Cl, Br; M = Al, Ga, In) and [Cl2(CH3)M.N(SnMe3)3] (M = Al, Ga) ; data_md433 _database_code_CSD 148506 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H27 Br3 In N Sn3' _chemical_formula_weight 859.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 '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' 'In' 'In' -0.7276 1.3100 '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 'cubic' _symmetry_space_group_name_H-M 'P2(1)3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' _cell_length_a 12.989(3) _cell_length_b 12.989(3) _cell_length_c 12.989(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2191.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 15.0 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 9.875 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.732 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 axs CCD 1000' _diffrn_measurement_method '\scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3882 _diffrn_reflns_av_R_equivalents 0.0701 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 3 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 24.97 _reflns_number_total 1277 _reflns_number_gt 1145 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART' _computing_cell_refinement 'SMART' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker axs SHELXTL-97' _computing_publication_material 'SHELXL-97' _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^)+(0.0141P)^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 SHELXL _refine_ls_extinction_coef 0.00083(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.028(17) _refine_ls_number_reflns 1277 _refine_ls_number_parameters 56 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0440 _refine_ls_wR_factor_gt 0.0425 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.10091(3) 0.27802(3) 0.82422(4) 0.02735(14) Uani 1 1 d . . . In1 In 0.34238(3) 0.15762(3) 0.84238(3) 0.0293(2) Uani 1 3 d S . . Br1 Br 0.52908(5) 0.18459(6) 0.80113(6) 0.0452(2) Uani 1 1 d . . . N1 N 0.2465(4) 0.2535(4) 0.7465(4) 0.027(2) Uani 1 3 d S . . C1 C 0.1269(5) 0.4005(5) 0.9287(5) 0.0381(18) Uani 1 1 d . . . H11 H 0.0631 0.4350 0.9426 0.057 Uiso 1 1 calc R . . H12 H 0.1748 0.4484 0.8991 0.057 Uiso 1 1 calc R . . H13 H 0.1547 0.3737 0.9917 0.057 Uiso 1 1 calc R . . C2 C 0.0606(5) 0.1385(5) 0.8996(6) 0.0398(19) Uani 1 1 d . . . H21 H 0.1116 0.0870 0.8850 0.060 Uiso 1 1 calc R . . H22 H -0.0053 0.1155 0.8754 0.060 Uiso 1 1 calc R . . H23 H 0.0574 0.1500 0.9726 0.060 Uiso 1 1 calc R . . C3 C -0.0095(5) 0.3193(6) 0.7087(6) 0.0450(19) Uani 1 1 d . . . H31 H -0.0778 0.3073 0.7344 0.067 Uiso 1 1 calc R . . H32 H 0.0016 0.2783 0.6482 0.067 Uiso 1 1 calc R . . H33 H -0.0018 0.3908 0.6916 0.067 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0246(3) 0.0292(3) 0.0283(3) 0.0008(2) 0.0018(2) 0.0032(2) In1 0.0293(2) 0.0293(2) 0.0293(2) 0.0052(2) -0.0052(2) 0.0052(2) Br1 0.0292(4) 0.0577(5) 0.0486(5) 0.0046(4) -0.0041(3) 0.0037(4) N1 0.027(2) 0.027(2) 0.027(2) 0.003(2) -0.003(2) 0.003(2) C1 0.041(5) 0.039(4) 0.033(4) -0.001(3) 0.009(3) 0.007(4) C2 0.037(4) 0.037(5) 0.045(5) 0.008(4) 0.009(4) 0.006(3) C3 0.035(4) 0.054(5) 0.046(5) 0.000(4) -0.009(4) 0.017(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 Sn1 C1 2.119(7) . ? Sn1 C2 2.125(6) . ? Sn1 C3 2.144(6) . ? Sn1 N1 2.167(3) . ? In1 N1 2.158(8) . ? In1 Br1 2.5081(9) 6_456 ? In1 Br1 2.5081(9) . ? In1 Br1 2.5081(9) 12_565 ? N1 Sn1 2.167(3) 12_565 ? N1 Sn1 2.167(3) 6_456 ? C1 H11 0.9600 . ? C1 H12 0.9600 . ? C1 H13 0.9600 . ? C2 H21 0.9600 . ? C2 H22 0.9600 . ? C2 H23 0.9600 . ? C3 H31 0.9600 . ? C3 H32 0.9600 . ? C3 H33 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sn1 C2 112.6(3) . . ? C1 Sn1 C3 111.6(3) . . ? C2 Sn1 C3 111.8(3) . . ? C1 Sn1 N1 105.64(19) . . ? C2 Sn1 N1 107.7(3) . . ? C3 Sn1 N1 107.1(3) . . ? N1 In1 Br1 110.75(2) . 6_456 ? N1 In1 Br1 110.75(2) . . ? Br1 In1 Br1 108.17(3) 6_456 . ? N1 In1 Br1 110.75(2) . 12_565 ? Br1 In1 Br1 108.17(3) 6_456 12_565 ? Br1 In1 Br1 108.17(3) . 12_565 ? In1 N1 Sn1 108.6(2) . 12_565 ? In1 N1 Sn1 108.6(2) . 6_456 ? Sn1 N1 Sn1 110.3(2) 12_565 6_456 ? In1 N1 Sn1 108.6(2) . . ? Sn1 N1 Sn1 110.3(2) 12_565 . ? Sn1 N1 Sn1 110.3(2) 6_456 . ? Sn1 C1 H11 109.5 . . ? Sn1 C1 H12 109.5 . . ? H11 C1 H12 109.5 . . ? Sn1 C1 H13 109.5 . . ? H11 C1 H13 109.5 . . ? H12 C1 H13 109.5 . . ? Sn1 C2 H21 109.5 . . ? Sn1 C2 H22 109.5 . . ? H21 C2 H22 109.5 . . ? Sn1 C2 H23 109.5 . . ? H21 C2 H23 109.5 . . ? H22 C2 H23 109.5 . . ? Sn1 C3 H31 109.5 . . ? Sn1 C3 H32 109.5 . . ? H31 C3 H32 109.5 . . ? Sn1 C3 H33 109.5 . . ? H31 C3 H33 109.5 . . ? H32 C3 H33 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br1 In1 N1 Sn1 -35.99(2) 6_456 . . 12_565 ? Br1 In1 N1 Sn1 84.01(2) . . . 12_565 ? Br1 In1 N1 Sn1 -155.99(2) 12_565 . . 12_565 ? Br1 In1 N1 Sn1 -155.99(2) 6_456 . . 6_456 ? Br1 In1 N1 Sn1 -35.99(2) . . . 6_456 ? Br1 In1 N1 Sn1 84.01(2) 12_565 . . 6_456 ? Br1 In1 N1 Sn1 84.01(2) 6_456 . . . ? Br1 In1 N1 Sn1 -155.99(2) . . . . ? Br1 In1 N1 Sn1 -35.99(2) 12_565 . . . ? C1 Sn1 N1 In1 82.8(2) . . . . ? C2 Sn1 N1 In1 -37.8(2) . . . . ? C3 Sn1 N1 In1 -158.2(2) . . . . ? C1 Sn1 N1 Sn1 -158.3(3) . . . 12_565 ? C2 Sn1 N1 Sn1 81.2(4) . . . 12_565 ? C3 Sn1 N1 Sn1 -39.2(4) . . . 12_565 ? C1 Sn1 N1 Sn1 -36.2(4) . . . 6_456 ? C2 Sn1 N1 Sn1 -156.7(3) . . . 