Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'ProfD Hubert Schmidbaur' _publ_contact_author_address ; Department Chemie Technische Universitat Munchen Lichtenbergstr. 4 Garching Bavaria 85748 GERMANY ; _publ_contact_author_email H.SCHMIDBAUR@LRZ.TUM.DE _publ_section_title ; Bromination of (Phosphine)gold(I) Bromide Complexes: Stoichiometry and Structure of Products ; loop_ _publ_author_name 'H. Schmidbaur' 'Daniel Schneider' 'Oliver Schuster' data_19cos _database_code_depnum_ccdc_archive 'CCDC 264733' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H9 Au Br5 P' _chemical_formula_weight 672.59 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' P P 0.1023 0.0942 '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' Au Au -2.0133 8.8022 '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 orthorhombic _symmetry_space_group_name_H-M Pnma 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 13.9810(10) _cell_length_b 7.2400(10) _cell_length_c 12.2090(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1235.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 28374 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 28.143 _exptl_absorpt_correction_type redelf _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 1.572 _exptl_absorpt_process_details ; Platon Delabs (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'NONIUS DIP 2020' _diffrn_measurement_method phi-rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28374 _diffrn_reflns_av_R_equivalents 0.053 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.44 _reflns_number_total 1224 _reflns_number_gt 1206 _reflns_threshold_expression >2sigma(I) _computing_data_collection XPRESS _computing_cell_refinement DENZO _computing_data_reduction SCALEPACK _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0252P)^2^+7.2641P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1224 _refine_ls_number_parameters 67 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0614 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 1.238 _refine_ls_restrained_S_all 1.238 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.006 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 Br4 Br 0.01594(6) 0.2500 0.46269(7) 0.0251(2) Uani 1 2 d S . . Br5 Br -0.00674(6) 0.2500 0.64938(7) 0.0252(2) Uani 1 2 d S . . C1 C 0.2670(4) 0.0469(9) 0.0181(6) 0.0275(13) Uani 1 1 d . . . C2 C 0.1912(6) 0.2500 -0.1636(8) 0.028(2) Uani 1 2 d S . . H2A H 0.1550 0.1414 -0.1877 0.042 Uiso 0.50 1 calc PR . . H2B H 0.2556 0.2462 -0.1954 0.042 Uiso 1 2 calc SR . . H2C H 0.1584 0.3624 -0.1879 0.042 Uiso 0.50 1 calc PR . . Au1 Au 0.05512(2) 0.2500 0.07631(2) 0.01664(13) Uani 1 2 d S . . Br1 Br -0.09398(6) 0.2500 0.18658(7) 0.0249(2) Uani 1 2 d S . . Br2 Br 0.15060(7) 0.2500 0.24160(7) 0.0324(2) Uani 1 2 d S . . Br3 Br -0.04055(6) 0.2500 -0.08983(7) 0.0215(2) Uani 1 2 d S . . P1 P 0.19979(14) 0.2500 -0.01691(18) 0.0184(4) Uani 1 2 d S . . H1A H 0.229(5) -0.062(11) 0.001(6) 0.028 Uiso 1 1 d . . . H1B H 0.285(5) 0.062(10) 0.097(6) 0.028 Uiso 1 1 d . . . H1C H 0.328(5) 0.047(10) -0.031(6) 0.028 Uiso 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 Br4 0.0365(5) 0.0179(4) 0.0210(4) 0.000 0.0045(3) 0.000 Br5 0.0305(4) 0.0264(5) 0.0187(4) 0.000 -0.0023(3) 0.000 C1 0.018(3) 0.020(3) 0.044(4) 0.003(3) 0.000(3) 0.005(2) C2 0.016(4) 0.028(5) 0.040(5) 0.000 0.002(4) 0.000 Au1 0.01672(19) 0.0168(2) 0.01643(19) 0.000 0.00085(11) 0.000 Br1 0.0255(4) 0.0237(5) 0.0256(4) 0.000 0.0098(3) 0.000 Br2 0.0315(4) 0.0468(6) 0.0190(4) 0.000 -0.0062(3) 0.000 Br3 0.0181(4) 0.0270(5) 0.0195(4) 0.000 -0.0011(3) 0.000 P1 0.0136(9) 0.0183(11) 0.0234(11) 0.000 0.0010(8) 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 Br4 Br5 2.3013(12) . ? Br4 Br2 3.2910(13) . ? Br4 Br1 3.7047(13) . ? C1 P1 1.796(6) . ? C1 H1A 0.97(7) . ? C1 H1B 1.01(7) . ? C1 H1C 1.04(7) . ? C2 P1 1.795(10) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? Au1 P1 2.321(2) . ? Au1 Br2 2.4197(9) . ? Au1 Br3 2.4296(8) . ? Au1 Br1 2.4815(8) . ? P1 C1 1.796(6) 7_565 ? 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 Br5 Br4 Br2 153.02(5) . . ? Br5 Br4 Br1 147.57(4) . . ? Br2 Br4 Br1 59.40(2) . . ? P1 C1 H1A 109(4) . . ? P1 C1 H1B 106(4) . . ? H1A C1 H1B 116(6) . . ? P1 C1 H1C 107(4) . . ? H1A C1 H1C 109(5) . . ? H1B C1 H1C 110(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 Au1 Br2 85.88(6) . . ? P1 Au1 Br3 94.04(6) . . ? Br2 Au1 Br3 179.92(3) . . ? P1 Au1 Br1 176.51(6) . . ? Br2 Au1 Br1 90.63(3) . . ? Br3 Au1 Br1 89.46(3) . . ? Au1 Br1 Br4 98.35(3) . . ? Au1 Br2 Br4 111.62(4) . . ? C2 P1 C1 105.8(3) . 7_565 ? C2 P1 C1 105.8(3) . . ? C1 P1 C1 109.9(4) 7_565 . ? C2 P1 Au1 115.5(3) . . ? C1 P1 Au1 109.8(2) 7_565 . ? C1 P1 Au1 109.8(2) . . ? 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 Br1 Br4 0.0 . . . . ? Br2 Au1 Br1 Br4 0.0 . . . . ? Br3 Au1 Br1 Br4 180.0 . . . . ? Br5 Br4 Br1 Au1 180.0 . . . . ? Br2 Br4 Br1 Au1 0.0 . . . . ? P1 Au1 Br2 Br4 180.0 . . . . ? Br3 Au1 Br2 Br4 180(15) . . . . ? Br1 Au1 Br2 Br4 0.0 . . . . ? Br5 Br4 Br2 Au1 180.0 . . . . ? Br1 Br4 Br2 Au1 0.0 . . . . ? Br2 Au1 P1 C2 180.0 . . . . ? Br3 Au1 P1 C2 0.0 . . . . ? Br1 Au1 P1 C2 180.0 . . . . ? Br2 Au1 P1 C1 -60.5(3) . . . 7_565 ? Br3 Au1 P1 C1 119.5(3) . . . 7_565 ? Br1 Au1 P1 C1 -60.5(3) . . . 7_565 ? Br2 Au1 P1 C1 60.5(3) . . . . ? Br3 Au1 P1 C1 -119.5(3) . . . . ? Br1 Au1 P1 C1 60.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.44 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.381 _refine_diff_density_min -1.567 _refine_diff_density_rms 0.377 #=== END data_21c2cos _database_code_depnum_ccdc_archive 'CCDC 264734' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H21 Au Br5 P' _chemical_formula_weight 756.74 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' P P 0.1023 0.0942 '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' Au Au -2.0133 8.8022 '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 Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 8.5738(2) _cell_length_b 15.1158(3) _cell_length_c 14.0133(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.6080(10) _cell_angle_gamma 90.00 _cell_volume 1804.06(7) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 20615 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.786 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 19.296 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.410 _exptl_absorpt_correction_T_max 0.800 _exptl_absorpt_process_details ; Platon Delabs (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'NONIUS DIP 2020' _diffrn_measurement_method phi-rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20615 _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 25.39 _reflns_number_total 3294 _reflns_number_gt 3263 _reflns_threshold_expression >2sigma(I) _computing_data_collection XPRESS _computing_cell_refinement DENZO _computing_data_reduction SCALEPACK _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0295P)^2^+15.7568P] 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 riding _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 0.011(11) _refine_ls_number_reflns 3294 _refine_ls_number_parameters 151 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0679 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 C11 C 0.5377(9) 0.2158(5) 0.6800(6) 0.0178(16) Uani 1 1 d . . . H11 H 0.5624 0.2487 0.7419 0.021 Uiso 1 1 calc R . . C12 C 0.5999(9) 0.1201(6) 0.6981(7) 0.0238(17) Uani 1 1 d . . . H12A H 0.5840 0.0864 0.6380 0.036 Uiso 1 1 calc R . . H12B H 0.5428 0.0916 0.7464 0.036 Uiso 1 1 calc R . . H12C H 0.7121 0.1219 0.7212 0.036 Uiso 1 1 calc R . . C13 C 0.6244(10) 0.2625(7) 0.6065(8) 0.032(2) Uani 1 1 d . . . H13A H 0.7348 0.2700 0.6321 0.047 Uiso 1 1 calc R . . H13B H 0.5768 0.3207 0.5921 0.047 Uiso 1 1 calc R . . H13C H 0.6176 0.2272 0.5475 0.047 Uiso 1 1 calc R . . C21 C 0.2643(11) 0.3330(6) 0.6419(8) 0.034(2) Uani 1 1 d . . . H21 H 0.3078 0.3554 0.5833 0.041 Uiso 1 1 calc R . . C22 C 0.3355(14) 0.3920(7) 0.7231(8) 0.042(3) Uani 1 1 d . . . H22A H 0.3045 0.4535 0.7093 0.063 Uiso 1 1 calc R . . H22B H 0.4502 0.3873 0.7291 0.063 Uiso 1 1 calc R . . H22C H 0.2977 0.3734 0.7834 0.063 Uiso 1 1 calc R . . C23 C 0.0845(11) 0.3446(6) 0.6207(9) 0.039(3) Uani 1 1 d . . . H23A H 