data_nb110478 _publ_section_references ; Bruker (2006). SAINT. Version 7.23A. Bruker AXS inc., Madison, Wisconsin, USA. Bruker (1999). SMART. Version 5.054. Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (2004), TWINABS 1.05. Bruker Nonius, Inc., Madison, Wisconsin,USA. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2008). SADABS 2008. Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (2008). CELL_NOW, V. 2008/2. Bruker AXS, Inc., Madison, Wisconsin, USA ; _publ_section_exptl_refinement ; The crystal was twinned and the orientation matrix for the major component was determined (CELL_NOW). The data were reduced and corrected for absorption (TWINABS). Hydrogen atoms were included in calculated positions and refined using a riding model. ; _publ_contact_author_name 'Andreas Decken' _publ_contact_author_address ;Department of Chemistry University of New Brunswick Fredericton, NB E3B 5A3 Canada ; _publ_contact_author_email adecken@unb.ca _publ_contact_author_phone '(506) 453-4875' _publ_contact_author_fax '(506) 453-4981' loop_ _publ_author_name _publ_author_address 'Andreas Decken' ;Department of Chemistry University of New Brunswick Fredericton, NB E3B 5A3 Canada ; 'Neil Burford' ;Department of Chemistry Dalhousie University Halifax, NS B4H 4J3 Canada ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C6 H18 Cl4 P2 Sn' _chemical_formula_sum 'C6 H18 Cl4 P2 Sn' _chemical_melting_point ? _exptl_crystal_description Irregular _exptl_crystal_colour Colourless _diffrn_ambient_temperature 188(1) _chemical_formula_weight 412.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.6923(14) _cell_length_b 8.4333(17) _cell_length_c 13.376(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.204(2) _cell_angle_gamma 90.00 _cell_volume 743.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 188(1) _cell_measurement_reflns_used 2215 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 28.38 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.844 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 2.617 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5607 _exptl_absorpt_correction_T_max 0.7798 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; Crystal decay was monitored by repeating the initial 50 frames at the end of the data collection and analyzing duplicate reflections ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type K760 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART1000/P4' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3093 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 27.49 _reflns_number_total 1656 _reflns_number_gt 1179 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Sheldrick, 2008)' _computing_publication_material 'Bruker SHELXTL (Sheldrick, 2008)' _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^)+(0.0230P)^2^+0.1551P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1656 _refine_ls_number_parameters 64 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0573 _refine_ls_wR_factor_gt 0.0538 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Sn1 Sn 0.5000 0.5000 0.5000 0.01720(8) Uani 1 2 d S . . Cl2 Cl 0.75576(10) 0.49717(7) 