Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'ProfD Hubert Schmidbaur' _publ_contact_author_address ; AC/Neue Materialien Technische Universitat Munchen Lichtenbergstrasse 4 Garching 85747 GERMANY ; _publ_contact_author_email H.SCHMIDBAUR@LRZ.TUM.DE _publ_section_title ; Governing the oxidative addition of iodine to gold(I) complexes by ligand tuning ; loop_ _publ_author_name 'Hubert Schmidbaur' 'Annette Schier' 'Daniel Schneider' data_[(Me3P)AuI3] _database_code_depnum_ccdc_archive 'CCDC 232528' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(Me3P)AuI3]' _chemical_formula_sum 'C3 H9 Au I3 P' _chemical_formula_weight 653.74 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.6198(1) _cell_length_b 12.1910(2) _cell_length_c 12.1256(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.967(1) _cell_angle_gamma 90.00 _cell_volume 1118.07(3) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 28524 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.884 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 21.516 _exptl_absorpt_correction_type DELABS _exptl_absorpt_correction_T_min 0.360 _exptl_absorpt_correction_T_max 0.774 _exptl_absorpt_process_details ? _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 HU' _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 28524 _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_av_sigmaI/netI 0.077 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.24 _reflns_number_total 2483 _reflns_number_gt 2469 _reflns_threshold_expression >2sigma(I) _computing_data_collection XPRESS _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _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^)+(0.0362P)^2^+8.8624P] 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 2483 _refine_ls_number_parameters 73 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0836 _refine_ls_wR_factor_gt 0.0834 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.142 _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 Au Au 0.03704(3) 0.391923(19) 0.668593(19) 0.01766(10) Uani 1 1 d . . . I1 I 0.16653(7) 0.35262(4) 0.48167(4) 0.03129(14) Uani 1 1 d . . . I2 I -0.08247(7) 0.41795(5) 0.86038(4) 0.03700(15) Uani 1 1 d . . . I3 I -0.22931(7) 0.25563(4) 0.60775(5) 0.03706(15) Uani 1 1 d . . . P P 0.2733(2) 0.50523(14) 0.73507(14) 0.0202(3) Uani 1 1 d . . . C1 C 0.4366(12) 0.5348(9) 0.6437(7) 0.042(2) Uani 1 1 d . . . H1A H 0.5276 0.5830 0.6817 0.063 Uiso 1 1 calc R . . H1B H 0.3799 0.5713 0.5767 0.063 Uiso 1 1 calc R . . H1C H 0.4912 0.4662 0.6231 0.063 Uiso 1 1 calc R . . C2 C 0.3988(11) 0.4461(9) 0.8553(7) 0.043(2) Uani 1 1 d . . . H2A H 0.4971 0.4949 0.8819 0.065 Uiso 1 1 calc R . . H2B H 0.4456 0.3747 0.8357 0.065 Uiso 1 1 calc R . . H2C H 0.3223 0.4362 0.9139 0.065 Uiso 1 1 calc R . . C3 C 0.1989(13) 0.6378(8) 0.7743(11) 0.051(3) Uani 1 1 d . . . H3A H 0.3012 0.6831 0.8019 0.077 Uiso 1 1 calc R . . H3B H 0.1219 0.6293 0.8329 0.077 Uiso 1 1 calc R . . H3C H 0.1330 0.6734 0.7096 0.077 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 Au 0.01924(15) 0.01443(16) 0.01883(15) -0.00013(8) 0.00037(10) 0.00032(8) I1 0.0403(3) 0.0322(3) 0.0221(2) -0.00669(19) 0.00680(19) -0.0005(2) I2 0.0297(3) 0.0575(4) 0.0254(3) 0.0004(2) 0.0101(2) -0.0008(2) I3 0.0264(3) 0.0271(3) 0.0562(3) -0.0082(2) -0.0014(2) -0.00725(18) P 0.0218(8) 0.0195(8) 0.0187(7) 0.0000(6) -0.0001(6) -0.0025(6) C1 0.040(4) 0.055(6) 0.032(4) 0.000(4) 0.009(3) -0.024(4) C2 0.031(4) 0.061(6) 0.034(4) 0.015(4) -0.009(3) -0.010(4) C3 0.037(5) 0.025(4) 0.090(8) -0.023(5) -0.004(5) -0.003(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 Au P 2.3340(17) . ? Au I2 2.6176(5) . ? Au I1 2.6235(5) . ? Au I3 2.6572(5) . ? P C2 1.795(8) . ? P C3 1.796(9) . ? P C1 1.800(8) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P Au I2 87.61(4) . . ? P Au I1 92.94(4) . . ? I2 Au I1 175.95(2) . . ? P Au I3 175.70(4) . . ? I2 Au I3 89.206(19) . . ? I1 Au I3 90.032(19) . . ? C2 P C3 107.5(6) . . ? C2 P C1 103.9(4) . . ? C3 P C1 104.3(5) . . ? C2 P Au 110.8(3) . . ? C3 P Au 111.6(3) . . ? C1 P Au 117.9(3) . . ? P C1 H1A 109.5 . . ? P C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P C2 H2A 109.5 . . ? P C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P C3 H3A 109.5 . . ? P C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag I2 Au P C2 61.2(4) . . . . ? I1 Au P C2 -114.8(4) . . . . ? I3 Au P C2 18.9(8) . . . . ? I2 Au P C3 -58.6(5) . . . . ? I1 Au P C3 125.5(5) . . . . ? I3 Au P C3 -100.9(7) . . . . ? I2 Au P C1 -179.3(4) . . . . ? I1 Au P C1 4.7(4) . . . . ? I3 Au P C1 138.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.24 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.864 _refine_diff_density_min -2.532 _refine_diff_density_rms 0.306 #===END data_[(Me2PhP)AuI30.75CH2Cl2] _database_code_depnum_ccdc_archive 'CCDC 232529' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(Me2PhP)AuI30.75CH2Cl2]' _chemical_formula_sum 'C8.75 H12.50 Au Cl1.50 I3 P' _chemical_formula_weight 779.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 35.9785(4) _cell_length_b 8.3066(1) _cell_length_c 25.1157(4) _cell_angle_alpha 90.00 _cell_angle_beta 116.494(1) _cell_angle_gamma 90.00 _cell_volume 6717.77(15) _cell_formula_units_Z 16 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 101645 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.083 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5496 _exptl_absorpt_coefficient_mu 14.582 _exptl_absorpt_correction_type DEABS _exptl_absorpt_correction_T_min 0.348 _exptl_absorpt_correction_T_max 0.787 _exptl_absorpt_process_details ? _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 HU' _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 101645 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_av_sigmaI/netI 0.064 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.29 _reflns_number_total 7357 _reflns_number_gt 7281 _reflns_threshold_expression >2sigma(I) _computing_data_collection XPRESS _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _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^)+(0.0053P)^2^+116.6794P] 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 7357 _refine_ls_number_parameters 276 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0839 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.223 _refine_ls_restrained_S_all 1.223 _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 0.215719(7) 0.86197(3) 0.162299(11) 0.02132(7) Uani 1 1 d . . . Au2 Au 0.367449(8) 0.81600(3) 0.122606(11) 0.02281(7) Uani 1 1 d . . . I1 I 0.213405(16) 1.14180(6) 0.11251(2) 0.03213(11) Uani 1 1 d . . . I2 I 0.277530(15) 0.77207(7) 0.13885(2) 0.03326(12) Uani 1 1 d . . . I3 I 0.211829(15) 0.56597(6) 0.19598(2) 0.03184(11) Uani 1 1 d . . . I4 I 0.408987(14) 0.56660(6) 0.18791(2) 0.03012(11) Uani 1 1 d . . . I5 I 0.338172(16) 0.63029(6) 0.02824(2) 0.03049(11) Uani 1 1 d . . . I6 I 0.39900(2) 0.99130(8) 0.21968(3) 0.05073(17) Uani 1 1 d . . . P1 P 0.16241(5) 0.9323(2) 0.18736(8) 0.0228(3) Uani 1 1 d . . . P2 P 0.33491(6) 1.0387(2) 0.06246(8) 0.0253(3) Uani 1 1 d . . . C11 C 0.1533(3) 1.1453(9) 0.1897(4) 0.0333(16) Uani 1 1 d . . . H11A H 0.1306 1.1619 0.2006 0.050 Uiso 1 1 calc R . . H11B H 0.1459 1.1927 0.1506 0.050 Uiso 1 1 calc R . . H11C H 0.1786 1.1968 0.2194 0.050 Uiso 1 1 calc R . . C12 C 0.1714(2) 0.8608(10) 0.2594(3) 0.0299(15) Uani 1 1 d . . . H12A H 0.1482 0.8933 0.2676 0.045 Uiso 1 1 calc R . . H12B H 0.1973 0.9069 0.2896 0.045 Uiso 1 1 calc R . . H12C H 0.1735 0.7431 0.2604 0.045 Uiso 1 1 calc R . . C21 C 0.2840(2) 1.0022(10) 0.0022(4) 0.0342(16) Uani 1 1 d . . . H21A H 0.2731 1.1022 -0.0201 0.051 Uiso 1 1 calc R . . H21B H 0.2653 0.9648 0.0185 0.051 Uiso 1 1 calc R . . H21C H 0.2860 0.9199 -0.0243 0.051 Uiso 1 1 calc R . . C22 C 0.3257(2) 1.2073(9) 0.0996(4) 0.0325(16) Uani 1 1 d . . . H22A H 0.3121 1.2934 0.0707 0.049 Uiso 1 1 calc R . . H22B H 0.3522 1.2465 0.1306 0.049 Uiso 1 1 calc R . . H22C H 0.3078 1.1740 0.1177 0.049 Uiso 1 1 calc R . . C111 C 0.1149(2) 0.8491(9) 0.1316(3) 0.0263(14) Uani 1 1 d . . . C112 C 0.0897(2) 0.7479(11) 0.1456(4) 0.0373(18) Uani 1 1 d . . . H11D H 0.0976 0.7195 0.1859 0.045 Uiso 1 1 calc R . . C113 C 0.0529(3) 0.6884(12) 0.1006(4) 0.046(2) Uani 1 1 d . . . H11E H 0.0356 0.6200 0.1103 0.055 Uiso 1 1 calc R . . C114 C 0.0414(2) 0.7283(11) 0.0420(4) 0.0416(19) Uani 1 1 d . . . H11F H 0.0163 0.6870 0.0114 0.050 Uiso 1 1 calc R . . C115 C 0.0661(3) 0.8275(12) 0.0278(4) 0.046(2) Uani 1 1 d . . . H11G H 0.0582 0.8551 -0.0126 0.055 Uiso 1 1 calc R . . C116 C 0.1028(2) 0.8878(11) 0.0726(4) 0.0359(17) Uani 1 1 d . . . H11H H 0.1198 0.9565 0.0626 0.043 Uiso 1 1 calc R . . C211 C 0.3688(2) 1.1045(9) 0.0308(3) 0.0290(15) Uani 1 1 d . . . C212 C 0.3639(3) 1.0408(10) -0.0231(3) 0.0354(17) Uani 1 1 d . . . H21D H 0.3426 0.9646 -0.0436 0.042 Uiso 1 1 calc R . . C213 C 0.3902(3) 1.0889(11) -0.0467(4) 0.0409(19) Uani 1 1 d . . . H21E H 0.3867 1.0468 -0.0839 0.049 Uiso 1 1 calc R . . C214 C 0.4215(3) 1.1982(12) -0.0166(4) 0.045(2) Uani 1 1 d . . . H21F H 0.4396 1.2298 -0.0330 0.054 Uiso 1 1 calc R . . C215 C 0.4270(2) 1.2624(12) 0.0375(4) 0.042(2) Uani 1 1 d . . . H21G H 0.4486 1.3372 0.0581 0.051 Uiso 1 1 calc R . . C216 C 0.4000(2) 1.2154(10) 0.0613(4) 0.0354(17) Uani 1 1 d . . . H21I H 0.4031 1.2591 0.0980 0.043 Uiso 1 1 calc R . . C1 C 0.0000 0.689(2) 0.2500 0.088(7) Uani 1 2 d S . . H1A H 0.0233 0.6235 0.2723 0.106 Uiso 1 1 d . . . C2 C -0.0037(3) 0.7688(12) -0.1595(4) 0.043(2) Uani 1 1 d . . . H2A H -0.0251 0.7296 -0.1984 0.052 Uiso 1 1 calc R . . H2B H 0.0138 0.8481 -0.1674 0.052 Uiso 1 1 calc R . . Cl11 Cl 0.01075(8) 0.8026(3) 0.20004(10) 0.0486(5) Uani 1 1 d . . . Cl21 Cl -0.02856(8) 0.8658(3) -0.12114(11) 0.0543(6) Uani 1 1 d . . . Cl22 Cl 0.02710(7) 0.6076(3) -0.11997(11) 0.0473(5) 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 Au1 0.01816(12) 0.02326(14) 0.02325(12) 0.00072(9) 0.00988(10) -0.00045(9) Au2 0.02017(13) 0.02347(14) 0.02499(13) -0.00070(9) 0.01026(10) -0.00074(9) I1 0.0361(3) 0.0272(3) 0.0379(3) 0.00638(18) 0.0208(2) 0.00015(18) I2 0.0255(2) 0.0440(3) 0.0356(2) 0.0067(2) 0.01834(19) 0.00708(19) I3 0.0302(2) 0.0238(2) 0.0424(3) 0.00482(18) 0.0170(2) 0.00092(17) I4 0.0266(2) 0.0295(3) 0.0315(2) 0.00445(18) 0.01041(18) 0.00201(17) I5 0.0374(3) 0.0264(3) 0.0269(2) -0.00248(17) 0.01375(19) -0.00060(18) I6 0.0480(3) 0.0447(3) 0.0380(3) -0.0170(2) -0.0001(2) 0.0084(3) P1 0.0210(8) 0.0243(9) 0.0263(8) 0.0003(6) 0.0133(7) 0.0003(6) P2 0.0235(8) 0.0228(9) 0.0301(9) 0.0013(7) 0.0123(7) -0.0001(6) C11 0.034(4) 0.030(4) 0.038(4) -0.002(3) 0.018(3) 0.008(3) C12 0.032(4) 0.034(4) 0.027(3) 0.001(3) 0.016(3) -0.001(3) C21 0.025(4) 0.031(4) 0.041(4) 0.006(3) 0.010(3) 0.003(3) C22 0.036(4) 0.025(4) 0.043(4) -0.002(3) 0.024(3) 0.003(3) C111 0.026(3) 0.022(3) 0.035(4) 0.000(3) 0.017(3) -0.001(3) C112 0.027(4) 0.047(5) 0.041(4) -0.001(4) 0.019(3) -0.013(3) C113 0.028(4) 0.054(6) 0.060(6) -0.007(4) 0.025(4) -0.009(4) C114 0.022(4) 0.048(5) 0.045(4) -0.010(4) 0.006(3) 0.000(3) C115 0.037(5) 0.055(6) 0.032(4) 0.000(4) 0.004(3) -0.009(4) C116 0.027(4) 0.043(5) 0.036(4) 0.002(3) 0.012(3) -0.007(3) C211 0.030(4) 0.027(4) 0.033(4) 0.007(3) 0.017(3) 0.003(3) C212 0.042(4) 0.032(4) 0.033(4) 0.004(3) 0.018(3) 0.005(3) C213 0.047(5) 0.042(5) 0.041(4) 0.010(4) 0.026(4) 0.014(4) C214 0.033(4) 0.059(6) 0.051(5) 0.027(4) 0.026(4) 0.016(4) C215 0.024(4) 0.052(5) 0.050(5) 0.009(4) 0.015(3) 0.000(3) C216 0.032(4) 0.036(4) 0.040(4) 0.004(3) 0.018(3) -0.001(3) C1 0.125(17) 0.042(10) 0.16(2) 0.000 0.121(17) 0.000 C2 0.039(5) 0.052(6) 0.037(4) 0.007(4) 0.016(4) 0.005(4) Cl11 0.0509(13) 0.0459(13) 0.0435(11) -0.0034(9) 0.0162(10) 0.0018(10) Cl21 0.0487(13) 0.0682(17) 0.0503(12) 0.0118(11) 0.0260(11) 0.0226(11) Cl22 0.0437(12) 0.0394(12) 0.0581(13) 0.0044(10) 0.0219(10) 0.0051(9) _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 2.3439(17) . ? Au1 I1 2.6231(5) . ? Au1 I3 2.6242(5) . ? Au1 I2 2.6493(5) . ? Au2 P2 2.3445(18) . ? Au2 I5 2.6228(5) . ? Au2 I6 2.6236(6) . ? Au2 I4 2.6511(5) . ? P1 C12 1.791(7) . ? P1 C111 1.796(7) . ? P1 C11 1.805(8) . ? P2 C22 1.793(8) . ? P2 C21 1.806(8) . ? P2 C211 1.812(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 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 . ? C111 C116 1.383(11) . ? C111 C112 1.392(10) . ? C112 C113 1.393(12) . ? C112 H11D 0.9500 . ? C113 C114 1.381(13) . ? C113 H11E 0.9500 . ? C114 C115 1.371(13) . ? C114 H11F 0.9500 . ? C115 C116 1.392(11) . ? C115 H11G 0.9500 . ? C116 H11H 0.9500 . ? C211 C216 1.389(11) . ? C211 C212 1.390(11) . ? C212 C213 1.380(12) . ? C212 H21D 0.9500 . ? C213 C214 1.382(14) . ? C213 H21E 0.9500 . ? C214 C215 1.390(13) . ? C214 H21F 0.9500 . ? C215 C216 1.402(11) . ? C215 H21G 0.9500 . ? C216 H21I 0.9500 . ? C1 Cl11 1.746(10) . ? C1 Cl11 1.746(10) 2 ? C1 H1A 0.9454 . ? C2 Cl22 1.740(9) . ? C2 Cl21 1.774(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? 