6_456 ? C3 Sn1 N1 Sn1 82.9(3) . . . 6_456 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.444 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.135 data_md453 _database_code_CSD 148507 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H27 Cl3 In N Sn3' _chemical_formula_weight 726.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'In' 'In' -0.7276 1.3100 '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 cubic _symmetry_space_group_name_H-M P2(1)3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' _cell_length_a 12.9021(12) _cell_length_b 12.9021(12) _cell_length_c 12.9021(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2147.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 4.867 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.764 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 axs CCD 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5260 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.03 _reflns_number_total 1277 _reflns_number_gt 1244 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART' _computing_cell_refinement 'SMART' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker axs SHELXTL-PLUS' _computing_publication_material 'SHELXL-97' _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^)+(0.0255P)^2^+1.7592P] 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 0.52(7) _refine_ls_number_reflns 1277 _refine_ls_number_parameters 55 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0227 _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0507 _refine_ls_wR_factor_gt 0.0503 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.92355(3) 0.02794(3) 0.14860(3) 0.03085(11) Uani 1 1 d . . . In1 In 0.90655(3) -0.09345(3) -0.09345(3) 0.03473(16) Uani 1 3 d S . . Cl1 Cl 0.94935(12) -0.07296(14) -0.27052(11) 0.0531(4) Uani 1 1 d . . . N1 N 1.0027(3) 0.0027(3) 0.0027(3) 0.0233(14) Uani 1 3 d S . . C1 C 1.0391(5) 0.0683(5) 0.2625(4) 0.0465(14) Uani 1 1 d . . . H1A H 1.0761 0.1288 0.2400 0.070 Uiso 1 1 calc R . . H1B H 1.0868 0.0118 0.2706 0.070 Uiso 1 1 calc R . . H1C H 1.0059 0.0823 0.3276 0.070 Uiso 1 1 calc R . . C2 C 0.8463(5) -0.1135(4) 0.1872(5) 0.0456(14) Uani 1 1 d . . . H2A H 0.8587 -0.1297 0.2588 0.068 Uiso 1 1 calc R . . H2B H 0.8724 -0.1685 0.1445 0.068 Uiso 1 1 calc R . . H2C H 0.7732 -0.1057 0.1758 0.068 Uiso 1 1 calc R . . C3 C 0.8154(4) 0.1504(5) 0.1223(4) 0.0405(13) Uani 1 1 d . . . H3A H 0.7534 0.1226 0.0920 0.061 Uiso 1 1 calc R . . H3B H 0.8454 0.2004 0.0761 0.061 Uiso 1 1 calc R . . H3C H 0.7989 0.1831 0.1870 0.061 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0317(2) 0.0319(2) 0.02895(19) -0.00309(14) 0.00218(14) -0.00102(14) In1 0.03473(16) 0.03473(16) 0.03473(16) -0.00629(15) -0.00629(15) -0.00629(15) Cl1 0.0590(9) 0.0667(10) 0.0334(7) -0.0046(7) -0.0066(6) -0.0068(8) N1 0.0233(14) 0.0233(14) 0.0233(14) -0.0027(15) -0.0027(15) -0.0027(15) C1 0.050(3) 0.053(4) 0.037(3) -0.010(3) -0.006(3) 0.001(3) C2 0.054(4) 0.040(3) 0.042(3) -0.001(2) 0.010(3) -0.017(3) C3 0.036(3) 0.042(3) 0.043(3) -0.008(3) 0.005(2) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C3 2.134(6) . ? Sn1 C2 2.138(5) . ? Sn1 C1 2.157(6) . ? Sn1 N1 2.166(2) . ? In1 N1 2.148(6) . ? In1 Cl1 2.3652(15) 9_654 ? In1 Cl1 2.3652(15) . ? In1 Cl1 2.3652(15) 5_645 ? N1 Sn1 2.166(2) 5_645 ? N1 Sn1 2.166(2) 9_654 ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? 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 C3 Sn1 C2 111.3(2) . . ? C3 Sn1 C1 112.4(2) . . ? C2 Sn1 C1 111.7(2) . . ? C3 Sn1 N1 106.34(15) . . ? C2 Sn1 N1 107.1(2) . . ? C1 Sn1 N1 107.6(2) . . ? N1 In1 Cl1 111.00(4) . 9_654 ? N1 In1 Cl1 111.00(4) . . ? Cl1 In1 Cl1 107.90(4) 9_654 . ? N1 In1 Cl1 111.00(4) . 5_645 ? Cl1 In1 Cl1 107.90(4) 9_654 5_645 ? Cl1 In1 Cl1 107.90(4) . 5_645 ? In1 N1 Sn1 108.46(15) . . ? In1 N1 Sn1 108.46(15) . 5_645 ? Sn1 N1 Sn1 110.46(15) . 5_645 ? In1 N1 Sn1 108.46(15) . 9_654 ? Sn1 N1 Sn1 110.46(15) . 9_654 ? Sn1 N1 Sn1 110.46(15) 5_645 9_654 ? Sn1 C1 H1A 109.5 . . ? Sn1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sn1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Sn1 C2 H2A 109.5 . . ? Sn1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sn1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Sn1 C3 H3A 109.5 . . ? Sn1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Sn1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 In1 N1 Sn1 -82.32(5) 9_654 . . . ? Cl1 In1 N1 Sn1 157.68(5) . . . . ? Cl1 In1 N1 Sn1 37.68(5) 5_645 . . . ? Cl1 In1 N1 Sn1 37.68(5) 9_654 . . 5_645 ? Cl1 In1 N1 Sn1 -82.32(5) . . . 5_645 ? Cl1 In1 N1 Sn1 157.68(5) 5_645 . . 5_645 ? Cl1 In1 N1 Sn1 157.68(5) 9_654 . . 9_654 ? Cl1 In1 N1 Sn1 37.68(5) . . . 9_654 ? Cl1 In1 N1 Sn1 -82.32(5) 5_645 . . 9_654 ? C3 Sn1 N1 In1 -81.73(17) . . . . ? C2 Sn1 N1 In1 37.40(18) . . . . ? C1 Sn1 N1 In1 157.60(18) . . . . ? C3 Sn1 N1 Sn1 159.5(2) . . . 5_645 ? C2 Sn1 N1 Sn1 -81.3(3) . . . 5_645 ? C1 Sn1 N1 Sn1 38.9(3) . . . 5_645 ? C3 Sn1 N1 Sn1 37.0(3) . . . 9_654 ? C2 Sn1 N1 Sn1 156.1(3) . . . 9_654 ? C1 Sn1 N1 Sn1 -83.6(3) . . . 