0.38902(4) 0.02740(14) Uani 1 1 d . . . Cl1 Cl 0.31468(9) 0.71173(6) 0.39346(4) 0.02674(15) Uani 1 1 d . . . P1 P 0.68708(9) 0.72113(7) 0.61071(4) 0.02086(15) Uani 1 1 d . . . C1 C 0.8253(4) 0.6499(3) 0.72983(16) 0.0283(6) Uani 1 1 d . . . H1A H 0.9314 0.5763 0.7172 0.042 Uiso 1 1 calc R . . H1B H 0.7321 0.5949 0.7669 0.042 Uiso 1 1 calc R . . H1C H 0.8877 0.7396 0.7703 0.042 Uiso 1 1 calc R . . C2 C 0.5050(4) 0.8647(3) 0.63882(18) 0.0292(6) Uani 1 1 d . . . H2A H 0.4233 0.8177 0.6852 0.044 Uiso 1 1 calc R . . H2B H 0.4159 0.8963 0.5757 0.044 Uiso 1 1 calc R . . H2C H 0.5767 0.9580 0.6708 0.044 Uiso 1 1 calc R . . C3 C 0.8620(4) 0.8256(3) 0.54681(18) 0.0326(6) Uani 1 1 d . . . H3A H 0.9204 0.9152 0.5887 0.049 Uiso 1 1 calc R . . H3B H 0.7901 0.8650 0.4813 0.049 Uiso 1 1 calc R . . H3C H 0.9708 0.7536 0.5356 0.049 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 0.01818(13) 0.01671(12) 0.01656(12) 0.00093(8) 0.00270(8) 0.00127(9) Cl2 0.0263(3) 0.0317(3) 0.0267(3) 0.0012(2) 0.0115(2) 0.0012(3) Cl1 0.0308(4) 0.0222(3) 0.0252(3) 0.0045(2) -0.0007(3) 0.0054(2) P1 0.0216(4) 0.0192(3) 0.0215(3) -0.0006(2) 0.0031(3) 0.0000(3) C1 0.0302(14) 0.0290(13) 0.0233(10) -0.0027(10) -0.0012(10) 0.0008(11) C2 0.0320(14) 0.0227(13) 0.0331(12) -0.0053(10) 0.0062(11) 0.0039(11) C3 0.0351(15) 0.0240(13) 0.0408(14) 0.0001(11) 0.0125(12) -0.0055(12) _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 Cl2 2.4565(7) 3_666 ? Sn1 Cl2 2.4565(7) . ? Sn1 Cl1 2.4762(6) 3_666 ? Sn1 Cl1 2.4762(6) . ? Sn1 P1 2.5654(7) 3_666 ? Sn1 P1 2.5654(7) . ? P1 C3 1.798(2) . ? P1 C1 1.798(2) . ? P1 C2 1.804(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Sn1 Cl2 180.0 3_666 . ? Cl2 Sn1 Cl1 89.47(2) 3_666 3_666 ? Cl2 Sn1 Cl1 90.53(2) . 3_666 ? Cl2 Sn1 Cl1 90.53(2) 3_666 . ? Cl2 Sn1 Cl1 89.47(2) . . ? Cl1 Sn1 Cl1 180.00(2) 3_666 . ? Cl2 Sn1 P1 92.00(2) 3_666 3_666 ? Cl2 Sn1 P1 88.00(2) . 3_666 ? Cl1 Sn1 P1 87.22(2) 3_666 3_666 ? Cl1 Sn1 P1 92.78(2) . 3_666 ? Cl2 Sn1 P1 88.00(2) 3_666 . ? Cl2 Sn1 P1 92.00(2) . . ? Cl1 Sn1 P1 92.78(2) 3_666 . ? Cl1 Sn1 P1 87.22(2) . . ? P1 Sn1 P1 180.000(17) 3_666 . ? C3 P1 C1 108.01(12) . . ? C3 P1 C2 106.92(12) . . ? C1 P1 C2 107.46(11) . . ? C3 P1 Sn1 111.97(8) . . ? C1 P1 Sn1 112.98(8) . . ? C2 P1 Sn1 109.23(8) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.551 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.082 _publ_requested_journal 'Chem. Commun.' #=============================================== data_nb111056 _publ_section_references ; Bruker (2006). SAINT. Version 7.23A. Bruker AXS inc., Madison, Wisconsin, USA. Bruker (1999). SMART. Version 5.054. Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2008). SADABS 2008. Bruker AXS Inc., Madison, Wisconsin, USA. ; _publ_section_exptl_refinement ; The AlCl~4~ anion was disordered over two positions and the site occupancies determined using an isotropic model as 0.58 (Cl(4)-Cl(5)), and 0.42 (Cl(6)-Cl(7)) and fixed in subsequent refinement cycles. Cl(4) and Cl(6) showed high thermal libration that could not be modelled with additional atom position disorder. The thermal parameters of these two atoms were refined with restraints to