# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address C.Russell ;School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS UK ; L.C.Forfar ;School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS UK ; T.J.Clark ;School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS UK ; M.Green ;School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS UK ; S.M.Mansell ;School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS UK ; ; R.A.Sanguramath ; ;School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS UK ; J.M.Slattery ;Department of Chemistry University of York Heslington York YO105DD UK ; _publ_contact_author_address ;School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS UK ; _publ_contact_author_email Chris.Russell@brs.ac.uk _publ_contact_author_fax '+44 (0)117 925 1295' _publ_contact_author_phone '+44 (0)117 928 7599' #TrackingRef '- Combined-revised.cif' _publ_contact_author_name 'Christopher A Russell' data_1 _database_code_depnum_ccdc_archive 'CCDC 841996' #TrackingRef '- Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Cl16 Cu4 Ga4 P8' _chemical_formula_sum 'Cl16 Cu4 Ga4 P8' _chemical_formula_weight 1348.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' Cu Cu 0.3201 1.2651 '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 Ccca _symmetry_space_group_name_Hall '-C 2b 2bc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1, -y+1/2, z' '-x+1/2, y+1/2, -z+1/2' 'x+1, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' '-x+1/2, -y+1/2, -z' 'x, y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' '-x, y+1/2, z-1/2' _cell_length_a 11.0651(3) _cell_length_b 11.4212(3) _cell_length_c 12.4657(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1575.37(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11058 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 28.2855 _exptl_crystal_description Block _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.842 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 7.776 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4596 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS-2008/1 - Bruker AXS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 Kappa-APEX-II area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20201 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0086 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 912 _reflns_number_gt 879 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2004)' _computing_cell_refinement 'APEX-II and SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT v7.51A (BRUKER)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0227P)^2^+1.4296P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 912 _refine_ls_number_parameters 38 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0149 _refine_ls_R_factor_gt 0.0142 _refine_ls_wR_factor_ref 0.0376 _refine_ls_wR_factor_gt 0.0372 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 Cu1 Cu 0.5000 0.98379(2) 0.2500 0.01845(9) Uani 1 2 d S . . P1 P 0.57573(4) 0.81063(4) 0.18254(3) 0.01650(11) Uani 1 1 d . . . Ga1 Ga 0.2500 1.0000 0.066636(17) 0.01094(8) Uani 1 2 d S . . Cl1 Cl 0.35991(3) 1.11102(3) 0.17532(3) 0.01327(9) Uani 1 1 d . . . Cl2 Cl 0.36380(3) 0.88814(3) -0.02766(3) 0.01711(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01913(14) 0.00972(15) 0.02650(16) 0.000 -0.00850(10) 0.000 P1 0.0169(2) 0.0116(2) 0.0210(2) 0.00112(14) 0.00380(14) -0.00180(14) Ga1 0.01155(12) 0.01282(14) 0.00845(12) 0.000 0.000 0.00029(7) Cl1 0.01409(17) 0.01167(19) 0.01405(17) -0.00151(12) -0.00306(11) 0.00121(12) Cl2 0.01866(18) 0.0191(2) 0.01354(17) -0.00388(13) 0.00378(12) 0.00193(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 P1 2.3067(5) 3_655 ? Cu1 P1 2.3067(5) . ? Cu1 Cl1 2.3197(4) . ? Cu1 Cl1 2.3198(4) 3_655 ? P1 P1 2.1742(8) 6_565 ? P1 P1 2.1787(8) 8_465 ? P1 P1 2.3744(7) 3_655 ? Ga1 Cl2 2.1447(4) . ? Ga1 Cl2 2.1447(4) 2_575 ? Ga1 Cl1 2.2186(4) 2_575 ? Ga1 Cl1 2.2186(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 P1 Cu1 P1 61.95(2) 3_655 . ? P1 Cu1 Cl1 116.144(13) 3_655 . ? P1 Cu1 Cl1 129.311(13) . . ? P1 Cu1 Cl1 129.313(13) 3_655 3_655 ? P1 Cu1 Cl1 116.145(13) . 3_655 ? Cl1 Cu1 Cl1 102.43(2) . 3_655 ? P1 P1 P1 66.12(2) 6_565 8_465 ? P1 P1 Cu1 105.43(2) 6_565 . ? P1 P1 Cu1 105.28(2) 8_465 . ? P1 P1 P1 57.03(2) 6_565 3_655 ? P1 P1 P1 56.85(2) 8_465 3_655 ? Cu1 P1 P1 59.024(10) . 3_655 ? Cl2 Ga1 Cl2 113.52(2) . 2_575 ? Cl2 Ga1 Cl1 108.426(15) . 2_575 ? Cl2 Ga1 Cl1 110.690(14) 2_575 2_575 ? Cl2 Ga1 Cl1 110.690(14) . . ? Cl2 Ga1 Cl1 108.427(15) 2_575 . ? Cl1 Ga1 Cl1 104.73(2) 2_575 . ? Ga1 Cl1 Cu1 104.676(16) . . ? 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 P1 Cu1 P1 P1 34.503(13) 3_655 . . 6_565 ? Cl1 Cu1 P1 P1 -67.562(19) . . . 6_565 ? Cl1 Cu1 P1 P1 157.061(13) 3_655 . . 6_565 ? P1 Cu1 P1 P1 -34.396(13) 3_655 . . 8_465 ? Cl1 Cu1 P1 P1 -136.461(17) . . . 8_465 ? Cl1 Cu1 P1 P1 88.162(14) 3_655 . . 8_465 ? Cl1 Cu1 P1 P1 -102.07(2) . . . 3_655 ? Cl1 Cu1 P1 P1 122.558(18) 3_655 . . 3_655 ? Cl2 Ga1 Cl1 Cu1 -45.437(18) . . . . ? Cl2 Ga1 Cl1 Cu1 -170.575(14) 2_575 . . . ? Cl1 Ga1 Cl1 Cu1 71.220(11) 2_575 . . . ? P1 Cu1 Cl1 Ga1 -48.256(19) 3_655 . . . ? P1 Cu1 Cl1 Ga1 25.78(2) . . . . ? Cl1 Cu1 Cl1 Ga1 165.559(18) 3_655 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.419 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.082 data_2 _database_code_depnum_ccdc_archive 'CCDC 841997' #TrackingRef '- Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Ag Cl4 Ga P4' _chemical_formula_sum 'Ag Cl4 Ga P4' _chemical_formula_weight 443.