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 I1 92.95(5) . . ? P1 Au1 I3 88.81(5) . . ? I1 Au1 I3 171.507(19) . . ? P1 Au1 I2 176.98(5) . . ? I1 Au1 I2 89.718(17) . . ? I3 Au1 I2 88.757(17) . . ? P2 Au2 I5 89.88(5) . . ? P2 Au2 I6 92.61(5) . . ? I5 Au2 I6 177.43(2) . . ? P2 Au2 I4 175.44(5) . . ? I5 Au2 I4 89.297(17) . . ? I6 Au2 I4 88.167(19) . . ? C12 P1 C111 109.8(3) . . ? C12 P1 C11 104.2(4) . . ? C111 P1 C11 106.3(4) . . ? C12 P1 Au1 112.9(3) . . ? C111 P1 Au1 107.6(2) . . ? C11 P1 Au1 115.8(3) . . ? C22 P2 C21 102.3(4) . . ? C22 P2 C211 108.0(4) . . ? C21 P2 C211 108.3(4) . . ? C22 P2 Au2 115.9(3) . . ? C21 P2 Au2 115.8(3) . . ? C211 P2 Au2 106.3(2) . . ? 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 . . ? 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 . . ? C116 C111 C112 118.9(7) . . ? C116 C111 P1 118.7(6) . . ? C112 C111 P1 122.4(6) . . ? C111 C112 C113 120.0(8) . . ? C111 C112 H11D 120.0 . . ? C113 C112 H11D 120.0 . . ? C114 C113 C112 120.2(8) . . ? C114 C113 H11E 119.9 . . ? C112 C113 H11E 119.9 . . ? C115 C114 C113 120.1(8) . . ? C115 C114 H11F 119.9 . . ? C113 C114 H11F 119.9 . . ? C114 C115 C116 119.8(8) . . ? C114 C115 H11G 120.1 . . ? C116 C115 H11G 120.1 . . ? C111 C116 C115 121.0(8) . . ? C111 C116 H11H 119.5 . . ? C115 C116 H11H 119.5 . . ? C216 C211 C212 120.6(7) . . ? C216 C211 P2 119.8(6) . . ? C212 C211 P2 119.7(6) . . ? C213 C212 C211 119.7(8) . . ? C213 C212 H21D 120.2 . . ? C211 C212 H21D 120.2 . . ? C214 C213 C212 120.2(8) . . ? C214 C213 H21E 119.9 . . ? C212 C213 H21E 119.9 . . ? C213 C214 C215 120.8(8) . . ? C213 C214 H21F 119.6 . . ? C215 C214 H21F 119.6 . . ? C214 C215 C216 119.2(8) . . ? C214 C215 H21G 120.4 . . ? C216 C215 H21G 120.4 . . ? C211 C216 C215 119.6(8) . . ? C211 C216 H21I 120.2 . . ? C215 C216 H21I 120.2 . . ? Cl11 C1 Cl11 114.5(10) . 2 ? Cl11 C1 H1A 108.3 . . ? Cl11 C1 H1A 108.0 2 . ? Cl22 C2 Cl21 112.7(5) . . ? Cl22 C2 H2A 109.0 . . ? Cl21 C2 H2A 109.0 . . ? Cl22 C2 H2B 109.0 . . ? Cl21 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? 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 I1 Au1 P1 C12 -140.3(3) . . . . ? I3 Au1 P1 C12 48.0(3) . . . . ? I2 Au1 P1 C12 11.6(10) . . . . ? I1 Au1 P1 C111 98.3(3) . . . . ? I3 Au1 P1 C111 -73.4(3) . . . . ? I2 Au1 P1 C111 -109.8(9) . . . . ? I1 Au1 P1 C11 -20.4(3) . . . . ? I3 Au1 P1 C11 167.9(3) . . . . ? I2 Au1 P1 C11 131.6(9) . . . . ? I5 Au2 P2 C22 158.5(3) . . . . ? I6 Au2 P2 C22 -22.1(3) . . . . ? I4 Au2 P2 C22 -121.9(6) . . . . ? I5 Au2 P2 C21 38.7(3) . . . . ? I6 Au2 P2 C21 -142.0(3) . . . . ? I4 Au2 P2 C21 118.3(6) . . . . ? I5 Au2 P2 C211 -81.6(3) . . . . ? I6 Au2 P2 C211 97.8(3) . . . . ? I4 Au2 P2 C211 -1.9(7) . . . . ? C12 P1 C111 C116 -178.9(6) . . . . ? C11 P1 C111 C116 69.0(7) . . . . ? Au1 P1 C111 C116 -55.6(7) . . . . ? C12 P1 C111 C112 1.5(8) . . . . ? C11 P1 C111 C112 -110.6(7) . . . . ? Au1 P1 C111 C112 124.8(6) . . . . ? C116 C111 C112 C113 -0.4(13) . . . . ? P1 C111 C112 C113 179.2(7) . . . . ? C111 C112 C113 C114 0.5(14) . . . . ? C112 C113 C114 C115 -0.3(14) . . . . ? C113 C114 C115 C116 0.1(15) . . . . ? C112 C111 C116 C115 0.2(13) . . . . ? P1 C111 C116 C115 -179.5(7) . . . . ? C114 C115 C116 C111 0.0(15) . . . . ? C22 P2 C211 C216 36.2(7) . . . . ? C21 P2 C211 C216 146.3(6) . . . . ? Au2 P2 C211 C216 -88.7(6) . . . . ? C22 P2 C211 C212 -145.1(6) . . . . ? C21 P2 C211 C212 -35.1(7) . . . . ? Au2 P2 C211 C212 89.9(6) . . . . ? C216 C211 C212 C213 -0.3(12) . . . . ? P2 C211 C212 C213 -179.0(6) . . . . ? C211 C212 C213 C214 0.9(12) . . . . ? C212 C213 C214 C215 -0.6(13) . . . . ? C213 C214 C215 C216 -0.2(13) . . . . ? C212 C211 C216 C215 -0.5(12) . . . . ? P2 C211 C216 C215 178.2(6) . . . . ? C214 C215 C216 C211 0.7(13) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.29 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 3.499 _refine_diff_density_min -3.515 _refine_diff_density_rms 0.219 #===END data_[(i-Pr)3PAuI1.5I2] _database_code_depnum_ccdc_archive 'CCDC 232530' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(i-Pr)3PAuI1.5I2]' _chemical_formula_sum 'C9 H21 Au I4 P' _chemical_formula_weight 864.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M C222(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.8516(1) _cell_length_b 12.4681(2) _cell_length_c 30.3821(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3731.86(9) _cell_formula_units_Z 8 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 51743 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 1.50 _exptl_crystal_size_mid 1.50 _exptl_crystal_size_min 1.00 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.078 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3048 _exptl_absorpt_coefficient_mu 14.566 _exptl_absorpt_correction_type DELABS _exptl_absorpt_correction_T_min 0.553 _exptl_absorpt_correction_T_max 0.863 _exptl_absorpt_process_details ? _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 HU' _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 51743 _diffrn_reflns_av_R_equivalents 0.062 _diffrn_reflns_av_sigmaI/netI 0.065 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 25.70 _reflns_number_total 3386 _reflns_number_gt 3379 _reflns_threshold_expression >2sigma(I) _computing_data_collection XPRESS _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _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^)+(0.0000P)^2^+2.7986P] 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 0.051(3) _refine_ls_number_reflns 3386 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0157 _refine_ls_R_factor_gt 0.0156 _refine_ls_wR_factor_ref 0.0446 _refine_ls_wR_factor_gt 0.0446 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au -0.213281(16) -0.893361(14) -0.132510(6) 0.01998(6) Uani 1 1 d . . . P1 P -0.42970(11) -0.90905(9) -0.10763(4) 0.0176(2) Uani 1 1 d . . . I2 I 0.03609(3) -0.88708(3) -0.158056(11) 0.02880(8) Uani 1 1 d . . . I3 I 0.00168(3) -0.96792(3) -0.043249(11) 0.03020(9) Uani 1 1 d . . . I4 I -0.21820(5) -1.04806(3) -0.228785(13) 0.04267(10) Uani 1 1 d . . . I5 I -0.32484(4) -1.19917(3) -0.282658(12) 0.03546(9) Uani 1 1 d . . . C111 C -0.4457(5) -0.8677(4) -0.04933(17) 0.0221(10) Uani 1 1 d . . . H11A H -0.4206 -0.9320 -0.0314 0.027 Uiso 1 1 calc R . . C112 C -0.3449(5) -0.7807(4) -0.03693(17) 0.0252(10) Uani 1 1 d . . . H11B H -0.3579 -0.7608 -0.0060 0.038 Uiso 1 1 calc R . . H11C H -0.3595 -0.7177 -0.0556 0.038 Uiso 1 1 calc R . . H11D H -0.2523 -0.8075 -0.0412 0.038 Uiso 1 1 calc R . . C113 C -0.5897(5) -0.8369(5) -0.0351(2) 0.0342(12) Uani 1 1 d . . . H11E H -0.5888 -0.8146 -0.0041 0.051 Uiso 1 1 calc R . . H11F H -0.6500 -0.8989 -0.0386 0.051 Uiso 1 1 calc R . . H11G H -0.6225 -0.7777 -0.0534 0.051 Uiso 1 1 calc R . . C121 C -0.4803(5) -1.0511(4) -0.11078(16) 0.0239(10) Uani 1 1 d . . . H12A H -0.4726 -1.0718 -0.1425 0.029 Uiso 1 1 calc R . . C122 C -0.6263(5) -1.0745(4) -0.0975(2) 0.0337(12) Uani 1 1 d . . . H12B H -0.6440 -1.1515 -0.1002 0.051 Uiso 1 1 calc R . . H12C H -0.6883 -1.0348 -0.1167 0.051 Uiso 1 1 calc R . . H12D H -0.6406 -1.0522 -0.0669 0.051 Uiso 1 1 calc R . . C123 C -0.3776(6) -1.1210(4) -0.0859(2) 0.0362(13) Uani 1 1 d . . . H12E H -0.4057 -1.1963 -0.0875 0.054 Uiso 1 1 calc R . . H12F H -0.3739 -1.0984 -0.0550 0.054 Uiso 1 1 calc R . . H12G H -0.2877 -1.1129 -0.0993 0.054 Uiso 1 1 calc R . . C131 C -0.5533(5) -0.8311(4) -0.13945(16) 0.0242(10) Uani 1 1 d . . . H13A H -0.6450 -0.8415 -0.1260 0.029 Uiso 1 1 calc R . . C132 C -0.5179(6) -0.7105(4) -0.13746(18) 0.0307(11) Uani 1 1 d . . . H13B H -0.5838 -0.6697 -0.1549 0.046 Uiso 1 1 calc R . . H13C H -0.4266 -0.6991 -0.1494 0.046 Uiso 1 1 calc R . . H13D H -0.5207 -0.6860 -0.1068 0.046 Uiso 1 1 calc R . . C133 C -0.5588(6) -0.8692(4) -0.18715(19) 0.0331(12) Uani 1 1 d . . . H13E H -0.6250 -0.8260 -0.2035 0.050 Uiso 1 1 calc R . . H13F H -0.5860 -0.9447 -0.1880 0.050 Uiso 1 1 calc R . . H13G H -0.4690 -0.8612 -0.2006 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01740(9) 0.02179(9) 0.02075(11) -0.00115(7) 0.00203(6) -0.00091(7) P1 0.0167(5) 0.0181(5) 0.0181(6) -0.0010(4) 0.0016(4) -0.0003(4) I2 0.01809(15) 0.03475(17) 0.03356(19) -0.00041(14) 0.00365(12) -0.00092(13) I3 0.03365(17) 0.02518(17) 0.0318(2) -0.00567(12) -0.00362(13) 0.00267(14) I4 0.0621(2) 0.03225(19) 0.0337(2) 0.00155(14) -0.01691(19) 0.00280(18) I5 0.0437(2) 0.03413(18) 0.0285(2) -0.00270(13) -0.00318(14) 0.00575(15) C111 0.025(2) 0.022(2) 0.020(3) -0.0003(16) 0.0024(18) 0.0024(18) C112 0.024(2) 0.025(2) 0.027(3) -0.0044(19) -0.0015(19) 0.000(2) C113 0.031(3) 0.040(3) 0.031(3) -0.010(2) 0.012(2) 0.001(2) C121 0.027(2) 0.026(2) 0.020(3) -0.0004(18) -0.0027(18) -0.002(2) C122 0.028(3) 0.033(3) 0.040(3) 0.002(2) 0.008(2) -0.009(2) C123 0.042(3) 0.023(3) 0.043(4) 0.000(2) -0.004(3) 0.001(2) C131 0.022(2) 0.025(2) 0.025(3) 0.005(2) 0.0004(19) -0.0003(18) C132 0.038(3) 0.028(3) 0.027(3) 0.000(2) -0.004(2) 0.009(2) C133 0.033(3) 0.039(3) 0.027(3) -0.002(2) -0.012(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.2706(11) . ? Au1 I2 2.5776(3) . ? P1 C131 1.834(5) . ? P1 C121 1.842(5) . ? P1 C111 1.851(5) . ? I3 I3 2.7470(7) 4_535 ? I4 I5 2.7078(5) . ? C111 C112 1.518(7) . ? C111 C113 1.533(7) . ? C111 H11A 1.0000 . ? C112 H11B 0.9800 . ? C112 H11C 0.9800 . ? C112 H11D 0.9800 . ? C113 H11E 0.9800 . ? C113 H11F 0.9800 . ? C113 H11G 0.9800 . ? C121 C122 1.522(7) . ? C121 C123 1.535(7) . ? C121 H12A 1.0000 . ? C122 H12B 0.9800 . ? C122 H12C 0.9800 . ? C122 H12D 0.9800 . ? C123 H12E 0.9800 . ? C123 H12F 0.9800 . ? C123 H12G 0.9800 . ? C131 C133 1.526(8) . ? C131 C132 1.545(7) . ? C131 H13A 1.0000 . ? C132 H13B 0.9800 . ? C132 H13C 0.9800 . ? C132 H13D 0.9800 . ? C133 H13E 0.9800 . ? C133 H13F 0.9800 . ? C133 H13G 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 I2 176.23(3) . . ? C131 P1 C121 107.6(2) . . ? C131 P1 C111 107.5(2) . . ? C121 P1 C111 107.1(2) . . ? C131 P1 Au1 113.73(16) . . ? C121 P1 Au1 108.64(16) . . ? C111 P1 Au1 111.98(15) . . ? C112 C111 C113 110.9(4) . . ? C112 C111 P1 112.4(3) . . ? C113 C111 P1 114.8(4) . . ? C112 C111 H11A 106.0 . . ? C113 C111 H11A 106.0 . . ? P1 C111 H11A 106.0 . . ? C111 C112 H11B 109.5 . . ? C111 C112 H11C 109.5 . . ? H11B C112 H11C 109.5 . . ? C111 C112 H11D 109.5 . . ? H11B C112 H11D 109.5 . . ? H11C C112 H11D 109.5 . . ? C111 C113 H11E 109.5 . . ? C111 C113 H11F 109.5 . . ? H11E C113 H11F 109.5 . . ? C111 C113 H11G 109.5 . . ? H11E C113 H11G 109.5 . . ? H11F C113 H11G 109.5 . . ? C122 C121 C123 112.5(4) . . ? C122 C121 P1 115.2(4) . . ? C123 C121 P1 110.0(3) . . ? C122 C121 H12A 106.1 . . ? C123 C121 H12A 106.1 . . ? P1 C121 H12A 106.1 . . ? C121 C122 H12B 109.5 . . ? C121 C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C121 C122 H12D 109.5 . . ? H12B C122 H12D 109.5 . . ? H12C C122 H12D 109.5 . . ? C121 C123 H12E 109.5 . . ? C121 C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C121 C123 H12G 109.5 . . ? H12E C123 H12G 109.5 . . ? H12F C123 H12G 109.5 . . ? C133 C131 C132 110.4(4) . . ? C133 C131 P1 111.1(4) . . ? C132 C131 P1 110.2(3) . . ? C133 C131 H13A 108.4 . . ? C132 C131 H13A 108.4 . . ? P1 C131 H13A 108.4 . . ? C131 C132 H13B 109.5 . . ? C131 C132 H13C 109.5 . . ? H13B C132 H13C 109.5 . . ? C131 C132 H13D 109.5 . . ? H13B C132 H13D 109.5 . . ? H13C C132 H13D 109.5 . . ? C131 C133 H13E 109.5 . . ? C131 C133 H13F 109.5 . . ? H13E C133 H13F 109.5 . . ? C131 C133 H13G 109.5 . . ? H13E C133 H13G 109.5 . . ? H13F C133 H13G 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 I2 Au1 P1 C131 -160.1(5) . . . . ? I2 Au1 P1 C121 -40.3(5) . . . . ? I2 Au1 P1 C111 77.8(5) . . . . ? C131 P1 C111 C112 -94.7(4) . . . . ? C121 P1 C111 C112 149.9(3) . . . . ? Au1 P1 C111 C112 30.9(4) . . . . ? C131 P1 C111 C113 33.2(4) . . . . ? C121 P1 C111 C113 -82.2(4) . . . . ? Au1 P1 C111 C113 158.8(3) . . . . ? C131 P1 C121 C122 -53.4(4) . . . . ? C111 P1 C121 C122 61.9(4) . . . . ? Au1 P1 C121 C122 -176.9(3) . . . . ? C131 P1 C121 C123 178.2(4) . . . . ? C111 P1 C121 C123 -66.5(4) . . . . ? Au1 P1 C121 C123 54.7(4) . . . . ? C121 P1 C131 C133 -58.3(4) . . . . ? C111 P1 C131 C133 -173.4(3) . . . . ? Au1 P1 C131 C133 62.0(4) . . . . ? C121 P1 C131 C132 179.0(3) . . . . ? C111 P1 C131 C132 64.0(4) . . . . ? Au1 P1 C131 C132 -60.