9_654 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.621 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.087 data_md499 _database_code_CSD 148508 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H30 Al Cl2 N Sn3' _chemical_formula_weight 618.30 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' 'Al' 'Al' 0.0645 0.0514 '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' 'N' 'N' 0.0061 0.0033 '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 12.7027(15) _cell_length_b 13.0934(15) _cell_length_c 12.7027(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2112.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 15.0 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.944 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 3.800 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.552 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 axs CCD1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4833 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.07 _reflns_number_total 2891 _reflns_number_gt 2846 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART' _computing_cell_refinement 'SMART' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker axs SHELXTL-PLUS' _computing_publication_material 'SHELXL-97' _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 w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+9.4503P] 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 0.02(6) _refine_ls_number_reflns 2891 _refine_ls_number_parameters 154 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1054 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.07309(4) 0.39571(4) 0.76515(6) 0.02983(18) Uani 1 d . . . C4 C 0.2596(8) 0.1785(9) 0.7071(10) 0.047(3) Uani 1 d . . . H4A H 0.3116 0.1254 0.7186 0.070 Uiso 1 calc R . . H4B H 0.2811 0.2402 0.7436 0.070 Uiso 1 calc R . . H4C H 0.2539 0.1924 0.6323 0.070 Uiso 1 calc R . . Sn2 Sn 0.11172(5) 0.12959(5) 0.76561(6) 0.03365(19) Uani 1 d . . . N1 N -0.0007(5) 0.2500(5) 0.7381(6) 0.0213(17) Uani 1 d . . . Sn3 Sn -0.13082(4) 0.23117(5) 0.84661(7) 0.03331(19) Uani 1 d . . . C1 C 0.1781(9) 0.3785(9) 0.8955(10) 0.046(3) Uani 1 d . . . H1A H 0.2129 0.4431 0.9093 0.069 Uiso 1 calc R . . H1B H 0.2304 0.3270 0.8789 0.069 Uiso 1 calc R . . H1C H 0.1386 0.3577 0.9572 0.069 Uiso 1 calc R . . C7 C -0.2651(8) 0.3102(8) 0.7887(10) 0.046(3) Uani 1 d . . . H7A H -0.2491 0.3824 0.7830 0.069 Uiso 1 calc R . . H7B H -0.3235 0.3006 0.8368 0.069 Uiso 1 calc R . . H7C H -0.2837 0.2836 0.7199 0.069 Uiso 1 calc R . . Al1 Al -0.0475(2) 0.2430(2) 0.5946(3) 0.0312(7) Uani 1 d . . . C2 C 0.1602(9) 0.4355(9) 0.6268(10) 0.045(3) Uani 1 d . . . H2A H 0.1944 0.5009 0.6373 0.068 Uiso 1 calc R . . H2B H 0.1127 0.4399 0.5672 0.068 Uiso 1 calc R . . H2C H 0.2130 0.3836 0.6132 0.068 Uiso 1 calc R . . Cl2 Cl -0.1105(2) 0.3903(2) 0.5553(3) 0.0505(7) Uani 1 d . . . C3 C -0.0437(9) 0.5077(8) 0.8026(9) 0.046(3) Uani 1 d . . . H3A H -0.0099 0.5732 0.8146 0.069 Uiso 1 calc R . . H3B H -0.0812 0.4871 0.8656 0.069 Uiso 1 calc R . . H3C H -0.0929 0.5137 0.7446 0.069 Uiso 1 calc R . . C8 C -0.1578(11) 0.0685(8) 0.8621(11) 0.055(3) Uani 1 d . . . H8A H -0.2156 0.0567 0.9105 0.082 Uiso 1 calc R . . H8B H -0.0947 0.0359 0.8890 0.082 Uiso 1 calc R . . H8C H -0.1751 0.0399 0.7938 0.082 Uiso 1 calc R . . Cl3 Cl -0.1787(2) 0.1372(2) 0.5885(3) 0.0495(7) Uani 1 d . . . C9 C -0.0852(9) 0.2958(9) 0.9934(9) 0.042(3) Uani 1 d . . . H9A H -0.0750 0.3687 0.9852 0.062 Uiso 1 calc R . . H9B H -0.0200 0.2646 1.0168 0.062 Uiso 1 calc R . . H9C H -0.1398 0.2834 1.0452 0.062 Uiso 1 calc R . . C10 C 0.0636(7) 0.1961(8) 0.4923(8) 0.030(2) Uani 1 d . . . H10A H 0.1228 0.2428 0.4944 0.045 Uiso 1 calc R . . H10B H 0.0344 0.1948 0.4217 0.045 Uiso 1 calc R . . H10C H 0.0871 0.1281 0.5114 0.045 Uiso 1 calc R . . C5 C 0.1183(10) 0.1054(10) 0.9327(11) 0.052(3) Uani 1 d . . . H5A H 0.1684 0.0516 0.9481 0.078 Uiso 1 calc R . . H5B H 0.0492 0.0858 0.9581 0.078 Uiso 1 calc R . . H5C H 0.1403 0.1680 0.9672 0.078 Uiso 1 calc R . . C6 C 0.0595(9) -0.0077(8) 0.6898(11) 0.047(3) Uani 1 d . . . H6A H 0.1103 -0.0617 0.7021 0.071 Uiso 1 calc R . . H6B H 0.0529 0.0042 0.6147 0.071 Uiso 1 calc R . . H6C H -0.0083 -0.0277 0.7183 0.071 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0281(3) 0.0244(3) 0.0370(4) -0.0025(4) -0.0012(3) -0.0020(2) C4 0.037(5) 0.049(6) 0.054(8) -0.001(6) 0.013(5) 0.006(5) Sn2 0.0319(3) 0.0296(3) 0.0394(4) -0.0002(4) 0.0011(4) 0.0072(2) N1 0.020(3) 0.015(3) 0.029(5) -0.007(3) -0.005(3) 0.000(2) Sn3 0.0289(3) 0.0320(3) 0.0389(5) -0.0035(3) 0.0061(3) -0.0007(2) C1 0.042(6) 0.040(6) 0.055(9) -0.018(5) -0.015(5) -0.005(4) C7 0.029(4) 0.050(6) 0.058(9) -0.003(6) 0.006(4) 0.013(4) Al1 0.0287(12) 0.0336(14) 0.031(2) -0.0041(13) -0.0028(12) 0.0023(11) C2 0.047(6) 0.037(6) 0.051(8) 0.007(5) 0.012(5) -0.012(5) Cl2 0.0535(16) 0.0492(17) 0.0486(19) 0.0052(13) -0.0082(13) 0.0134(13) C3 0.059(7) 0.025(5) 0.053(8) -0.013(5) -0.009(5) 0.012(5) C8 0.086(8) 0.030(5) 0.047(8) -0.010(6) 0.026(7) -0.020(5) Cl3 0.0361(12) 0.0511(15) 0.061(2) -0.0193(14) -0.0075(12) -0.0089(10) C9 0.050(6) 0.049(6) 0.026(7) -0.003(5) 0.003(5) 0.008(5) C10 0.033(4) 0.043(5) 0.014(6) -0.004(4) 0.011(4) -0.007(4) C5 0.062(8) 0.058(8) 0.035(8) 0.019(6) 0.008(6) 0.025(6) C6 0.057(6) 0.027(5) 0.057(8) -0.025(6) -0.002(6) 0.010(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 Sn1 C1 2.138(11) . ? Sn1 C3 2.140(10) . ? Sn1 C2 2.141(11) . ? Sn1 N1 2.154(6) . ? C4 Sn2 2.120(11) . ? Sn2 C6 2.144(10) . ? Sn2 C5 2.147(13) . ? Sn2 N1 2.156(6) . ? N1 Al1 1.919(8) . ? N1 