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 12.0275(9) _cell_length_b 7.0253(5) _cell_length_c 12.6877(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1072.07(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7250 _cell_measurement_theta_min 2.902 _cell_measurement_theta_max 28.381 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 5.862 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2512 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS-2008/1 - Bruker AXS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 Kappa-APEX-II area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9158 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 27.47 _reflns_number_total 1312 _reflns_number_gt 1293 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2004)' _computing_cell_refinement 'APEX-II and SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT v7.51A (BRUKER)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+0.7176P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1312 _refine_ls_number_parameters 55 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0173 _refine_ls_R_factor_gt 0.0170 _refine_ls_wR_factor_ref 0.0470 _refine_ls_wR_factor_gt 0.0468 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _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 Ag1 Ag 0.418631(17) 0.7500 0.574499(15) 0.01899(8) Uani 1 2 d S . . P1 P 0.37642(6) 0.7500 0.77147(6) 0.02106(16) Uani 1 2 d S . . P2 P 0.56412(6) 0.7500 0.72283(6) 0.02365(17) Uani 1 2 d S . . P3 P 0.50183(5) 0.90772(11) 0.85756(5) 0.03695(16) Uani 1 1 d . . . Ga1 Ga 0.30601(2) 1.2500 0.59216(2) 0.01189(9) Uani 1 2 d S . . Cl1 Cl 0.26184(4) 0.99985(6) 0.49936(3) 0.01869(11) Uani 1 1 d . . . Cl2 Cl 0.48845(5) 1.2500 0.61079(5) 0.01914(14) Uani 1 2 d S . . Cl3 Cl 0.23364(6) 1.2500 0.74578(5) 0.02367(15) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02294(13) 0.02046(13) 0.01357(12) 0.000 -0.00178(7) 0.000 P1 0.0153(3) 0.0325(4) 0.0154(3) 0.000 0.0008(2) 0.000 P2 0.0154(3) 0.0388(4) 0.0167(3) 0.000 0.0015(3) 0.000 P3 0.0333(3) 0.0542(4) 0.0233(3) -0.0185(3) -0.0002(2) -0.0088(3) Ga1 0.01312(15) 0.01138(15) 0.01116(14) 0.000 0.00062(9) 0.000 Cl1 0.0219(2) 0.0130(2) 0.0211(2) -0.00424(16) -0.00630(16) 0.00223(16) Cl2 0.0133(3) 0.0297(3) 0.0145(3) 0.000 -0.0006(2) 0.000 Cl3 0.0267(3) 0.0284(4) 0.0159(3) 0.000 0.0094(2) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P1 2.5501(8) . ? Ag1 P2 2.5698(8) . ? Ag1 Cl2 2.6030(7) 5_676 ? Ag1 Cl1 2.7470(5) . ? Ag1 Cl1 2.7470(5) 7_575 ? P1 P3 2.1670(8) 7_575 ? P1 P3 2.1670(8) . ? P1 P2 2.3403(9) . ? P2 P3 2.1704(9) 7_575 ? P2 P3 2.1705(9) . ? P3 P3 2.2161(16) 7_575 ? Ga1 Cl3 2.1346(7) . ? Ga1 Cl1 2.1811(4) . ? Ga1 Cl1 2.1811(5) 7_585 ? Ga1 Cl2 2.2069(7) . ? Cl2 Ag1 2.6030(7) 5_676 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Ag1 P2 54.40(2) . . ? P1 Ag1 Cl2 166.06(2) . 