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.70 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.539 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.110 #===END data_[(Ph3P)AuII2] _database_code_depnum_ccdc_archive 'CCDC 232531' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(Ph3P)AuII2]' _chemical_formula_sum 'C18 H15 Au I3 P' _chemical_formula_weight 839.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.2140(1) _cell_length_b 12.5045(1) _cell_length_c 16.7349(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.354(1) _cell_angle_gamma 90.00 _cell_volume 2061.11(4) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 53934 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.707 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 11.706 _exptl_absorpt_correction_type DELABS _exptl_absorpt_correction_T_min 0.465 _exptl_absorpt_correction_T_max 0.826 _exptl_absorpt_process_details ? _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 HU' _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 53934 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.046 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 27.19 _reflns_number_total 4557 _reflns_number_gt 4519 _reflns_threshold_expression >2sigma(I) _computing_data_collection XPRESS _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _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^)+(0.0198P)^2^+5.4440P] 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 4557 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0261 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0664 _refine_ls_wR_factor_gt 0.0663 _refine_ls_goodness_of_fit_ref 1.262 _refine_ls_restrained_S_all 1.262 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 1.403484(16) 0.361133(14) 0.718483(10) 0.02594(6) Uani 1 1 d . . . I1 I 1.61257(3) 0.43228(3) 0.676053(18) 0.03116(8) Uani 1 1 d . . . P1 P 1.22604(11) 0.30430(9) 0.76397(7) 0.0233(2) Uani 1 1 d . . . I2 I 1.26423(3) 0.19368(3) 0.35969(2) 0.03237(8) Uani 1 1 d . . . I3 I 1.39740(4) 0.29494(3) 0.50289(2) 0.04066(9) Uani 1 1 d . . . C111 C 1.1016(4) 0.2217(4) 0.6925(3) 0.0250(8) Uani 1 1 d . . . C112 C 0.9625(5) 0.2325(4) 0.6845(3) 0.0325(10) Uani 1 1 d . . . H11A H 0.9300 0.2875 0.7134 0.039 Uiso 1 1 calc R . . C113 C 0.8724(5) 0.1620(5) 0.6341(3) 0.0394(12) Uani 1 1 d . . . H11B H 0.7776 0.1703 0.6272 0.047 Uiso 1 1 calc R . . C114 C 0.9190(6) 0.0796(4) 0.5936(3) 0.0399(12) Uani 1 1 d . . . H11C H 0.8566 0.0308 0.5602 0.048 Uiso 1 1 calc R . . C115 C 1.0560(6) 0.0688(4) 0.6020(3) 0.0393(12) Uani 1 1 d . . . H11D H 1.0880 0.0119 0.5746 0.047 Uiso 1 1 calc R . . C116 C 1.1486(6) 0.1406(4) 0.6504(3) 0.0339(11) Uani 1 1 d . . . H11E H 1.2428 0.1341 0.6544 0.041 Uiso 1 1 calc R . . C121 C 1.2777(5) 0.2248(4) 0.8579(3) 0.0256(8) Uani 1 1 d . . . C122 C 1.4087(5) 0.2358(4) 0.9095(3) 0.0303(9) Uani 1 1 d . . . H12A H 1.4696 0.2859 0.8962 0.036 Uiso 1 1 calc R . . C123 C 1.4502(5) 0.1731(5) 0.9806(3) 0.0390(11) Uani 1 1 d . . . H12B H 1.5399 0.1794 1.0155 0.047 Uiso 1 1 calc R . . C124 C 1.3597(6) 0.1017(5) 1.0001(3) 0.0398(12) Uani 1 1 d . . . H12C H 1.3878 0.0588 1.0485 0.048 Uiso 1 1 calc R . . C125 C 1.2294(6) 0.0921(4) 0.9501(3) 0.0370(11) Uani 1 1 d . . . H12D H 1.1676 0.0438 0.9646 0.044 Uiso 1 1 calc R . . C126 C 1.1883(5) 0.1531(4) 0.8787(3) 0.0309(10) Uani 1 1 d . . . H12E H 1.0988 0.1458 0.8438 0.037 Uiso 1 1 calc R . . C131 C 1.1297(4) 0.4159(4) 0.7871(3) 0.0254(8) Uani 1 1 d . . . C132 C 1.0724(5) 0.4869(4) 0.7225(3) 0.0311(9) Uani 1 1 d . . . H13A H 1.0887 0.4774 0.6697 0.037 Uiso 1 1 calc R . . C133 C 0.9920(5) 0.5710(4) 0.7353(4) 0.0377(11) Uani 1 1 d . . . H13B H 0.9494 0.6167 0.6907 0.045 Uiso 1 1 calc R . . C134 C 0.9740(5) 0.5881(4) 0.8133(4) 0.0410(13) Uani 1 1 d . . . H13C H 0.9207 0.6468 0.8224 0.049 Uiso 1 1 calc R . . C135 C 1.0333(6) 0.5202(4) 0.8785(4) 0.0427(13) Uani 1 1 d . . . H13D H 1.0215 0.5331 0.9321 0.051 Uiso 1 1 calc R . . C136 C 1.1099(5) 0.4335(4) 0.8654(3) 0.0313(10) Uani 1 1 d . . . H13E H 1.1487 0.3861 0.9097 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.02453(10) 0.02699(11) 0.02815(10) 0.00145(6) 0.01021(7) -0.00093(6) I1 0.02618(15) 0.03764(18) 0.03120(15) 0.00453(12) 0.01033(11) -0.00298(11) P1 0.0235(5) 0.0235(5) 0.0238(5) -0.0010(4) 0.0080(4) -0.0005(4) I2 0.02904(15) 0.03184(17) 0.03674(16) 0.00216(12) 0.00962(12) 0.00453(11) I3 0.0507(2) 0.03203(18) 0.03657(17) 0.00223(13) 0.00677(14) 0.00048(14) C111 0.029(2) 0.026(2) 0.0206(18) 0.0006(16) 0.0075(16) 0.0006(16) C112 0.030(2) 0.037(3) 0.035(2) -0.008(2) 0.0150(19) -0.0078(19) C113 0.029(2) 0.053(3) 0.039(3) -0.009(2) 0.014(2) -0.011(2) C114 0.054(3) 0.036(3) 0.028(2) -0.0010(19) 0.007(2) -0.018(2) C115 0.051(3) 0.029(3) 0.032(2) -0.0064(19) 0.000(2) 0.007(2) C116 0.040(3) 0.029(3) 0.030(2) -0.0032(18) 0.003(2) 0.0080(19) C121 0.030(2) 0.023(2) 0.024(2) -0.0003(16) 0.0079(17) 0.0038(16) C122 0.024(2) 0.034(3) 0.032(2) -0.0035(19) 0.0060(17) -0.0036(17) C123 0.031(2) 0.051(3) 0.030(2) -0.002(2) -0.0005(19) 0.003(2) C124 0.049(3) 0.038(3) 0.029(2) 0.004(2) 0.005(2) 0.009(2) C125 0.046(3) 0.033(3) 0.031(2) 0.007(2) 0.008(2) -0.004(2) C126 0.031(2) 0.031(2) 0.030(2) 0.0040(18) 0.0057(18) -0.0032(18) C131 0.0230(19) 0.024(2) 0.031(2) -0.0042(16) 0.0088(16) -0.0029(16) C132 0.030(2) 0.029(2) 0.033(2) 0.0010(18) 0.0062(18) -0.0007(18) C133 0.027(2) 0.029(3) 0.055(3) 0.002(2) 0.009(2) 0.0022(18) C134 0.035(3) 0.024(2) 0.074(4) -0.008(2) 0.033(3) -0.0020(19) C135 0.060(3) 0.027(3) 0.056(3) -0.008(2) 0.040(3) -0.009(2) C136 0.039(3) 0.026(2) 0.034(2) -0.0028(18) 0.019(2) -0.0061(18) _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 2.2583(11) . ? Au1 I1 2.5806(3) . ? P1 C131 1.807(5) . ? P1 C121 1.816(4) . ? P1 C111 1.819(5) . ? I2 I3 2.7331(5) . ? C111 C116 1.391(6) . ? C111 C112 1.398(6) . ? C112 C113 1.387(7) . ? C112 H11A 0.9500 . ? C113 C114 1.385(8) . ? C113 H11B 0.9500 . ? C114 C115 1.376(8) . ? C114 H11C 0.9500 . ? C115 C116 1.396(7) . ? C115 H11D 0.9500 . ? C116 H11E 0.9500 . ? C121 C126 1.389(7) . ? C121 C122 1.394(6) . ? C122 C123 1.394(7) . ? C122 H12A 0.9500 . ? C123 C124 1.386(8) . ? C123 H12B 0.9500 . ? C124 C125 1.377(8) . ? C124 H12C 0.9500 . ? C125 C126 1.385(7) . ? C125 H12D 0.9500 . ? C126 H12E 0.9500 . ? C131 C136 1.395(6) . ? C131 C132 1.402(7) . ? C132 C133 1.384(7) . ? C132 H13A 0.9500 . ? C133 C134 1.383(8) . ? C133 H13B 0.9500 . ? C134 C135 1.389(9) . ? C134 H13C 0.9500 . ? C135 C136 1.388(7) . ? C135 H13D 0.9500 . ? C136 H13E 0.9500 . ? 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 I1 176.14(3) . . ? C131 P1 C121 106.7(2) . . ? C131 P1 C111 104.7(2) . . ? C121 P1 C111 104.5(2) . . ? C131 P1 Au1 111.12(15) . . ? C121 P1 Au1 112.86(15) . . ? C111 P1 Au1 116.12(14) . . ? C116 C111 C112 120.0(4) . . ? C116 C111 P1 118.2(4) . . ? C112 C111 P1 121.6(3) . . ? C113 C112 C111 119.4(5) . . ? C113 C112 H11A 120.3 . . ? C111 C112 H11A 120.3 . . ? C114 C113 C112 120.8(5) . . ? C114 C113 H11B 119.6 . . ? C112 C113 H11B 119.6 . . ? C115 C114 C113 119.7(5) . . ? C115 C114 H11C 120.2 . . ? C113 C114 H11C 120.2 . . ? C114 C115 C116 120.7(5) . . ? C114 C115 H11D 119.6 . . ? C116 C115 H11D 119.6 . . ? C111 C116 C115 119.4(5) . . ? C111 C116 H11E 120.3 . . ? C115 C116 H11E 120.3 . . ? C126 C121 C122 119.7(4) . . ? C126 C121 P1 120.7(3) . . ? C122 C121 P1 119.6(4) . . ? C121 C122 C123 119.9(5) . . ? C121 C122 H12A 120.0 . . ? C123 C122 H12A 120.0 . . ? C124 C123 C122 119.5(5) . . ? C124 C123 H12B 120.2 . . ? C122 C123 H12B 120.2 . . ? C125 C124 C123 120.7(5) . . ? C125 C124 H12C 119.7 . . ? C123 C124 H12C 119.7 . . ? C124 C125 C126 120.0(5) . . ? C124 C125 H12D 120.0 . . ? C126 C125 H12D 120.0 . . ? C125 C126 C121 120.2(5) . . ? C125 C126 H12E 119.9 . . ? C121 C126 H12E 119.9 . . ? C136 C131 C132 119.2(4) . . ? C136 C131 P1 123.1(4) . . ? C132 C131 P1 117.7(4) . . ? C133 C132 C131 120.4(5) . . ? C133 C132 H13A 119.8 . . ? C131 C132 H13A 119.8 . . ? C134 C133 C132 119.8(5) . . ? C134 C133 H13B 120.1 . . ? C132 C133 H13B 120.1 . . ? C133 C134 C135 120.5(5) . . ? C133 C134 H13C 119.8 . . ? C135 C134 H13C 119.8 . . ? C136 C135 C134 120.0(5) . . ? C136 C135 H13D 120.0 . . ? C134 C135 H13D 120.0 . . ? C135 C136 C131 120.0(5) . . ? C135 C136 H13E 120.0 . . ? C131 C136 H13E 120.0 . . ? 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 I1 Au1 P1 C131 61.9(5) . . . . ? I1 Au1 P1 C121 -57.8(5) . . . . ? I1 Au1 P1 C111 -179(20) . . . . ? C131 P1 C111 C116 167.4(4) . . . . ? C121 P1 C111 C116 -80.6(4) . . . . ? Au1 P1 C111 C116 44.5(4) . . . . ? C131 P1 C111 C112 -17.9(4) . . . . ? C121 P1 C111 C112 94.1(4) . . . . ? Au1 P1 C111 C112 -140.9(3) . . . . ? C116 C111 C112 C113 -0.3(7) . . . . ? P1 C111 C112 C113 -174.9(4) . . . . ? C111 C112 C113 C114 1.9(8) . . . . ? C112 C113 C114 C115 -1.4(8) . . . . ? C113 C114 C115 C116 -0.6(8) . . . . ? C112 C111 C116 C115 -1.6(7) . . . . ? P1 C111 C116 C115 173.2(4) . . . . ? C114 C115 C116 C111 2.1(8) . . . . ? C131 P1 C121 C126 80.7(4) . . . . ? C111 P1 C121 C126 -29.9(4) . . . . ? Au1 P1 C121 C126 -157.0(3) . . . . ? C131 P1 C121 C122 -99.5(4) . . . . ? C111 P1 C121 C122 149.9(4) . . . . ? Au1 P1 C121 C122 22.8(4) . . . . ? C126 C121 C122 C123 1.4(7) . . . . ? P1 C121 C122 C123 -178.4(4) . . . . ? C121 C122 C123 C124 -1.2(8) . . . . ? C122 C123 C124 C125 -0.1(9) . . . . ? C123 C124 C125 C126 1.1(9) . . . . ? C124 C125 C126 C121 -0.8(8) . . . . ? C122 C121 C126 C125 -0.4(7) . . . . ? P1 C121 C126 C125 179.4(4) . . . . ? C121 P1 C131 C136 2.7(4) . . . . ? C111 P1 C131 C136 113.1(4) . . . . ? Au1 P1 C131 C136 -120.7(4) . . . . ? C121 P1 C131 C132 -177.0(4) . . . . ? C111 P1 C131 C132 -66.5(4) . . . . ? Au1 P1 C131 C132 59.6(4) . . . . ? C136 C131 C132 C133 -2.8(7) . . . . ? P1 C131 C132 C133 176.9(4) . . . . ? C131 C132 C133 C134 3.4(7) . . . . ? C132 C133 C134 C135 -1.5(8) . . . . ? C133 C134 C135 C136 -0.9(8) . . . . ? C134 C135 C136 C131 1.4(8) . . . . ? C132 C131 C136 C135 0.4(7) . . . . ? P1 C131 C136 C135 -179.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.19 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.972 _refine_diff_density_min -0.822 _refine_diff_density_rms 0.152 #===END data_[(Ph3P)AuBr3] _database_code_depnum_ccdc_archive 'CCDC 232532' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(Ph3P)AuBr3]' _chemical_formula_sum 'C18 H15 Au Br3 P' _chemical_formula_weight 698.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.9533(1) _cell_length_b 14.0747(2) _cell_length_c 9.3338(1) _cell_angle_alpha 90.00 _cell_angle_beta 112.967(1) _cell_angle_gamma 90.00 _cell_volume 962.00(2) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 24415 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.70 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 13.956 _exptl_absorpt_correction_type DELABS _exptl_absorpt_correction_T_min 0.491 _exptl_absorpt_correction_T_max 0.837 _exptl_absorpt_process_details ? _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 HU' _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 23415 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_av_sigmaI/netI 0.063 _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 -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.15 _reflns_number_total 4196 _reflns_number_gt 4170 _reflns_threshold_expression >2sigma(I) _computing_data_collection XPRESS _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 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 0.022(5) _refine_ls_number_reflns 4196 _refine_ls_number_parameters 208 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0198 _refine_ls_R_factor_gt 0.0196 _refine_ls_wR_factor_ref 0.0512 _refine_ls_wR_factor_gt 0.0510 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 0.824275(16) 0.193658(13) 0.382808(14) 0.01923(5) Uani 1 1 d . . . Br1 Br 0.90276(6) 0.03487(3) 0.48591(6) 0.03056(10) Uani 1 1 d . . . Br2 Br 0.76092(5) 0.35047(3) 0.26626(5) 0.02988(10) Uani 1 1 d . . . Br3 Br 1.10579(6) 0.25511(4) 0.58521(6) 0.04236(12) Uani 1 1 d . . . P1 P 0.55210(12) 0.14213(7) 0.18944(11) 0.01781(18) Uani 1 1 d . . . C111 C 0.4578(5) 0.0336(3) 0.2307(4) 0.0215(7) Uani 1 1 d . . . C112 C 0.5154(6) -0.0540(3) 0.1942(6) 0.0302(9) Uani 1 1 d . . . H11A H 0.6014 -0.0558 0.1466 0.036 Uiso 1 1 calc R . . C113 C 0.4472(6) -0.1378(3) 0.2273(5) 