behave approximately isotropic. Hydrogen atoms were included in calculated positions and refined using a riding model. ; _publ_contact_author_name 'Andreas Decken' _publ_contact_author_address ;Department of Chemistry University of New Brunswick Fredericton, NB E3B 5A3 Canada ; _publ_contact_author_email adecken@unb.ca _publ_contact_author_phone '(506) 453-4875' _publ_contact_author_fax '(506) 453-4981' loop_ _publ_author_name _publ_author_address 'Andreas Decken' ;Department of Chemistry University of New Brunswick Fredericton, NB E3B 5A3 Canada ; 'Neil Burford' ;Department of Chemistry University of Victoria P.O. Box 3065, Stn CSC Victoria, BC V8W 3V6 Canada ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C6 H18 Cl3 P2 Sn, Al Cl4' _chemical_formula_sum 'C6 H18 Al Cl7 P2 Sn' _exptl_crystal_recrystallization_method CH2Cl2/Toluene _chemical_melting_point ? _exptl_crystal_description Irregular _exptl_crystal_colour Colourless _diffrn_ambient_temperature 198(1) _chemical_formula_weight 545.96 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m' _symmetry_space_group_name_Hall '-P 2yb' _symmetry_int_tables_number 11 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.164(3) _cell_length_b 10.897(3) _cell_length_c 10.684(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.708(3) _cell_angle_gamma 90.00 _cell_volume 1027.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 198(1) _cell_measurement_reflns_used 5717 _cell_measurement_theta_min 2.3085 _cell_measurement_theta_max 28.3845 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.765 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 2.334 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4955 _exptl_absorpt_correction_T_max 0.7210 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; Crystal decay was monitored by repeating the initial 50 frames at the end of the data collection and analyzing duplicate reflections ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type K760 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART1000/P4' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7106 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2430 _reflns_number_gt 2299 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Sheldrick, 2008)' _computing_publication_material 'Bruker SHELXTL (Sheldrick, 2008)' _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^)+(0.0323P)^2^+0.9662P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2430 _refine_ls_number_parameters 110 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0262 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0674 _refine_ls_wR_factor_gt 0.0662 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.334 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.71487(3) 0.7500 0.51532(3) 0.02775(10) Uani 1 2 d S . . Cl1 Cl 0.47282(12) 0.7500 0.36749(11) 0.0473(3) Uani 1 2 d S . . Cl2 Cl 0.81213(10) 0.95160(7) 0.57717(9) 0.0457(2) Uani 1 1 d . . . P1 P 0.85784(12) 0.7500 0.34174(11) 0.0319(2) Uani 1 2 d S . . P2 P 0.60542(12) 0.7500 0.70925(10) 0.0304(2) Uani 1 2 d S . . C1 C 1.0566(5) 0.7500 0.4220(5) 0.0403(10) Uani 1 2 d S . . H1A H 1.0795 0.6842 0.4869 0.060 