Sn3 2.166(7) . ? Sn3 C7 2.126(10) . ? Sn3 C9 2.128(12) . ? Sn3 C8 2.166(10) . ? Al1 C10 2.014(9) . ? Al1 Cl2 2.148(4) . ? Al1 Cl3 2.168(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sn1 C3 109.4(4) . . ? C1 Sn1 C2 109.8(5) . . ? C3 Sn1 C2 112.0(5) . . ? C1 Sn1 N1 107.6(4) . . ? C3 Sn1 N1 109.9(4) . . ? C2 Sn1 N1 108.0(4) . . ? C4 Sn2 C6 111.7(5) . . ? C4 Sn2 C5 110.9(5) . . ? C6 Sn2 C5 109.4(5) . . ? C4 Sn2 N1 108.0(4) . . ? C6 Sn2 N1 109.6(3) . . ? C5 Sn2 N1 107.1(4) . . ? Al1 N1 Sn1 109.2(4) . . ? Al1 N1 Sn2 108.9(3) . . ? Sn1 N1 Sn2 109.5(3) . . ? Al1 N1 Sn3 111.3(3) . . ? Sn1 N1 Sn3 109.3(3) . . ? Sn2 N1 Sn3 108.6(3) . . ? C7 Sn3 C9 109.2(4) . . ? C7 Sn3 N1 109.7(4) . . ? C9 Sn3 N1 107.7(4) . . ? C7 Sn3 C8 112.5(5) . . ? C9 Sn3 C8 110.7(5) . . ? N1 Sn3 C8 106.9(4) . . ? N1 Al1 C10 114.3(4) . . ? N1 Al1 Cl2 107.1(3) . . ? C10 Al1 Cl2 112.6(4) . . ? N1 Al1 Cl3 107.6(3) . . ? C10 Al1 Cl3 108.7(3) . . ? Cl2 Al1 Cl3 106.19(16) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 2.183 _refine_diff_density_min -1.037 _refine_diff_density_rms 0.174 data_MD520 _database_code_CSD 148509 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H30 Cl2 Ga N Sn3' _chemical_formula_weight 661.04 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' 'Sn' 'Sn' -0.6537 1.4246 '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' _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 12.719(3) _cell_length_b 13.047(3) _cell_length_c 12.719(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2110.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 15.0 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.080 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 5.011 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6760 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 axs CCD 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4848 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.13 _reflns_number_total 2947 _reflns_number_gt 2696 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART' _computing_cell_refinement 'SMART' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'bruker axs SHELXTL-PLUS' _computing_publication_material 'SHELXL-97' _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 w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+53.6694P] 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 0.46(8) _refine_ls_number_reflns 2947 _refine_ls_number_parameters 154 _refine_ls_number_restraints 67 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.1909 _refine_ls_wR_factor_gt 0.1869 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.005 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.07321(9) 0.39621(9) 0.86825(15) 0.0292(3) Uani 1 d . . . Sn2 Sn 0.11142(10) 0.12901(10) 0.86993(15) 0.0345(4) Uani 1 d . . . N1 N -0.0006(11) 0.2512(10) 0.8451(12) 0.018(3) Uani 1 d U . . Sn3 Sn -0.13100(11) 0.23157(11) 0.95015(13) 0.0354(4) Uani 1 d . . . Ga1 Ga -0.04651(19) 0.24250(18) 0.6948(2) 0.0349(6) Uani 1 d . . . Cl1 Cl -0.1131(5) 0.3946(5) 0.6591(5) 0.0481(15) Uani 1 d . . . Cl2 Cl -0.1832(5) 0.1363(5) 0.6943(6) 0.0476(14) Uani 1 d . . . C10 C 0.0622(15) 0.1943(16) 0.5897(17) 0.030(4) Uani 1 d U . . H10A H 0.1216 0.2408 0.5902 0.045 Uiso 1 calc R . . H10B H 0.0313 0.1929 0.5199 0.045 Uiso 1 calc R . . H10C H 0.0857 0.1260 0.6085 0.045 Uiso 1 calc R . . C1 C -0.0404(18) 0.5085(14) 0.9030(18) 0.035(5) Uani 1 d U . . H1A H -0.0767 0.4902 0.9674 0.053 Uiso 1 calc R . . H1B H -0.0907 0.5126 0.8458 0.053 Uiso 1 calc R . . H1C H -0.0062 0.5744 0.9118 0.053 Uiso 1 calc R . . C2 C 0.1584(16) 0.4364(16) 0.7245(18) 0.031(5) Uani 1 d U . . H2A H 0.1088 0.4443 0.6671 0.047 Uiso 1 calc R . . H2B H 0.2080 0.3825 0.7076 0.047 Uiso 1 calc R . . H2C H 0.1959 0.5003 0.7351 0.047 Uiso 1 calc R . . C3 C 0.180(2) 0.3816(16) 0.997(2) 0.045(6) Uani 1 d U . . H3A H 0.1415 0.3656 1.0607 0.067 Uiso 1 calc R . . H3B H 0.2180 0.4455 1.0066 0.067 Uiso 1 calc R . . H3C H 0.2300 0.3270 0.9825 0.067 Uiso 1 calc R . . C6 C -0.2615(16) 0.3150(18) 0.8926(17) 0.037(5) Uani 1 d U . . H6A H -0.2814 0.2887 0.8241 0.056 Uiso 1 calc R . . H6B H -0.2429 0.3868 0.8865 0.056 Uiso 1 calc R . . H6C H -0.3201 0.3077 0.9409 0.056 Uiso 1 calc R . . C5 C -0.1553(19) 0.0697(15) 0.964(2) 0.043(5) Uani 1 d U . . H5A H -0.1741 0.0417 0.8958 0.065 Uiso 1 calc R . . H5B H -0.2116 0.0566 1.0136 0.065 Uiso 1 calc R . . H5C H -0.0912 0.0374 0.9887 0.065 Uiso 1 calc R . . C9 C 0.0588(18) -0.0054(15) 0.7908(19) 0.038(5) Uani 1 d U . . H9A H 0.0583 0.0067 0.7156 0.057 Uiso 1 calc R . . H9B H -0.0117 -0.0223 0.8142 0.057 Uiso 1 calc R . . H9C H 0.1058 -0.0619 0.8068 0.057 Uiso 1 calc R . . C7 C 0.112(2) 0.097(2) 1.040(2) 0.043(6) Uani 1 d U . . H7A H 0.1606 0.0418 1.0554 0.064 Uiso 1 calc R . . H7B H 0.0415 0.0767 1.0624 0.064 Uiso 1 calc R . . H7C H 0.1326 0.1579 1.0785 0.064 Uiso 1 calc R . . C8 C 0.2562(19) 0.1762(17) 0.808(2) 0.042(5) Uani 1 d U . . H8A H 0.2490 0.1886 0.7335 0.063 Uiso 1 calc R . . H8B H 0.3083 0.1231 0.8201 0.063 Uiso 1 calc R . . H8C H 0.2784 0.2388 0.8430 0.063 Uiso 1 calc R . . C4 C -0.086(2) 0.293(2) 1.1031(19) 0.046(6) Uani 1 d U . . H4A H -0.0754 0.3662 1.0976 0.069 Uiso 1 calc R . . H4B H -0.0205 0.2608 1.1257 0.069 Uiso 1 calc R . . H4C H -0.1404 0.2785 1.1539 0.069 