0.0283(9) Uani 1 1 d . . . H11B H 0.4828 -0.1969 0.1986 0.034 Uiso 1 1 calc R . . C114 C 0.3264(6) -0.1359(3) 0.3026(5) 0.0287(8) Uani 1 1 d . . . H11C H 0.2824 -0.1936 0.3278 0.034 Uiso 1 1 calc R . . C115 C 0.2710(6) -0.0502(3) 0.3404(6) 0.0292(9) Uani 1 1 d . . . H11D H 0.1884 -0.0491 0.3914 0.035 Uiso 1 1 calc R . . C116 C 0.3355(5) 0.0352(3) 0.3043(5) 0.0257(8) Uani 1 1 d . . . H11E H 0.2959 0.0942 0.3300 0.031 Uiso 1 1 calc R . . C121 C 0.5903(5) 0.1215(3) 0.0136(5) 0.0219(7) Uani 1 1 d . . . C122 C 0.4495(6) 0.0827(3) -0.1148(5) 0.0274(8) Uani 1 1 d . . . H12A H 0.3369 0.0666 -0.1079 0.033 Uiso 1 1 calc R . . C123 C 0.4733(7) 0.0675(3) -0.2530(5) 0.0336(10) Uani 1 1 d . . . H12B H 0.3773 0.0411 -0.3406 0.040 Uiso 1 1 calc R . . C124 C 0.6370(7) 0.0912(3) -0.2617(6) 0.0353(10) Uani 1 1 d . . . H12C H 0.6534 0.0805 -0.3559 0.042 Uiso 1 1 calc R . . C125 C 0.7786(7) 0.1302(3) -0.1352(6) 0.0317(9) Uani 1 1 d . . . H12D H 0.8905 0.1466 -0.1431 0.038 Uiso 1 1 calc R . . C126 C 0.7555(6) 0.1453(3) 0.0038(5) 0.0264(8) Uani 1 1 d . . . H12E H 0.8518 0.1717 0.0912 0.032 Uiso 1 1 calc R . . C131 C 0.3790(5) 0.2326(3) 0.1571(5) 0.0211(7) Uani 1 1 d . . . C132 C 0.2733(5) 0.2638(3) 0.0079(5) 0.0283(8) Uani 1 1 d . . . H13A H 0.2891 0.2362 -0.0789 0.034 Uiso 1 1 calc R . . C133 C 0.1444(6) 0.3354(4) -0.0156(6) 0.0349(11) Uani 1 1 d . . . H13B H 0.0738 0.3574 -0.1178 0.042 Uiso 1 1 calc R . . C134 C 0.1199(7) 0.3741(3) 0.1102(7) 0.0393(11) Uani 1 1 d . . . H13C H 0.0301 0.4218 0.0947 0.047 Uiso 1 1 calc R . . C135 C 0.2248(7) 0.3439(3) 0.2582(6) 0.0355(11) Uani 1 1 d . . . H13D H 0.2088 0.3721 0.3446 0.043 Uiso 1 1 calc R . . C136 C 0.3543(6) 0.2725(3) 0.2832(5) 0.0271(8) Uani 1 1 d . . . H13E H 0.4251 0.2513 0.3858 0.033 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 0.01870(7) 0.01979(7) 0.01769(8) 0.00072(5) 0.00548(5) 0.00137(5) Br1 0.02645(19) 0.0280(2) 0.0390(3) 0.01402(17) 0.01467(17) 0.00838(16) Br2 0.02638(19) 0.01803(17) 0.0394(2) 0.00308(16) 0.00644(16) -0.00098(15) Br3 0.0345(2) 0.0472(3) 0.0282(3) 0.0001(2) -0.00643(18) -0.0080(2) P1 0.0176(4) 0.0181(5) 0.0180(5) -0.0013(4) 0.0073(3) -0.0005(3) C111 0.0187(16) 0.0225(17) 0.0218(19) 0.0028(14) 0.0061(13) 0.0032(14) C112 0.032(2) 0.0228(19) 0.041(3) -0.0049(17) 0.0205(19) -0.0006(16) C113 0.032(2) 0.0221(19) 0.029(2) -0.0008(17) 0.0102(17) -0.0004(16) C114 0.030(2) 0.025(2) 0.031(2) 0.0035(16) 0.0105(17) -0.0056(15) C115 0.030(2) 0.030(2) 0.033(2) -0.0038(18) 0.0182(19) -0.0063(17) C116 0.0243(19) 0.027(2) 0.029(2) -0.0005(16) 0.0141(16) 0.0024(16) C121 0.0244(18) 0.0166(16) 0.026(2) -0.0015(14) 0.0109(14) 0.0002(13) C122 0.029(2) 0.028(2) 0.027(2) -0.0065(16) 0.0132(16) -0.0073(16) C123 0.048(3) 0.033(2) 0.024(2) -0.0086(19) 0.0186(19) -0.013(2) C124 0.059(3) 0.023(2) 0.034(3) -0.0004(18) 0.029(2) 0.0040(19) C125 0.039(2) 0.026(2) 0.042(3) 0.0016(18) 0.0277(18) 0.0058(19) C126 0.0245(18) 0.027(2) 0.029(2) 0.0007(17) 0.0116(16) 0.0036(16) C131 0.0149(15) 0.0195(16) 0.031(2) 0.0001(15) 0.0112(14) 0.0000(13) C132 0.0197(18) 0.031(2) 0.030(2) 0.0012(17) 0.0051(15) 0.0008(15) C133 0.023(2) 0.040(3) 0.037(3) 0.007(2) 0.0064(18) 0.0047(18) C134 0.027(2) 0.033(2) 0.058(3) 0.004(2) 0.017(2) 0.0087(19) C135 0.037(2) 0.027(2) 0.052(3) -0.003(2) 0.027(2) 0.0042(19) C136 0.030(2) 0.021(2) 0.032(2) -0.0043(16) 0.0134(17) 0.0005(15) _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 2.3282(9) . ? Au1 Br1 2.4170(4) . ? Au1 Br2 2.4251(4) . ? Au1 Br3 2.4554(4) . ? P1 C121 1.806(4) . ? P1 C111 1.808(4) . ? P1 C131 1.813(4) . ? C111 C116 1.394(5) . ? C111 C112 1.404(5) . ? C112 C113 1.382(6) . ? C112 H11A 0.9500 . ? C113 C114 1.395(6) . ? C113 H11B 0.9500 . ? C114 C115 1.376(6) . ? C114 H11C 0.9500 . ? C115 C116 1.399(6) . ? C115 H11D 0.9500 . ? C116 H11E 0.9500 . ? C121 C126 1.393(5) . ? C121 C122 1.393(6) . ? C122 C123 1.392(6) . ? C122 H12A 0.9500 . ? C123 C124 1.377(7) . ? C123 H12B 0.9500 . ? C124 C125 1.388(8) . ? C124 H12C 0.9500 . ? C125 C126 1.396(6) . ? C125 H12D 0.9500 . ? C126 H12E 0.9500 . ? C131 C136 1.385(6) . ? C131 C132 1.387(6) . ? C132 C133 1.393(6) . ? C132 H13A 0.9500 . ? C133 C134 1.375(8) . ? C133 H13B 0.9500 . ? C134 C135 1.373(8) . ? C134 H13C 0.9500 . ? C135 C136 1.393(6) . ? C135 H13D 0.9500 . ? C136 H13E 0.9500 . ? 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 Br1 92.19(3) . . ? P1 Au1 Br2 88.18(3) . . ? Br1 Au1 Br2 175.107(15) . . ? P1 Au1 Br3 177.48(3) . . ? Br1 Au1 Br3 90.177(16) . . ? Br2 Au1 Br3 89.541(16) . . ? C121 P1 C111 106.77(17) . . ? C121 P1 C131 110.37(18) . . ? C111 P1 C131 106.14(17) . . ? C121 P1 Au1 108.63(13) . . ? C111 P1 Au1 115.83(13) . . ? C131 P1 Au1 109.04(13) . . ? C116 C111 C112 119.4(4) . . ? C116 C111 P1 121.3(3) . . ? C112 C111 P1 119.3(3) . . ? C113 C112 C111 120.2(4) . . ? C113 C112 H11A 119.9 . . ? C111 C112 H11A 119.9 . . ? C112 C113 C114 120.2(4) . . ? C112 C113 H11B 119.9 . . ? C114 C113 H11B 119.9 . . ? C115 C114 C113 119.9(4) . . ? C115 C114 H11C 120.0 . . ? C113 C114 H11C 120.0 . . ? C114 C115 C116 120.5(4) . . ? C114 C115 H11D 119.7 . . ? C116 C115 H11D 119.7 . . ? C111 C116 C115 119.8(4) . . ? C111 C116 H11E 120.1 . . ? C115 C116 H11E 120.1 . . ? C126 C121 C122 120.0(3) . . ? C126 C121 P1 121.2(3) . . ? C122 C121 P1 118.7(3) . . ? C123 C122 C121 120.2(4) . . ? C123 C122 H12A 119.9 . . ? C121 C122 H12A 119.9 . . ? C124 C123 C122 119.4(4) . . ? C124 C123 H12B 120.3 . . ? C122 C123 H12B 120.3 . . ? C123 C124 C125 121.2(4) . . ? C123 C124 H12C 119.4 . . ? C125 C124 H12C 119.4 . . ? C124 C125 C126 119.5(4) . . ? C124 C125 H12D 120.2 . . ? C126 C125 H12D 120.2 . . ? C121 C126 C125 119.6(4) . . ? C121 C126 H12E 120.2 . . ? C125 C126 H12E 120.2 . . ? C136 C131 C132 119.6(4) . . ? C136 C131 P1 119.6(3) . . ? C132 C131 P1 120.9(3) . . ? C131 C132 C133 120.5(4) . . ? C131 C132 H13A 119.8 . . ? C133 C132 H13A 119.8 . . ? C134 C133 C132 119.5(5) . . ? C134 C133 H13B 120.2 . . ? C132 C133 H13B 120.2 . . ? C135 C134 C133 120.3(4) . . ? C135 C134 H13C 119.8 . . ? C133 C134 H13C 119.8 . . ? C134 C135 C136 120.7(4) . . ? C134 C135 H13D 119.7 . . ? C136 C135 H13D 119.7 . . ? C131 C136 C135 119.4(4) . . ? C131 C136 H13E 120.3 . . ? C135 C136 H13E 120.3 . . ? 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 Br1 Au1 P1 C121 -95.57(13) . . . . ? Br2 Au1 P1 C121 79.54(13) . . . . ? Br3 Au1 P1 C121 104.7(6) . . . . ? Br1 Au1 P1 C111 24.51(14) . . . . ? Br2 Au1 P1 C111 -160.37(14) . . . . ? Br3 Au1 P1 C111 -135.2(6) . . . . ? Br1 Au1 P1 C131 144.10(14) . . . . ? Br2 Au1 P1 C131 -40.78(13) . . . . ? Br3 Au1 P1 C131 -15.6(7) . . . . ? C121 P1 C111 C116 -148.6(3) . . . . ? C131 P1 C111 C116 -30.9(4) . . . . ? Au1 P1 C111 C116 90.3(3) . . . . ? C121 P1 C111 C112 34.3(4) . . . . ? C131 P1 C111 C112 152.0(3) . . . . ? Au1 P1 C111 C112 -86.8(3) . . . . ? C116 C111 C112 C113 1.8(6) . . . . ? P1 C111 C112 C113 178.9(4) . . . . ? C111 C112 C113 C114 -2.5(7) . . . . ? C112 C113 C114 C115 1.8(7) . . . . ? C113 C114 C115 C116 -0.2(7) . . . . ? C112 C111 C116 C115 -0.3(6) . . . . ? P1 C111 C116 C115 -177.3(3) . . . . ? C114 C115 C116 C111 -0.5(7) . . . . ? C111 P1 C121 C126 -132.0(3) . . . . ? C131 P1 C121 C126 113.0(3) . . . . ? Au1 P1 C121 C126 -6.5(4) . . . . ? C111 P1 C121 C122 49.3(4) . . . . ? C131 P1 C121 C122 -65.7(4) . . . . ? Au1 P1 C121 C122 174.9(3) . . . . ? C126 C121 C122 C123 0.1(6) . . . . ? P1 C121 C122 C123 178.8(3) . . . . ? C121 C122 C123 C124 0.0(7) . . . . ? C122 C123 C124 C125 -0.3(7) . . . . ? C123 C124 C125 C126 0.5(7) . . . . ? C122 C121 C126 C125 0.1(6) . . . . ? P1 C121 C126 C125 -178.6(3) . . . . ? C124 C125 C126 C121 -0.4(6) . . . . ? C121 P1 C131 C136 -167.4(3) . . . . ? C111 P1 C131 C136 77.3(3) . . . . ? Au1 P1 C131 C136 -48.2(3) . . . . ? C121 P1 C131 C132 11.3(4) . . . . ? C111 P1 C131 C132 -104.0(3) . . . . ? Au1 P1 C131 C132 130.6(3) . . . . ? C136 C131 C132 C133 0.6(6) . . . . ? P1 C131 C132 C133 -178.1(3) . . . . ? C131 C132 C133 C134 -1.1(7) . . . . ? C132 C133 C134 C135 1.5(7) . . . . ? C133 C134 C135 C136 -1.4(7) . . . . ? C132 C131 C136 C135 -0.6(6) . . . . ? P1 C131 C136 C135 178.2(3) . . . . ? C134 C135 C136 C131 1.0(7) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.15 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.929 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.116 #===END data_[(BzMePhP)AuBr3] _database_code_depnum_ccdc_archive 'CCDC 232533' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(BzMePhP)AuBr3]' _chemical_formula_sum 'C14 H15 Au Br3 P' _chemical_formula_weight 650.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 9.573(1) _cell_length_b 14.264(1) _cell_length_c 12.973(1) _cell_angle_alpha 90.00 _cell_angle_beta 104.10(1) _cell_angle_gamma 90.00 _cell_volume 1718.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 199(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13 _cell_measurement_theta_max 16 _exptl_crystal_description 'transparent needles' _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 15.617 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.129 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 199(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 'Enraf Nonius CAD4' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number '2 -7 1 / 1 2 6 / 2 4 4' _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 1.3 _diffrn_reflns_number 3940 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 26.97 _reflns_number_total 3720 _reflns_number_gt 3111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Software (Enraf Nonius 1989)' _computing_cell_refinement 'CAD4 Software (Enraf Nonius 1989)' _computing_data_reduction 'SDP-Plus (Enraf Nonius 1988)' _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^)+(0.0831P)^2^+6.9454P] 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 3720 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1198 _refine_ls_wR_factor_gt 0.1133 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Au Au 0.97025(3) 0.491301(19) 0.15307(2) 0.02192(12) Uani 1 1 d . . . Br1 Br 0.91854(10) 0.63526(6) 0.05346(7) 0.0337(2) Uani 1 1 d . . . Br2 Br 1.02698(10) 0.34754(6) 0.25426(7) 0.0337(2) Uani 1 1 d . . . Br3 Br 0.71731(11) 0.44180(8) 0.08613(7) 0.0435(2) Uani 1 1 d . . . P P 1.2028(2) 0.53856(14) 0.23179(14) 0.0212(4) Uani 1 1 d . . . C11 C 1.3320(9) 0.4557(6) 0.2082(6) 0.0292(17) Uani 1 1 d . . . H111 H 1.4273 0.4771 0.2417 0.044 Uiso 1 1 d R . . H112 H 1.3156 0.3959 0.2371 0.044 Uiso 1 1 d R . . H113 H 1.3224 0.4498 0.1330 0.044 Uiso 1 1 d R . . C211 C 1.2127(9) 0.5486(5) 0.3722(6) 0.0241(15) Uani 1 1 d . . . C212 C 1.3061(10) 0.4949(6) 0.4466(7) 0.0294(17) Uani 1 1 d . . . H212 H 1.3661 0.4488 0.4247 0.044 Uiso 1 1 d R . . C213 C 1.3133(11) 0.5088(7) 0.5539(7) 0.036(2) Uani 1 1 d . . . H213 H 1.3779 0.4718 0.6065 0.054 Uiso 1 1 d R . . C214 C 1.2281(13) 0.5752(8) 0.5847(6) 0.046(3) Uani 1 1 d . . . H214 H 1.2344 0.5848 0.6590 0.070 Uiso 1 1 d R . . C215 C 1.1333(13) 0.6278(8) 0.5106(8) 0.050(3) Uani 1 1 d . . . H215 H 1.0728 0.6736 0.5325 0.074 Uiso 1 1 d R . . C216 C 1.1254(11) 0.6139(7) 0.4027(7) 0.037(2) Uani 1 1 d . . . H216 H 1.0601 0.6505 0.3501 0.056 Uiso 1 1 d R . . C31 C 1.2571(9) 0.6535(6) 0.1900(6) 0.0273(16) Uani 1 1 d . . . H31 H 1.1939 0.7011 0.2048 0.041 Uiso 1 1 d R . . H32 H 1.2487 0.6528 0.1148 0.041 Uiso 1 1 d R . . C311 C 1.4088(9) 0.6760(5) 0.2463(6) 0.0251(16) Uani 1 1 d . . . C312 C 1.5195(10) 0.6565(6) 0.1967(7) 0.0349(19) Uani 1 1 d . . . H312 H 1.4975 0.6294 0.1268 0.052 Uiso 1 1 d R . . C313 C 1.6633(10) 0.6752(6) 0.2493(7) 0.036(2) Uani 1 1 d . . . H313 H 1.7399 0.6607 0.2160 0.054 Uiso 1 1 d R . . C314 C 1.6935(10) 0.7158(6) 0.3491(8) 0.0362(19) Uani 1 1 d . . . H314 H 1.7914 0.7294 0.3854 0.054 Uiso 1 1 d R . . C315 C 1.5848(11) 0.7359(7) 0.3972(8) 0.040(2) Uani 1 1 d . . . H315 H 1.6068 0.7635 0.4667 0.061 Uiso 1 1 d R . . C316 C 1.4421(10) 0.7168(6) 0.3461(7) 0.0317(18) Uani 1 1 d . . . H316 H 1.3662 0.7322 0.3798 0.048 Uiso 1 1 d 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 Au 0.02199(18) 0.02257(17) 0.02139(17) -0.00162(10) 0.00563(12) -0.00156(11) Br1 0.0319(5) 0.0331(4) 0.0339(4) 0.0077(3) 0.0036(3) 0.0037(3) Br2 0.0378(5) 0.0241(4) 0.0417(4) 0.0044(3) 0.0144(4) -0.0012(3) Br3 0.0340(5) 0.0530(6) 0.0418(5) -0.0059(4) 0.0060(4) -0.0123(4) P 0.0205(10) 0.0209(9) 0.0216(8) -0.0008(7) 0.0038(7) 0.0008(7) C11 0.024(4) 0.029(4) 0.034(4) -0.006(3) 0.005(3) 0.000(3) C211 0.028(4) 0.023(3) 0.021(3) 0.004(3) 0.006(3) -0.004(3) C212 0.028(4) 0.029(4) 0.031(4) 