0.0354 0.3327 0.6792 0.059 Uiso 1 1 calc R . . H23B H 0.0435 0.3031 0.5702 0.059 Uiso 1 1 calc R . . H23C H 0.0606 0.4053 0.5992 0.059 Uiso 1 1 calc R . . C31 C 0.2409(10) 0.1572(6) 0.7476(6) 0.0248(19) Uani 1 1 d . . . H31 H 0.2835 0.0957 0.7462 0.030 Uiso 1 1 calc R . . C32 C 0.2961(14) 0.1937(8) 0.8496(7) 0.039(2) Uani 1 1 d . . . H32A H 0.2407 0.2490 0.8596 0.059 Uiso 1 1 calc R . . H32B H 0.4094 0.2048 0.8555 0.059 Uiso 1 1 calc R . . H32C H 0.2730 0.1502 0.8979 0.059 Uiso 1 1 calc R . . C33 C 0.0621(11) 0.1478(7) 0.7330(8) 0.036(2) Uani 1 1 d . . . H33A H 0.0298 0.1022 0.7764 0.054 Uiso 1 1 calc R . . H33B H 0.0283 0.1307 0.6664 0.054 Uiso 1 1 calc R . . H33C H 0.0136 0.2043 0.7470 0.054 Uiso 1 1 calc R . . P1 P 0.3236(2) 0.21720(13) 0.65205(14) 0.0140(4) Uani 1 1 d . . . Br1 Br 0.23638(9) 0.00318(5) 0.57680(6) 0.02349(18) Uani 1 1 d . . . Br2 Br 0.25374(10) 0.06918(7) 0.34366(6) 0.0317(2) Uani 1 1 d . . . Br3 Br 0.29742(12) 0.28136(7) 0.41574(7) 0.0368(2) Uani 1 1 d . . . Br4 Br 0.86805(11) 0.03040(7) 0.48180(7) 0.0356(2) Uani 1 1 d . . . Br5 Br 0.60383(10) 0.04378(7) 0.42174(7) 0.0316(2) Uani 1 1 d . . . Au1 Au 0.27205(3) 0.145482(17) 0.50286(2) 0.01476(9) 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 C11 0.016(4) 0.019(4) 0.018(4) -0.004(3) -0.004(3) -0.003(3) C12 0.019(4) 0.020(4) 0.032(5) -0.002(4) 0.000(3) 0.011(3) C13 0.016(4) 0.031(5) 0.048(6) 0.009(4) 0.003(4) 0.003(3) C21 0.029(5) 0.022(5) 0.050(7) 0.002(5) -0.003(4) 0.006(4) C22 0.063(7) 0.025(5) 0.037(6) -0.009(5) 0.002(5) 0.012(5) C23 0.029(5) 0.025(5) 0.061(7) 0.010(5) -0.007(5) 0.012(4) C31 0.024(4) 0.034(5) 0.019(4) 0.001(4) 0.013(3) -0.005(3) C32 0.060(7) 0.043(6) 0.016(5) -0.008(4) 0.008(4) -0.008(5) C33 0.023(5) 0.047(7) 0.040(6) 0.000(4) 0.009(4) 0.000(4) P1 0.0145(9) 0.0134(9) 0.0140(9) -0.0007(8) 0.0005(7) 0.0012(7) Br1 0.0263(4) 0.0123(4) 0.0316(5) 0.0012(3) 0.0022(3) -0.0017(3) Br2 0.0283(4) 0.0453(6) 0.0202(4) -0.0139(4) -0.0024(3) 0.0039(4) Br3 0.0548(6) 0.0286(5) 0.0267(5) 0.0146(4) 0.0041(4) -0.0050(4) Br4 0.0270(4) 0.0371(5) 0.0424(6) -0.0061(5) 0.0029(4) -0.0028(4) Br5 0.0260(4) 0.0382(5) 0.0314(5) -0.0120(4) 0.0062(3) -0.0025(4) Au1 0.01536(13) 0.01554(14) 0.01297(13) 0.00017(12) -0.00018(8) 0.00015(11) _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 C11 C13 1.513(12) . ? C11 C12 1.553(11) . ? C11 P1 1.833(7) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C21 C22 1.518(15) . ? C21 C23 1.546(13) . ? C21 P1 1.824(10) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C31 C33 1.530(13) . ? C31 C32 1.554(13) . ? C31 P1 1.826(8) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? P1 Au1 2.3513(19) . ? Br1 Au1 2.4222(8) . ? Br2 Au1 2.5003(9) . ? Br3 Au1 2.4118(9) . ? Br4 Br5 2.3329(12) . ? 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 C13 C11 C12 111.1(7) . . ? C13 C11 P1 114.0(6) . . ? C12 C11 P1 111.2(5) . . ? C13 C11 H11 106.7 . . ? C12 C11 H11 106.7 . . ? P1 C11 H11 106.7 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C22 C21 C23 112.5(9) . . ? C22 C21 P1 114.9(7) . . ? C23 C21 P1 112.7(7) . . ? C22 C21 H21 105.2 . . ? C23 C21 H21 105.2 . . ? P1 C21 H21 105.2 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C33 C31 C32 110.5(8) . . ? C33 C31 P1 114.6(7) . . ? C32 C31 P1 113.3(7) . . ? C33 C31 H31 105.9 . . ? C32 C31 H31 105.9 . . ? P1 C31 H31 105.9 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C21 P1 C31 113.9(5) . . ? C21 P1 C11 106.9(4) . . ? C31 P1 C11 107.5(4) . . ? C21 P1 Au1 110.6(4) . . ? C31 P1 Au1 111.9(3) . . ? C11 P1 Au1 105.4(3) . . ? P1 Au1 Br3 92.22(5) . . ? P1 Au1 Br1 92.81(5) . . ? Br3 Au1 Br1 174.83(4) . . ? P1 Au1 Br2 172.81(5) . . ? Br3 Au1 Br2 86.63(4) . . ? Br1 Au1 Br2 88.51(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 C22 C21 P1 C31 70.8(9) . . . . ? C23 C21 P1 C31 -60.0(9) . . . . ? C22 C21 P1 C11 -47.8(9) . . . . ? C23 C21 P1 C11 -178.6(8) . . . . ? C22 C21 P1 Au1 -162.1(7) . . . . ? C23 C21 P1 Au1 67.1(9) . . . . ? C33 C31 P1 C21 64.7(8) . . . . ? C32 C31 P1 C21 -63.4(8) . . . . ? C33 C31 P1 C11 -177.0(7) . . . . ? C32 C31 P1 C11 54.9(8) . . . . ? C33 C31 P1 Au1 -61.7(7) . . . . ? C32 C31 P1 Au1 170.3(6) . . . . ? C13 C11 P1 C21 -57.8(8) . . . . ? C12 C11 P1 C21 175.6(6) . . . . ? C13 C11 P1 C31 179.5(6) . . . . ? C12 C11 P1 C31 52.9(7) . . . . ? C13 C11 P1 Au1 59.8(6) . . . . ? C12 C11 P1 Au1 -66.7(6) . . . . ? C21 P1 Au1 Br3 27.5(4) . . . . ? C31 P1 Au1 Br3 155.7(3) . . . . ? C11 P1 Au1 Br3 -87.7(3) . . . . ? C21 P1 Au1 Br1 -151.3(4) . . . . ? C31 P1 Au1 Br1 -23.2(3) . . . . ? C11 P1 Au1 Br1 93.5(3) . . . . ? C21 P1 Au1 Br2 108.2(5) . . . . ? C31 P1 Au1 Br2 -123.6(5) . . . . ? C11 P1 Au1 Br2 -7.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.768 _refine_diff_density_min -1.442 _refine_diff_density_rms 0.196 #=== END data_24p-1 _database_code_depnum_ccdc_archive 'CCDC 264735' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H33 Au Br5 P' _chemical_formula_weight 985.02 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' Br Br -0.2901 2.4595 '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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2777(2) _cell_length_b 8.6329(2) _cell_length_c 21.4606(5) _cell_angle_alpha 82.4810(10) _cell_angle_beta 88.8960(10) _cell_angle_gamma 85.9630(10) _cell_volume 1516.55(6) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 34935 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 11.505 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.545 _exptl_absorpt_correction_T_max 0.859 _exptl_absorpt_process_details ; Platon Delabs (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'NONIUS DIP 2020' _diffrn_measurement_method phi-rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34935 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.47 _reflns_number_total 5187 _reflns_number_gt 4698 _reflns_threshold_expression >2sigma(I) _computing_data_collection XPRESS _computing_cell_refinement DENZO _computing_data_reduction SCALEPACK _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0346P)^2^+4.4964P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5187 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0815 _refine_ls_wR_factor_gt 0.0789 _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 C11 C 0.9682(6) 0.5769(6) 0.8264(2) 0.0235(11) Uani 1 1 d . . . C12 C 1.0416(7) 0.6857(6) 0.8580(3) 0.0287(12) Uani 1 1 d . . . C13 C 1.1348(7) 0.6329(7) 0.9111(3) 0.0334(13) Uani 1 1 d . . . H13 H 1.1851 0.7068 0.9322 0.040 Uiso 1 1 calc R . . C14 C 1.1556(7) 0.4744(7) 0.9338(3) 0.0312(12) Uani 1 1 d . . . C15 C 1.0898(7) 0.3687(7) 0.9003(3) 0.0296(12) Uani 1 1 d . . . H15 H 1.1071 0.2601 0.9147 0.036 Uiso 1 1 calc R . . C16 C 0.9989(6) 0.4142(6) 0.8460(2) 0.0250(11) Uani 1 1 d . . . C17 C 1.0343(8) 0.8621(7) 0.8380(3) 0.0361(13) Uani 1 1 d . . . H17A H 0.9616 0.9146 0.8665 0.054 Uiso 1 1 calc R . . H17B H 0.9937 0.8857 0.7950 0.054 Uiso 1 1 calc R . . H17C H 1.1431 0.8994 0.8398 0.054 Uiso 1 1 calc R . . C18 C 1.2498(8) 0.4197(9) 0.9927(3) 0.0444(16) Uani 1 1 d . . . H18A H 1.1992 0.3306 1.0164 0.067 Uiso 1 1 calc R . . H18B H 1.2502 0.5052 1.0185 0.067 Uiso 1 1 calc R . . H18C H 1.3614 0.3875 0.9815 0.067 Uiso 1 1 calc R . . C19 C 0.9503(7) 0.2840(6) 0.8113(3) 0.0326(13) Uani 1 1 d . . . H19A H 1.0272 0.1927 0.8204 0.049 Uiso 1 1 calc R . . H19B H 0.9506 0.3193 0.7660 0.049 Uiso 1 1 calc R . . H19C H 0.8414 0.2555 0.8249 0.049 Uiso 1 1 calc R . . C21 C 0.6887(6) 0.5046(6) 0.7467(2) 0.0255(11) Uani 1 1 d . . . C22 C 0.5713(6) 0.4470(6) 0.7909(2) 0.0245(11) Uani 1 1 d . . . C23 C 0.4541(7) 0.3552(7) 0.7711(3) 0.0311(12) Uani 1 1 d . . . H23 H 0.3706 0.3222 0.7997 0.037 Uiso 1 1 calc R . . C24 C 0.4551(7) 0.3110(7) 0.7119(3) 0.0294(12) Uani 1 1 d . . . C25 C 0.5810(7) 0.3572(6) 0.6711(3) 0.0277(12) Uani 1 1 d . . . H25 H 0.5863 0.3221 0.6310 0.033 Uiso 1 1 calc R . . C26 C 0.6994(7) 0.4524(6) 0.6864(2) 0.0273(11) Uani 1 1 d . . . C27 C 0.5646(7) 0.4692(7) 0.8596(3) 0.0340(13) Uani 1 1 d . . . H27A H 0.6701 0.4989 0.8723 0.051 Uiso 1 1 calc R . . H27B H 0.5382 0.3711 0.8849 0.051 Uiso 1 1 calc R . . H27C H 0.4813 0.5520 0.8662 0.051 Uiso 1 1 calc R . . C28 C 0.3228(8) 0.2188(8) 0.6909(3) 0.0401(14) Uani 1 1 d . . . H28A H 0.2970 0.1364 0.7248 0.060 