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0266(7) 0.0285(6) 0.0326(7) -0.0022(7) -0.0005(7) -0.0018(4) Sn2 0.0323(7) 0.0340(7) 0.0373(8) 0.0002(8) -0.0001(8) 0.0067(5) N1 0.024(6) 0.015(5) 0.016(6) 0.000(5) 0.000(5) 0.001(5) Sn3 0.0288(7) 0.0401(7) 0.0372(8) -0.0047(7) 0.0059(7) -0.0013(6) Ga1 0.0304(12) 0.0415(12) 0.0329(13) -0.0054(11) -0.0026(10) 0.0032(9) Cl1 0.056(4) 0.052(4) 0.037(3) 0.006(3) -0.006(3) 0.015(3) Cl2 0.036(3) 0.050(3) 0.056(4) -0.021(3) -0.005(3) -0.011(2) C10 0.019(9) 0.043(10) 0.027(10) 0.007(8) -0.002(7) -0.005(7) C1 0.050(11) 0.016(8) 0.041(11) -0.001(7) 0.005(8) 0.001(8) C2 0.030(10) 0.030(9) 0.033(11) 0.010(8) 0.013(8) -0.010(7) C3 0.054(12) 0.026(9) 0.055(13) -0.030(9) -0.001(10) -0.007(9) C6 0.027(9) 0.059(11) 0.026(11) -0.004(8) 0.004(8) 0.009(8) C5 0.050(12) 0.030(9) 0.050(13) -0.007(9) 0.009(10) -0.006(8) C9 0.049(11) 0.026(9) 0.039(11) -0.017(9) 0.002(9) 0.008(8) C7 0.047(12) 0.057(12) 0.025(10) 0.004(9) 0.002(9) 0.013(9) C8 0.043(11) 0.042(10) 0.041(12) -0.003(9) 0.004(9) 0.003(9) C4 0.065(13) 0.050(11) 0.023(10) -0.013(9) -0.009(10) 0.016(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C1 2.10(2) . ? Sn1 N1 2.132(13) . ? Sn1 C3 2.14(3) . ? Sn1 C2 2.19(2) . ? Sn2 C8 2.09(2) . ? Sn2 C9 2.13(2) . ? Sn2 N1 2.161(14) . ? Sn2 C7 2.21(3) . ? N1 Ga1 2.001(15) . ? N1 Sn3 2.146(15) . ? Sn3 C6 2.12(2) . ? Sn3 C5 2.14(2) . ? Sn3 C4 2.18(2) . ? Ga1 C10 2.02(2) . ? Ga1 Cl1 2.205(7) . ? Ga1 Cl2 2.223(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sn1 N1 110.1(7) . . ? C1 Sn1 C3 109.8(9) . . ? N1 Sn1 C3 107.9(7) . . ? C1 Sn1 C2 110.4(8) . . ? N1 Sn1 C2 108.4(7) . . ? C3 Sn1 C2 110.3(9) . . ? C8 Sn2 C9 110.0(9) . . ? C8 Sn2 N1 107.9(7) . . ? C9 Sn2 N1 109.3(7) . . ? C8 Sn2 C7 115.0(10) . . ? C9 Sn2 C7 107.9(10) . . ? N1 Sn2 C7 106.5(7) . . ? Ga1 N1 Sn1 108.1(6) . . ? Ga1 N1 Sn3 111.2(7) . . ? Sn1 N1 Sn3 111.1(6) . . ? Ga1 N1 Sn2 106.9(6) . . ? Sn1 N1 Sn2 110.1(6) . . ? Sn3 N1 Sn2 109.3(6) . . ? C6 Sn3 C5 115.0(10) . . ? C6 Sn3 N1 109.3(7) . . ? C5 Sn3 N1 106.3(7) . . ? C6 Sn3 C4 109.2(9) . . ? C5 Sn3 C4 109.0(11) . . ? N1 Sn3 C4 107.9(9) . . ? N1 Ga1 C10 116.7(7) . . ? N1 Ga1 Cl1 104.9(4) . . ? C10 Ga1 Cl1 113.9(6) . . ? N1 Ga1 Cl2 105.5(4) . . ? C10 Ga1 Cl2 109.8(6) . . ? Cl1 Ga1 Cl2 105.1(3) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 25.13 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 4.403 _refine_diff_density_min -1.124 _refine_diff_density_rms 0.311 data_md351 _database_code_CSD 161554 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H27 Cl3 Ga N Sn3' _chemical_formula_weight 681.46 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' '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 12.6570(13) _cell_length_b 13.0934(13) _cell_length_c 12.6714(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2099.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 10.0? _cell_measurement_theta_max 15.0 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 5.163 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.570 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 axs CCD 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4843 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2156 _reflns_number_gt 2089 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART' _computing_cell_refinement 'SMART' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker axs SHELXTL-PLUS' _computing_publication_material 'SHELXL-97' _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^)+(0.0796P)^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 0.00(4) _refine_ls_number_reflns 2156 _refine_ls_number_parameters 175 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1001 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 Sn31 Sn 1.1030(10) 0.8424(9) 0.2578(10) 0.030(3) Uiso 0.05 1 d PD A 1 Sn21 Sn 0.9906(11) 0.5978(7) 0.2871(11) 0.030(3) Uiso 0.05 1 d PD B 1 Sn11 Sn 0.8392(8) 0.8125(11) 0.3550(11) 0.039(3) Uiso 0.05 1 d PD C 1 Ga1 Ga 1.05031(9) 0.74442(8) 0.49509(8) 0.0276(3) Uani 1 1 d . D 2 Cl1 Cl 1.1814(2) 0.6361(2) 0.5095(2) 0.0467(7) Uani 1 1 d . D 2 Cl2 Cl 0.9280(2) 0.6970(3) 0.6058(2) 0.0498(7) Uani 1 1 d . D 2 Cl3 Cl 1.1087(3) 0.8945(2) 0.5424(2) 0.0448(7) Uani 1 1 d . D 2 N1 N 0.9979(5) 0.7498(4) 0.3505(6) 0.0206(15) Uani 1 1 d D D 2 Sn1 Sn 0.92515(5) 0.89657(4) 0.32459(6) 0.0272(2) Uani 0.95 1 d P D 2 C11 C 0.8409(11) 0.9355(10) 0.4649(9) 0.049(3) Uani 1 1 d . D 2 H11A H 0.7934 0.9909 0.4504 0.074 Uiso 1 1 calc R D 2 H11B H 0.8900 0.9556 0.5187 0.074 Uiso 1 1 calc R D 2 H11C H 0.8013 0.8773 0.4887 0.074 Uiso 1 1 calc R D 2 C12 C 1.0464(10) 1.0070(8) 0.2904(10) 0.047(3) Uani 1 1 d . D 2 H12A H 1.0853 0.9858 0.2292 0.070 Uiso 1 1 calc R D 2 H12B H 1.0934 1.0123 0.3495 0.070 Uiso 1 1 calc R D 2 H12C H 1.0145 1.0723 0.2771 0.070 Uiso 1 1 calc R D 2 C13 C 0.8193(8) 0.8770(9) 0.1962(9) 0.039(2) Uani 1 1 d . D 2 H13A H 0.7669 0.9300 0.1977 0.058 Uiso 1 1 calc R D 2 H13B H 0.7853 0.8116 0.2018 0.058 Uiso 1 1 calc R D 2 H13C H 0.8577 0.8805 0.1310 0.058 Uiso 1 1 calc R D 2 Sn2 Sn 0.88397(5) 0.62897(5) 0.32774(5) 0.0296(2) Uani 0.95 1 d P D 2 C21 C 0.8787(11) 0.6041(11) 0.1607(10) 0.055(4) Uani 1 1 d . D 2 H21A H 0.9223 0.6537 0.1259 0.082 Uiso 1 1 calc R D 2 H21B H 0.8072 0.6107 0.1364 0.082 Uiso 1 1 calc R D 2 H21C H 0.9041 0.5367 0.1451 