0.001(3) 0.007(3) 0.000(3) C213 0.030(5) 0.047(5) 0.029(4) 0.006(4) 0.003(4) 0.002(4) C214 0.063(7) 0.056(6) 0.018(4) 0.001(4) 0.006(4) 0.001(5) C215 0.063(7) 0.051(6) 0.037(5) -0.006(4) 0.018(5) 0.014(5) C216 0.040(5) 0.045(5) 0.026(4) 0.005(4) 0.006(4) 0.015(4) C31 0.025(4) 0.027(4) 0.030(4) 0.004(3) 0.006(3) -0.001(3) C311 0.026(4) 0.020(3) 0.029(4) -0.003(3) 0.007(3) -0.004(3) C312 0.034(5) 0.038(4) 0.035(4) -0.007(4) 0.013(4) -0.008(4) C313 0.030(5) 0.036(5) 0.047(5) -0.003(4) 0.019(4) -0.010(4) C314 0.027(5) 0.030(4) 0.049(5) -0.003(4) 0.006(4) -0.011(4) C315 0.045(6) 0.038(5) 0.041(5) -0.011(4) 0.017(4) -0.015(4) C316 0.032(5) 0.027(4) 0.039(4) -0.008(3) 0.015(4) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au P 2.312(2) . ? Au Br1 2.4124(8) . ? Au Br2 2.4241(8) . ? Au Br3 2.4681(10) . ? P C11 1.790(8) . ? P C211 1.807(7) . ? P C31 1.841(8) . ? C11 H111 0.9600 . ? C11 H112 0.9600 . ? C11 H113 0.9600 . ? C211 C216 1.372(12) . ? C211 C212 1.377(11) . ? C212 C213 1.391(12) . ? C212 H212 0.9600 . ? C213 C214 1.372(14) . ? C213 H213 0.9600 . ? C214 C215 1.374(14) . ? C214 H214 0.9601 . ? C215 C216 1.397(12) . ? C215 H215 0.9600 . ? C216 H216 0.9600 . ? C31 C311 1.493(11) . ? C31 H31 0.9600 . ? C31 H32 0.9600 . ? C311 C316 1.383(11) . ? C311 C312 1.396(12) . ? C312 C313 1.405(13) . ? C312 H312 0.9600 . ? C313 C314 1.383(13) . ? C313 H313 0.9600 . ? C314 C315 1.368(14) . ? C314 H314 0.9600 . ? C315 C316 1.393(13) . ? C315 H315 0.9600 . ? C316 H316 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P Au Br1 92.19(5) . . ? P Au Br2 86.72(5) . . ? Br1 Au Br2 178.91(3) . . ? P Au Br3 174.49(5) . . ? Br1 Au Br3 89.96(3) . . ? Br2 Au Br3 91.13(3) . . ? C11 P C211 110.9(4) . . ? C11 P C31 106.3(4) . . ? C211 P C31 106.1(4) . . ? C11 P Au 111.3(3) . . ? C211 P Au 106.1(3) . . ? C31 P Au 116.1(3) . . ? P C11 H111 109.4 . . ? P C11 H112 109.5 . . ? H111 C11 H112 109.5 . . ? P C11 H113 109.5 . . ? H111 C11 H113 109.5 . . ? H112 C11 H113 109.5 . . ? C216 C211 C212 120.9(7) . . ? C216 C211 P 117.3(6) . . ? C212 C211 P 121.8(7) . . ? C211 C212 C213 119.1(8) . . ? C211 C212 H212 120.4 . . ? C213 C212 H212 120.4 . . ? C214 C213 C212 120.2(8) . . ? C214 C213 H213 119.9 . . ? C212 C213 H213 120.0 . . ? C213 C214 C215 120.7(8) . . ? C213 C214 H214 119.6 . . ? C215 C214 H214 119.6 . . ? C214 C215 C216 119.3(9) . . ? C214 C215 H215 120.5 . . ? C216 C215 H215 120.2 . . ? C211 C216 C215 119.8(8) . . ? C211 C216 H216 120.1 . . ? C215 C216 H216 120.1 . . ? C311 C31 P 111.0(5) . . ? C311 C31 H31 109.6 . . ? P C31 H31 109.5 . . ? C311 C31 H32 109.3 . . ? P C31 H32 109.3 . . ? H31 C31 H32 108.1 . . ? C316 C311 C312 119.2(8) . . ? C316 C311 C31 121.5(8) . . ? C312 C311 C31 119.3(7) . . ? C311 C312 C313 120.1(8) . . ? C311 C312 H312 119.9 . . ? C313 C312 H312 120.0 . . ? C314 C313 C312 119.4(8) . . ? C314 C313 H313 120.1 . . ? C312 C313 H313 120.4 . . ? C315 C314 C313 120.4(9) . . ? C315 C314 H314 119.6 . . ? C313 C314 H314 120.0 . . ? C314 C315 C316 120.6(8) . . ? C314 C315 H315 119.8 . . ? C316 C315 H315 119.5 . . ? C311 C316 C315 120.2(8) . . ? C311 C316 H316 119.7 . . ? C315 C316 H316 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br1 Au P C11 -123.7(3) . . . . ? Br2 Au P C11 56.2(3) . . . . ? Br3 Au P C11 123.4(6) . . . . ? Br1 Au P C211 115.6(3) . . . . ? Br2 Au P C211 -64.5(3) . . . . ? Br3 Au P C211 2.7(7) . . . . ? Br1 Au P C31 -1.9(3) . . . . ? Br2 Au P C31 178.0(3) . . . . ? Br3 Au P C31 -114.9(6) . . . . ? C11 P C211 C216 176.2(7) . . . . ? C31 P C211 C216 61.2(8) . . . . ? Au P C211 C216 -62.8(7) . . . . ? C11 P C211 C212 -2.3(8) . . . . ? C31 P C211 C212 -117.3(7) . . . . ? Au P C211 C212 118.7(7) . . . . ? C216 C211 C212 C213 -1.3(13) . . . . ? P C211 C212 C213 177.1(7) . . . . ? C211 C212 C213 C214 0.2(14) . . . . ? C212 C213 C214 C215 0.9(17) . . . . ? C213 C214 C215 C216 -0.7(18) . . . . ? C212 C211 C216 C215 1.5(15) . . . . ? P C211 C216 C215 -177.1(8) . . . . ? C214 C215 C216 C211 -0.4(17) . . . . ? C11 P C31 C311 -55.7(6) . . . . ? C211 P C31 C311 62.4(7) . . . . ? Au P C31 C311 179.9(5) . . . . ? P C31 C311 C316 -84.9(8) . . . . ? P C31 C311 C312 95.9(8) . . . . ? C316 C311 C312 C313 2.2(13) . . . . ? C31 C311 C312 C313 -178.6(8) . . . . ? C311 C312 C313 C314 -2.0(14) . . . . ? C312 C313 C314 C315 1.3(14) . . . . ? C313 C314 C315 C316 -0.7(15) . . . . ? C312 C311 C316 C315 -1.6(12) . . . . ? C31 C311 C316 C315 179.3(8) . . . . ? C314 C315 C316 C311 0.8(14) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.97 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.704 _refine_diff_density_min -1.727 _refine_diff_density_rms 0.271 #===END data_[(oTol3P)AuI] _database_code_depnum_ccdc_archive 'CCDC 232534' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(oTol3P)AuI]' _chemical_formula_sum 'C21 H21 Au I P' _chemical_formula_weight 628.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.0151(2) _cell_length_b 20.1112(2) _cell_length_c 28.2688(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7967.86(18) _cell_formula_units_Z 16 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 208102 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4704 _exptl_absorpt_coefficient_mu 9.015 _exptl_absorpt_correction_type DELABS _exptl_absorpt_correction_T_min 0.526 _exptl_absorpt_correction_T_max 0.852 _exptl_absorpt_process_details ? _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 HU' _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 208102 _diffrn_reflns_av_R_equivalents 0.062 _diffrn_reflns_av_sigmaI/netI 0.046 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.20 _reflns_number_total 8431 _reflns_number_gt 7618 _reflns_threshold_expression >2sigma(I) _computing_data_collection XPRESS _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _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^)+(0.0250P)^2^+45.1985P] 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 8431 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0719 _refine_ls_wR_factor_gt 0.0696 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 0.286139(14) 0.033115(11) 0.510952(7) 0.02840(6) Uani 1 1 d . . . I1 I 0.32607(3) 0.122114(19) 0.573013(13) 0.03312(9) Uani 1 1 d . . . P1 P 0.25999(9) -0.04430(7) 0.45392(5) 0.0256(3) Uani 1 1 d . . . Au2 Au 0.273730(15) 0.138784(10) 0.233282(7) 0.02868(6) Uani 1 1 d . . . I2 I 0.26603(4) 0.05412(2) 0.166027(15) 0.04960(12) Uani 1 1 d . . . P2 P 0.26787(9) 0.21629(7) 0.29128(5) 0.0241(3) Uani 1 1 d . . . C111 C 0.1350(4) -0.0564(3) 0.43798(18) 0.0285(11) Uani 1 1 d . . . C112 C 0.0719(4) -0.0025(3) 0.43340(19) 0.0307(11) Uani 1 1 d . . . C113 C -0.0208(4) -0.0158(3) 0.4183(2) 0.0413(14) Uani 1 1 d . . . H11A H -0.0643 0.0201 0.4150 0.050 Uiso 1 1 calc R . . C114 C -0.0513(4) -0.0794(4) 0.4079(2) 0.0441(15) Uani 1 1 d . . . H11B H -0.1147 -0.0867 0.3972 0.053 Uiso 1 1 calc R . . C115 C 0.0105(4) -0.1323(3) 0.4131(2) 0.0396(14) Uani 1 1 d . . . H11C H -0.0104 -0.1764 0.4067 0.048 Uiso 1 1 calc R . . C116 C 0.1032(4) -0.1206(3) 0.4275(2) 0.0344(12) Uani 1 1 d . . . H11D H 0.1462 -0.1569 0.4304 0.041 Uiso 1 1 calc R . . C117 C 0.0995(5) 0.0688(3) 0.4438(2) 0.0411(14) Uani 1 1 d . . . H11E H 0.1615 0.0785 0.4293 0.049 Uiso 1 1 calc R . . H11F H 0.1037 0.0753 0.4781 0.049 Uiso 1 1 calc R . . H11G H 0.0511 0.0988 0.4307 0.049 Uiso 1 1 calc R . . C121 C 0.3192(4) -0.0248(2) 0.39744(18) 0.0255(10) Uani 1 1 d . . . C122 C 0.4145(3) -0.0030(3) 0.39587(19) 0.0271(11) Uani 1 1 d . . . C123 C 0.4550(4) 0.0083(3) 0.3519(2) 0.0335(12) Uani 1 1 d . . . H12A H 0.5198 0.0219 0.3501 0.040 Uiso 1 1 calc R . . C124 C 0.4033(4) 0.0004(3) 0.31024(19) 0.0320(12) Uani 1 1 d . . . H12B H 0.4325 0.0093 0.2806 0.038 Uiso 1 1 calc R . . C125 C 0.3101(4) -0.0202(3) 0.31217(19) 0.0312(12) Uani 1 1 d . . . H12C H 0.2745 -0.0257 0.2838 0.037 Uiso 1 1 calc R . . C126 C 0.2677(4) -0.0332(3) 0.35571(18) 0.0285(11) Uani 1 1 d . . . H12D H 0.2034 -0.0480 0.3570 0.034 Uiso 1 1 calc R . . C127 C 0.4739(4) 0.0070(3) 0.4396(2) 0.0329(12) Uani 1 1 d . . . H12E H 0.4760 -0.0345 0.4578 0.039 Uiso 1 1 calc R . . H12F H 0.4455 0.0422 0.4591 0.039 Uiso 1 1 calc R . . H12G H 0.5388 0.0199 0.4306 0.039 Uiso 1 1 calc R . . C131 C 0.3041(4) -0.1263(3) 0.47097(19) 0.0283(11) Uani 1 1 d . . . C132 C 0.2696(4) -0.1588(3) 0.51205(19) 0.0342(12) Uani 1 1 d . . . C133 C 0.3079(4) -0.2204(3) 0.5240(2) 0.0387(13) Uani 1 1 d . . . H13A H 0.2859 -0.2424 0.5517 0.046 Uiso 1 1 calc R . . C134 C 0.3770(4) -0.2501(3) 0.4965(2) 0.0391(14) Uani 1 1 d . . . H13B H 0.4017 -0.2923 0.5054 0.047 Uiso 1 1 calc R . . C135 C 0.4106(4) -0.2192(3) 0.4564(2) 0.0357(13) Uani 1 1 d . . . H13C H 0.4582 -0.2399 0.4375 0.043 Uiso 1 1 calc R . . C136 C 0.3742(4) -0.1573(3) 0.44381(19) 0.0312(12) Uani 1 1 d . . . H13D H 0.3975 -0.1359 0.4162 0.037 Uiso 1 1 calc R . . C137 C 0.1910(5) -0.1297(4) 0.5419(2) 0.0513(17) Uani 1 1 d . . . H13E H 0.1860 -0.1547 0.5716 0.062 Uiso 1 1 calc R . . H13F H 0.1304 -0.1326 0.5247 0.062 Uiso 1 1 calc R . . H13G H 0.2053 -0.0831 0.5489 0.062 Uiso 1 1 calc R . . C211 C 0.3094(4) 0.2973(3) 0.27088(18) 0.0268(11) Uani 1 1 d . . . C212 C 0.2742(4) 0.3262(3) 0.22922(18) 0.0312(12) Uani 1 1 d . . . C213 C 0.3119(4) 0.3871(3) 0.2147(2) 0.0350(12) Uani 1 1 d . . . H21A H 0.2884 0.4073 0.1866 0.042 Uiso 1 1 calc R . . C214 C 0.3823(4) 0.4187(3) 0.2403(2) 0.0361(13) Uani 1 1 d . . . H21B H 0.4075 0.4598 0.2294 0.043 Uiso 1 1 calc R . . C215 C 0.4165(4) 0.3912(3) 0.2817(2) 0.0365(13) Uani 1 1 d . . . H21C H 0.4645 0.4133 0.2994 0.044 Uiso 1 1 calc R . . C216 C 0.3800(4) 0.3308(3) 0.29706(19) 0.0301(11) Uani 1 1 d . . . H21D H 0.4030 0.3118 0.3256 0.036 Uiso 1 1 calc R . . C217 C 0.1959(4) 0.2958(3) 0.1995(2) 0.0392(13) Uani 1 1 d . . . H21E H 0.1843 0.3238 0.1717 0.047 Uiso 1 1 calc R . . H21F H 0.1373 0.2925 0.2182 0.047 Uiso 1 1 calc R . . H21G H 0.2153 0.2512 0.1892 0.047 Uiso 1 1 calc R . . C221 C 0.1460(4) 0.2286(3) 0.31196(17) 0.0250(10) Uani 1 1 d . . . C222 C 0.0856(4) 0.1746(3) 0.32317(18) 0.0267(11) Uani 1 1 d . . . C223 C -0.0067(4) 0.1881(3) 0.33758(19) 0.0323(12) Uani 1 1 d . . . H22A H -0.0478 0.1521 0.3452 0.039 Uiso 1 1 calc R . . C224 C -0.0411(4) 0.2529(3) 0.34117(19) 0.0342(12) Uani 1 1 d . . . H22B H -0.1053 0.2607 0.3505 0.041 Uiso 1 1 calc R . . C225 C 0.0178(4) 0.3053(3) 0.3312(2) 0.0351(13) Uani 1 1 d . . . H22C H -0.0050 0.3496 0.3342 0.042 Uiso 1 1 calc R . . C226 C 0.1113(4) 0.2935(3) 0.31664(19) 0.0295(11) Uani 1 1 d . . . H22D H 0.1520 0.3300 0.3098 0.035 Uiso 1 1 calc R . . C227 C 0.1181(4) 0.1033(3) 0.3194(2) 0.0360(13) Uani 1 1 d . . . H22E H 0.1810 0.0986 0.3342 0.043 Uiso 1 1 calc R . . H22F H 0.1221 0.0905 0.2860 0.043 Uiso 1 1 calc R . . H22G H 0.0722 0.0744 0.3356 0.043 Uiso 1 1 calc R . . C231 C 0.3389(4) 0.1981(3) 0.34418(18) 0.0269(11) Uani 1 1 d . . . C232 C 0.4360(4) 0.1806(3) 0.3403(2) 0.0305(11) Uani 1 1 d . . . C233 C 0.4866(4) 0.1709(3) 0.3821(2) 0.0356(13) Uani 1 1 d . . . H23A H 0.5526 0.1604 0.3803 0.043 Uiso 1 1 calc R . . C234 C 0.4444(5) 0.1761(3) 0.4262(2) 0.0383(13) Uani 1 1 d . . . H23B H 0.4811 0.1690 0.4540 0.046 Uiso 1 1 calc R . . C235 C 0.3482(4) 0.1916(3) 0.4296(2) 0.0367(13) Uani 1 1 d . . . H23C H 0.3181 0.1940 0.4596 0.044 Uiso 1 1 calc R . . C236 C 0.2962(4) 0.2034(3) 0.38855(19) 0.0313(12) Uani 1 1 d . . . H23D H 0.2308 0.2154 0.3908 0.038 Uiso 1 1 calc R . . C237 C 0.4867(4) 0.1732(3) 0.2937(2) 0.0368(13) Uani 1 1 d . . . H23E H 0.4526 0.1409 0.2740 0.044 Uiso 1 1 calc R . . H23F H 0.5520 0.1575 0.2992 0.044 Uiso 1 1 calc R . . H23G H 0.4885 0.2162 0.2775 0.044 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 0.02767(11) 0.03037(12) 0.02717(10) -0.00595(8) -0.00285(8) 0.00238(8) I1 0.03265(19) 0.0353(2) 0.03141(18) -0.00854(14) -0.00261(14) 0.00003(14) P1 0.0241(6) 0.0265(7) 0.0262(6) -0.0039(5) -0.0019(5) 0.0027(5) Au2 0.03111(11) 0.02761(12) 0.02731(10) -0.00284(7) 0.00451(8) -0.00210(8) I2 0.0677(3) 0.0407(2) 0.0404(2) -0.01413(17) 0.0214(2) -0.0207(2) P2 0.0235(6) 0.0239(7) 0.0248(6) -0.0003(5) 0.0007(5) 0.0011(5) C111 0.026(3) 0.032(3) 0.028(3) -0.005(2) 0.003(2) -0.001(2) C112 0.024(3) 0.040(3) 0.028(3) -0.003(2) -0.002(2) 0.004(2) C113 0.032(3) 0.053(4) 0.038(3) -0.009(3) -0.001(2) 0.009(3) C114 0.021(3) 0.063(4) 0.048(4) -0.011(3) -0.001(2) -0.004(3) C115 0.032(3) 0.046(4) 0.041(3) -0.005(3) 0.004(2) -0.013(3) C116 0.031(3) 0.038(3) 0.034(3) -0.004(2) 0.000(2) 0.000(2) C117 0.043(3) 0.034(3) 0.046(3) -0.010(3) -0.008(3) 0.013(3) C121 0.024(2) 0.021(3) 