Uiso 1 1 calc R . . H28B H 0.3595 0.1712 0.6537 0.060 Uiso 1 1 calc R . . H28C H 0.2260 0.2889 0.6807 0.060 Uiso 1 1 calc R . . C29 C 0.8332(7) 0.4849(8) 0.6386(3) 0.0363(14) Uani 1 1 d . . . H29A H 0.8406 0.4037 0.6105 0.054 Uiso 1 1 calc R . . H29B H 0.9364 0.4845 0.6603 0.054 Uiso 1 1 calc R . . H29C H 0.8095 0.5875 0.6139 0.054 Uiso 1 1 calc R . . C31 C 0.8965(6) 0.7722(6) 0.6982(2) 0.0255(11) Uani 1 1 d . . . C32 C 0.7814(7) 0.8710(7) 0.6609(3) 0.0292(12) Uani 1 1 d . . . C33 C 0.8401(7) 0.9807(7) 0.6148(3) 0.0325(13) Uani 1 1 d . . . H33 H 0.7648 1.0510 0.5906 0.039 Uiso 1 1 calc R . . C34 C 1.0050(7) 0.9927(7) 0.6022(3) 0.0319(12) Uani 1 1 d . . . C35 C 1.1124(7) 0.8829(7) 0.6361(3) 0.0315(12) Uani 1 1 d . . . H35 H 1.2247 0.8841 0.6262 0.038 Uiso 1 1 calc R . . C36 C 1.0613(7) 0.7715(6) 0.6841(3) 0.0265(11) Uani 1 1 d . . . C37 C 0.5997(7) 0.8651(9) 0.6649(3) 0.0427(15) Uani 1 1 d . . . H37A H 0.5545 0.9433 0.6908 0.064 Uiso 1 1 calc R . . H37B H 0.5723 0.7606 0.6838 0.064 Uiso 1 1 calc R . . H37C H 0.5544 0.8877 0.6225 0.064 Uiso 1 1 calc R . . C38 C 1.0623(9) 1.1157(8) 0.5527(3) 0.0430(15) Uani 1 1 d . . . H38A H 1.1014 1.2015 0.5727 0.064 Uiso 1 1 calc R . . H38B H 0.9725 1.1560 0.5247 0.064 Uiso 1 1 calc R . . H38C H 1.1505 1.0702 0.5283 0.064 Uiso 1 1 calc R . . C39 C 1.1924(6) 0.6572(7) 0.7137(3) 0.0317(12) Uani 1 1 d . . . H39A H 1.2314 0.6948 0.7515 0.048 Uiso 1 1 calc R . . H39B H 1.2823 0.6478 0.6838 0.048 Uiso 1 1 calc R . . H39C H 1.1488 0.5546 0.7252 0.048 Uiso 1 1 calc R . . Br1 Br 0.66114(7) 0.81372(6) 0.81433(3) 0.03210(14) Uani 1 1 d . . . Br11 Br 0.22815(8) -0.06643(9) 0.03170(3) 0.04634(18) Uani 1 1 d . . . Br12 Br 0.58390(7) -0.03628(7) 0.10825(3) 0.03843(15) Uani 1 1 d . . . Br21 Br 0.51161(8) 0.78125(7) 0.49656(3) 0.04023(16) Uani 1 1 d . . . Br22 Br 0.77222(8) 0.47602(8) 0.45682(3) 0.04351(17) Uani 1 1 d . . . Au1 Au 0.5000 0.0000 0.0000 0.02593(9) Uani 1 2 d S . . Au2 Au 0.5000 0.5000 0.5000 0.02887(10) Uani 1 2 d S . . P1 P 0.81963(16) 0.64924(15) 0.76658(6) 0.0232(3) 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 C11 0.023(3) 0.025(3) 0.021(2) -0.002(2) 0.001(2) 0.000(2) C12 0.029(3) 0.027(3) 0.030(3) -0.004(2) -0.004(2) -0.001(2) C13 0.032(3) 0.042(3) 0.027(3) -0.008(3) -0.004(2) -0.004(3) C14 0.024(3) 0.042(3) 0.025(3) 0.003(3) 0.000(2) 0.003(2) C15 0.027(3) 0.028(3) 0.032(3) 0.003(2) 0.006(2) 0.002(2) C16 0.021(3) 0.027(3) 0.026(3) -0.004(2) 0.007(2) 0.000(2) C17 0.042(3) 0.030(3) 0.039(3) -0.008(3) 0.000(3) -0.011(3) C18 0.034(3) 0.064(4) 0.031(3) 0.002(3) -0.006(3) 0.007(3) C19 0.029(3) 0.023(3) 0.044(3) 0.000(3) -0.002(2) 0.001(2) C21 0.025(3) 0.027(3) 0.025(3) -0.003(2) 0.000(2) -0.001(2) C22 0.020(3) 0.029(3) 0.023(3) -0.001(2) -0.001(2) 0.003(2) C23 0.023(3) 0.031(3) 0.037(3) 0.003(3) 0.000(2) -0.001(2) C24 0.026(3) 0.029(3) 0.033(3) -0.003(2) -0.004(2) -0.004(2) C25 0.034(3) 0.027(3) 0.022(3) -0.005(2) -0.005(2) 0.005(2) C26 0.032(3) 0.028(3) 0.021(3) 0.001(2) -0.001(2) -0.001(2) C27 0.038(3) 0.039(3) 0.025(3) -0.002(3) 0.005(2) -0.010(3) C28 0.036(3) 0.038(3) 0.048(4) -0.009(3) -0.009(3) -0.007(3) C29 0.040(3) 0.042(3) 0.030(3) -0.016(3) 0.006(3) -0.010(3) C31 0.022(3) 0.028(3) 0.026(3) -0.006(2) -0.002(2) 0.005(2) C32 0.030(3) 0.029(3) 0.027(3) 0.000(2) 0.001(2) 0.000(2) C33 0.041(3) 0.026(3) 0.030(3) 0.001(2) -0.006(2) 0.001(2) C34 0.042(3) 0.029(3) 0.025(3) -0.002(2) 0.000(2) -0.007(2) C35 0.028(3) 0.034(3) 0.033(3) -0.004(3) -0.003(2) -0.008(2) C36 0.027(3) 0.025(3) 0.028(3) -0.005(2) -0.005(2) 0.000(2) C37 0.030(3) 0.056(4) 0.038(3) 0.007(3) -0.005(3) 0.004(3) C38 0.050(4) 0.041(3) 0.037(3) 0.006(3) -0.005(3) -0.017(3) C39 0.020(3) 0.037(3) 0.037(3) -0.003(3) 0.003(2) 0.001(2) Br1 0.0325(3) 0.0319(3) 0.0313(3) -0.0062(2) 0.0027(2) 0.0048(2) Br11 0.0310(3) 0.0632(4) 0.0484(4) -0.0143(3) 0.0109(3) -0.0184(3) Br12 0.0397(3) 0.0443(3) 0.0310(3) -0.0079(3) -0.0017(2) 0.0052(3) Br21 0.0472(4) 0.0306(3) 0.0428(3) -0.0025(3) -0.0022(3) -0.0059(3) Br22 0.0375(3) 0.0421(3) 0.0490(4) 0.0001(3) 0.0089(3) -0.0028(3) Au1 0.02474(16) 0.02448(15) 0.02917(16) -0.00519(12) 0.00311(11) -0.00362(11) Au2 0.03225(17) 0.02913(17) 0.02448(16) 0.00030(12) -0.00240(12) -0.00335(12) P1 0.0222(7) 0.0238(6) 0.0230(6) -0.0018(5) -0.0003(5) -0.0008(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 C11 C12 1.405(8) . ? C11 C16 1.419(7) . ? C11 P1 1.815(5) . ? C12 C13 1.396(8) . ? C12 C17 1.524(8) . ? C13 C14 1.391(9) . ? C13 H13 0.9500 . ? C14 C15 1.381(8) . ? C14 C18 1.501(8) . ? C15 C16 1.396(8) . ? C15 H15 0.9500 . ? C16 C19 1.508(8) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 C22 1.414(7) . ? C21 C26 1.424(8) . ? C21 P1 1.806(5) . ? C22 C23 1.401(8) . ? C22 C27 1.510(7) . ? C23 C24 1.372(8) . ? C23 H23 0.9500 . ? C24 C25 1.394(8) . ? C24 C28 1.507(8) . ? C25 C26 1.393(8) . ? C25 H25 0.9500 . ? C26 C29 1.512(8) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 C36 1.391(8) . ? C31 C32 1.418(7) . ? C31 P1 1.827(6) . ? C32 C33 1.384(8) . ? C32 C37 1.508(8) . ? C33 C34 1.394(9) . ? C33 H33 0.9500 . ? C34 C35 1.395(8) . ? C34 C38 1.494(8) . ? C35 C36 1.394(8) . ? C35 H35 0.9500 . ? C36 C39 1.506(7) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? Br1 P1 2.2032(15) . ? Br11 Au1 2.4241(6) . ? Br12 Au1 2.4121(6) . ? Br21 Au2 2.4281(6) . ? Br22 Au2 2.4255(6) . ? Au1 Br12 2.4121(6) 2_655 ? Au1 Br11 2.4241(6) 2_655 ? Au2 Br22 2.4255(6) 2_666 ? Au2 Br21 2.4281(6) 2_666 ? 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 C12 C11 C16 119.7(5) . . ? C12 C11 P1 118.6(4) . . ? C16 C11 P1 121.4(4) . . ? C13 C12 C11 119.6(5) . . ? C13 C12 C17 115.0(5) . . ? C11 C12 C17 125.4(5) . . ? C14 C13 C12 121.3(6) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C15 C14 C13 118.2(5) . . ? C15 C14 C18 120.9(6) . . ? C13 C14 C18 120.8(6) . . ? C14 C15 C16 122.9(5) . . ? C14 C15 H15 118.5 . . ? C16 C15 H15 118.5 . . ? C15 C16 C11 117.9(5) . . ? C15 C16 C19 116.2(5) . . ? C11 C16 C19 125.8(5) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C21 C26 120.0(5) . . ? C22 C21 P1 119.4(4) . . ? C26 C21 P1 120.6(4) . . ? C23 C22 C21 118.3(5) . . ? C23 C22 C27 116.0(5) . . ? C21 C22 C27 125.6(5) . . ? C24 C23 C22 122.7(5) . . ? C24 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? C23 C24 C25 117.8(5) . . ? C23 C24 C28 121.4(5) . . ? C25 C24 C28 120.8(5) . . ? C26 C25 C24 123.2(5) . . ? C26 C25 H25 118.4 . . ? C24 C25 H25 118.4 . . ? C25 C26 C21 117.5(5) . . ? C25 C26 C29 116.8(5) . . ? C21 C26 C29 125.5(5) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C36 C31 C32 121.4(5) . . ? C36 C31 P1 121.4(4) . . ? C32 C31 P1 117.1(4) . . ? C33 C32 C31 117.4(5) . . ? C33 C32 C37 116.1(5) . . ? C31 C32 C37 126.5(5) . . ? C32 C33 C34 122.9(5) . . ? C32 C33 H33 118.5 . . ? C34 C33 H33 118.5 . . ? C33 C34 C35 117.3(5) . . ? C33 C34 C38 120.8(5) . . ? C35 C34 C38 121.9(6) . . ? C36 C35 C34 122.5(5) . . ? C36 C35 H35 118.7 . . ? C34 C35 H35 118.7 . . ? C31 C36 C35 117.9(5) . . ? C31 C36 C39 126.5(5) . . ? C35 C36 C39 115.5(5) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Br12 Au1 Br12 180.00(3) . 2_655 ? Br12 Au1 Br11 89.26(2) . 2_655 ? Br12 Au1 Br11 90.74(2) 2_655 2_655 ? Br12 Au1 Br11 90.74(2) . . ? Br12 Au1 Br11 89.26(2) 2_655 . ? Br11 Au1 Br11 180.00(5) 2_655 . ? Br22 Au2 Br22 180.0 . 2_666 ? Br22 Au2 Br21 91.28(2) . . ? Br22 Au2 Br21 88.72(2) 2_666 . ? Br22 Au2 Br21 88.72(2) . 2_666 ? Br22 Au2 Br21 91.28(2) 2_666 2_666 ? Br21 Au2 Br21 180.0 . 2_666 ? C21 P1 C11 114.8(2) . . ? C21 P1 C31 113.6(2) . . ? C11 P1 C31 115.4(2) . . ? C21 P1 Br1 105.11(18) . . ? C11 P1 Br1 102.39(18) . . ? C31 P1 Br1 103.60(17) . . ? 