0.082 Uiso 1 1 calc R D 2 C22 C 0.7320(10) 0.6806(10) 0.3876(10) 0.052(3) Uani 1 1 d . D 2 H22A H 0.6911 0.7086 0.3307 0.077 Uiso 1 1 calc R D 2 H22B H 0.7429 0.7321 0.4404 0.077 Uiso 1 1 calc R D 2 H22C H 0.6948 0.6240 0.4181 0.077 Uiso 1 1 calc R D 2 C23 C 0.9366(9) 0.4948(8) 0.4057(10) 0.047(3) Uani 1 1 d . D 2 H23A H 0.9102 0.4357 0.3693 0.070 Uiso 1 1 calc R D 2 H23B H 0.9110 0.4946 0.4770 0.070 Uiso 1 1 calc R D 2 H23C H 1.0125 0.4932 0.4061 0.070 Uiso 1 1 calc R D 2 Sn3 Sn 1.13001(5) 0.72866(5) 0.24309(6) 0.0289(2) Uani 0.95 1 d P D 2 C31 C 1.1565(12) 0.5684(8) 0.2319(10) 0.054(3) Uani 1 1 d . D 2 H31A H 1.1918 0.5449 0.2944 0.081 Uiso 1 1 calc R D 2 H31B H 1.1996 0.5542 0.1713 0.081 Uiso 1 1 calc R D 2 H31C H 1.0900 0.5338 0.2249 0.081 Uiso 1 1 calc R D 2 C32 C 1.2654(8) 0.8085(9) 0.3042(8) 0.043(3) Uani 1 1 d . D 2 H32A H 1.3049 0.7637 0.3494 0.065 Uiso 1 1 calc R D 2 H32B H 1.2424 0.8669 0.3437 0.065 Uiso 1 1 calc R D 2 H32C H 1.3093 0.8304 0.2467 0.065 Uiso 1 1 calc R D 2 C33 C 1.0853(9) 0.7932(9) 0.0940(9) 0.041(2) Uani 1 1 d . D 2 H33A H 1.0465 0.7435 0.0540 0.062 Uiso 1 1 calc R D 2 H33B H 1.1476 0.8127 0.0557 0.062 Uiso 1 1 calc R D 2 H33C H 1.0419 0.8522 0.1056 0.062 Uiso 1 1 calc R D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.0310(5) 0.0313(5) 0.0206(5) 0.0043(4) -0.0026(4) -0.0028(4) Cl1 0.0367(14) 0.0511(16) 0.0521(17) 0.0181(13) -0.0061(12) 0.0079(11) Cl2 0.0516(17) 0.0656(19) 0.0322(13) 0.0108(13) 0.0132(11) -0.0063(14) Cl3 0.0574(17) 0.0449(16) 0.0319(13) -0.0053(11) -0.0083(13) -0.0132(12) N1 0.026(4) 0.019(3) 0.017(3) 0.000(2) 0.000(3) 0.001(3) Sn1 0.0302(4) 0.0241(3) 0.0273(3) 0.0018(3) -0.0015(3) 0.0019(2) C11 0.068(8) 0.050(7) 0.030(5) -0.002(5) 0.016(6) 0.015(6) C12 0.062(7) 0.025(5) 0.052(6) 0.015(5) -0.010(6) -0.007(5) C13 0.025(5) 0.052(6) 0.039(6) 0.003(5) -0.012(5) 0.002(4) Sn2 0.0345(4) 0.0277(4) 0.0265(3) 0.0001(3) 0.0013(3) -0.0084(2) C21 0.076(10) 0.059(9) 0.029(6) -0.008(6) -0.008(6) -0.034(6) C22 0.051(7) 0.060(7) 0.044(6) -0.001(6) 0.004(6) -0.016(6) C23 0.046(6) 0.040(6) 0.055(6) 0.009(6) -0.003(5) -0.014(5) Sn3 0.0302(3) 0.0303(4) 0.0261(4) 0.0038(3) 0.0067(3) 0.0013(2) C31 0.088(9) 0.034(6) 0.041(6) 0.006(5) 0.029(7) 0.030(6) C32 0.025(5) 0.069(7) 0.034(6) 0.002(5) -0.001(4) -0.017(5) C33 0.042(6) 0.050(7) 0.031(5) 0.016(5) 0.004(5) -0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N1 1.950(7) . ? Ga1 Cl2 2.180(3) . ? Ga1 Cl3 2.183(3) . ? Ga1 Cl1 2.190(3) . ? N1 Sn1 2.156(6) . ? N1 Sn2 2.161(6) . ? N1 Sn3 2.174(7) . ? Sn1 C13 2.123(10) . ? Sn1 C11 2.135(11) . ? Sn1 C12 2.153(11) . ? Sn2 C23 2.123(11) . ? Sn2 C21 2.142(12) . ? Sn2 C22 2.176(13) . ? Sn3 C31 2.130(10) . ? Sn3 C33 2.145(11) . ? Sn3 C32 2.151(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ga1 Cl2 111.9(2) . . ? N1 Ga1 Cl3 109.91(19) . . ? Cl2 Ga1 Cl3 108.66(13) . . ? N1 Ga1 Cl1 111.1(2) . . ? Cl2 Ga1 Cl1 107.45(12) . . ? Cl3 Ga1 Cl1 107.66(13) . . ? Ga1 N1 Sn1 108.7(3) . . ? Ga1 N1 Sn2 109.0(3) . . ? Sn1 N1 Sn2 110.3(3) . . ? Ga1 N1 Sn3 108.8(3) . . ? Sn1 N1 Sn3 110.3(3) . . ? Sn2 N1 Sn3 109.7(3) . . ? C13 Sn1 C11 110.6(5) . . ? C13 Sn1 C12 112.1(4) . . ? C11 Sn1 C12 111.3(5) . . ? C13 Sn1 N1 106.2(4) . . ? C11 Sn1 N1 107.4(4) . . ? C12 Sn1 N1 109.0(4) . . ? C23 Sn2 C21 110.1(6) . . ? C23 Sn2 N1 109.5(3) . . ? C21 Sn2 N1 105.3(4) . . ? C23 Sn2 C22 111.9(5) . . ? C21 Sn2 C22 111.3(5) . . ? N1 Sn2 C22 108.4(4) . . ? C31 Sn3 C33 111.8(5) . . ? C31 Sn3 C32 112.2(5) . . ? C33 Sn3 C32 109.6(4) . . ? C31 Sn3 N1 106.8(4) . . ? C33 Sn3 N1 107.4(4) . . ? C32 Sn3 N1 109.0(3) . . ? 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 Cl2 Ga1 N1 Sn1 85.3(3) . . . . ? Cl3 Ga1 N1 Sn1 -35.5(3) . . . . ? Cl1 Ga1 N1 Sn1 -154.5(2) . . . . ? Cl2 Ga1 N1 Sn2 -35.0(3) . . . . ? Cl3 Ga1 N1 Sn2 -155.8(2) . . . . ? Cl1 Ga1 N1 Sn2 85.2(3) . . . . ? Cl2 Ga1 N1 Sn3 -154.52(19) . . . . ? Cl3 Ga1 N1 Sn3 84.6(3) . . . . ? Cl1 Ga1 N1 Sn3 -34.4(3) . . . . ? Ga1 N1 Sn1 C13 -157.6(4) . . . . ? Sn2 N1 Sn1 C13 -38.1(5) . . . . ? Sn3 N1 Sn1 C13 83.2(4) . . . . ? Ga1 N1 Sn1 C11 -39.2(5) . . . . ? Sn2 N1 Sn1 C11 80.3(5) . . . . ? Sn3 N1 Sn1 C11 -158.4(5) . . . . ? Ga1 N1 Sn1 C12 81.5(4) . . . . ? Sn2 N1 Sn1 C12 -159.0(4) . . . . ? Sn3 N1 Sn1 C12 -37.7(5) . . . . ? Ga1 N1 Sn2 C23 -39.9(5) . . . . ? Sn1 N1 Sn2 C23 -159.2(4) . . . . ? Sn3 N1 Sn2 C23 79.1(5) . . . . ? Ga1 N1 Sn2 C21 -158.3(5) . . . . ? Sn1 N1 Sn2 C21 82.4(5) . . . . ? Sn3 N1 Sn2 C21 -39.3(6) . . . . ? Ga1 N1 Sn2 C22 82.4(4) . . . . ? Sn1 N1 Sn2 C22 -36.9(5) . . . . ? Sn3 N1 Sn2 C22 -158.6(4) . . . . ? Ga1 N1 Sn3 C31 82.4(5) . . . . ? Sn1 N1 Sn3 C31 -158.4(5) . . . . ? Sn2 N1 Sn3 C31 -36.7(5) . . . . ? Ga1 N1 Sn3 C33 -157.6(4) . . . . ? Sn1 N1 Sn3 C33 -38.4(5) . . . . ? Sn2 N1 Sn3 C33 83.3(4) . . . . ? Ga1 N1 Sn3 C32 -38.9(4) . . . . ? Sn1 N1 Sn3 C32 80.2(5) . . . . ? Sn2 N1 Sn3 C32 -158.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 2.023 _refine_diff_density_min -1.661 _refine_diff_density_rms 0.222 data_md394 _database_code_CSD 161555 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H27 Br3 Ga N Sn3' _chemical_formula_weight 814.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M P2(1)3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' _cell_length_a 12.9467(10) _cell_length_b 12.9467(10) _cell_length_c 12.9467(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2170.