0.032(3) -0.0002(19) 0.000(2) 0.0044(19) C122 0.020(2) 0.030(3) 0.032(3) -0.003(2) -0.004(2) 0.004(2) C123 0.029(3) 0.034(3) 0.037(3) 0.000(2) 0.002(2) -0.001(2) C124 0.035(3) 0.033(3) 0.028(3) 0.001(2) 0.003(2) 0.003(2) C125 0.033(3) 0.034(3) 0.026(3) -0.002(2) -0.006(2) 0.007(2) C126 0.028(3) 0.028(3) 0.030(3) -0.006(2) -0.002(2) 0.003(2) C127 0.023(3) 0.040(3) 0.035(3) 0.002(2) -0.007(2) 0.001(2) C131 0.028(3) 0.030(3) 0.027(3) -0.002(2) -0.002(2) -0.002(2) C132 0.038(3) 0.039(3) 0.026(3) 0.000(2) -0.002(2) -0.006(2) C133 0.048(4) 0.037(3) 0.031(3) 0.004(2) -0.008(3) -0.007(3) C134 0.046(4) 0.028(3) 0.044(3) 0.001(2) -0.012(3) 0.001(2) C135 0.038(3) 0.028(3) 0.041(3) -0.004(2) -0.004(2) 0.005(2) C136 0.034(3) 0.031(3) 0.029(3) -0.003(2) -0.002(2) 0.002(2) C137 0.059(4) 0.057(5) 0.038(4) 0.002(3) 0.014(3) 0.005(3) C211 0.023(2) 0.027(3) 0.029(3) 0.002(2) 0.005(2) 0.0027(19) C212 0.030(3) 0.038(3) 0.026(3) 0.000(2) 0.006(2) -0.001(2) C213 0.038(3) 0.033(3) 0.034(3) 0.005(2) 0.009(2) 0.005(2) C214 0.038(3) 0.026(3) 0.045(3) 0.005(2) 0.013(3) 0.000(2) C215 0.035(3) 0.032(3) 0.043(3) -0.006(2) 0.007(2) -0.006(2) C216 0.026(3) 0.032(3) 0.032(3) -0.002(2) 0.000(2) 0.000(2) C217 0.046(4) 0.039(4) 0.032(3) 0.006(2) -0.005(3) -0.001(3) C221 0.024(2) 0.026(3) 0.025(2) 0.0000(19) -0.0025(19) 0.0001(19) C222 0.024(3) 0.032(3) 0.024(2) -0.002(2) -0.0004(19) -0.002(2) C223 0.027(3) 0.043(3) 0.027(3) -0.004(2) 0.001(2) -0.005(2) C224 0.025(3) 0.046(4) 0.032(3) -0.002(2) -0.002(2) 0.007(2) C225 0.034(3) 0.039(3) 0.032(3) -0.001(2) -0.002(2) 0.012(2) C226 0.029(3) 0.028(3) 0.032(3) 0.000(2) 0.000(2) 0.004(2) C227 0.035(3) 0.032(3) 0.041(3) 0.003(2) 0.008(2) -0.006(2) C231 0.029(3) 0.024(3) 0.028(3) -0.0002(19) -0.002(2) 0.002(2) C232 0.029(3) 0.024(3) 0.039(3) 0.000(2) -0.001(2) 0.000(2) C233 0.033(3) 0.027(3) 0.047(3) 0.003(2) -0.009(2) 0.002(2) C234 0.046(4) 0.031(3) 0.038(3) 0.001(2) -0.015(3) -0.002(2) C235 0.047(3) 0.034(3) 0.029(3) 0.001(2) 0.000(2) 0.001(2) C236 0.036(3) 0.027(3) 0.031(3) 0.000(2) 0.001(2) -0.001(2) C237 0.027(3) 0.043(4) 0.040(3) 0.000(3) 0.002(2) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.2710(13) . ? Au1 I1 2.5680(4) . ? P1 C111 1.826(5) . ? P1 C131 1.827(6) . ? P1 C121 1.841(5) . ? Au2 P2 2.2636(13) . ? Au2 I2 2.5544(4) . ? P2 C221 1.823(5) . ? P2 C211 1.824(5) . ? P2 C231 1.833(5) . ? C111 C116 1.397(8) . ? C111 C112 1.404(8) . ? C112 C113 1.393(8) . ? C112 C117 1.516(8) . ? C113 C114 1.380(9) . ? C113 H11A 0.9500 . ? C114 C115 1.381(9) . ? C114 H11B 0.9500 . ? C115 C116 1.382(8) . ? C115 H11C 0.9500 . ? C116 H11D 0.9500 . ? C117 H11E 0.9800 . ? C117 H11F 0.9800 . ? C117 H11G 0.9800 . ? C121 C126 1.393(7) . ? C121 C122 1.408(7) . ? C122 C123 1.385(8) . ? C122 C127 1.504(7) . ? C123 C124 1.392(8) . ? C123 H12A 0.9500 . ? C124 C125 1.372(8) . ? C124 H12B 0.9500 . ? C125 C126 1.391(8) . ? C125 H12C 0.9500 . ? C126 H12D 0.9500 . ? C127 H12E 0.9800 . ? C127 H12F 0.9800 . ? C127 H12G 0.9800 . ? C131 C136 1.394(8) . ? C131 C132 1.418(8) . ? C132 C133 1.392(9) . ? C132 C137 1.507(9) . ? C133 C134 1.378(9) . ? C133 H13A 0.9500 . ? C134 C135 1.376(9) . ? C134 H13B 0.9500 . ? C135 C136 1.392(8) . ? C135 H13C 0.9500 . ? C136 H13D 0.9500 . ? C137 H13E 0.9800 . ? C137 H13F 0.9800 . ? C137 H13G 0.9800 . ? C211 C212 1.402(7) . ? C211 C216 1.407(7) . ? C212 C213 1.396(8) . ? C212 C217 1.513(8) . ? C213 C214 1.379(9) . ? C213 H21A 0.9500 . ? C214 C215 1.379(8) . ? C214 H21B 0.9500 . ? C215 C216 1.388(8) . ? C215 H21C 0.9500 . ? C216 H21D 0.9500 . ? C217 H21E 0.9800 . ? C217 H21F 0.9800 . ? C217 H21G 0.9800 . ? C221 C226 1.400(7) . ? C221 C222 1.412(7) . ? C222 C223 1.383(7) . ? C222 C227 1.509(8) . ? C223 C224 1.393(8) . ? C223 H22A 0.9500 . ? C224 C225 1.368(8) . ? C224 H22B 0.9500 . ? C225 C226 1.394(8) . ? C225 H22C 0.9500 . ? C226 H22D 0.9500 . ? C227 H22E 0.9800 . ? C227 H22F 0.9800 . ? C227 H22G 0.9800 . ? C231 C236 1.393(7) . ? C231 C232 1.411(7) . ? C232 C233 1.394(8) . ? C232 C237 1.504(8) . ? C233 C234 1.383(9) . ? C233 H23A 0.9500 . ? C234 C235 1.388(9) . ? C234 H23B 0.9500 . ? C235 C236 1.391(8) . ? C235 H23C 0.9500 . ? C236 H23D 0.9500 . ? C237 H23E 0.9800 . ? C237 H23F 0.9800 . ? C237 H23G 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 I1 176.35(4) . . ? C111 P1 C131 105.7(2) . . ? C111 P1 C121 104.3(2) . . ? C131 P1 C121 105.6(2) . . ? C111 P1 Au1 114.92(17) . . ? C131 P1 Au1 112.16(17) . . ? C121 P1 Au1 113.39(17) . . ? P2 Au2 I2 175.19(4) . . ? C221 P2 C211 106.2(2) . . ? C221 P2 C231 105.9(2) . . ? C211 P2 C231 105.2(2) . . ? C221 P2 Au2 111.07(17) . . ? C211 P2 Au2 112.01(17) . . ? C231 P2 Au2 115.72(17) . . ? C116 C111 C112 119.5(5) . . ? C116 C111 P1 118.8(4) . . ? C112 C111 P1 121.6(4) . . ? C113 C112 C111 117.9(5) . . ? C113 C112 C117 118.6(5) . . ? C111 C112 C117 123.5(5) . . ? C114 C113 C112 122.1(6) . . ? C114 C113 H11A 118.9 . . ? C112 C113 H11A 118.9 . . ? C113 C114 C115 119.8(5) . . ? C113 C114 H11B 120.1 . . ? C115 C114 H11B 120.1 . . ? C114 C115 C116 119.3(6) . . ? C114 C115 H11C 120.4 . . ? C116 C115 H11C 120.4 . . ? C115 C116 C111 121.3(6) . . ? C115 C116 H11D 119.3 . . ? C111 C116 H11D 119.3 . . ? C112 C117 H11E 109.5 . . ? C112 C117 H11F 109.5 . . ? H11E C117 H11F 109.5 . . ? C112 C117 H11G 109.5 . . ? H11E C117 H11G 109.5 . . ? H11F C117 H11G 109.5 . . ? C126 C121 C122 120.2(5) . . ? C126 C121 P1 118.4(4) . . ? C122 C121 P1 121.4(4) . . ? C123 C122 C121 117.9(5) . . ? C123 C122 C127 119.3(5) . . ? C121 C122 C127 122.7(5) . . ? C122 C123 C124 121.9(5) . . ? C122 C123 H12A 119.1 . . ? C124 C123 H12A 119.1 . . ? C125 C124 C123 119.8(5) . . ? C125 C124 H12B 120.1 . . ? C123 C124 H12B 120.1 . . ? C124 C125 C126 119.9(5) . . ? C124 C125 H12C 120.1 . . ? C126 C125 H12C 120.1 . . ? C125 C126 C121 120.4(5) . . ? C125 C126 H12D 119.8 . . ? C121 C126 H12D 119.8 . . ? C122 C127 H12E 109.5 . . ? C122 C127 H12F 109.5 . . ? H12E C127 H12F 109.5 . . ? C122 C127 H12G 109.5 . . ? H12E C127 H12G 109.5 . . ? H12F C127 H12G 109.5 . . ? C136 C131 C132 119.0(5) . . ? C136 C131 P1 119.8(4) . . ? C132 C131 P1 121.1(4) . . ? C133 C132 C131 118.6(5) . . ? C133 C132 C137 119.4(5) . . ? C131 C132 C137 122.0(6) . . ? C134 C133 C132 121.3(6) . . ? C134 C133 H13A 119.4 . . ? C132 C133 H13A 119.4 . . ? C135 C134 C133 120.7(6) . . ? C135 C134 H13B 119.7 . . ? C133 C134 H13B 119.7 . . ? C134 C135 C136 119.3(6) . . ? C134 C135 H13C 120.4 . . ? C136 C135 H13C 120.4 . . ? C135 C136 C131 121.2(5) . . ? C135 C136 H13D 119.4 . . ? C131 C136 H13D 119.4 . . ? C132 C137 H13E 109.5 . . ? C132 C137 H13F 109.5 . . ? H13E C137 H13F 109.5 . . ? C132 C137 H13G 109.5 . . ? H13E C137 H13G 109.5 . . ? H13F C137 H13G 109.5 . . ? C212 C211 C216 119.4(5) . . ? C212 C211 P2 121.5(4) . . ? C216 C211 P2 119.1(4) . . ? C213 C212 C211 118.5(5) . . ? C213 C212 C217 117.8(5) . . ? C211 C212 C217 123.7(5) . . ? C214 C213 C212 121.4(5) . . ? C214 C213 H21A 119.3 . . ? C212 C213 H21A 119.3 . . ? C215 C214 C213 120.6(5) . . ? C215 C214 H21B 119.7 . . ? C213 C214 H21B 119.7 . . ? C214 C215 C216 119.3(6) . . ? C214 C215 H21C 120.4 . . ? C216 C215 H21C 120.4 . . ? C215 C216 C211 120.9(5) . . ? C215 C216 H21D 119.6 . . ? C211 C216 H21D 119.6 . . ? C212 C217 H21E 109.5 . . ? C212 C217 H21F 109.5 . . ? H21E C217 H21F 109.5 . . ? C212 C217 H21G 109.5 . . ? H21E C217 H21G 109.5 . . ? H21F C217 H21G 109.5 . . ? C226 C221 C222 119.2(5) . . ? C226 C221 P2 118.8(4) . . ? C222 C221 P2 122.0(4) . . ? C223 C222 C221 118.4(5) . . ? C223 C222 C227 119.3(5) . . ? C221 C222 C227 122.3(5) . . ? C222 C223 C224 121.9(5) . . ? C222 C223 H22A 119.0 . . ? C224 C223 H22A 119.0 . . ? C225 C224 C223 119.8(5) . . ? C225 C224 H22B 120.1 . . ? C223 C224 H22B 120.1 . . ? C224 C225 C226 119.8(5) . . ? C224 C225 H22C 120.1 . . ? C226 C225 H22C 120.1 . . ? C225 C226 C221 120.8(5) . . ? C225 C226 H22D 119.6 . . ? C221 C226 H22D 119.6 . . ? C222 C227 H22E 109.5 . . ? C222 C227 H22F 109.5 . . ? H22E C227 H22F 109.5 . . ? C222 C227 H22G 109.5 . . ? H22E C227 H22G 109.5 . . ? H22F C227 H22G 109.5 . . ? C236 C231 C232 120.3(5) . . ? C236 C231 P2 119.1(4) . . ? C232 C231 P2 120.6(4) . . ? C233 C232 C231 117.3(5) . . ? C233 C232 C237 119.3(5) . . ? C231 C232 C237 123.3(5) . . ? C234 C233 C232 122.5(5) . . ? C234 C233 H23A 118.8 . . ? C232 C233 H23A 118.8 . . ? C233 C234 C235 119.6(5) . . ? C233 C234 H23B 120.2 . . ? C235 C234 H23B 120.2 . . ? C234 C235 C236 119.4(5) . . ? C234 C235 H23C 120.3 . . ? C236 C235 H23C 120.3 . . ? C235 C236 C231 120.8(5) . . ? C235 C236 H23D 119.6 . . ? C231 C236 H23D 119.6 . . ? C232 C237 H23E 109.5 . . ? C232 C237 H23F 109.5 . . ? H23E C237 H23F 109.5 . . ? C232 C237 H23G 109.5 . . ? H23E C237 H23G 109.5 . . ? H23F C237 H23G 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 I1 Au1 P1 C111 -150.3(6) . . . . ? I1 Au1 P1 C131 89.0(6) . . . . ? I1 Au1 P1 C121 -30.4(6) . . . . ? I2 Au2 P2 C221 28.3(5) . . . . ? I2 Au2 P2 C211 -90.3(5) . . . . ? I2 Au2 P2 C231 149.1(4) . . . . ? C131 P1 C111 C116 -18.5(5) . . . . ? C121 P1 C111 C116 92.5(5) . . . . ? Au1 P1 C111 C116 -142.7(4) . . . . ? C131 P1 C111 C112 165.2(4) . . . . ? C121 P1 C111 C112 -83.7(5) . . . . ? Au1 P1 C111 C112 41.0(5) . . . . ? C116 C111 C112 C113 -0.2(8) . . . . ? P1 C111 C112 C113 176.1(4) . . . . ? C116 C111 C112 C117 -179.9(5) . . . . ? P1 C111 C112 C117 -3.6(8) . . . . ? C111 C112 C113 C114 0.0(9) . . . . ? C117 C112 C113 C114 179.7(6) . . . . ? C112 C113 C114 C115 0.9(10) . . . . ? C113 C114 C115 C116 -1.6(9) . . . . ? C114 C115 C116 C111 1.4(9) . . . . ? C112 C111 C116 C115 -0.5(8) . . . . ? P1 C111 C116 C115 -176.9(5) . . . . ? C111 P1 C121 C126 -10.1(5) . . . . ? C131 P1 C121 C126 101.0(4) . . . . ? Au1 P1 C121 C126 -135.9(4) . . . . ? C111 P1 C121 C122 170.9(4) . . . . ? C131 P1 C121 C122 -78.0(5) . . . . ? Au1 P1 C121 C122 45.2(5) . . . . ? C126 C121 C122 C123 -1.2(8) . . . . ? P1 C121 C122 C123 177.7(4) . . . . ? C126 C121 C122 C127 -180.0(5) . . . . ? P1 C121 C122 C127 -1.0(7) . . . . ? C121 C122 C123 C124 1.8(8) . . . . ? C127 C122 C123 C124 -179.5(5) . . . . ? C122 C123 C124 C125 -1.1(9) . . . . ? C123 C124 C125 C126 -0.1(8) . . . . ? C124 C125 C126 C121 0.6(8) . . . . ? C122 C121 C126 C125 0.1(8) . . . . ? P1 C121 C126 C125 -178.9(4) . . . . ? C111 P1 C131 C136 114.5(4) . . . . ? C121 P1 C131 C136 4.4(5) . . . . ? Au1 P1 C131 C136 -119.6(4) . . . . ? C111 P1 C131 C132 -66.7(5) . . . . ? C121 P1 C131 C132 -176.8(4) . . . . ? Au1 P1 C131 C132 59.3(5) . . . . ? C136 C131 C132 C133 0.7(8) . . . . ? P1 C131 C132 C133 -178.2(4) . . . . ? C136 C131 C132 C137 -177.3(6) . . . . ? P1 C131 C132 C137 3.9(8) . . . . ? C131 C132 C133 C134 -0.8(9) . . . . ? C137 C132 C133 C134 177.2(6) . . . . ? C132 C133 C134 C135 0.4(9) . . . . ? C133 C134 C135 C136 0.1(9) . . . . ? C134 C135 C136 C131 -0.2(8) . . . . ? C132 C131 C136 C135 -0.2(8) . . . . ? P1 C131 C136 C135 178.7(4) . . . . ? C221 P2 C211 C212 -71.3(5) . . . . ? C231 P2 C211 C212 176.7(4) . . . . ? Au2 P2 C211 C212 50.1(5) . . . . ? C221 P2 C211 C216 110.2(4) . . . . ? C231 P2 C211 C216 -1.8(5) . . . . ? Au2 P2 C211 C216 -128.4(4) . . . . ? C216 C211 C212 C213 0.9(8) . . . . ? P2 C211 C212 C213 -177.6(4) . . . . ? C216 C211 C212 C217 -177.6(5) . . . . ? P2 C211 C212 C217 3.9(8) . . . . ? C211 C212 C213 C214 0.3(8) . . . . ? C217 C212 C213 C214 178.9(5) . . . . ? C212 C213 C214 C215 -1.1(9) . . . . ? C213 C214 C215 C216 0.7(9) . . . . ? C214 C215 C216 C211 0.5(8) . . . . ? C212 C211 C216 C215 -1.3(8) . . . . ? P2 C211 C216 C215 177.2(4) . . . . ? C211 P2 C221 C226 -10.3(5) . . . . ? C231 P2 C221 C226 101.3(4) . . . . ? Au2 P2 C221 C226 -132.3(4) . . . . ? C211 P2 C221 C222 169.5(4) . . . . ? C231 P2 C221 C222 -79.0(5) . . . . ? Au2 P2 C221 C222 47.4(4) . . . . ? C226 C221 C222 C223 1.2(7) . . . . ? P2 C221 C222 C223 -178.5(4) . . . . ? C226 C221 C222 C227 -179.4(5) . . . . ? P2 C221 C222 C227 0.8(7) . . . . ? C221 C222 C223 C224 0.1(8) . . . . ? C227 C222 C223 C224 -179.3(5) . . . . ? C222 C223 C224 C225 -1.3(8) . . . . ? C223 C224 C225 C226 1.2(8) . . . . ? C224 C225 C226 C221 0.2(8) . . . . ? C222 C221 C226 C225 -1.4(8) . . . . ? P2 C221 C226 C225 178.4(4) . . . . ? C221 P2 C231 C236 -6.8(5) . . . . ? C211 P2 C231 C236 105.5(5) . . . . ? Au2 P2 C231 C236 -130.3(4) . . . . ? C221 P2 C231 C232 174.8(4) . . . . ? C211 P2 C231 C232 -72.9(5) . . . . ? Au2 P2 C231 C232 51.3(5) . . . . ? C236 C231 C232 C233 -1.6(8) . . . . ? P2 C231 C232 C233 176.7(4) . . . . ? C236 C231 C232 C237 179.3(5) . . . . ? P2 C231 C232 C237 -2.3(8) . . . . ? C231 C232 C233 C234 1.8(8) . . . . ? C237 C232 C233 C234 -179.1(5) . . . . ? C232 C233 C234 C235 -0.1(9) . . . . ? C233 C234 C235 C236 -1.7(9) . . . . ? C234 C235 C236 C231 1.9(9) . . . . ? C232 C231 C236 C235 -0.2(8) . . . . ? P2 C231 C236 C235 -178.