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 C16 C11 C12 C13 -4.5(8) . . . . ? P1 C11 C12 C13 169.2(4) . . . . ? C16 C11 C12 C17 173.1(5) . . . . ? P1 C11 C12 C17 -13.2(8) . . . . ? C11 C12 C13 C14 -0.6(9) . . . . ? C17 C12 C13 C14 -178.4(5) . . . . ? C12 C13 C14 C15 3.9(9) . . . . ? C12 C13 C14 C18 -177.2(6) . . . . ? C13 C14 C15 C16 -2.3(8) . . . . ? C18 C14 C15 C16 178.8(5) . . . . ? C14 C15 C16 C11 -2.6(8) . . . . ? C14 C15 C16 C19 174.0(5) . . . . ? C12 C11 C16 C15 6.0(8) . . . . ? P1 C11 C16 C15 -167.5(4) . . . . ? C12 C11 C16 C19 -170.2(5) . . . . ? P1 C11 C16 C19 16.3(7) . . . . ? C26 C21 C22 C23 -8.3(8) . . . . ? P1 C21 C22 C23 169.7(4) . . . . ? C26 C21 C22 C27 168.6(5) . . . . ? P1 C21 C22 C27 -13.4(7) . . . . ? C21 C22 C23 C24 4.3(8) . . . . ? C27 C22 C23 C24 -173.0(5) . . . . ? C22 C23 C24 C25 1.6(8) . . . . ? C22 C23 C24 C28 -177.0(5) . . . . ? C23 C24 C25 C26 -3.6(8) . . . . ? C28 C24 C25 C26 175.0(5) . . . . ? C24 C25 C26 C21 -0.4(8) . . . . ? C24 C25 C26 C29 176.7(5) . . . . ? C22 C21 C26 C25 6.4(8) . . . . ? P1 C21 C26 C25 -171.5(4) . . . . ? C22 C21 C26 C29 -170.4(5) . . . . ? P1 C21 C26 C29 11.7(8) . . . . ? C36 C31 C32 C33 -8.0(8) . . . . ? P1 C31 C32 C33 170.7(4) . . . . ? C36 C31 C32 C37 169.7(6) . . . . ? P1 C31 C32 C37 -11.6(8) . . . . ? C31 C32 C33 C34 2.8(9) . . . . ? C37 C32 C33 C34 -175.1(6) . . . . ? C32 C33 C34 C35 3.2(9) . . . . ? C32 C33 C34 C38 -178.6(6) . . . . ? C33 C34 C35 C36 -4.5(8) . . . . ? C38 C34 C35 C36 177.4(6) . . . . ? C32 C31 C36 C35 6.8(8) . . . . ? P1 C31 C36 C35 -171.8(4) . . . . ? C32 C31 C36 C39 -170.5(5) . . . . ? P1 C31 C36 C39 10.9(8) . . . . ? C34 C35 C36 C31 -0.4(8) . . . . ? C34 C35 C36 C39 177.2(5) . . . . ? C22 C21 P1 C11 69.9(5) . . . . ? C26 C21 P1 C11 -112.1(5) . . . . ? C22 C21 P1 C31 -154.4(4) . . . . ? C26 C21 P1 C31 23.6(5) . . . . ? C22 C21 P1 Br1 -41.8(4) . . . . ? C26 C21 P1 Br1 136.2(4) . . . . ? C12 C11 P1 C21 -161.5(4) . . . . ? C16 C11 P1 C21 12.1(5) . . . . ? C12 C11 P1 C31 63.6(5) . . . . ? C16 C11 P1 C31 -122.9(4) . . . . ? C12 C11 P1 Br1 -48.2(4) . . . . ? C16 C11 P1 Br1 125.4(4) . . . . ? C36 C31 P1 C21 -117.0(5) . . . . ? C32 C31 P1 C21 64.4(5) . . . . ? C36 C31 P1 C11 18.5(6) . . . . ? C32 C31 P1 C11 -160.2(4) . . . . ? C36 C31 P1 Br1 129.6(4) . . . . ? C32 C31 P1 Br1 -49.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.47 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 1.431 _refine_diff_density_min -0.827 _refine_diff_density_rms 0.149 #=== END data_25p1 _database_code_depnum_ccdc_archive 'CCDC 264736' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H54 Au Br5 P2' _chemical_formula_weight 1001.13 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' Au Au -2.0133 8.8022 '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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6524(3) _cell_length_b 8.9391(3) _cell_length_c 11.6377(4) _cell_angle_alpha 82.4755(13) _cell_angle_beta 74.3263(17) _cell_angle_gamma 88.7371(14) _cell_volume 859.10(5) _cell_formula_units_Z 1 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 19895 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.935 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 482 _exptl_absorpt_coefficient_mu 10.200 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.226 _exptl_absorpt_correction_T_max 0.689 _exptl_absorpt_process_details ; Platon Delabs (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'NONIUS DIP 2020' _diffrn_measurement_method phi-rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19895 _diffrn_reflns_av_R_equivalents 0.074 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.19 _reflns_number_total 2848 _reflns_number_gt 2729 _reflns_threshold_expression >2sigma(I) _computing_data_collection XPRESS _computing_cell_refinement DENZO _computing_data_reduction SCALEPACK _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0824P)^2^+2.8662P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2848 _refine_ls_number_parameters 157 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1298 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _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 0.5000 0.0000 0.0000 0.02578(18) Uani 1 2 d S . . P1 P 0.3604(2) 0.03862(19) 0.19402(16) 0.0241(4) Uani 1 1 d . . . Br1 Br 0.20473(11) 0.47786(10) 0.62284(8) 0.0478(3) Uani 1 1 d . . . Br2 Br 0.0000 0.5000 0.5000 0.0374(3) Uani 1 2 d S . . Br3 Br 0.94864(11) 0.51510(9) 0.10219(10) 0.0491(3) Uani 1 1 d . . . C11 C 0.4209(10) 0.2320(8) 0.2187(7) 0.0355(17) Uani 1 1 d . . . C12 C 0.5995(12) 0.2569(10) 0.1639(9) 0.050(2) Uani 1 1 d . . . H6A H 0.6297 0.3583 0.1742 0.075 Uiso 1 1 calc R . . H6B H 0.6262 0.2468 0.0779 0.075 Uiso 1 1 calc R . . H6C H 0.6582 0.1816 0.2040 0.075 Uiso 1 1 calc R . . C13 C 0.3758(10) 0.2595(9) 0.3515(8) 0.0392(18) Uani 1 1 d . . . H7A H 0.4431 0.1975 0.3940 0.059 Uiso 1 1 calc R . . H7B H 0.2626 0.2323 0.3890 0.059 Uiso 1 1 calc R . . H7C H 0.3930 0.3663 0.3561 0.059 Uiso 1 1 calc R . . C14 C 0.3406(12) 0.3553(9) 0.1473(9) 0.046(2) Uani 1 1 d . . . H1A H 0.3750 0.4555 0.1571 0.069 Uiso 1 1 calc R . . H1B H 0.2236 0.3457 0.1780 0.069 Uiso 1 1 calc R . . H1C H 0.3727 0.3424 0.0617 0.069 Uiso 1 1 calc R . . C21 C 0.1389(9) 0.0278(9) 0.2063(7) 0.0339(16) Uani 1 1 d . . . C22 C 0.0861(10) -0.1373(10) 0.2133(9) 0.044(2) Uani 1 1 d . . . H9A H 0.0845 -0.1914 0.2925 0.066 Uiso 1 1 calc R . . H9B H 0.1617 -0.1856 0.1505 0.066 Uiso 1 1 calc R . . H9C H -0.0216 -0.1399 0.2013 0.066 Uiso 1 1 calc R . . C23 C 0.0299(10) 0.0971(11) 0.3142(8) 0.047(2) Uani 1 1 d . . . H14A H -0.0829 0.0835 0.3159 0.071 Uiso 1 1 calc R . . H14B H 0.0547 0.2051 0.3059 0.071 Uiso 1 1 calc R . . H14C H 0.0486 0.0468 0.3891 0.071 Uiso 1 1 calc R . . C24 C 0.1083(10) 0.1089(10) 0.0887(8) 0.0396(18) Uani 1 1 d . . . H10A H -0.0069 0.1059 0.0949 0.059 Uiso 1 1 calc R . . H10B H 0.1670 0.0580 0.0206 0.059 Uiso 1 1 calc R . . H10C H 0.1453 0.2141 0.0762 0.059 Uiso 1 1 calc R . . C31 C 0.4160(10) -0.1144(8) 0.3037(7) 0.0340(16) Uani 1 1 d . . . C32 C 0.3069(12) -0.1269(10) 0.4309(8) 0.046(2) Uani 1 1 d . . . H5A H 0.1973 -0.1513 0.4303 0.069 Uiso 1 1 calc R . . H5B H 0.3076 -0.0306 0.4626 0.069 Uiso 1 1 calc R . . H5C H 0.3454 -0.2068 0.4821 0.069 Uiso 1 1 calc R . . C33 C 0.4249(12) -0.2673(9) 0.2561(8) 0.045(2) Uani 1 1 d . . . H2A H 0.4542 -0.3454 0.3136 0.067 Uiso 1 1 calc R . . H2B H 0.5060 -0.2618 0.1784 0.067 Uiso 1 1 calc R . . H2C H 0.3201 -0.2924 0.2459 0.067 Uiso 1 1 calc R . . C34 C 0.5907(11) -0.0825(10) 0.3080(9) 0.046(2) Uani 1 1 d . . . H3A H 0.5916 0.0056 0.3500 0.069 Uiso 1 1 calc R . . H3B H 0.6606 -0.0625 0.2258 0.069 Uiso 1 1 calc R . . H3C H 0.6297 -0.1706 0.3511 0.069 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 Au1 0.0252(3) 0.0295(2) 0.0224(3) -0.00732(15) -0.00430(18) 0.00126(15) P1 0.0234(9) 0.0276(8) 0.0207(9) -0.0072(7) -0.0032(8) 0.0009(7) Br1 0.0506(6) 0.0464(5) 0.0481(6) -0.0017(4) -0.0188(5) 0.0047(4) Br2 0.0418(6) 0.0310(5) 0.0358(6) -0.0026(4) -0.0057(5) 0.0061(4) Br3 0.0406(5) 0.0355(4) 0.0755(7) -0.0047(4) -0.0244(5) 0.0012(3) C11 0.042(4) 0.031(4) 0.037(4) -0.012(3) -0.012(4) 0.000(3) C12 0.054(5) 0.040(4) 0.058(6) -0.013(4) -0.013(5) -0.018(4) C13 0.042(5) 0.043(4) 0.040(5) -0.019(4) -0.017(4) 0.003(3) C14 0.064(6) 0.030(4) 0.050(5) -0.002(3) -0.027(5) 0.000(4) C21 0.024(4) 0.043(4) 0.035(4) -0.009(3) -0.005(3) -0.005(3) C22 0.032(4) 0.050(5) 0.054(6) -0.007(4) -0.016(4) -0.011(4) C23 0.029(4) 0.074(6) 0.038(5) -0.016(4) -0.004(4) 0.009(4) C24 0.037(4) 0.051(4) 0.039(5) -0.014(4) -0.022(4) 0.005(3) C31 0.038(4) 0.036(4) 0.028(4) -0.002(3) -0.011(4) 0.006(3) C32 0.062(6) 0.044(4) 0.028(4) 0.007(3) -0.010(4) -0.005(4) C33 0.059(6) 0.036(4) 0.047(5) -0.011(4) -0.026(5) 0.011(4) C34 0.040(5) 0.047(4) 0.057(6) -0.011(4) -0.023(4) 0.012(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 Au1 P1 2.3213(17) . ? Au1 P1 2.3213(17) 2_655 ? P1 C21 1.887(8) . ? P1 C31 1.891(7) . ? P1 C11 1.896(7) . ? Br1 Br2 2.5494(9) . ? Br2 Br1 2.5494(9) 2_566 ? Br3 Br3 2.353(2) 2_765 ? C11 C12 1.513(12) . ? C11 C13 1.540(11) . ? C11 C14 1.558(11) . ? C12 H6A 0.9800 . ? C12 H6B 0.9800 . ? C12 H6C 0.9800 . ? C13 H7A 0.9800 . ? C13 H7B 0.9800 . ? C13 H7C 0.9800 . ? C14 H1A 0.9800 . ? C14 H1B 0.9800 . ? C14 H1C 0.9800 . ? C21 C22 1.540(11) . ? C21 C23 1.546(11) . ? C21 C24 1.547(11) . ? C22 H9A 0.9800 . ? C22 H9B 0.9800 . ? C22 H9C 0.9800 . ? C23 H14A 0.9800 . ? C23 H14B 0.9800 . ? C23 H14C 0.9800 . ? C24 H10A 0.9800 . ? C24 H10B 0.9800 . ? C24 H10C 0.9800 . ? C31 C32 1.517(12) . ? C31 C33 1.534(11) . ? C31 C34 1.560(12) . ? C32 H5A 0.9800 . ? C32 H5B 0.9800 . ? C32 H5C 0.9800 . ? C33 H2A 0.9800 . ? C33 H2B 0.9800 . ? C33 H2C 0.9800 . ? C34 H3A 0.9800 . ? C34 H3B 0.9800 . ? C34 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 P1 Au1 P1 180.00(9) . 