5_676 ? P2 Ag1 Cl2 111.66(2) . 5_676 ? P1 Ag1 Cl1 101.739(16) . . ? P2 Ag1 Cl1 136.188(11) . . ? Cl2 Ag1 Cl1 88.929(15) 5_676 . ? P1 Ag1 Cl1 101.738(16) . 7_575 ? P2 Ag1 Cl1 136.188(12) . 7_575 ? Cl2 Ag1 Cl1 88.930(15) 5_676 7_575 ? Cl1 Ag1 Cl1 79.430(19) . 7_575 ? P3 P1 P3 61.50(5) 7_575 . ? P3 P1 P2 57.42(3) 7_575 . ? P3 P1 P2 57.42(3) . . ? P3 P1 Ag1 110.82(3) 7_575 . ? P3 P1 Ag1 110.82(3) . . ? P2 P1 Ag1 63.23(3) . . ? P3 P2 P3 61.40(5) 7_575 . ? P3 P2 P1 57.28(3) 7_575 . ? P3 P2 P1 57.28(3) . . ? P3 P2 Ag1 109.98(3) 7_575 . ? P3 P2 Ag1 109.98(3) . . ? P1 P2 Ag1 62.37(3) . . ? P1 P3 P2 65.31(3) . . ? P1 P3 P3 59.25(2) . 7_575 ? P2 P3 P3 59.30(2) . 7_575 ? Cl3 Ga1 Cl1 113.179(17) . . ? Cl3 Ga1 Cl1 113.178(17) . 7_585 ? Cl1 Ga1 Cl1 107.36(3) . 7_585 ? Cl3 Ga1 Cl2 107.92(3) . . ? Cl1 Ga1 Cl2 107.456(17) . . ? Cl1 Ga1 Cl2 107.457(17) 7_585 . ? Ga1 Cl1 Ag1 99.223(17) . . ? Ga1 Cl2 Ag1 109.28(3) . 5_676 ? 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 P2 Ag1 P1 P3 -33.16(3) . . . 7_575 ? Cl2 Ag1 P1 P3 -33.16(3) 5_676 . . 7_575 ? Cl1 Ag1 P1 P3 -172.42(3) . . . 7_575 ? Cl1 Ag1 P1 P3 106.10(3) 7_575 . . 7_575 ? P2 Ag1 P1 P3 33.16(3) . . . . ? Cl2 Ag1 P1 P3 33.16(3) 5_676 . . . ? Cl1 Ag1 P1 P3 -106.10(3) . . . . ? Cl1 Ag1 P1 P3 172.42(3) 7_575 . . . ? Cl2 Ag1 P1 P2 0.0 5_676 . . . ? Cl1 Ag1 P1 P2 -139.260(10) . . . . ? Cl1 Ag1 P1 P2 139.261(10) 7_575 . . . ? P3 P1 P2 P3 74.72(6) . . . 7_575 ? Ag1 P1 P2 P3 -142.64(3) . . . 7_575 ? P3 P1 P2 P3 -74.72(5) 7_575 . . . ? Ag1 P1 P2 P3 142.64(3) . . . . ? P3 P1 P2 Ag1 142.64(3) 7_575 . . . ? P3 P1 P2 Ag1 -142.64(3) . . . . ? P1 Ag1 P2 P3 32.90(3) . . . 7_575 ? Cl2 Ag1 P2 P3 -147.10(3) 5_676 . . 7_575 ? Cl1 Ag1 P2 P3 100.27(3) . . . 7_575 ? Cl1 Ag1 P2 P3 -34.46(4) 7_575 . . 7_575 ? P1 Ag1 P2 P3 -32.90(3) . . . . ? Cl2 Ag1 P2 P3 147.10(3) 5_676 . . . ? Cl1 Ag1 P2 P3 34.46(4) . . . . ? Cl1 Ag1 P2 P3 -100.27(3) 7_575 . . . ? Cl2 Ag1 P2 P1 180.0 5_676 . . . ? Cl1 Ag1 P2 P1 67.36(2) . . . . ? Cl1 Ag1 P2 P1 -67.36(2) 7_575 . . . ? P3 P1 P3 P2 67.65(3) 7_575 . . . ? Ag1 P1 P3 P2 -35.42(3) . . . . ? P2 P1 P3 P3 -67.65(3) . . . 7_575 ? Ag1 P1 P3 P3 -103.07(2) . . . 7_575 ? P3 P2 P3 P1 -67.57(2) 7_575 . . . ? Ag1 P2 P3 P1 34.90(3) . . . . ? P1 P2 P3 P3 67.57(2) . . . 7_575 ? Ag1 P2 P3 P3 102.47(2) . . . 7_575 ? Cl3 Ga1 Cl1 Ag1 -83.67(3) . . . . ? Cl1 Ga1 Cl1 Ag1 150.704(12) 7_585 . . . ? Cl2 Ga1 Cl1 Ag1 35.37(2) . . . . ? P1 Ag1 Cl1 Ga1 57.93(2) . . . . ? P2 Ag1 Cl1 Ga1 7.89(3) . . . . ? Cl2 Ag1 Cl1 Ga1 -113.023(18) 5_676 . . . ? Cl1 Ag1 Cl1 Ga1 157.866(10) 7_575 . . . ? Cl3 Ga1 Cl2 Ag1 180.0 . . . 5_676 ? Cl1 Ga1 Cl2 Ag1 57.633(15) . . . 5_676 ? Cl1 Ga1 Cl2 Ag1 -57.634(15) 7_585 . . 