Uiso 0.50 1 calc PR . . H1B H 1.0853 0.8292 0.4650 0.060 Uiso 0.50 1 calc PR . . H1C H 1.1139 0.7365 0.3579 0.060 Uiso 0.50 1 calc PR . . C2 C 0.8131(4) 0.8842(4) 0.2417(3) 0.0474(8) Uani 1 1 d . . . H2A H 0.8711 0.8833 0.1770 0.071 Uiso 1 1 calc R . . H2B H 0.8394 0.9576 0.2961 0.071 Uiso 1 1 calc R . . H2C H 0.7045 0.8849 0.1975 0.071 Uiso 1 1 calc R . . C3 C 0.7511(6) 0.7500 0.8594(5) 0.0506(12) Uani 1 2 d S . . H3A H 0.8012 0.8303 0.8722 0.076 Uiso 0.50 1 calc PR . . H3B H 0.8257 0.6862 0.8569 0.076 Uiso 0.50 1 calc PR . . H3C H 0.7064 0.7335 0.9312 0.076 Uiso 0.50 1 calc PR . . C4 C 0.4902(4) 0.8838(4) 0.7022(4) 0.0504(8) Uani 1 1 d . . . H4A H 0.4112 0.8852 0.6194 0.076 Uiso 1 1 calc R . . H4B H 0.5534 0.9574 0.7093 0.076 Uiso 1 1 calc R . . H4C H 0.4429 0.8822 0.7742 0.076 Uiso 1 1 calc R . . Al1 Al 0.2331(2) 0.7500 0.98747(15) 0.0560(4) Uani 1 2 d S . . Cl3 Cl 0.13042(15) 0.7500 0.78323(12) 0.0563(3) Uani 1 2 d P A 1 Cl4 Cl 0.4569(3) 0.7500 1.0250(3) 0.1168(17) Uani 0.58 2 d PU A 1 Cl5 Cl 0.1430(3) 0.9054(3) 1.0714(3) 0.0980(8) Uani 0.58 1 d P A 1 Cl6 Cl 0.1066(5) 0.7500 1.1030(4) 0.124(2) Uani 0.42 2 d PU A 2 Cl7 Cl 0.4006(5) 0.9051(3) 1.0211(3) 0.0939(11) Uani 0.42 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.03033(16) 0.02558(16) 0.02846(16) 0.000 0.00987(11) 0.000 Cl1 0.0344(5) 0.0706(8) 0.0343(5) 0.000 0.0046(4) 0.000 Cl2 0.0585(5) 0.0309(4) 0.0500(5) -0.0057(3) 0.0187(4) -0.0127(3) P1 0.0304(5) 0.0334(5) 0.0341(5) 0.000 0.0128(4) 0.000 P2 0.0321(5) 0.0316(5) 0.0287(5) 0.000 0.0105(4) 0.000 C1 0.033(2) 0.037(2) 0.051(3) 0.000 0.0108(19) 0.000 C2 0.0488(18) 0.052(2) 0.0448(18) 0.0151(16) 0.0175(15) 0.0085(16) C3 0.046(3) 0.070(4) 0.032(2) 0.000 0.005(2) 0.000 C4 0.0554(19) 0.049(2) 0.054(2) 0.0026(17) 0.0277(17) 0.0166(17) Al1 0.0672(10) 0.0682(11) 0.0292(7) 0.000 0.0075(7) 0.000 Cl3 0.0473(6) 0.0875(10) 0.0305(5) 0.000 0.0043(5) 0.000 Cl4 0.0387(12) 0.274(5) 0.0391(13) 0.000 0.0123(10) 0.000 Cl5 0.123(2) 0.0888(17) 0.0957(17) -0.0459(15) 0.0528(15) -0.0140(15) Cl6 0.062(2) 0.268(7) 0.050(2) 0.000 0.0283(18) 0.000 Cl7 0.124(3) 0.088(2) 0.0506(14) 0.0019(15) -0.0083(15) -0.040(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 Cl1 2.3490(12) . ? Sn1 Cl2 2.3955(10) . ? Sn1 Cl2 2.3955(10) 4_575 ? Sn1 P2 2.5347(12) . ? Sn1 P1 2.5439(12) . ? P1 C1 1.791(5) . ? P1 C2 1.791(4) 4_575 ? P1 C2 1.791(4) . ? P2 C3 1.788(5) . ? P2 C4 1.790(3) 4_575 ? P2 C4 1.790(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? Al1 Cl6 1.908(4) . ? Al1 Cl4 1.981(3) . ? Al1 Cl3 2.130(2) . ? Al1 Cl5 2.180(3) . ? Al1 Cl5 2.180(3) 4_575 ? Al1 Cl7 2.246(4) . ? Al1 Cl7 2.246(4) 4_575 ? 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 Cl1 Sn1 Cl2 113.49(2) . . ? Cl1 Sn1 Cl2 113.49(2) . 4_575 ? Cl2 Sn1 Cl2 133.00(5) . 4_575 ? Cl1 Sn1 P2 92.23(4) . . ? Cl2 Sn1 P2 88.54(2) . . ? Cl2 Sn1 P2 88.54(2) 4_575 . ? Cl1 Sn1 P1 95.10(5) . . ? Cl2 Sn1 P1 88.54(3) . . ? Cl2 Sn1 P1 88.54(3) 4_575 . ? P2 Sn1 P1 172.67(4) . . ? C1 P1 C2 108.92(15) . 4_575 ? C1 P1 C2 108.92(15) . . ? C2 P1 C2 109.4(3) 4_575 . ? C1 P1 Sn1 108.00(17) . . ? C2 P1 Sn1 110.79(12) 4_575 . ? C2 P1 Sn1 110.79(12) . . ? C3 P2 C4 109.05(16) . 