2_655 ? C21 P1 C31 110.2(4) . . ? C21 P1 C11 111.4(3) . . ? C31 P1 C11 111.0(3) . . ? C21 P1 Au1 108.0(3) . . ? C31 P1 Au1 108.6(2) . . ? C11 P1 Au1 107.5(3) . . ? Br1 Br2 Br1 180.0 2_566 . ? C12 C11 C13 109.9(7) . . ? C12 C11 C14 104.9(7) . . ? C13 C11 C14 108.5(7) . . ? C12 C11 P1 109.7(5) . . ? C13 C11 P1 114.3(5) . . ? C14 C11 P1 109.2(5) . . ? C11 C12 H6A 109.5 . . ? C11 C12 H6B 109.5 . . ? H6A C12 H6B 109.5 . . ? C11 C12 H6C 109.5 . . ? H6A C12 H6C 109.5 . . ? H6B C12 H6C 109.5 . . ? C11 C13 H7A 109.5 . . ? C11 C13 H7B 109.5 . . ? H7A C13 H7B 109.5 . . ? C11 C13 H7C 109.5 . . ? H7A C13 H7C 109.5 . . ? H7B C13 H7C 109.5 . . ? C11 C14 H1A 109.5 . . ? C11 C14 H1B 109.5 . . ? H1A C14 H1B 109.5 . . ? C11 C14 H1C 109.5 . . ? H1A C14 H1C 109.5 . . ? H1B C14 H1C 109.5 . . ? C22 C21 C23 108.8(7) . . ? C22 C21 C24 105.2(6) . . ? C23 C21 C24 108.8(7) . . ? C22 C21 P1 110.2(5) . . ? C23 C21 P1 114.6(5) . . ? C24 C21 P1 108.8(5) . . ? C21 C22 H9A 109.5 . . ? C21 C22 H9B 109.5 . . ? H9A C22 H9B 109.5 . . ? C21 C22 H9C 109.5 . . ? H9A C22 H9C 109.5 . . ? H9B C22 H9C 109.5 . . ? C21 C23 H14A 109.5 . . ? C21 C23 H14B 109.5 . . ? H14A C23 H14B 109.5 . . ? C21 C23 H14C 109.5 . . ? H14A C23 H14C 109.5 . . ? H14B C23 H14C 109.5 . . ? C21 C24 H10A 109.5 . . ? C21 C24 H10B 109.5 . . ? H10A C24 H10B 109.5 . . ? C21 C24 H10C 109.5 . . ? H10A C24 H10C 109.5 . . ? H10B C24 H10C 109.5 . . ? C32 C31 C33 110.0(7) . . ? C32 C31 C34 108.4(7) . . ? C33 C31 C34 104.6(7) . . ? C32 C31 P1 114.7(6) . . ? C33 C31 P1 110.3(5) . . ? C34 C31 P1 108.3(6) . . ? C31 C32 H5A 109.5 . . ? C31 C32 H5B 109.5 . . ? H5A C32 H5B 109.5 . . ? C31 C32 H5C 109.5 . . ? H5A C32 H5C 109.5 . . ? H5B C32 H5C 109.5 . . ? C31 C33 H2A 109.5 . . ? C31 C33 H2B 109.5 . . ? H2A C33 H2B 109.5 . . ? C31 C33 H2C 109.5 . . ? H2A C33 H2C 109.5 . . ? H2B C33 H2C 109.5 . . ? C31 C34 H3A 109.5 . . ? C31 C34 H3B 109.5 . . ? H3A C34 H3B 109.5 . . ? C31 C34 H3C 109.5 . . ? H3A C34 H3C 109.5 . . ? H3B C34 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 C21 P1 C11 C12 -158.8(6) . . . . ? C31 P1 C11 C12 77.9(7) . . . . ? Au1 P1 C11 C12 -40.7(6) . . . . ? C21 P1 C11 C13 77.3(6) . . . . ? C31 P1 C11 C13 -45.9(7) . . . . ? Au1 P1 C11 C13 -164.6(5) . . . . ? C21 P1 C11 C14 -44.4(7) . . . . ? C31 P1 C11 C14 -167.6(6) . . . . ? Au1 P1 C11 C14 73.7(6) . . . . ? C31 P1 C21 C22 -44.1(7) . . . . ? C11 P1 C21 C22 -167.8(6) . . . . ? Au1 P1 C21 C22 74.4(6) . . . . ? C31 P1 C21 C23 79.0(7) . . . . ? C11 P1 C21 C23 -44.7(7) . . . . ? Au1 P1 C21 C23 -162.5(6) . . . . ? C31 P1 C21 C24 -159.0(5) . . . . ? C11 P1 C21 C24 77.3(6) . . . . ? Au1 P1 C21 C24 -40.5(5) . . . . ? C21 P1 C31 C32 -48.2(7) . . . . ? C11 P1 C31 C32 75.8(7) . . . . ? Au1 P1 C31 C32 -166.3(5) . . . . ? C21 P1 C31 C33 76.8(7) . . . . ? C11 P1 C31 C33 -159.3(6) . . . . ? Au1 P1 C31 C33 -41.4(6) . . . . ? C21 P1 C31 C34 -169.4(5) . . . . ? C11 P1 C31 C34 -45.4(6) . . . . ? Au1 P1 C31 C34 72.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 1.598 _refine_diff_density_min -1.912 _refine_diff_density_rms 0.216 #=== END data_30p1cos _database_code_depnum_ccdc_archive 'CCDC 264737' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H9 Au I4 P' _chemical_formula_weight 780.64 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/c 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 7.71990(10) _cell_length_b 23.7025(4) _cell_length_c 15.9063(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.2520(9) _cell_angle_gamma 90.00 _cell_volume 2610.35(6) _cell_formula_units_Z 8 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 59562 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.973 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 20.800 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.340 _exptl_absorpt_correction_T_max 0.763 _exptl_absorpt_process_details ; Platon Delabs (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'NONIUS DIP 2020' _diffrn_measurement_method phi-rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59562 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.46 _reflns_number_total 4522 _reflns_number_gt 4512 _reflns_threshold_expression >2sigma(I) _computing_data_collection XPRESS _computing_cell_refinement DENZO _computing_data_reduction SCALEPACK _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0502P)^2^+49.8084P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4522 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1076 _refine_ls_wR_factor_gt 0.1076 _refine_ls_goodness_of_fit_ref 1.240 _refine_ls_restrained_S_all 1.240 _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 Au1 Au -0.00823(6) 0.209902(16) 0.51663(3) 0.01573(13) Uani 1 1 d . . . P1 P 0.1698(5) 0.25246(12) 0.4479(2) 0.0218(6) Uani 1 1 d . . . I1 I 0.27490(11) -0.03524(3) 0.51461(5) 0.02190(18) Uani 1 1 d . . . Au2 Au 0.80904(6) 0.056001(17) 0.04301(3) 0.01699(13) Uani 1 1 d . . . P2 P 0.9580(4) 0.02478(12) 0.19854(19) 0.0186(6) Uani 1 1 d . . . I2 I 0.31101(12) 0.07015(3) 0.58968(5) 0.02610(19) Uani 1 1 d . . . I11 I -0.29671(12) 0.20214(4) 0.34877(5) 0.0281(2) Uani 1 1 d . . . C11 C 0.231(2) 0.1983(6) 0.3862(10) 0.031(3) Uani 1 1 d . . . H11A H 0.3203 0.2137 0.3632 0.046 Uiso 1 1 calc R . . H11B H 0.1137 0.1849 0.3329 0.046 Uiso 1 1 calc R . . H11C H 0.2934 0.1667 0.4287 0.046 Uiso 1 1 calc R . . I12 I -0.22365(11) 0.16176(3) 0.58897(5) 0.02202(18) Uani 1 1 d . . . C12 C 0.043(3) 0.3082(6) 0.3678(11) 0.041(4) Uani 1 1 d . . . H12A H -0.0107 0.3343 0.3978 0.061 Uiso 1 1 calc R . . H12B H -0.0616 0.2921 0.3115 0.061 Uiso 1 1 calc R . . H12C H 0.1329 0.3285 0.3503 0.061 Uiso 1 1 calc R . . I13 I 0.29183(12) 0.20618(3) 0.68157(5) 0.02509(19) Uani 1 1 d . . . C13 C 0.391(2) 0.2871(5) 0.5248(11) 0.034(3) Uani 1 1 d . . . H13A H 0.4440 0.3071 0.4873 0.051 Uiso 1 1 calc R . . H13B H 0.4848 0.2589 0.5642 0.051 Uiso 1 1 calc R . . H13C H 0.3655 0.3141 0.5645 0.051 Uiso 1 1 calc R . . I21 I 0.71803(12) -0.04635(3) -0.02529(5) 0.02456(19) Uani 1 1 d . . . C21 C 1.209(2) 0.0444(5) 0.2589(9) 0.030(3) Uani 1 1 d . . . H21A H 1.2583 0.0353 0.3256 0.044 Uiso 1 1 calc R . . H21B H 1.2216 0.0851 0.2517 0.044 Uiso 1 1 calc R . . H21C H 1.2825 0.0237 0.2323 0.044 Uiso 1 1 calc R . . I22 I 0.61756(12) 0.09661(4) -0.12930(5) 0.0285(2) Uani 1 1 d . . . C22 C 0.835(2) 0.0540(6) 0.2616(10) 0.034(3) Uani 1 1 d . . . H22A H 0.6991 0.0421 0.2316 0.051 Uiso 1 1 calc R . . H22B H 0.8414 0.0953 0.2608 0.051 Uiso 1 1 calc R . . H22C H 0.8961 0.0406 0.3265 0.051 Uiso 1 1 calc R . . I23 I 0.91612(13) 0.15908(3) 0.10452(6) 0.0282(2) Uani 1 1 d . . . C23 C 0.955(2) -0.0490(5) 0.2168(9) 0.032(3) Uani 1 1 d . . . H23A H 1.0357 -0.0681 0.1921 0.048 Uiso 1 1 calc R . . H23B H 0.8224 -0.0630 0.1844 0.048 Uiso 1 1 calc R . . H23C H 1.0061 -0.0567 0.2841 0.048 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 Au1 0.0177(3) 0.0128(2) 0.0144(2) 0.00060(14) 0.0049(2) 0.00133(14) P1 0.0242(17) 0.0175(14) 0.0251(15) 0.0047(11) 0.0123(14) 0.0031(11) I1 0.0226(4) 0.0209(4) 0.0212(4) -0.0006(3) 0.0088(3) -0.0033(3) Au2 0.0198(3) 0.0141(2) 0.0149(2) 0.00223(14) 0.0057(2) 0.00082(15) P2 0.0231(17) 0.0178(14) 0.0126(13) 0.0039(10) 0.0060(13) 0.0032(11) I2 0.0289(5) 0.0228(4) 0.0265(4) -0.0045(3) 0.0123(4) -0.0045(3) I11 0.0207(5) 0.0410(5) 0.0160(4) 0.0010(3) 0.0021(4) 0.0010(3) C11 0.026(7) 0.032(7) 0.036(7) 0.000(5) 0.015(7) 0.005(5) I12 0.0260(4) 0.0182(4) 0.0232(4) 0.0029(3) 0.0120(3) -0.0005(3) C12 0.067(11) 0.021(6) 0.039(8) 0.009(6) 0.026(8) 0.006(7) I13 0.0243(5) 0.0267(4) 0.0161(4) -0.0024(3) 0.0015(3) 0.0014(3) C13 0.022(8) 0.019(6) 0.043(8) 0.005(5) -0.001(7) -0.006(5) I21 0.0310(5) 0.0183(4) 0.0229(4) -0.0045(3) 0.0106(4) -0.0031(3) C21 0.035(8) 0.028(6) 0.024(6) 0.001(5) 0.012(6) -0.001(5) I22 0.0260(5) 0.0343(4) 0.0186(4) 0.0105(3) 0.0039(4) 0.0000(3) C22 0.048(9) 0.031(7) 0.033(7) 0.009(5) 0.027(7) 0.009(6) I23 0.0411(5) 0.0136(4) 0.0259(4) 0.0012(3) 0.0111(4) -0.0011(3) C23 0.056(10) 0.015(6) 0.026(6) 0.002(5) 0.017(7) -0.007(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 Au1 P1 2.330(3) . ? Au1 I11 2.6196(9) . ? Au1 I13 2.6231(9) . ? Au1 I12 2.6617(8) . ? P1 C12 1.795(14) . ? P1 C13 1.801(14) . ? P1 C11 1.804(13) . ? I1 I2 2.7294(11) . ? Au2 P2 2.340(3) . ? Au2 I21 2.6238(8) . ? Au2 I23 2.6257(8) . ? Au2 I22 2.6532(8) . ? P2 C23 1.775(12) . ? P2 C22 