5_676 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.486 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.120 data_3 _database_code_depnum_ccdc_archive 'CCDC 841998' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Au Cl4 Ga P8' _chemical_formula_weight 656.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 16.6593(12) _cell_length_b 14.3369(10) _cell_length_c 6.0051(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1434.27(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9964 _cell_measurement_theta_min 2.8265 _cell_measurement_theta_max 28.3265 _exptl_crystal_description Rod _exptl_crystal_colour Orange _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.039 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 13.691 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3868 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS-2008/1 - Bruker AXS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 Kappa-APEX-II area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_reflns_number 20315 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1706 _reflns_number_gt 1545 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2004)' _computing_cell_refinement 'APEX-II and SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT v7.51A (BRUKER)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+2.0095P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1706 _refine_ls_number_parameters 70 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0201 _refine_ls_R_factor_gt 0.0175 _refine_ls_wR_factor_ref 0.0499 _refine_ls_wR_factor_gt 0.0485 _refine_ls_goodness_of_fit_ref 1.171 _refine_ls_restrained_S_all 1.171 _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 Au1 Au 0.874239(9) 0.7500 0.22675(3) 0.01561(7) Uani 1 2 d S . . P1 P 0.86307(5) 0.60178(6) 0.42429(13) 0.01737(16) Uani 1 1 d . . . P2 P 0.88729(5) 0.60171(6) 0.02873(13) 0.01852(17) Uani 1 1 d . . . P3 P 0.94174(5) 0.50268(6) 0.25794(14) 0.02046(19) Uani 1 1 d . . . P4 P 0.81144(5) 0.49981(6) 0.19807(14) 0.01972(17) Uani 1 1 d . . . Ga1 Ga 0.12538(2) 0.7500 0.48535(8) 0.01324(11) Uani 1 2 d S . . Cl1 Cl 0.12743(4) 0.62664(6) 0.27263(12) 0.02166(19) Uani 1 1 d . . . Cl2 Cl 0.01640(6) 0.7500 0.68513(18) 0.0207(2) Uani 1 2 d S . . Cl3 Cl 0.22964(6) 0.7500 0.70430(18) 0.0221(2) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01751(11) 0.01109(10) 0.01824(10) 0.000 0.00056(6) 0.000 P1 0.0250(4) 0.0137(4) 0.0134(4) -0.0006(3) 0.0014(3) -0.0018(3) P2 0.0277(4) 0.0143(4) 0.0135(4) 0.0000(3) 0.0025(3) 0.0023(3) P3 0.0170(4) 0.0176(5) 0.0268(4) 0.0022(3) -0.0004(3) 0.0042(3) P4 0.0175(4) 0.0167(4) 0.0249(4) -0.0012(3) -0.0037(3) -0.0041(3) Ga1 0.0127(2) 0.0109(2) 0.0162(2) 0.000 0.00133(16) 0.000 Cl1 0.0294(5) 0.0144(4) 0.0211(4) -0.0048(3) 0.0033(3) -0.0003(3) Cl2 0.0150(5) 0.0193(5) 0.0278(5) 0.000 