4_575 ? C3 P2 C4 109.05(16) . . ? C4 P2 C4 109.1(3) 4_575 . ? C3 P2 Sn1 111.63(18) . . ? C4 P2 Sn1 108.98(13) 4_575 . ? C4 P2 Sn1 108.98(13) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P2 C3 H3A 109.5 . . ? P2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Cl6 Al1 Cl4 130.27(18) . . ? Cl6 Al1 Cl3 119.04(18) . . ? Cl4 Al1 Cl3 110.69(12) . . ? Cl6 Al1 Cl5 50.94(9) . . ? Cl4 Al1 Cl5 113.81(10) . . ? Cl3 Al1 Cl5 108.06(10) . . ? Cl6 Al1 Cl5 50.94(9) . 4_575 ? Cl4 Al1 Cl5 113.81(10) . 4_575 ? Cl3 Al1 Cl5 108.06(11) . 4_575 ? Cl5 Al1 Cl5 101.89(18) . 4_575 ? Cl6 Al1 Cl7 113.90(15) . . ? Cl4 Al1 Cl7 48.85(13) . . ? Cl3 Al1 Cl7 104.91(10) . . ? Cl5 Al1 Cl7 70.64(14) . . ? Cl5 Al1 Cl7 146.84(14) 4_575 . ? Cl6 Al1 Cl7 113.90(15) . 4_575 ? Cl4 Al1 Cl7 48.85(13) . 4_575 ? Cl3 Al1 Cl7 104.91(10) . 4_575 ? Cl5 Al1 Cl7 146.84(14) . 4_575 ? Cl5 Al1 Cl7 70.64(14) 4_575 4_575 ? Cl7 Al1 Cl7 97.6(2) . 4_575 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.871 _refine_diff_density_min -0.701 _refine_diff_density_rms 0.077 _publ_requested_journal 'Chem. Commun.' #=============================================== data_nb120297 _publ_section_references ; Bruker (2006). SAINT. Version 7.23A. Bruker AXS inc., Madison, Wisconsin, USA. Bruker (1999). SMART. Version 5.054. Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2008). SADABS 2008. Bruker AXS Inc., Madison, Wisconsin, USA. ; _publ_section_exptl_refinement ; Hydrogen atoms were included in calculated positions and refined using a riding model. ; _publ_contact_author_name 'Andreas Decken' _publ_contact_author_address ;Department of Chemistry University of New Brunswick Fredericton, NB E3B 5A3 Canada ; _publ_contact_author_email adecken@unb.ca _publ_contact_author_phone '(506) 453-4875' _publ_contact_author_fax '(506) 453-4981' loop_ _publ_author_name _publ_author_address 'Andreas Decken' ;Department of Chemistry University of New Brunswick Fredericton, NB E3B 5A3 Canada ; 'Neil Burford' ;Department of Chemistry University of Victoria P.O. Box 3065, Stn CSC Victoria, BC V8W 3V6 Canada ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C6 H18 Al2 Cl10 P2 Sn' _chemical_formula_sum 'C6 H18 Al2 Cl10 P2 Sn' _exptl_crystal_recrystallization_method CH2Cl2/Toluene _chemical_melting_point ? _exptl_crystal_description Parallelpiped _exptl_crystal_colour Colourless _diffrn_ambient_temperature 173(1) _chemical_formula_weight 679.29 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? 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 7.2557(10) _cell_length_b 13.2556(18) _cell_length_c 25.966(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.068(2) _cell_angle_gamma 90.00 _cell_volume 2487.