1.799(13) . ? P2 C21 1.800(14) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 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 P1 Au1 I11 87.95(8) . . ? P1 Au1 I13 92.32(8) . . ? I11 Au1 I13 173.52(3) . . ? P1 Au1 I12 177.82(8) . . ? I11 Au1 I12 89.91(3) . . ? I13 Au1 I12 89.85(3) . . ? C12 P1 C13 101.6(7) . . ? C12 P1 C11 109.2(7) . . ? C13 P1 C11 107.1(7) . . ? C12 P1 Au1 113.8(6) . . ? C13 P1 Au1 117.3(5) . . ? C11 P1 Au1 107.4(5) . . ? P2 Au2 I21 93.54(7) . . ? P2 Au2 I23 88.50(7) . . ? I21 Au2 I23 175.68(3) . . ? P2 Au2 I22 174.73(8) . . ? I21 Au2 I22 89.02(3) . . ? I23 Au2 I22 89.26(3) . . ? C23 P2 C22 103.9(6) . . ? C23 P2 C21 104.8(7) . . ? C22 P2 C21 108.2(7) . . ? C23 P2 Au2 116.7(5) . . ? C22 P2 Au2 109.5(5) . . ? C21 P2 Au2 113.1(4) . . ? P1 C11 H11A 109.5 . . ? P1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P1 C12 H12A 109.5 . . ? P1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P2 C21 H21A 109.5 . . ? P2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? P2 C22 H22A 109.5 . . ? P2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P2 C23 H23A 109.5 . . ? P2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 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 I11 Au1 P1 C12 48.3(6) . . . . ? I13 Au1 P1 C12 -138.2(6) . . . . ? I12 Au1 P1 C12 36(2) . . . . ? I11 Au1 P1 C13 166.7(5) . . . . ? I13 Au1 P1 C13 -19.8(5) . . . . ? I12 Au1 P1 C13 155(2) . . . . ? I11 Au1 P1 C11 -72.6(5) . . . . ? I13 Au1 P1 C11 100.9(5) . . . . ? I12 Au1 P1 C11 -85(2) . . . . ? I21 Au2 P2 C23 -1.3(6) . . . . ? I23 Au2 P2 C23 -177.5(6) . . . . ? I22 Au2 P2 C23 117.5(10) . . . . ? I21 Au2 P2 C22 -118.9(5) . . . . ? I23 Au2 P2 C22 64.9(5) . . . . ? I22 Au2 P2 C22 -0.1(11) . . . . ? I21 Au2 P2 C21 120.3(5) . . . . ? I23 Au2 P2 C21 -55.8(5) . . . . ? I22 Au2 P2 C21 -120.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 25.46 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 3.041 _refine_diff_density_min -2.313 _refine_diff_density_rms 0.371 #=== END data_31p2cos _database_code_depnum_ccdc_archive 'CCDC 264738' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H21 Au Br3 P' _chemical_formula_weight 741.04 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' P P 0.1023 0.0942 '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' Au Au -2.0133 8.8022 '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 P2(1)/c 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 8.51070(10) _cell_length_b 35.9228(4) _cell_length_c 15.5325(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.2154(4) _cell_angle_gamma 90.00 _cell_volume 4729.06(10) _cell_formula_units_Z 8 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 85564 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.082 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 11.362 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.765 _exptl_absorpt_correction_T_max 1.755 _exptl_absorpt_process_details ; Platon Delabs (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'NONIUS DIP 2020' _diffrn_measurement_method phi-rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 85564 _diffrn_reflns_av_R_equivalents 0.061 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 25.44 _reflns_number_total 8397 _reflns_number_gt 7907 _reflns_threshold_expression >2sigma(I) _computing_data_collection XPRESS _computing_cell_refinement DENZO _computing_data_reduction SCALEPACK _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. During the structure refinement, the atoms of a dichloromethane molecule were observed but could not be modelled satisfactorily. The SQUEEZE routine in PLATON was used to modify the HKL file. ; _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^)+(0.0402P)^2^+18.4634P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8397 _refine_ls_number_parameters 475 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0847 _refine_ls_wR_factor_gt 0.0832 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 0.54072(3) 0.061298(6) -0.158465(15) 0.02429(7) Uani 1 1 d . . . P1 P 0.63206(16) 0.09863(4) -0.04027(9) 0.0186(3) Uani 1 1 d . . . Au2 Au 0.22142(2) 0.194805(5) 0.355035(14) 0.01973(7) Uani 1 1 d . . . P2 P 0.39639(16) 0.17201(4) 0.46896(10) 0.0194(3) Uani 1 1 d . . . Br11 Br 0.81131(8) 0.057955(17) -0.19706(4) 0.03465(15) Uani 1 1 d . . . Br12 Br 0.45469(10) 0.02108(2) -0.28179(5) 0.0513(2) Uani 1 1 d . . . Br13 Br 0.26587(7) 0.070653(18) -0.13391(4) 0.03419(15) Uani 1 1 d . . . Br21 Br 0.07627(7) 0.137136(16) 0.36400(4) 0.03244(15) Uani 1 1 d . . . Br22 Br 0.02637(7) 0.216267(16) 0.23856(4) 0.02926(14) Uani 1 1 d . . . Br23 Br 0.34355(7) 0.255702(16) 0.34945(5) 0.03594(16) Uani 1 1 d . . . C111 C 0.7643(6) 0.07404(14) 0.0393(4) 0.0216(11) Uani 1 1 d . . . C112 C 0.8041(7) 0.03734(15) 0.0214(4) 0.0265(13) Uani 1 1 d . . . H112 H 0.7690 0.0264 -0.0327 0.032 Uiso 1 1 calc R . . C113 C 0.8966(7) 0.01666(15) 0.0840(4) 0.0293(13) Uani 1 1 d . . . H113 H 0.9268 -0.0081 0.0718 0.035 Uiso 1 1 calc R . . C114 C 0.9432(8) 0.03234(17) 0.1628(4) 0.0332(14) Uani 1 1 d . . . H114 H 1.0041 0.0183 0.2055 0.040 Uiso 1 1 calc R . . C115 C 0.9020(7) 0.06832(17) 0.1800(4) 0.0306(13) Uani 1 1 d . . . H115 H 0.9351 0.0786 0.2350 0.037 Uiso 1 1 calc R . . C116 C 0.8134(6) 0.09035(15) 0.1198(4) 0.0235(12) Uani 1 1 d . . . C117 C 0.7758(7) 0.12981(15) 0.1466(4) 0.0289(13) Uani 1 1 d . . . H11A H 0.6748 0.1300 0.1723 0.043 Uiso 1 1 calc R . . H11B H 0.7690 0.1461 0.0957 0.043 Uiso 1 1 calc R . . H11C H 0.8594 0.1388 0.1891 0.043 Uiso 1 1 calc R . . C121 C 0.4766(6) 0.11644(15) 0.0211(4) 0.0219(11) Uani 1 1 d . . . C122 C 0.4457(6) 0.15426(16) 0.0216(4) 0.0248(12) Uani 1 1 d . . . H122 H 0.5024 0.1705 -0.0127 0.030 Uiso 1 1 calc R . . C123 C 0.3325(7) 0.16888(18) 0.0718(4) 0.0340(15) Uani 1 1 d . . . H123 H 0.3114 0.1949 0.0715 0.041 Uiso 1 1 calc R . . C124 C 0.2519(8) 0.1452(2) 0.1215(5) 0.0389(16) Uani 1 1 d . . . H124 H 0.1743 0.1548 0.1557 0.047 Uiso 1 1 calc R . . C125 C 0.2828(7) 0.1074(2) 0.1221(4) 0.0353(15) Uani 1 1 d . . . H125 H 0.2265 0.0915 0.1574 0.042 Uiso 1 1 calc R . . C126 C 0.3942(6) 0.09202(16) 0.0723(4) 0.0257(12) Uani 1 1 d . . . C127 C 0.4211(7) 0.05040(17) 0.0786(4) 0.0315(14) Uani 1 1 d . . . H12A H 0.5077 0.0452 0.1230 0.047 Uiso 1 1 calc R . . H12B H 0.4482 0.0409 0.0227 0.047 Uiso 1 1 calc R . . H12C H 0.3247 0.0382 0.0943 0.047 Uiso 1 1 calc R . . C131 C 0.7392(6) 0.13696(14) -0.0849(4) 0.0226(12) Uani 1 1 d . . . C132 C 0.8983(7) 0.14128(15) -0.0558(4) 0.0260(12) Uani 1 1 d . . . H132 H 0.9444 0.1255 -0.0115 0.031 Uiso 1 1 calc R . . C133 C 0.9898(7) 0.16815(18) -0.0906(4) 0.0318(14) Uani 1 1 d . . . H133 H 1.0979 0.1709 -0.0703 0.038 Uiso 1 1 calc R . . C134 C 0.9221(8) 0.19109(17) -0.1554(4) 0.0326(14) Uani 1 1 d . . . H134 H 0.9833 0.2101 -0.1788 0.039 Uiso 1 1 calc R . . C135 C 0.7668(8) 0.18651(16) -0.1860(4) 0.0306(14) Uani 1 1 d . . . H135 H 0.7224 0.2023 -0.2308 0.037 Uiso 1 1 calc R . . C136 C 0.6718(7) 0.15894(15) -0.1523(4) 0.0243(12) Uani 1 1 d . . . C137 C 0.5048(7) 0.15377(16) -0.1946(4) 0.0286(13) Uani 1 1 d . . . H13A H 0.5030 0.1331 -0.2358 0.043 Uiso 1 1 calc R . . H13B H 0.4704 0.1766 -0.2251 0.043 Uiso 1 1 calc R . . H13C H 0.4336 0.1482 -0.1501 0.043 Uiso 1 1 calc R . . C211 C 0.5122(7) 0.13278(15) 0.4360(4) 0.0238(12) Uani 1 1 d . . . C212 C 0.4802(8) 0.11828(16) 0.3531(4) 0.0300(13) Uani 1 1 d . . . H212 H 0.3975 0.1287 0.3154 0.036 Uiso 1 1 calc R . . C213 C 0.5676(9) 0.08892(18) 0.3252(5) 0.0401(16) Uani 1 1 d . . . H213 H 0.5435 0.0786 0.2692 0.048 Uiso 1 1 calc R . . C214 C 0.6909(9) 0.07464(19) 0.3801(5) 0.0459(18) Uani 1 1 d . . . H214 H 0.7533 0.0549 0.3611 0.055 Uiso 1 1 calc R . . C215 C 0.7226(8) 0.08888(18) 0.4611(5) 0.0406(16) Uani 1 1 d . . . H215 H 0.8065 0.0784 0.4977 0.049 Uiso 1 1 calc R . . C216 C 0.6374(7) 0.11815(16) 0.4923(4) 0.0286(13) Uani 1 1 d . . . C217 C 0.6836(8) 0.1322(2) 0.5825(5) 0.0415(17) Uani 1 1 d . . . H21A H 0.7222 0.1115 0.6195 0.062 Uiso 1 1 calc R . . H21B H 0.5915 0.1435 0.6059 0.062 Uiso 1 1 calc R . . H21C H 0.7670 0.1510 0.5808 0.062 Uiso 1 1 calc R . . C221 C 0.5315(6) 0.20730(15) 0.5126(4) 0.0282(13) Uani 1 1 d . . . C222 C 0.5091(8) 0.22270(18) 0.5936(5) 0.0408(17) Uani 1 1 d . . . H222 H 0.4296 