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 15.0 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 10.151 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.609 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 axs CCD 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5337 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.05 _reflns_number_total 1299 _reflns_number_gt 1265 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART' _computing_cell_refinement 'SMART' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER axs SHELXTL-PLUS' _computing_publication_material 'SHELXL-97' _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^)+(0.0001P)^2^+195.7444P] 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 0.49(7) _refine_ls_number_reflns 1299 _refine_ls_number_parameters 52 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.1921 _refine_ls_wR_factor_gt 0.1918 _refine_ls_goodness_of_fit_ref 1.203 _refine_ls_restrained_S_all 1.203 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.92217(14) 1.02577(14) 1.14592(14) 0.0265(4) Uani 1 1 d . . . Br1 Br 0.9486(2) 0.9370(3) 0.7366(2) 0.0417(8) Uani 1 1 d . . . Ga1 Ga 0.9120 0.9120 0.9120 0.0270(10) Uani 1 3 d S . . N1 N 0.9992 0.9992 0.9992 0.020(7) Uiso 1 3 d S . . C1 C 1.044(3) 1.068(2) 1.254(2) 0.042(8) Uani 1 1 d . . . H1A H 1.0145 1.0774 1.3216 0.063 Uiso 1 1 calc R . . H1B H 1.0754 1.1314 1.2320 0.063 Uiso 1 1 calc R . . H1C H 1.0946 1.0144 1.2563 0.063 Uiso 1 1 calc R . . C2 C 0.820(3) 1.155(2) 1.119(2) 0.044(8) Uani 1 1 d . . . H2A H 0.7633 1.1333 1.0766 0.066 Uiso 1 1 calc R . . H2B H 0.8574 1.2091 1.0844 0.066 Uiso 1 1 calc R . . H2C H 0.7945 1.1802 1.1838 0.066 Uiso 1 1 calc R . . C3 C 0.853(3) 0.883(3) 1.194(3) 0.061(11) Uani 1 1 d . . . H3A H 0.7809 0.8942 1.2089 0.091 Uiso 1 1 calc R . . H3B H 0.8871 0.8575 1.2541 0.091 Uiso 1 1 calc R . . H3C H 0.8586 0.8330 1.1390 0.091 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0259(9) 0.0285(10) 0.0251(9) -0.0038(7) 0.0016(8) -0.0033(7) Br1 0.0437(18) 0.054(2) 0.0278(14) -0.0048(13) -0.0035(12) -0.0045(14) Ga1 0.0270(10) 0.0270(10) 0.0270(10) -0.0027(12) -0.0027(12) -0.0027(12) C1 0.07(2) 0.042(17) 0.017(12) -0.006(12) 0.018(13) 0.011(16) C2 0.06(2) 0.040(18) 0.034(17) -0.006(14) -0.007(14) -0.008(15) C3 0.05(2) 0.10(3) 0.037(18) -0.010(18) -0.017(16) 0.01(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C3 2.15(4) . ? Sn1 C2 2.16(3) . ? Sn1 N1 2.1731(18) . ? Sn1 C1 2.18(3) . ? Br1 Ga1 2.342(3) . ? Ga1 N1 1.95385(16) . ? Ga1 Br1 2.342(3) 9 ? Ga1 Br1 2.342(3) 5 ? N1 Sn1 2.1731(18) 5 ? N1 Sn1 2.1731(18) 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 C3 Sn1 C2 117.2(13) . . ? C3 Sn1 N1 107.9(10) . . ? C2 Sn1 N1 105.2(8) . . ? C3 Sn1 C1 109.6(12) . . ? C2 Sn1 C1 110.5(11) . . ? N1 Sn1 C1 105.7(7) . . ? N1 Ga1 Br1 111.31(8) . . ? N1 Ga1 Br1 111.31(8) . 9 ? Br1 Ga1 Br1 107.58(8) . 9 ? N1 Ga1 Br1 111.31(8) . 5 ? Br1 Ga1 Br1 107.58(8) . 5 ? Br1 Ga1 Br1 107.58(8) 9 5 ? Ga1 N1 Sn1 109.36(5) . 5 ? Ga1 N1 Sn1 109.36(5) . . ? Sn1 N1 Sn1 109.58(5) 5 . ? Ga1 N1 Sn1 109.36(5) . 9 ? Sn1 N1 Sn1 109.58(5) 5 9 ? Sn1 N1 Sn1 109.58(5) . 9 ? 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 Br1 Ga1 N1 Sn1 -84.76(10) . . . 5 ? Br1 Ga1 N1 Sn1 35.24(10) 9 . . 5 ? Br1 Ga1 N1 Sn1 155.24(10) 5 . . 5 ? Br1 Ga1 N1 Sn1 155.24(10) . . . . ? Br1 Ga1 N1 Sn1 -84.76(10) 9 . . . ? Br1 Ga1 N1 Sn1 35.24(10) 5 . . . ? Br1 Ga1 N1 Sn1 35.24(10) . . . 9 ? Br1 Ga1 N1 Sn1 155.24(10) 9 . . 9 ? Br1 Ga1 N1 Sn1 -84.76(10) 5 . . 9 ? C3 Sn1 N1 Ga1 41.2(10) . . . . ? C2 Sn1 N1 Ga1 -84.6(9) . . . . ? C1 Sn1 N1 Ga1 158.4(8) . . . . ? C3 Sn1 N1 Sn1 -78.6(10) . . . 5 ? C2 Sn1 N1 Sn1 155.5(9) . . . 5 ? C1 Sn1 N1 Sn1 38.6(8) . . . 5 ? C3 Sn1 N1 Sn1 161.1(10) . . . 9 ? C2 Sn1 N1 Sn1 35.3(9) . . . 9 ? C1 Sn1 N1 Sn1 -81.7(8) . . . 9 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.486 _refine_diff_density_min -2.025 _refine_diff_density_rms 0.389 data_cheng _database_code_CSD 145599 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H27 Al Cl3 N Si0 Sn3' _chemical_formula_weight 638.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 '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' 'N' 'N' 0.0061 0.0033 '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 12.6514(15) _cell_length_b 13.0879(16) _cell_length_c 12.6514(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2094.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 89 _cell_measurement_theta_min 4.01 _cell_measurement_theta_max 23.7 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.025 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 3.959 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5345 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 axs CCD 1000' _diffrn_measurement_method 'omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4832 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.07 _reflns_number_total 2941 _reflns_number_gt 2806 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART' _computing_cell_refinement 'SMART' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER axs SHELXTL-PLUS' _computing_publication_material 'SHELXL-97' _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 w=1/[\s^2^(Fo^2^)+(0.1335P)^2^+22.9284P] 