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6152 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 28.23 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 2.291 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4609 _exptl_absorpt_correction_T_max 0.6267 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; Crystal decay was monitored by repeating the initial 50 frames at the end of the data collection and analyzing duplicate reflections ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type K760 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART1000/P4' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16786 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5573 _reflns_number_gt 5087 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Sheldrick, 2008)' _computing_publication_material 'Bruker SHELXTL (Sheldrick, 2008)' _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^)+(0.0275P)^2^+1.4371P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5573 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0569 _refine_ls_wR_factor_gt 0.0550 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.972758(18) 0.240648(9) 0.099990(5) 0.01848(5) Uani 1 1 d . . . Al1 Al 0.68623(9) 0.52888(5) 0.12889(2) 0.02600(13) Uani 1 1 d . . . Al2 Al 0.70504(9) -0.06651(5) 0.14039(2) 0.02619(13) Uani 1 1 d . . . Cl1 Cl 1.16235(7) 0.10719(4) 0.07609(2) 0.03004(11) Uani 1 1 d . . . Cl2 Cl 1.14647(7) 0.38252(4) 0.08158(2) 0.02925(11) Uani 1 1 d . . . Cl3 Cl 0.69053(7) 0.36464(4) 0.142988(19) 0.02749(11) Uani 1 1 d . . . Cl4 Cl 0.42359(7) 0.57771(4) 0.14858(2) 0.03670(13) Uani 1 1 d . . . Cl5 Cl 0.90649(8) 0.59601(5) 0.17525(3) 0.04780(16) Uani 1 1 d . . . Cl6 Cl 0.71413(9) 0.54522(4) 0.04888(2) 0.04172(14) Uani 1 1 d . . . Cl7 Cl 0.67885(7) 0.09697(4) 0.127284(19) 0.02739(11) Uani 1 1 d . . . Cl8 Cl 0.89266(10) -0.08533(5) 0.20664(3) 0.05102(17) Uani 1 1 d . . . Cl9 Cl 0.79453(10) -0.13074(5) 0.07225(3) 0.04782(16) Uani 1 1 d . . . Cl10 Cl 0.43421(8) -0.11713(5) 0.15137(2) 0.03977(13) Uani 1 1 d . . . P1 P 1.06897(8) 0.23357(4) 0.19643(2) 0.02440(11) Uani 1 1 d . . . P2 P 0.75631(7) 0.23567(4) 0.01767(2) 0.02081(10) Uani 1 1 d . . . C1 C 0.8896(3) 0.20754(18) 0.23733(8) 0.0315(5) Uani 1 1 d . . . H1A H 0.9409 0.2085 0.2735 0.047 Uiso 1 1 calc R . . H1B H 0.8368 0.1409 0.2289 0.047 Uiso 1 1 calc R . . H1C H 0.7927 0.2589 0.2320 0.047 Uiso 1 1 calc R . . C2 C 1.1718(4) 0.3531(2) 0.21371(9) 0.0455(6) Uani 1 1 d . . . H2A H 1.0782 0.4063 0.2085 0.068 Uiso 1 1 calc R . . H2B H 1.2727 0.3667 0.1919 0.068 Uiso 1 1 calc R . . H2C H 1.2209 0.3518 0.2501 0.068 Uiso 1 1 calc R . . C3 C 1.2424(4) 0.1373(2) 0.20686(10) 0.0516(7) Uani 1 1 d . . . H3A H 1.2834 0.1334 0.2438 0.077 Uiso 1 1 calc R . . H3B H 1.3481 0.1539 0.1874 0.077 Uiso 1 1 calc R . . H3C H 1.1904 0.0722 0.1951 0.077 Uiso 1 1 calc R . . C4 C 0.5242(3) 0.27231(17) 0.02574(9) 0.0315(5) Uani 1 1 d . . . H4A H 0.5221 0.3431 0.0365 0.047 Uiso 1 1 calc R . . H4B H 0.4749 0.2299 0.0522 0.047 Uiso 1 1 calc R . . H4C H 0.4480 0.2640 -0.0071 0.047 Uiso 1 1 calc R . . C5 C 0.7563(3) 0.10999(16) -0.00786(8) 0.0312(5) Uani 1 1 d . . . H5A H 0.7076 0.0633 0.0168 0.047 Uiso 1 1 calc R . . H5B H 0.8830 0.0905 -0.0138 0.047 Uiso 1 1 calc R . . H5C H 0.6783 0.1075 -0.0406 0.047 Uiso 1 1 calc R . . C6 C 0.8515(3) 0.31842(17) -0.02767(8) 0.0333(5) Uani 1 1 d . . . H6A H 0.7774 0.3142 -0.0610 0.050 Uiso 1 1 calc R . . H6B H 0.9792 0.2984 -0.0320 0.050 Uiso 1 1 calc R . . H6C H 0.8499 0.3879 -0.0148 0.050 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 0.01922(8) 0.02076(7) 0.01555(7) -0.00073(4) 0.00211(5) 