0.2131 0.6266 0.049 Uiso 1 1 calc R . . C223 C 0.6042(11) 0.25218(19) 0.6255(6) 0.061(3) Uani 1 1 d . . . H223 H 0.5888 0.2624 0.6805 0.073 Uiso 1 1 calc R . . C224 C 0.7164(11) 0.2663(2) 0.5802(7) 0.069(3) Uani 1 1 d . . . H224 H 0.7785 0.2867 0.6023 0.083 Uiso 1 1 calc R . . C225 C 0.7417(8) 0.2510(2) 0.5011(7) 0.058(3) Uani 1 1 d . . . H225 H 0.8225 0.2611 0.4698 0.069 Uiso 1 1 calc R . . C226 C 0.6518(7) 0.22089(18) 0.4652(5) 0.0386(17) Uani 1 1 d . . . C227 C 0.6893(8) 0.2050(2) 0.3802(6) 0.051(2) Uani 1 1 d . . . H22A H 0.7527 0.1824 0.3903 0.076 Uiso 1 1 calc R . . H22B H 0.7488 0.2233 0.3495 0.076 Uiso 1 1 calc R . . H22C H 0.5910 0.1989 0.3453 0.076 Uiso 1 1 calc R . . C231 C 0.2752(6) 0.15719(16) 0.5527(4) 0.0241(12) Uani 1 1 d . . . C232 C 0.2880(7) 0.12044(18) 0.5823(4) 0.0325(14) Uani 1 1 d . . . H232 H 0.3575 0.1036 0.5576 0.039 Uiso 1 1 calc R . . C233 C 0.1994(8) 0.1086(2) 0.6475(5) 0.0441(18) Uani 1 1 d . . . H233 H 0.2100 0.0839 0.6690 0.053 Uiso 1 1 calc R . . C234 C 0.0954(8) 0.1330(3) 0.6813(5) 0.052(2) Uani 1 1 d . . . H234 H 0.0339 0.1249 0.7258 0.063 Uiso 1 1 calc R . . C235 C 0.0803(8) 0.1690(3) 0.6509(5) 0.050(2) Uani 1 1 d . . . H235 H 0.0099 0.1854 0.6759 0.060 Uiso 1 1 calc R . . C236 C 0.1652(7) 0.1818(2) 0.5847(4) 0.0354(15) Uani 1 1 d . . . C237 C 0.1313(9) 0.2199(2) 0.5495(5) 0.0473(19) Uani 1 1 d . . . H23A H 0.0430 0.2188 0.5044 0.071 Uiso 1 1 calc R . . H23B H 0.2249 0.2296 0.5248 0.071 Uiso 1 1 calc R . . H23C H 0.1036 0.2363 0.5961 0.071 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 Au1 0.03374(13) 0.02068(11) 0.01843(15) -0.00246(8) 0.00226(9) -0.00150(8) P1 0.0219(6) 0.0179(6) 0.0162(8) -0.0001(5) 0.0031(5) -0.0002(5) Au2 0.02053(11) 0.02312(11) 0.01547(14) -0.00007(7) 0.00117(8) 0.00174(7) P2 0.0189(6) 0.0228(6) 0.0163(8) -0.0015(5) 0.0007(5) 0.0004(5) Br11 0.0402(3) 0.0382(3) 0.0270(4) -0.0005(2) 0.0114(3) 0.0117(3) Br12 0.0698(5) 0.0452(4) 0.0372(5) -0.0224(3) -0.0038(4) -0.0034(3) Br13 0.0304(3) 0.0470(3) 0.0250(4) -0.0014(3) 0.0012(2) -0.0130(3) Br21 0.0337(3) 0.0331(3) 0.0284(4) 0.0039(2) -0.0092(3) -0.0103(2) Br22 0.0345(3) 0.0324(3) 0.0197(3) 0.0001(2) -0.0042(2) 0.0085(2) Br23 0.0320(3) 0.0265(3) 0.0478(4) 0.0091(3) -0.0040(3) -0.0022(2) C111 0.025(3) 0.020(2) 0.021(3) 0.002(2) 0.006(2) 0.000(2) C112 0.032(3) 0.023(3) 0.025(4) 0.001(2) 0.011(3) 0.002(2) C113 0.034(3) 0.019(3) 0.036(4) 0.008(2) 0.012(3) 0.006(2) C114 0.040(3) 0.031(3) 0.029(4) 0.010(3) 0.004(3) 0.009(3) C115 0.036(3) 0.032(3) 0.024(4) 0.002(2) 0.004(3) 0.001(3) C116 0.022(3) 0.023(3) 0.025(3) 0.001(2) 0.006(2) -0.003(2) C117 0.035(3) 0.023(3) 0.027(4) -0.002(2) -0.003(3) -0.003(2) C121 0.021(3) 0.027(3) 0.017(3) -0.002(2) 0.000(2) -0.002(2) C122 0.024(3) 0.029(3) 0.020(3) -0.003(2) -0.006(2) 0.001(2) C123 0.030(3) 0.038(3) 0.033(4) -0.014(3) -0.006(3) 0.010(3) C124 0.031(3) 0.060(4) 0.026(4) -0.019(3) 0.005(3) 0.008(3) C125 0.029(3) 0.057(4) 0.021(4) -0.005(3) 0.007(3) -0.004(3) C126 0.022(3) 0.035(3) 0.020(3) -0.004(2) 0.002(2) -0.004(2) C127 0.032(3) 0.033(3) 0.030(4) 0.004(3) 0.009(3) -0.012(3) C131 0.024(3) 0.023(3) 0.022(3) -0.006(2) 0.008(2) -0.003(2) C132 0.030(3) 0.026(3) 0.023(3) 0.004(2) 0.007(2) 0.002(2) C133 0.030(3) 0.041(3) 0.025(4) 0.003(3) 0.007(3) -0.006(3) C134 0.040(3) 0.034(3) 0.025(4) 0.003(2) 0.007(3) -0.013(3) C135 0.049(4) 0.026(3) 0.018(4) 0.004(2) 0.007(3) -0.004(3) C136 0.030(3) 0.022(3) 0.022(3) -0.005(2) 0.008(2) 0.000(2) C137 0.035(3) 0.025(3) 0.024(4) 0.004(2) -0.007(3) 0.000(2) C211 0.027(3) 0.022(3) 0.022(3) 0.001(2) 0.004(2) 0.005(2) C212 0.038(3) 0.031(3) 0.022(4) -0.002(2) 0.006(3) -0.001(2) C213 0.056(4) 0.033(3) 0.034(4) -0.008(3) 0.014(3) 0.010(3) C214 0.057(4) 0.032(3) 0.052(5) 0.003(3) 0.022(4) 0.018(3) C215 0.045(4) 0.034(3) 0.042(5) 0.005(3) 0.004(3) 0.019(3) C216 0.031(3) 0.031(3) 0.023(4) 0.005(2) 0.004(3) 0.006(2) C217 0.039(4) 0.047(4) 0.036(4) 0.006(3) -0.011(3) 0.009(3) C221 0.021(3) 0.020(3) 0.041(4) 0.001(2) -0.008(2) 0.001(2) C222 0.047(4) 0.033(3) 0.039(5) -0.004(3) -0.019(3) 0.006(3) C223 0.084(6) 0.025(3) 0.063(6) -0.014(3) -0.049(5) 0.005(4) C224 0.067(6) 0.028(4) 0.098(8) 0.014(4) -0.070(6) -0.013(4) C225 0.035(4) 0.035(4) 0.097(8) 0.031(4) -0.030(4) -0.014(3) C226 0.020(3) 0.034(3) 0.059(5) 0.013(3) -0.009(3) -0.004(2) C227 0.029(3) 0.049(4) 0.077(6) 0.024(4) 0.022(4) 0.008(3) C231 0.023(3) 0.041(3) 0.007(3) 0.001(2) -0.005(2) -0.001(2) C232 0.027(3) 0.042(3) 0.027(4) 0.000(3) 0.000(3) -0.006(3) C233 0.044(4) 0.060(4) 0.027(4) 0.015(3) -0.004(3) -0.016(3) C234 0.035(4) 0.101(7) 0.022(4) 0.006(4) 0.009(3) -0.010(4) C235 0.030(3) 0.095(6) 0.024(4) 0.006(4) 0.003(3) 0.003(4) C236 0.028(3) 0.061(4) 0.016(4) 0.000(3) -0.001(3) 0.009(3) C237 0.046(4) 0.063(5) 0.034(5) -0.003(3) 0.012(3) 0.025(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 Au1 P1 2.3481(14) . ? Au1 Br13 2.4273(7) . ? Au1 Br11 2.4348(6) . ? Au1 Br12 2.4573(7) . ? P1 C121 1.816(6) . ? P1 C111 1.823(6) . ? P1 C131 1.823(6) . ? Au2 P2 2.3537(14) . ? Au2 Br21 2.4225(6) . ? Au2 Br23 2.4269(6) . ? Au2 Br22 2.4652(6) . ? P2 C221 1.802(6) . ? P2 C231 1.812(6) . ? P2 C211 1.819(5) . ? C111 C112 1.396(8) . ? C111 C116 1.409(8) . ? C112 C113 1.406(8) . ? C112 H112 0.9500 . ? C113 C114 1.373(9) . ? C113 H113 0.9500 . ? C114 C115 1.372(9) . ? C114 H114 0.9500 . ? C115 C116 1.392(8) . ? C115 H115 0.9500 . ? C116 C117 1.520(8) . ? C117 H11A 0.9800 . ? C117 H11B 0.9800 . ? C117 H11C 0.9800 . ? C121 C122 1.384(8) . ? C121 C126 1.413(8) . ? C122 C123 1.396(8) . ? C122 H122 0.9500 . ? C123 C124 1.375(10) . ? C123 H123 0.9500 . ? C124 C125 1.382(10) . ? C124 H124 0.9500 . ? C125 C126 1.390(8) . ? C125 H125 0.9500 . ? C126 C127 1.514(8) . ? C127 H12A 0.9800 . ? C127 H12B 0.9800 . ? C127 H12C 0.9800 . ? C131 C136 1.392(8) . ? C131 C132 1.397(8) . ? C132 C133 1.380(8) . ? C132 H132 0.9500 . ? C133 C134 1.385(9) . ? C133 H133 0.9500 . ? C134 C135 1.373(9) . ? C134 H134 0.9500 . ? C135 C136 1.409(8) . ? C135 H135 0.9500 . ? C136 C137 1.522(8) . ? C137 H13A 0.9800 . ? C137 H13B 0.9800 . ? C137 H13C 0.9800 . ? C211 C212 1.393(9) . ? C211 C216 1.416(8) . ? C212 C213 1.383(9) . ? C212 H212 0.9500 . ? C213 C214 1.388(11) . ? C213 H213 0.9500 . ? C214 C215 1.362(11) . ? C214 H214 0.9500 . ? C215 C216 1.390(9) . ? C215 H215 0.9500 . ? C216 C217 1.508(10) . ? C217 H21A 0.9800 . ? C217 H21B 0.9800 . ? C217 H21C 0.9800 . ? C221 C226 1.402(9) . ? C221 C222 1.404(10) . ? C222 C223 1.396(10) . ? C222 H222 0.9500 . ? C223 C224 1.336(15) . ? C223 H223 0.9500 . ? C224 C225 1.380(14) . ? C224 H224 0.9500 . ? C225 C226 1.409(10) . ? C225 H225 0.9500 . ? C226 C227 1.499(12) . ? C227 H22A 0.9800 . ? C227 H22B 0.9800 . ? C227 H22C 0.9800 . ? C231 C232 1.399(9) . ? C231 C236 1.410(9) . ? C232 C233 1.384(9) . ? C232 H232 0.9500 . ? C233 C234 1.381(12) . ? C233 H233 0.9500 . ? C234 C235 1.378(12) . ? C234 H234 0.9500 . ? C235 C236 1.389(10) . ? C235 H235 0.9500 . ? C236 C237 1.492(10) . ? C237 H23A 0.9800 . ? C237 H23B 0.9800 . ? C237 H23C 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 P1 Au1 Br13 93.06(4) . . ? P1 Au1 Br11 88.13(4) . . ? Br13 Au1 Br11 172.77(2) . . ? P1 Au1 Br12 177.88(4) . . ? Br13 Au1 Br12 88.90(3) . . ? Br11 Au1 Br12 90.03(3) . . ? C121 P1 C111 104.4(3) . . ? C121 P1 C131 110.3(2) . . ? C111 P1 C131 108.9(3) . . ? C121 P1 Au1 113.97(18) . . ? C111 P1 Au1 113.18(18) . . ? C131 P1 Au1 105.99(19) . . ? P2 Au2 Br21 87.15(4) . . ? P2 Au2 Br23 95.55(4) . . ? Br21 Au2 Br23 174.38(2) . . ? P2 Au2 Br22 176.69(4) . . ? Br21 Au2 Br22 89.81(2) . . ? Br23 Au2 Br22 87.36(2) . . ? C221 P2 C231 108.8(3) . . ? C221 P2 C211 107.9(3) . . ? C231 P2 C211 109.4(3) . . ? C221 P2 Au2 112.12(19) . . ? C231 P2 Au2 106.21(18) . . ? C211 P2 Au2 112.3(2) . . ? C112 C111 C116 120.8(5) . . ? C112 C111 P1 117.9(5) . . ? C116 C111 P1 121.0(4) . . ? C111 C112 C113 119.4(6) . . ? C111 C112 H112 120.3 . . ? C113 C112 H112 120.3 . . ? C114 C113 C112 119.9(5) . . ? C114 C113 H113 120.1 . . ? C112 C113 H113 120.1 . . ? C115 C114 C113 120.1(6) . . ? C115 C114 H114 120.0 . . ? C113 C114 H114 120.0 . . ? C114 C115 C116 122.5(6) . . ? C114 C115 H115 118.7 . . ? C116 C115 H115 118.7 . . ? C115 C116 C111 117.2(5) . . ? C115 C116 C117 117.5(5) . . ? C111 C116 C117 125.3(5) . . ? C116 C117 