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 27.20 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 3.864 _refine_diff_density_min -3.306 _refine_diff_density_rms 0.129 #===END data_[(oTol3P)AuI0.5I2] _database_code_depnum_ccdc_archive 'CCDC 232535' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(oTol3P)AuI0.5I2]' _chemical_formula_sum 'C21 H21 Au I2 P' _chemical_formula_weight 755.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9024(1) _cell_length_b 11.6435(2) _cell_length_c 11.7222(2) _cell_angle_alpha 105.877(1) _cell_angle_beta 95.169(1) _cell_angle_gamma 103.724(1) _cell_volume 1119.62(3) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 29379 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _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 2.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 694 _exptl_absorpt_coefficient_mu 9.400 _exptl_absorpt_correction_type DELABS _exptl_absorpt_correction_T_min 0.386 _exptl_absorpt_correction_T_max 0.788 _exptl_absorpt_process_details ? _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 HU' _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 29379 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.039 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 27.24 _reflns_number_total 4650 _reflns_number_gt 4607 _reflns_threshold_expression >2sigma(I) _computing_data_collection XPRESS _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _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^)+(0.0319P)^2^+1.0491P] 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 4650 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0256 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0683 _refine_ls_wR_factor_gt 0.0681 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _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 0.288575(14) 0.242128(12) 0.183668(11) 0.02389(6) Uani 1 1 d . . . I1 I 0.43780(3) 0.32981(3) 0.03584(2) 0.03261(8) Uani 1 1 d . . . P1 P 0.16380(10) 0.15633(9) 0.31298(8) 0.02220(18) Uani 1 1 d . . . I2 I 0.12341(3) 0.45150(3) 0.01579(2) 0.03500(8) Uani 1 1 d . . . C111 C 0.2089(4) 0.0103(3) 0.3065(3) 0.0251(7) Uani 1 1 d . . . C112 C 0.1979(4) -0.0816(4) 0.1954(4) 0.0288(7) Uani 1 1 d . . . C113 C 0.2487(5) -0.1848(4) 0.1974(4) 0.0356(9) Uani 1 1 d . . . H11A H 0.2433 -0.2462 0.1234 0.043 Uiso 1 1 calc R . . C114 C 0.3073(5) -0.2017(4) 0.3036(5) 0.0443(11) Uani 1 1 d . . . H11B H 0.3418 -0.2733 0.3018 0.053 Uiso 1 1 calc R . . C115 C 0.3149(5) -0.1133(4) 0.4120(4) 0.0410(10) Uani 1 1 d . . . H11C H 0.3531 -0.1250 0.4852 0.049 Uiso 1 1 calc R . . C116 C 0.2671(4) -0.0077(4) 0.4145(4) 0.0312(8) Uani 1 1 d . . . H11D H 0.2736 0.0529 0.4893 0.037 Uiso 1 1 calc R . . C117 C 0.1328(5) -0.0724(4) 0.0757(4) 0.0365(9) Uani 1 1 d . . . H11E H 0.2056 -0.0057 0.0561 0.044 Uiso 1 1 calc R . . H11F H 0.0311 -0.0542 0.0801 0.044 Uiso 1 1 calc R . . H11G H 0.1194 -0.1513 0.0130 0.044 Uiso 1 1 calc R . . C121 C -0.0480(4) 0.1223(4) 0.2790(3) 0.0296(8) Uani 1 1 d . . . C122 C -0.1192(5) 0.2156(5) 0.2684(4) 0.0375(9) Uani 1 1 d . . . C123 C -0.2836(6) 0.1805(7) 0.2361(4) 0.0573(16) Uani 1 1 d . . . H12A H -0.3341 0.2415 0.2268 0.069 Uiso 1 1 calc R . . C124 C -0.3726(6) 0.0628(7) 0.2178(5) 0.067(2) Uani 1 1 d . . . H12B H -0.4830 0.0426 0.1942 0.080 Uiso 1 1 calc R . . C125 C -0.3044(5) -0.0265(6) 0.2331(5) 0.0595(17) Uani 1 1 d . . . H12C H -0.3670 -0.1079 0.2236 0.071 Uiso 1 1 calc R . . C126 C -0.1414(5) 0.0034(5) 0.2629(4) 0.0405(10) Uani 1 1 d . . . H12D H -0.0936 -0.0589 0.2723 0.049 Uiso 1 1 calc R . . C127 C -0.0269(7) 0.3506(5) 0.2957(6) 0.0543(14) Uani 1 1 d . . . H12E H -0.0971 0.3984 0.2763 0.065 Uiso 1 1 calc R . . H12F H 0.0571 0.3558 0.2472 0.065 Uiso 1 1 calc R . . H12G H 0.0187 0.3846 0.3813 0.065 Uiso 1 1 calc R . . C131 C 0.2151(4) 0.2491(3) 0.4716(3) 0.0245(7) Uani 1 1 d . . . C132 C 0.3696(4) 0.3194(3) 0.5243(3) 0.0264(7) Uani 1 1 d . . . C133 C 0.3969(5) 0.3868(4) 0.6463(3) 0.0309(8) Uani 1 1 d . . . H13A H 0.4998 0.4367 0.6832 0.037 Uiso 1 1 calc R . . C134 C 0.2782(5) 0.3827(4) 0.7148(4) 0.0366(9) Uani 1 1 d . . . H13B H 0.3007 0.4284 0.7978 0.044 Uiso 1 1 calc R . . C135 C 0.1269(5) 0.3123(5) 0.6627(4) 0.0386(9) Uani 1 1 d . . . H13C H 0.0449 0.3094 0.7093 0.046 Uiso 1 1 calc R . . C136 C 0.0966(5) 0.2460(4) 0.5412(4) 0.0343(9) Uani 1 1 d . . . H13D H -0.0071 0.1976 0.5049 0.041 Uiso 1 1 calc R . . C137 C 0.5055(4) 0.3238(4) 0.4560(4) 0.0323(8) Uani 1 1 d . . . H13E H 0.5035 0.2392 0.4100 0.039 Uiso 1 1 calc R . . H13F H 0.6042 0.3623 0.5128 0.039 Uiso 1 1 calc R . . H13G H 0.4971 0.3726 0.4009 0.039 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 0.02515(9) 0.02430(10) 0.02284(9) 0.00772(7) 0.00476(5) 0.00702(6) I1 0.03542(14) 0.03310(15) 0.02850(13) 0.01186(11) 0.00849(10) 0.00381(11) P1 0.0221(4) 0.0229(5) 0.0213(4) 0.0058(4) 0.0041(3) 0.0066(3) I2 0.03591(14) 0.03413(16) 0.03185(14) 0.00519(12) 0.01074(10) 0.00752(11) C111 0.0221(15) 0.0249(18) 0.0280(17) 0.0090(15) 0.0051(13) 0.0040(13) C112 0.0256(17) 0.0258(19) 0.0309(18) 0.0035(16) 0.0049(14) 0.0052(14) C113 0.034(2) 0.025(2) 0.043(2) 0.0013(18) 0.0069(16) 0.0095(15) C114 0.034(2) 0.032(2) 0.069(3) 0.018(2) 0.000(2) 0.0145(17) C115 0.043(2) 0.035(2) 0.046(2) 0.016(2) -0.0040(19) 0.0109(18) C116 0.0303(18) 0.029(2) 0.0329(19) 0.0092(17) 0.0006(15) 0.0077(15) C117 0.048(2) 0.033(2) 0.0263(18) 0.0046(17) 0.0058(16) 0.0111(18) C121 0.0236(16) 0.042(2) 0.0232(16) 0.0057(16) 0.0050(13) 0.0137(15) C122 0.038(2) 0.056(3) 0.0292(19) 0.016(2) 0.0114(16) 0.027(2) C123 0.045(3) 0.105(5) 0.034(2) 0.015(3) 0.009(2) 0.048(3) C124 0.023(2) 0.114(6) 0.042(3) -0.011(3) 0.0014(18) 0.020(3) C125 0.025(2) 0.072(4) 0.047(3) -0.026(3) 0.0083(18) 0.000(2) C126 0.0276(19) 0.042(3) 0.038(2) -0.0036(19) 0.0059(16) 0.0027(17) C127 0.068(3) 0.061(3) 0.068(3) 0.042(3) 0.036(3) 0.045(3) C131 0.0276(17) 0.0211(17) 0.0229(16) 0.0046(14) 0.0029(13) 0.0057(13) C132 0.0297(18) 0.0226(18) 0.0269(17) 0.0071(15) 0.0037(14) 0.0081(14) C133 0.0342(19) 0.027(2) 0.0257(18) 0.0022(16) 0.0007(14) 0.0059(15) C134 0.043(2) 0.037(2) 0.0244(17) 0.0022(17) 0.0042(16) 0.0093(18) C135 0.038(2) 0.048(3) 0.0280(19) 0.0076(19) 0.0116(16) 0.0114(18) C136 0.0310(19) 0.040(2) 0.0285(19) 0.0083(18) 0.0074(15) 0.0040(16) C137 0.0281(18) 0.035(2) 0.0332(19) 0.0100(17) 0.0043(15) 0.0075(15) _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 2.2661(9) . ? Au1 I1 2.5591(3) . ? P1 C121 1.815(4) . ? P1 C111 1.821(4) . ? P1 C131 1.829(4) . ? I2 I2 2.7388(6) 2_565 ? C111 C116 1.412(5) . ? C111 C112 1.419(5) . ? C112 C113 1.386(6) . ? C112 C117 1.511(5) . ? C113 C114 1.387(7) . ? C113 H11A 0.9500 . ? C114 C115 1.384(7) . ? C114 H11B 0.9500 . ? C115 C116 1.388(6) . ? C115 H11C 0.9500 . ? C116 H11D 0.9500 . ? C117 H11E 0.9800 . ? C117 H11F 0.9800 . ? C117 H11G 0.9800 . ? C121 C126 1.388(6) . ? C121 C122 1.408(6) . ? C122 C123 1.408(6) . ? C122 C127 1.521(8) . ? C123 C124 1.358(10) . ? C123 H12A 0.9500 . ? C124 C125 1.366(10) . ? C124 H12B 0.9500 . ? C125 C126 1.397(6) . ? C125 H12C 0.9500 . ? C126 H12D 0.9500 . ? C127 H12E 0.9800 . ? C127 H12F 0.9800 . ? C127 H12G 0.9800 . ? C131 C136 1.390(5) . ? C131 C132 1.407(5) . ? C132 C133 1.397(5) . ? C132 C137 1.508(5) . ? C133 C134 1.383(6) . ? C133 H13A 0.9500 . ? C134 C135 1.383(6) . ? C134 H13B 0.9500 . ? C135 C136 1.388(6) . ? C135 H13C 0.9500 . ? C136 H13D 0.9500 . ? C137 H13E 0.9800 . ? C137 H13F 0.9800 . ? C137 H13G 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 I1 176.82(2) . . ? C121 P1 C111 107.01(18) . . ? C121 P1 C131 104.88(17) . . ? C111 P1 C131 105.51(16) . . ? C121 P1 Au1 113.02(13) . . ? C111 P1 Au1 109.92(12) . . ? C131 P1 Au1 115.86(12) . . ? C116 C111 C112 119.3(4) . . ? C116 C111 P1 118.8(3) . . ? C112 C111 P1 121.7(3) . . ? C113 C112 C111 118.2(4) . . ? C113 C112 C117 118.6(4) . . ? C111 C112 C117 123.2(4) . . ? C112 C113 C114 122.4(4) . . ? C112 C113 H11A 118.8 . . ? C114 C113 H11A 118.8 . . ? C115 C114 C113 119.4(4) . . ? C115 C114 H11B 120.3 . . ? C113 C114 H11B 120.3 . . ? C114 C115 C116 120.3(4) . . ? C114 C115 H11C 119.8 . . ? C116 C115 H11C 119.8 . . ? C115 C116 C111 120.4(4) . . ? C115 C116 H11D 119.8 . . ? C111 C116 H11D 119.8 . . ? C112 C117 H11E 109.5 . . ? C112 C117 H11F 109.5 . . ? H11E C117 H11F 109.5 . . ? C112 C117 H11G 109.5 . . ? H11E C117 H11G 109.5 . . ? H11F C117 H11G 109.5 . . ? C126 C121 C122 119.4(4) . . ? C126 C121 P1 120.1(3) . . ? C122 C121 P1 120.6(3) . . ? C121 C122 C123 117.2(5) . . ? C121 C122 C127 122.7(4) . . ? C123 C122 C127 120.0(4) . . ? C124 C123 C122 122.5(5) . . ? C124 C123 H12A 118.8 . . ? C122 C123 H12A 118.8 . . ? C123 C124 C125 120.4(4) . . ? C123 C124 H12B 119.8 . . ? C125 C124 H12B 119.8 . . ? C124 C125 C126 119.2(5) . . ? C124 C125 H12C 120.4 . . ? C126 C125 H12C 120.4 . . ? C121 C126 C125 121.3(5) . . ? C121 C126 H12D 119.3 . . ? C125 C126 H12D 119.3 . . ? C122 C127 H12E 109.5 . . ? C122 C127 H12F 109.5 . . ? H12E C127 H12F 109.5 . . ? C122 C127 H12G 109.5 . . ? H12E C127 H12G 109.5 . . ? H12F C127 H12G 109.5 . . ? C136 C131 C132 120.0(3) . . ? C136 C131 P1 117.9(3) . . ? C132 C131 P1 122.0(3) . . ? C133 C132 C131 117.7(4) . . ? C133 C132 C137 119.1(3) . . ? C131 C132 C137 123.2(3) . . ? C134 C133 C132 121.8(4) . . ? C134 C133 H13A 119.1 . . ? C132 C133 H13A 119.1 . . ? C133 C134 C135 120.2(4) . . ? C133 C134 H13B 119.9 . . ? C135 C134 H13B 119.9 . . ? C134 C135 C136 119.0(4) . . ? C134 C135 H13C 120.5 . . ? C136 C135 H13C 120.5 . . ? C135 C136 C131 121.3(4) . . ? C135 C136 H13D 119.3 . . ? C131 C136 H13D 119.3 . . ? C132 C137 H13E 109.5 . . ? C132 C137 H13F 109.5 . . ? H13E C137 H13F 109.5 . . ? C132 C137 H13G 109.5 . . ? H13E C137 H13G 109.5 . . ? H13F C137 H13G 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 I1 Au1 P1 C121 -128.3(4) . . . . ? I1 Au1 P1 C111 -8.9(5) . . . . ? I1 Au1 P1 C131 110.6(4) . . . . ? C121 P1 C111 C116 -110.0(3) . . . . ? C131 P1 C111 C116 1.3(3) . . . . ? Au1 P1 C111 C116 126.9(3) . . . . ? C121 P1 C111 C112 74.7(3) . . . . ? C131 P1 C111 C112 -174.0(3) . . . . ? Au1 P1 C111 C112 -48.4(3) . . . . ? C116 C111 C112 C113 -1.5(5) . . . . ? P1 C111 C112 C113 173.8(3) . . . . ? C116 C111 C112 C117 178.2(4) . . . . ? P1 C111 C112 C117 -6.5(5) . . . . ? C111 C112 C113 C114 0.9(6) . . . . ? C117 C112 C113 C114 -178.7(4) . . . . ? C112 C113 C114 C115 0.4(7) . . . . ? C113 C114 C115 C116 -1.2(7) . . . . ? C114 C115 C116 C111 0.6(6) . . . . ? C112 C111 C116 C115 0.8(6) . . . . ? P1 C111 C116 C115 -174.7(3) . . . . ? C111 P1 C121 C126 4.5(4) . . . . ? C131 P1 C121 C126 -107.3(3) . . . . ? Au1 P1 C121 C126 125.6(3) . . . . ? C111 P1 C121 C122 -175.4(3) . . . . ? C131 P1 C121 C122 72.9(3) . . . . ? Au1 P1 C121 C122 -54.2(3) . . . . ? C126 C121 C122 C123 -2.9(6) . . . . ? P1 C121 C122 C123 177.0(3) . . . . ? C126 C121 C122 C127 174.3(4) . . . . ? P1 C121 C122 C127 -5.8(6) . . . . ? C121 C122 C123 C124 1.3(7) . . . . ? C127 C122 C123 C124 -176.0(5) . . . . ? C122 C123 C124 C125 1.5(8) . . . . ? C123 C124 C125 C126 -2.6(8) . . . . ? C122 C121 C126 C125 1.8(6) . . . . ? P1 C121 C126 C125 -178.0(4) . . . . ? C124 C125 C126 C121 1.0(7) . . . . ? C121 P1 C131 C136 17.8(4) . . . . ? C111 P1 C131 C136 -95.0(3) . . . . ? Au1 P1 C131 C136 143.2(3) . . . . ? C121 P1 C131 C132 -163.9(3) . . . . ? C111 P1 C131 C132 83.3(3) . . . . ? Au1 P1 C131 C132 -38.6(3) . . . . ? C136 C131 C132 C133 -1.5(6) . . . . ? P1 C131 C132 C133 -179.7(3) . . . . ? C136 C131 C132 C137 177.7(4) . . . . ? P1 C131 C132 C137 -0.5(5) . . . . ? C131 C132 C133 C134 1.7(6) . . . . ? C137 C132 C133 C134 -177.5(4) . . . . ? C132 C133 C134 C135 -1.1(7) . . . . ? C133 C134 C135 C136 0.1(7) . . . . ? C134 C135 C136 C131 0.1(7) . . . . ? C132 C131 C136 C135 0.7(6) . . . . ? P1 C131 C136 C135 178.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 27.24 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 1.321 _refine_diff_density_min -1.772 _refine_diff_density_rms 0.148 #===END data_[(dppm)(AuBr)2] _database_code_depnum_ccdc_archive 'CCDC 232536' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(dppm)(AuBr)2]' _chemical_formula_sum 'C25 H22 Au2 Br2 P2' _chemical_formula_weight 938.