0.00055(4) Al1 0.0279(3) 0.0230(3) 0.0268(3) -0.0031(2) 0.0006(2) 0.0016(2) Al2 0.0302(3) 0.0253(3) 0.0231(3) 0.0015(2) 0.0020(2) -0.0007(2) Cl1 0.0284(3) 0.0301(2) 0.0318(3) -0.0073(2) 0.0036(2) 0.0082(2) Cl2 0.0297(3) 0.0288(2) 0.0298(3) 0.00092(19) 0.0054(2) -0.00800(19) Cl3 0.0323(3) 0.0250(2) 0.0258(2) 0.00246(18) 0.00628(19) 0.00622(19) Cl4 0.0278(3) 0.0343(3) 0.0473(3) -0.0124(2) -0.0004(2) 0.0054(2) Cl5 0.0318(3) 0.0519(4) 0.0582(4) -0.0210(3) -0.0043(3) -0.0045(3) Cl6 0.0606(4) 0.0350(3) 0.0301(3) 0.0085(2) 0.0073(3) 0.0028(3) Cl7 0.0297(2) 0.0252(2) 0.0277(2) 0.00312(18) 0.00512(19) -0.00187(19) Cl8 0.0549(4) 0.0454(3) 0.0483(4) 0.0113(3) -0.0210(3) -0.0017(3) Cl9 0.0600(4) 0.0412(3) 0.0452(4) -0.0133(3) 0.0210(3) -0.0001(3) Cl10 0.0360(3) 0.0436(3) 0.0402(3) 0.0121(2) 0.0062(2) -0.0087(2) P1 0.0251(3) 0.0312(3) 0.0166(2) -0.00013(19) 0.0004(2) 0.0024(2) P2 0.0223(3) 0.0224(2) 0.0175(2) 0.00001(18) 0.00072(19) 0.00065(18) C1 0.0382(12) 0.0382(11) 0.0189(10) 0.0034(9) 0.0062(9) 0.0004(10) C2 0.0551(16) 0.0548(15) 0.0256(12) -0.0059(11) -0.0017(11) -0.0251(13) C3 0.0496(16) 0.0734(19) 0.0306(13) 0.0033(12) -0.0042(11) 0.0331(14) C4 0.0222(10) 0.0378(11) 0.0337(12) -0.0002(9) -0.0024(9) 0.0040(9) C5 0.0418(12) 0.0280(10) 0.0229(10) -0.0066(8) -0.0026(9) -0.0007(9) C6 0.0434(13) 0.0359(11) 0.0207(10) 0.0062(8) 0.0040(9) -0.0043(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 Cl2 2.3367(5) . ? Sn1 Cl1 2.3575(5) . ? Sn1 P2 2.5390(6) . ? Sn1 P1 2.5414(6) . ? Sn1 Cl3 2.9233(6) . ? Sn1 Cl7 2.9907(6) . ? Al1 Cl5 2.1107(9) . ? Al1 Cl6 2.1164(9) . ? Al1 Cl4 2.1176(8) . ? Al1 Cl3 2.2073(8) . ? Al2 Cl8 2.1120(9) . ? Al2 Cl9 2.1166(9) . ? Al2 Cl10 2.1194(9) . ? Al2 Cl7 2.1993(8) . ? P1 C1 1.785(2) . ? P1 C2 1.792(2) . ? P1 C3 1.796(2) . ? P2 C4 1.783(2) . ? P2 C6 1.792(2) . ? P2 C5 1.793(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Sn1 Cl1 102.25(2) . . ? Cl2 Sn1 P2 98.825(19) . . ? Cl1 Sn1 P2 95.209(19) . . ? Cl2 Sn1 P1 97.185(19) . . ? Cl1 Sn1 P1 96.654(19) . . ? P2 Sn1 P1 157.554(19) . . ? Cl2 Sn1 Cl3 91.968(19) . . ? Cl1 Sn1 Cl3 165.284(17) . . ? P2 Sn1 Cl3 86.219(18) . . ? P1 Sn1 Cl3 77.591(17) . . ? Cl2 Sn1 Cl7 165.882(17) . . ? Cl1 Sn1 Cl7 91.68(2) . . ? P2 Sn1 Cl7 77.407(17) . . ? P1 Sn1 Cl7 83.254(17) . . ? Cl3 Sn1 Cl7 74.296(17) . . ? Cl5 Al1 Cl6 112.55(4) . . ? Cl5 Al1 Cl4 112.68(4) . . ? Cl6 Al1 Cl4 111.83(4) . . ? Cl5 Al1 Cl3 108.80(4) . . ? Cl6 Al1 Cl3 105.22(3) . . ? Cl4 Al1 Cl3 105.15(3) . . ? Cl8 Al2 Cl9 114.21(4) . . ? Cl8 Al2 Cl10 113.06(4) . . ? Cl9 Al2 Cl10 109.98(4) . . ? Cl8 Al2 Cl7 106.44(3) . . ? Cl9 Al2 Cl7 107.20(4) . . ? Cl10 Al2 Cl7 105.33(3) . . ? Al1 Cl3 Sn1 119.43(3) . . ? Al2 Cl7 Sn1 127.63(3) . . ? C1 P1 C2 109.37(12) . . ? C1 P1 C3 108.13(13) . . ? C2 P1 C3 108.65(15) . . ? C1 P1 Sn1 116.25(8) . . ? C2 P1 Sn1 106.62(8) . . ? C3 P1 Sn1 107.61(9) . . ? C4 P2 C6 109.47(11) . . ? C4 P2 C5 109.11(11) . . ? C6 P2 C5 108.26(11) . . ? C4 P2 Sn1 114.48(8) . . ? C6 P2 Sn1 106.96(8) . . ? C5 P2 Sn1 108.37(7) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.867 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.073 _publ_requested_journal 'Chem. Commun.'