H11A 109.5 . . ? C116 C117 H11B 109.5 . . ? H11A C117 H11B 109.5 . . ? C116 C117 H11C 109.5 . . ? H11A C117 H11C 109.5 . . ? H11B C117 H11C 109.5 . . ? C122 C121 C126 120.1(5) . . ? C122 C121 P1 119.8(4) . . ? C126 C121 P1 120.0(4) . . ? C121 C122 C123 120.9(6) . . ? C121 C122 H122 119.5 . . ? C123 C122 H122 119.5 . . ? C124 C123 C122 119.0(6) . . ? C124 C123 H123 120.5 . . ? C122 C123 H123 120.5 . . ? C123 C124 C125 120.6(6) . . ? C123 C124 H124 119.7 . . ? C125 C124 H124 119.7 . . ? C124 C125 C126 121.6(6) . . ? C124 C125 H125 119.2 . . ? C126 C125 H125 119.2 . . ? C125 C126 C121 117.7(6) . . ? C125 C126 C127 117.5(6) . . ? C121 C126 C127 124.7(5) . . ? C126 C127 H12A 109.5 . . ? C126 C127 H12B 109.5 . . ? H12A C127 H12B 109.5 . . ? C126 C127 H12C 109.5 . . ? H12A C127 H12C 109.5 . . ? H12B C127 H12C 109.5 . . ? C136 C131 C132 120.1(5) . . ? C136 C131 P1 121.9(4) . . ? C132 C131 P1 117.7(4) . . ? C133 C132 C131 121.0(6) . . ? C133 C132 H132 119.5 . . ? C131 C132 H132 119.5 . . ? C132 C133 C134 119.2(6) . . ? C132 C133 H133 120.4 . . ? C134 C133 H133 120.4 . . ? C135 C134 C133 120.3(6) . . ? C135 C134 H134 119.9 . . ? C133 C134 H134 119.9 . . ? C134 C135 C136 121.5(6) . . ? C134 C135 H135 119.2 . . ? C136 C135 H135 119.2 . . ? C131 C136 C135 117.8(5) . . ? C131 C136 C137 124.1(5) . . ? C135 C136 C137 118.0(5) . . ? C136 C137 H13A 109.5 . . ? C136 C137 H13B 109.5 . . ? H13A C137 H13B 109.5 . . ? C136 C137 H13C 109.5 . . ? H13A C137 H13C 109.5 . . ? H13B C137 H13C 109.5 . . ? C212 C211 C216 120.3(5) . . ? C212 C211 P2 118.9(4) . . ? C216 C211 P2 120.7(4) . . ? C213 C212 C211 120.6(6) . . ? C213 C212 H212 119.7 . . ? C211 C212 H212 119.7 . . ? C212 C213 C214 119.2(7) . . ? C212 C213 H213 120.4 . . ? C214 C213 H213 120.4 . . ? C215 C214 C213 120.2(6) . . ? C215 C214 H214 119.9 . . ? C213 C214 H214 119.9 . . ? C214 C215 C216 122.7(6) . . ? C214 C215 H215 118.6 . . ? C216 C215 H215 118.6 . . ? C215 C216 C211 116.9(6) . . ? C215 C216 C217 118.6(6) . . ? C211 C216 C217 124.5(5) . . ? C216 C217 H21A 109.5 . . ? C216 C217 H21B 109.5 . . ? H21A C217 H21B 109.5 . . ? C216 C217 H21C 109.5 . . ? H21A C217 H21C 109.5 . . ? H21B C217 H21C 109.5 . . ? C226 C221 C222 119.9(6) . . ? C226 C221 P2 121.3(5) . . ? C222 C221 P2 118.7(5) . . ? C223 C222 C221 119.7(8) . . ? C223 C222 H222 120.2 . . ? C221 C222 H222 120.2 . . ? C224 C223 C222 121.3(9) . . ? C224 C223 H223 119.3 . . ? C222 C223 H223 119.3 . . ? C223 C224 C225 119.7(7) . . ? C223 C224 H224 120.2 . . ? C225 C224 H224 120.2 . . ? C224 C225 C226 122.3(8) . . ? C224 C225 H225 118.8 . . ? C226 C225 H225 118.8 . . ? C221 C226 C225 117.1(8) . . ? C221 C226 C227 123.6(6) . . ? C225 C226 C227 119.3(7) . . ? C226 C227 H22A 109.5 . . ? C226 C227 H22B 109.5 . . ? H22A C227 H22B 109.5 . . ? C226 C227 H22C 109.5 . . ? H22A C227 H22C 109.5 . . ? H22B C227 H22C 109.5 . . ? C232 C231 C236 120.7(6) . . ? C232 C231 P2 118.7(5) . . ? C236 C231 P2 120.5(5) . . ? C233 C232 C231 119.9(6) . . ? C233 C232 H232 120.1 . . ? C231 C232 H232 120.1 . . ? C234 C233 C232 119.7(7) . . ? C234 C233 H233 120.1 . . ? C232 C233 H233 120.1 . . ? C235 C234 C233 120.4(7) . . ? C235 C234 H234 119.8 . . ? C233 C234 H234 119.8 . . ? C234 C235 C236 121.8(7) . . ? C234 C235 H235 119.1 . . ? C236 C235 H235 119.1 . . ? C235 C236 C231 117.4(7) . . ? C235 C236 C237 118.7(6) . . ? C231 C236 C237 123.9(6) . . ? C236 C237 H23A 109.5 . . ? C236 C237 H23B 109.5 . . ? H23A C237 H23B 109.5 . . ? C236 C237 H23C 109.5 . . ? H23A C237 H23C 109.5 . . ? H23B C237 H23C 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 Br13 Au1 P1 C121 2.7(2) . . . . ? Br11 Au1 P1 C121 175.5(2) . . . . ? Br12 Au1 P1 C121 -154.6(11) . . . . ? Br13 Au1 P1 C111 121.82(19) . . . . ? Br11 Au1 P1 C111 -65.32(19) . . . . ? Br12 Au1 P1 C111 -35.5(12) . . . . ? Br13 Au1 P1 C131 -118.84(19) . . . . ? Br11 Au1 P1 C131 54.02(19) . . . . ? Br12 Au1 P1 C131 83.9(11) . . . . ? Br21 Au2 P2 C221 -169.6(2) . . . . ? Br23 Au2 P2 C221 5.5(2) . . . . ? Br22 Au2 P2 C221 -145.7(6) . . . . ? Br21 Au2 P2 C231 -50.9(2) . . . . ? Br23 Au2 P2 C231 124.2(2) . . . . ? Br22 Au2 P2 C231 -27.0(7) . . . . ? Br21 Au2 P2 C211 68.7(2) . . . . ? Br23 Au2 P2 C211 -116.2(2) . . . . ? Br22 Au2 P2 C211 92.6(7) . . . . ? C121 P1 C111 C112 127.6(4) . . . . ? C131 P1 C111 C112 -114.5(5) . . . . ? Au1 P1 C111 C112 3.1(5) . . . . ? C121 P1 C111 C116 -46.7(5) . . . . ? C131 P1 C111 C116 71.1(5) . . . . ? Au1 P1 C111 C116 -171.2(4) . . . . ? C116 C111 C112 C113 -1.1(8) . . . . ? P1 C111 C112 C113 -175.4(4) . . . . ? C111 C112 C113 C114 1.8(9) . . . . ? C112 C113 C114 C115 -1.1(9) . . . . ? C113 C114 C115 C116 -0.2(10) . . . . ? C114 C115 C116 C111 0.9(9) . . . . ? C114 C115 C116 C117 -179.8(6) . . . . ? C112 C111 C116 C115 -0.2(8) . . . . ? P1 C111 C116 C115 174.0(4) . . . . ? C112 C111 C116 C117 -179.4(5) . . . . ? P1 C111 C116 C117 -5.2(8) . . . . ? C111 P1 C121 C122 122.7(5) . . . . ? C131 P1 C121 C122 5.7(5) . . . . ? Au1 P1 C121 C122 -113.3(4) . . . . ? C111 P1 C121 C126 -53.4(5) . . . . ? C131 P1 C121 C126 -170.3(4) . . . . ? Au1 P1 C121 C126 70.6(5) . . . . ? C126 C121 C122 C123 -0.6(8) . . . . ? P1 C121 C122 C123 -176.7(4) . . . . ? C121 C122 C123 C124 0.4(9) . . . . ? C122 C123 C124 C125 0.2(10) . . . . ? C123 C124 C125 C126 -0.7(10) . . . . ? C124 C125 C126 C121 0.5(9) . . . . ? C124 C125 C126 C127 179.1(6) . . . . ? C122 C121 C126 C125 0.2(8) . . . . ? P1 C121 C126 C125 176.2(5) . . . . ? C122 C121 C126 C127 -178.3(6) . . . . ? P1 C121 C126 C127 -2.3(8) . . . . ? C121 P1 C131 C136 -71.0(5) . . . . ? C111 P1 C131 C136 174.9(4) . . . . ? Au1 P1 C131 C136 52.8(5) . . . . ? C121 P1 C131 C132 115.8(5) . . . . ? C111 P1 C131 C132 1.7(5) . . . . ? Au1 P1 C131 C132 -120.4(4) . . . . ? C136 C131 C132 C133 2.6(9) . . . . ? P1 C131 C132 C133 175.9(5) . . . . ? C131 C132 C133 C134 -0.1(9) . . . . ? C132 C133 C134 C135 -1.5(10) . . . . ? C133 C134 C135 C136 0.7(10) . . . . ? C132 C131 C136 C135 -3.3(8) . . . . ? P1 C131 C136 C135 -176.3(4) . . . . ? C132 C131 C136 C137 173.6(5) . . . . ? P1 C131 C136 C137 0.5(8) . . . . ? C134 C135 C136 C131 1.7(9) . . . . ? C134 C135 C136 C137 -175.3(6) . . . . ? C221 P2 C211 C212 -129.2(5) . . . . ? C231 P2 C211 C212 112.5(5) . . . . ? Au2 P2 C211 C212 -5.2(5) . . . . ? C221 P2 C211 C216 48.1(6) . . . . ? C231 P2 C211 C216 -70.1(5) . . . . ? Au2 P2 C211 C216 172.2(4) . . . . ? C216 C211 C212 C213 1.5(9) . . . . ? P2 C211 C212 C213 178.8(5) . . . . ? C211 C212 C213 C214 -1.8(10) . . . . ? C212 C213 C214 C215 1.5(11) . . . . ? C213 C214 C215 C216 -1.0(12) . . . . ? C214 C215 C216 C211 0.7(10) . . . . ? C214 C215 C216 C217 -179.1(7) . . . . ? C212 C211 C216 C215 -0.9(9) . . . . ? P2 C211 C216 C215 -178.2(5) . . . . ? C212 C211 C216 C217 178.9(6) . . . . ? P2 C211 C216 C217 1.6(9) . . . . ? C231 P2 C221 C226 172.7(5) . . . . ? C211 P2 C221 C226 54.1(5) . . . . ? Au2 P2 C221 C226 -70.1(5) . . . . ? C231 P2 C221 C222 -10.9(5) . . . . ? C211 P2 C221 C222 -129.5(5) . . . . ? Au2 P2 C221 C222 106.3(5) . . . . ? C226 C221 C222 C223 1.7(9) . . . . ? P2 C221 C222 C223 -174.8(5) . . . . ? C221 C222 C223 C224 0.3(10) . . . . ? C222 C223 C224 C225 -1.4(11) . . . . ? C223 C224 C225 C226 0.6(11) . . . . ? C222 C221 C226 C225 -2.4(8) . . . . ? P2 C221 C226 C225 174.0(5) . . . . ? C222 C221 C226 C227 177.0(6) . . . . ? P2 C221 C226 C227 -6.6(8) . . . . ? C224 C225 C226 C221 1.3(9) . . . . ? C224 C225 C226 C227 -178.1(6) . . . . ? C221 P2 C231 C232 -115.5(5) . . . . ? C211 P2 C231 C232 2.2(5) . . . . ? Au2 P2 C231 C232 123.6(4) . . . . ? C221 P2 C231 C236 67.2(5) . . . . ? C211 P2 C231 C236 -175.2(5) . . . . ? Au2 P2 C231 C236 -53.7(5) . . . . ? C236 C231 C232 C233 -4.1(9) . . . . ? P2 C231 C232 C233 178.5(5) . . . . ? C231 C232 C233 C234 1.8(10) . . . . ? C232 C233 C234 C235 -0.5(11) . . . . ? C233 C234 C235 C236 1.5(12) . . . . ? C234 C235 C236 C231 -3.6(11) . . . . ? C234 C235 C236 C237 174.2(7) . . . . ? C232 C231 C236 C235 4.9(9) . . . . ? P2 C231 C236 C235 -177.8(5) . . . . ? C232 C231 C236 C237 -172.8(6) . . . . ? P2 C231 C236 C237 4.5(9) . . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 25.44 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 1.951 _refine_diff_density_min -0.981 _refine_diff_density_rms 0.167 #=== END