0.0065(4) 0.000 Cl3 0.0160(5) 0.0221(6) 0.0280(5) 0.000 -0.0048(4) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.4408(8) 7_575 ? Au1 P1 2.4408(8) . ? Au1 P2 2.4457(8) . ? Au1 P2 2.4457(8) 7_575 ? P1 P4 2.1731(11) . ? P1 P3 2.1757(12) . ? P1 P2 2.4094(12) . ? P2 P3 2.1755(12) . ? P2 P4 2.1829(11) . ? P3 P4 2.2007(14) . ? Ga1 Cl2 2.1761(11) . ? Ga1 Cl3 2.1784(11) . ? Ga1 Cl1 2.1820(9) . ? Ga1 Cl1 2.1820(9) 7_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 P1 Au1 P1 121.06(4) 7_575 . ? P1 Au1 P2 179.27(3) 7_575 . ? P1 Au1 P2 59.08(3) . . ? P1 Au1 P2 59.08(3) 7_575 7_575 ? P1 Au1 P2 179.27(3) . 7_575 ? P2 Au1 P2 120.76(4) . 7_575 ? P4 P1 P3 60.80(4) . . ? P4 P1 P2 56.61(3) . . ? P3 P1 P2 56.37(3) . . ? P4 P1 Au1 108.18(4) . . ? P3 P1 Au1 107.42(4) . . ? P2 P1 Au1 60.56(3) . . ? P3 P2 P4 60.65(4) . . ? P3 P2 P1 56.38(3) . . ? P4 P2 P1 56.23(3) . . ? P3 P2 Au1 107.26(4) . . ? P4 P2 Au1 107.69(4) . . ? P1 P2 Au1 60.36(3) . . ? P2 P3 P1 67.25(4) . . ? P2 P3 P4 59.84(4) . . ? P1 P3 P4 59.54(4) . . ? P1 P4 P2 67.16(4) . . ? P1 P4 P3 59.66(4) . . ? P2 P4 P3 59.51(4) . . ? Cl2 Ga1 Cl3 109.42(5) . . ? Cl2 Ga1 Cl1 109.62(3) . . ? Cl3 Ga1 Cl1 109.93(3) . . ? Cl2 Ga1 Cl1 109.62(3) . 7_575 ? Cl3 Ga1 Cl1 109.93(3) . 7_575 ? Cl1 Ga1 Cl1 108.30(5) . 7_575 ? 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 P1 Au1 P1 P4 149.10(3) 7_575 . . . ? P2 Au1 P1 P4 -31.74(4) . . . . ? P2 Au1 P1 P4 -109.4(19) 7_575 . . . ? P1 Au1 P1 P3 -146.69(3) 7_575 . . . ? P2 Au1 P1 P3 32.47(4) . . . . ? P2 Au1 P1 P3 -45.2(19) 7_575 . . . ? P1 Au1 P1 P2 -179.16(3) 7_575 . . . ? P2 Au1 P1 P2 -77.6(19) 7_575 . . . ? P4 P1 P2 P3 -74.73(5) . . . . ? Au1 P1 P2 P3 142.03(4) . . . . ? P3 P1 P2 P4 74.73(5) . . . . ? Au1 P1 P2 P4 -143.24(4) . . . . ? P4 P1 P2 Au1 143.24(4) . . . . ? P3 P1 P2 Au1 -142.03(4) . . . . ? P1 Au1 P2 P3 69.5(19) 7_575 . . . ? P1 Au1 P2 P3 -32.44(4) . . . . ? P2 Au1 P2 P3 146.73(3) 7_575 . . . ? P1 Au1 P2 P4 133.4(19) 7_575 . . . ? P1 Au1 P2 P4 31.48(4) . . . . ? P2 Au1 P2 P4 -149.35(3) 7_575 . . . ? P1 Au1 P2 P1 102.0(19) 7_575 . . . ? P2 Au1 P2 P1 179.17(3) 7_575 . . . ? P4 P2 P3 P1 -66.92(4) . . . . ? Au1 P2 P3 P1 34.05(4) . . . . ? P1 P2 P3 P4 66.92(4) . . . . ? Au1 P2 P3 P4 100.97(4) . . . . ? P4 P1 P3 P2 67.33(4) . . . . ? Au1 P1 P3 P2 -34.16(4) . . . . ? P2 P1 P3 P4 -67.33(4) . . . . ? Au1 P1 P3 P4 -101.49(4) . . . . ? P3 P1 P4 P2 -66.95(4) . . . . ? Au1 P1 P4 P2 33.27(4) . . . . ? P2 P1 P4 P3 66.95(4) . . . . ? Au1 P1 P4 P3 100.23(4) . . . . ? P3 P2 P4 P1 67.16(4) . . . . ? Au1 P2 P4 P1 -33.09(4) . . . . ? P1 P2 P4 P3 -67.16(4) . . . . ? Au1 P2 P4 P3 -100.26(4) . . . . ? P2 P3 P4 P1 -79.79(4) . . . . ? P1 P3 P4 P2 79.79(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.446 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.125