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 0.00 _refine_ls_number_reflns 2941 _refine_ls_number_parameters 154 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1687 _refine_ls_wR_factor_gt 0.1597 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.076 _refine_ls_shift/su_mean 0.013 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.07457(8) 0.89584(6) 0.72229(10) 0.0280(3) Uani 1 d . . . N1 N -0.0016(9) 0.7481(7) 0.7523(9) 0.017(2) Uani 1 d . . . Sn2 Sn 0.11494(8) 0.62888(7) 0.72464(10) 0.0300(3) Uani 1 d . . . Sn3 Sn -0.13032(8) 0.72898(7) 0.64109(10) 0.0292(3) Uani 1 d . . . Cl2 Cl -0.1072(4) 0.8912(3) 0.9380(4) 0.0401(10) Uani 1 d . . . Cl3 Cl -0.1765(4) 0.6376(3) 0.9052(4) 0.0422(11) Uani 1 d . . . Cl1 Cl 0.0727(4) 0.6967(4) 0.9996(3) 0.0423(10) Uani 1 d . . . Al1 Al -0.0504(4) 0.7439(3) 0.8919(4) 0.0256(9) Uani 1 d . . . C1 C 0.2653(15) 0.6840(13) 0.7864(16) 0.043(4) Uani 1 d . . . H1A H 0.3194 0.6326 0.7751 0.064 Uiso 1 calc R . . H1B H 0.2584 0.6975 0.8615 0.064 Uiso 1 calc R . . H1C H 0.2850 0.7465 0.7501 0.064 Uiso 1 calc R . . C2 C 0.1856(16) 0.8738(16) 0.5939(16) 0.049(5) Uani 1 d . . . H2A H 0.2209 0.9379 0.5786 0.073 Uiso 1 calc R . . H2B H 0.1480 0.8506 0.5316 0.073 Uiso 1 calc R . . H2C H 0.2376 0.8229 0.6142 0.073 Uiso 1 calc R . . C3 C 0.1661(15) 0.9357(14) 0.8602(14) 0.041(4) Uani 1 d . . . H3A H 0.1192 0.9454 0.9200 0.061 Uiso 1 calc R . . H3B H 0.2047 0.9984 0.8469 0.061 Uiso 1 calc R . . H3C H 0.2157 0.8812 0.8758 0.061 Uiso 1 calc R . . C4 C -0.1528(19) 0.5635(12) 0.6279(17) 0.053(5) Uani 1 d . . . H4A H -0.1752 0.5364 0.6956 0.079 Uiso 1 calc R . . H4B H -0.0867 0.5317 0.6072 0.079 Uiso 1 calc R . . H4C H -0.2063 0.5493 0.5751 0.079 Uiso 1 calc R . . C5 C 0.1190(17) 0.6062(14) 0.5580(15) 0.046(6) Uani 1 d . . . H5A H 0.1701 0.5535 0.5411 0.070 Uiso 1 calc R . . H5B H 0.1391 0.6695 0.5235 0.070 Uiso 1 calc R . . H5C H 0.0496 0.5854 0.5335 0.070 Uiso 1 calc R . . C6 C -0.0847(15) 0.7958(15) 0.4931(14) 0.040(4) Uani 1 d . . . H6A H -0.0777 0.8691 0.5014 0.059 Uiso 1 calc R . . H6B H -0.1382 0.7812 0.4403 0.059 Uiso 1 calc R . . H6C H -0.0176 0.7672 0.4706 0.059 Uiso 1 calc R . . C7 C -0.0418(18) 1.0057(12) 0.6845(15) 0.051(5) Uani 1 d . . . H7A H -0.0912 1.0119 0.7429 0.076 Uiso 1 calc R . . H7B H -0.0795 0.9845 0.6215 0.076 Uiso 1 calc R . . H7C H -0.0082 1.0712 0.6720 0.076 Uiso 1 calc R . . C8 C -0.264(2) 0.8081(14) 0.7018(17) 0.056(6) Uani 1 d . . . H8A H -0.2485 0.8806 0.7054 0.084 Uiso 1 calc R . . H8B H -0.2802 0.7828 0.7721 0.084 Uiso 1 calc R . . H8C H -0.3241 0.7969 0.6558 0.084 Uiso 1 calc R . . C9 C 0.0608(19) 0.4930(12) 0.8014(18) 0.055(6) Uani 1 d . . . H9A H 0.1115 0.4385 0.7902 0.083 Uiso 1 calc R . . H9B H -0.0071 0.4732 0.7722 0.083 Uiso 1 calc R . . H9C H 0.0534 0.5058 0.8766 0.083 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0297(6) 0.0221(4) 0.0324(5) 0.0017(5) 0.0001(5) -0.0023(3) N1 0.018(6) 0.013(4) 0.020(6) -0.001(4) 0.006(4) 0.000(4) Sn2 0.0318(6) 0.0255(5) 0.0328(6) 0.0001(5) -0.0008(6) 0.0076(3) Sn3 0.0296(6) 0.0267(5) 0.0313(6) 0.0036(4) -0.0046(5) -0.0010(4) Cl2 0.051(3) 0.034(2) 0.035(2) -0.0052(15) 0.006(2) 0.0112(17) Cl3 0.031(3) 0.047(2) 0.048(3) 0.0180(18) 0.0044(19) -0.0091(16) Cl1 0.043(3) 0.051(2) 0.033(2) 0.0084(18) -0.0122(18) 0.0049(18) Al1 0.027(3) 0.0254(19) 0.024(2) 0.0062(17) 0.0028(19) 0.0036(16) C1 0.032(11) 0.041(9) 0.056(12) 0.009(8) -0.001(9) 0.008(7) C2 0.031(12) 0.073(13) 0.042(11) 0.009(9) 0.016(9) -0.006(8) C3 0.043(11) 0.039(9) 0.040(10) -0.012(7) -0.009(9) -0.004(8) C4 0.082(15) 0.025(8) 0.051(13) 0.006(8) 0.011(11) -0.009(8) C5 0.065(14) 0.043(10) 0.031(10) -0.027(8) -0.024(9) 0.035(9) C6 0.030(10) 0.054(10) 0.035(10) 0.003(8) -0.007(7) 0.003(7) C7 0.079(15) 0.015(6) 0.057(11) 0.015(7) -0.014(10) -0.002(8) C8 0.074(16) 0.042(9) 0.052(14) 0.006(8) -0.011(10) -0.007(9) C9 0.082(16) 0.026(8) 0.057(12) 0.017(9) 0.022(11) 0.015(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C7 2.113(19) . ? Sn1 C3 2.159(17) . ? Sn1 C2 2.166(19) . ? Sn1 N1 2.194(10) . ? N1 Al1 1.872(12) . ? N1 Sn3 2.166(12) . ? N1 Sn2 2.175(10) . ? Sn2 C9 2.139(17) . ? Sn2 C1 2.179(19) . ? Sn2 C5 2.129(19) . ? Sn3 C8 2.13(2) . ? Sn3 C6 2.145(18) . ? Sn3 C4 2.190(16) . ? Cl2 Al1 2.138(6) . ? Cl3 Al1 2.124(6) . ? Cl1 Al1 2.159(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Sn1 C3 113.1(7) . . ? C7 Sn1 C2 111.9(8) . . ? C3 Sn1 C2 106.9(8) . . ? C7 Sn1 N1 109.4(6) . . ? C3 Sn1 N1 108.0(6) . . ? C2 Sn1 N1 107.3(6) . . ? Al1 N1 Sn3 111.2(5) . . ? Al1 N1 Sn2 110.7(5) . . ? Sn3 N1 Sn2 108.8(4) . . ? Al1 N1 Sn1 109.5(5) . . ? Sn3 N1 Sn1 108.7(5) . . ? Sn2 N1 Sn1 107.8(5) . . ? C9 Sn2 C1 113.1(8) . . ? C9 Sn2 C5 110.0(9) . . ? C1 Sn2 C5 112.3(8) . . ? C9 Sn2 N1 107.8(6) . . ? C1 Sn2 N1 107.3(5) . . ? C5 Sn2 N1 106.0(5) . . ? C8 Sn3 N1 107.9(6) . . ? C8 Sn3 C6 109.3(7) . . ? N1 Sn3 C6 108.5(6) . . ? C8 Sn3 C4 113.9(8) . . ? N1 Sn3 C4 105.1(7) . . ? C6 Sn3 C4 111.8(8) . . ? N1 Al1 Cl3 110.0(4) . . ? N1 Al1 Cl2 110.0(4) . . ? Cl3 Al1 Cl2 108.4(3) . . ? N1 Al1 Cl1 111.5(4) . . ? Cl3 Al1 Cl1 107.7(2) . . ? Cl2 Al1 Cl1 109.2(3) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 3.734 _refine_diff_density_min -1.395 _refine_diff_density_rms 0.263 #===================================================================== #===== #== #