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 22.3810(3) _cell_length_b 7.3200(1) _cell_length_c 18.3500(3) _cell_angle_alpha 90.00 _cell_angle_beta 122.226(1) _cell_angle_gamma 90.00 _cell_volume 2543.15(6) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 32750 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 14.804 _exptl_absorpt_correction_type DELABS _exptl_absorpt_correction_T_min 0.488 _exptl_absorpt_correction_T_max 0.836 _exptl_absorpt_process_details ? _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 HU' _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 32750 _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_av_sigmaI/netI 0.050 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 27.31 _reflns_number_total 2823 _reflns_number_gt 2474 _reflns_threshold_expression >2sigma(I) _computing_data_collection XPRESS _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _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^)+(0.0249P)^2^+28.6543P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom (Ph), difmap (CH)' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2823 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0717 _refine_ls_wR_factor_gt 0.0687 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 -0.000207(11) 0.62427(3) 0.343616(13) 0.02189(8) Uani 1 1 d . . . Br1 Br -0.06954(4) 0.36667(8) 0.33879(5) 0.03318(15) Uani 1 1 d . . . P1 P 0.05807(7) 0.8736(2) 0.34375(9) 0.0191(3) Uani 1 1 d . . . C1 C 0.0000 1.0161(11) 0.2500 0.0195(15) Uani 1 2 d S . . H1 H 0.022(5) 1.087(12) 0.236(6) 0.050 Uiso 1 1 d . . . C111 C 0.1356(3) 0.8259(8) 0.3392(3) 0.0187(11) Uani 1 1 d . . . C112 C 0.1720(3) 0.6653(9) 0.3753(4) 0.0310(14) Uani 1 1 d . . . H11A H 0.1541 0.5794 0.3977 0.037 Uiso 1 1 calc R . . C113 C 0.2346(4) 0.6272(10) 0.3793(5) 0.0393(16) Uani 1 1 d . . . H11B H 0.2595 0.5173 0.4053 0.047 Uiso 1 1 calc R . . C114 C 0.2601(3) 0.7496(10) 0.3455(4) 0.0307(14) Uani 1 1 d . . . H11C H 0.3029 0.7243 0.3482 0.037 Uiso 1 1 calc R . . C115 C 0.2235(3) 0.9098(10) 0.3074(4) 0.0325(14) Uani 1 1 d . . . H11D H 0.2407 0.9923 0.2829 0.039 Uiso 1 1 calc R . . C116 C 0.1619(3) 0.9504(9) 0.3048(4) 0.0263(12) Uani 1 1 d . . . H11E H 0.1377 1.0618 0.2800 0.032 Uiso 1 1 calc R . . C211 C 0.0881(3) 1.0228(8) 0.4354(4) 0.0226(11) Uani 1 1 d . . . C212 C 0.1225(4) 1.1888(9) 0.4423(4) 0.0294(13) Uani 1 1 d . . . H21A H 0.1315 1.2231 0.3991 0.035 Uiso 1 1 calc R . . C213 C 0.1430(4) 1.3008(9) 0.5117(4) 0.0367(16) Uani 1 1 d . . . H21B H 0.1653 1.4138 0.5156 0.044 Uiso 1 1 calc R . . C214 C 0.1315(4) 1.2513(10) 0.5762(4) 0.0353(15) Uani 1 1 d . . . H21C H 0.1462 1.3299 0.6240 0.042 Uiso 1 1 calc R . . C215 C 0.0985(3) 1.0873(10) 0.5707(4) 0.0308(14) Uani 1 1 d . . . H21D H 0.0908 1.0524 0.6149 0.037 Uiso 1 1 calc R . . C216 C 0.0768(3) 0.9733(9) 0.4998(4) 0.0254(12) Uani 1 1 d . . . H21E H 0.0541 0.8609 0.4958 0.030 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 0.02273(12) 0.02053(12) 0.02330(12) -0.00017(9) 0.01288(9) -0.00194(9) Br1 0.0382(3) 0.0227(3) 0.0495(4) -0.0064(3) 0.0306(3) -0.0076(3) P1 0.0191(6) 0.0204(6) 0.0161(6) 0.0006(6) 0.0082(5) -0.0007(6) C1 0.016(3) 0.020(4) 0.015(4) 0.000 0.003(3) 0.000 C111 0.016(2) 0.021(3) 0.013(2) -0.004(2) 0.004(2) 0.000(2) C112 0.030(3) 0.029(3) 0.036(3) 0.008(3) 0.019(3) 0.003(3) C113 0.035(3) 0.037(4) 0.045(4) 0.008(3) 0.020(3) 0.014(3) C114 0.017(3) 0.047(4) 0.026(3) 0.000(3) 0.011(2) 0.004(3) C115 0.025(3) 0.046(4) 0.027(3) 0.003(3) 0.015(3) -0.004(3) C116 0.023(3) 0.026(3) 0.029(3) 0.004(2) 0.013(3) 0.000(2) C211 0.019(3) 0.026(3) 0.017(3) 0.002(2) 0.006(2) 0.002(2) C212 0.038(3) 0.027(3) 0.020(3) 0.001(2) 0.014(3) -0.004(3) C213 0.046(4) 0.026(3) 0.024(3) -0.002(3) 0.010(3) -0.002(3) C214 0.033(3) 0.042(4) 0.023(3) -0.006(3) 0.010(3) 0.006(3) C215 0.025(3) 0.046(4) 0.020(3) -0.005(3) 0.011(2) 0.004(3) C216 0.017(3) 0.036(3) 0.020(3) 0.001(2) 0.008(2) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.2425(15) . ? Au1 Br1 2.4135(6) . ? P1 C211 1.807(6) . ? P1 C111 1.814(6) . ? P1 C1 1.831(5) . ? C1 P1 1.831(5) 2 ? C1 H1 0.85(8) . ? C111 C112 1.382(8) . ? C111 C116 1.406(8) . ? C112 C113 1.389(9) . ? C112 H11A 0.9500 . ? C113 C114 1.377(10) . ? C113 H11B 0.9500 . ? C114 C115 1.388(10) . ? C114 H11C 0.9500 . ? C115 C116 1.385(9) . ? C115 H11D 0.9500 . ? C116 H11E 0.9500 . ? C211 C216 1.382(8) . ? C211 C212 1.408(9) . ? C212 C213 1.371(9) . ? C212 H21A 0.9500 . ? C213 C214 1.386(10) . ? C213 H21B 0.9500 . ? C214 C215 1.385(10) . ? C214 H21C 0.9500 . ? C215 C216 1.396(9) . ? C215 H21D 0.9500 . ? C216 H21E 0.9500 . ? 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 Br1 176.48(4) . . ? C211 P1 C111 105.6(3) . . ? C211 P1 C1 104.8(3) . . ? C111 P1 C1 106.49(19) . . ? C211 P1 Au1 114.8(2) . . ? C111 P1 Au1 114.38(19) . . ? C1 P1 Au1 109.98(18) . . ? P1 C1 P1 110.5(4) 2 . ? P1 C1 H1 107(6) 2 . ? P1 C1 H1 114(6) . . ? C112 C111 C116 119.0(5) . . ? C112 C111 P1 118.5(5) . . ? C116 C111 P1 122.4(4) . . ? C111 C112 C113 121.1(6) . . ? C111 C112 H11A 119.4 . . ? C113 C112 H11A 119.4 . . ? C114 C113 C112 119.7(6) . . ? C114 C113 H11B 120.2 . . ? C112 C113 H11B 120.2 . . ? C113 C114 C115 120.0(6) . . ? C113 C114 H11C 120.0 . . ? C115 C114 H11C 120.0 . . ? C116 C115 C114 120.6(6) . . ? C116 C115 H11D 119.7 . . ? C114 C115 H11D 119.7 . . ? C115 C116 C111 119.6(6) . . ? C115 C116 H11E 120.2 . . ? C111 C116 H11E 120.2 . . ? C216 C211 C212 119.3(6) . . ? C216 C211 P1 119.4(5) . . ? C212 C211 P1 121.3(5) . . ? C213 C212 C211 119.7(6) . . ? C213 C212 H21A 120.1 . . ? C211 C212 H21A 120.1 . . ? C212 C213 C214 120.9(7) . . ? C212 C213 H21B 119.5 . . ? C214 C213 H21B 119.5 . . ? C215 C214 C213 119.9(6) . . ? C215 C214 H21C 120.1 . . ? C213 C214 H21C 120.1 . . ? C214 C215 C216 119.6(6) . . ? C214 C215 H21D 120.2 . . ? C216 C215 H21D 120.2 . . ? C211 C216 C215 120.6(6) . . ? C211 C216 H21E 119.7 . . ? C215 C216 H21E 119.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br1 Au1 P1 C211 89.5(7) . . . . ? Br1 Au1 P1 C111 -148.1(6) . . . . ? Br1 Au1 P1 C1 -28.4(7) . . . . ? C211 P1 C1 P1 -160.6(2) . . . 2 ? C111 P1 C1 P1 87.7(2) . . . 2 ? Au1 P1 C1 P1 -36.70(6) . . . 2 ? C211 P1 C111 C112 97.4(5) . . . . ? C1 P1 C111 C112 -151.6(5) . . . . ? Au1 P1 C111 C112 -29.9(5) . . . . ? C211 P1 C111 C116 -79.0(5) . . . . ? C1 P1 C111 C116 32.0(6) . . . . ? Au1 P1 C111 C116 153.7(4) . . . . ? C116 C111 C112 C113 1.2(10) . . . . ? P1 C111 C112 C113 -175.3(6) . . . . ? C111 C112 C113 C114 -1.2(11) . . . . ? C112 C113 C114 C115 -0.1(11) . . . . ? C113 C114 C115 C116 1.6(10) . . . . ? C114 C115 C116 C111 -1.6(10) . . . . ? C112 C111 C116 C115 0.2(9) . . . . ? P1 C111 C116 C115 176.6(5) . . . . ? C111 P1 C211 C216 -124.2(5) . . . . ? C1 P1 C211 C216 123.6(5) . . . . ? Au1 P1 C211 C216 2.8(5) . . . . ? C111 P1 C211 C212 56.0(6) . . . . ? C1 P1 C211 C212 -56.2(5) . . . . ? Au1 P1 C211 C212 -177.0(4) . . . . ? C216 C211 C212 C213 -1.4(10) . . . . ? P1 C211 C212 C213 178.4(5) . . . . ? C211 C212 C213 C214 1.2(11) . . . . ? C212 C213 C214 C215 -0.4(11) . . . . ? C213 C214 C215 C216 -0.3(10) . . . . ? C212 C211 C216 C215 0.7(9) . . . . ? P1 C211 C216 C215 -179.1(5) . . . . ? C214 C215 C216 C211 0.2(9) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.31 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.348 _refine_diff_density_min -1.423 _refine_diff_density_rms 0.181 #===END data_[(dppm)(AuI)2] _database_code_depnum_ccdc_archive 'CCDC 232537' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(dppm)(AuI)2]' _chemical_formula_sum 'C25 H22 Au2 I2 P2' _chemical_formula_weight 1032.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 22.4894(2) _cell_length_b 7.5585(1) _cell_length_c 18.7126(3) _cell_angle_alpha 90.00 _cell_angle_beta 123.579(1) _cell_angle_gamma 90.00 _cell_volume 2650.07(6) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 35673 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour dark-yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 13.521 _exptl_absorpt_correction_type DELABS _exptl_absorpt_correction_T_min 0.323 _exptl_absorpt_correction_T_max 0.754 _exptl_absorpt_process_details ? _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 HU' _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 35673 _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_av_sigmaI/netI 0.079 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 27.19 _reflns_number_total 2939 _reflns_number_gt 2932 _reflns_threshold_expression >2sigma(I) _computing_data_collection XPRESS _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _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^)+(0.0099P)^2^+23.3731P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'difmap (CH2), geom (Ph)' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2939 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0261 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0670 _refine_ls_wR_factor_gt 0.0670 _refine_ls_goodness_of_fit_ref 1.195 _refine_ls_restrained_S_all 1.195 _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 0.000034(9) 0.64578(2) 0.345552(11) 0.01884(8) Uani 1 1 d . . . I1 I -0.070112(19) 0.37825(4) 0.34487(3) 0.02886(10) Uani 1 1 d . . . P1 P 0.05866(6) 0.88561(16) 0.34375(7) 0.0152(2) Uani 1 1 d . . . C1 C 0.0000 1.0240(8) 0.2500 0.0161(11) Uani 1 2 d S . . H1 H 0.027(4) 1.104(10) 0.237(5) 0.050 Uiso 1 1 d . . . C111 C 0.1348(2) 0.8306(6) 0.3391(3) 0.0175(9) Uani 1 1 d . . . C112 C 0.1723(3) 0.6767(8) 0.3805(4) 0.0289(11) Uani 1 1 d . . . H11A H 0.1558 0.6026 0.4071 0.035 Uiso 1 1 calc R . . C113 C 0.2331(3) 0.6303(8) 0.3835(4) 0.0351(13) Uani 1 1 d . . . H11B H 0.2580 0.5249 0.4119 0.042 Uiso 1 1 calc R . . C114 C 0.2575(3) 0.7365(8) 0.3453(3) 0.0292(11) Uani 1 1 d . . . H11C H 0.2995 0.7049 0.3478 0.035 Uiso 1 1 calc R . . C115 C 0.2207(3) 0.8899(7) 0.3030(3) 0.0259(10) Uani 1 1 d . . . H11D H 0.2370 0.9620 0.2755 0.031 Uiso 1 1 calc R . . C116 C 0.1599(2) 0.9378(7) 0.3008(3) 0.0222(9) Uani 1 1 d . . . H11E H 0.1355 1.0441 0.2730 0.027 Uiso 1 1 calc R . . C211 C 0.0925(2) 1.0343(6) 0.4344(3) 0.0187(9) Uani 1 1 d . . . C212 C 0.1318(3) 1.1844(7) 0.4428(3) 0.0242(10) Uani 1 1 d . . . H21A H 0.1412 1.2114 0.4004 0.029 Uiso 1 1 calc R . . C213 C 0.1572(3) 1.2942(8) 0.5130(3) 0.0326(12) Uani 1 1 d . . . H21B H 0.1846 1.3956 0.5192 0.039 Uiso 1 1 calc R . . C214 C 0.1425(3) 1.2565(8) 0.5744(3) 0.0303(11) Uani 1 1 d . . . H21C H 0.1594 1.3333 0.6221 0.036 Uiso 1 1 calc R . . C215 C 0.1037(3) 1.1083(8) 0.5665(3) 0.0302(11) Uani 1 1 d . . . H21D H 0.0938 1.0833 0.6087 0.036 Uiso 1 1 calc R . . C216 C 0.0789(2) 0.9950(7) 0.4968(3) 0.0227(10) Uani 1 1 d . . . H21E H 0.0528 0.8916 0.4918 0.027 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 0.01784(11) 0.01823(12) 0.02049(11) 0.00048(6) 0.01062(8) -0.00159(6) I1 0.03187(19) 0.01812(17) 0.0464(2) -0.00450(13) 0.02777(17) -0.00524(12) P1 0.0131(5) 0.0181(5) 0.0122(5) 0.0005(4) 0.0056(4) -0.0004(4) C1 0.013(3) 0.016(3) 0.014(3) 0.000 0.004(2) 0.000 C111 0.0121(19) 0.023(2) 0.0123(19) 0.0006(17) 0.0037(16) 0.0013(16) C112 0.027(3) 0.030(3) 0.032(3) 0.016(2) 0.018(2) 0.009(2) C113 0.025(3) 0.038(3) 0.037(3) 0.016(2) 0.014(2) 0.014(2) C114 0.015(2) 0.041(3) 0.028(2) -0.001(2) 0.0097(19) 0.005(2) C115 0.021(2) 0.033(3) 0.027(2) 0.003(2) 0.015(2) -0.002(2) C116 0.020(2) 0.025(2) 0.022(2) 0.0041(19) 0.0117(18) 0.0025(18) C211 0.016(2) 0.022(2) 0.0116(18) 0.0000(17) 0.0039(16) 0.0030(16) C212 0.027(2) 0.024(2) 0.017(2) -0.0021(19) 0.0088(19) -0.003(2) C213 0.036(3) 0.023(3) 0.023(2) -0.001(2) 0.007(2) -0.002(2) C214 0.028(2) 0.037(3) 0.017(2) -0.007(2) 0.0068(19) 0.006(2) C215 0.023(2) 0.048(3) 0.019(2) -0.003(2) 0.012(2) 0.005(2) C216 0.017(2) 0.031(3) 0.018(2) 0.0011(19) 0.0081(17) 0.0025(18) _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 2.2528(12) . ? Au1 I1 2.5604(4) . ? P1 C111 1.811(5) . ? P1 C211 1.814(5) . ? P1 C1 1.831(4) . ? C1 P1 1.831(4) 2 ? C1 H1 0.98(7) . ? C111 C116 1.392(7) . ? C111 C112 1.393(7) . ? C112 C113 1.383(8) . ? C112 H11A 0.9500 . ? C113 C114 1.375(8) . ? C113 H11B 0.9500 . ? C114 C115 1.389(8) . ? C114 H11C 0.9500 . ? C115 C116 1.393(7) . ? C115 H11D 0.9500 . ? C116 H11E 0.9500 . ? C211 C212 1.392(7) . ? C211 C216 1.393(6) . ? C212 C213 1.381(7) . ? C212 H21A 0.9500 . ? C213 C214 1.389(8) . ? C213 H21B 0.9500 . ? C214 C215 1.377(9) . ? C214 H21C 0.9500 . ? C215 C216 1.394(7) . ? C215 H21D 0.9500 . ? C216 H21E 0.9500 . ? 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 I1 178.29(3) . . ? C111 P1 C211 105.5(2) . . ? C111 P1 C1 106.55(15) . . ? C211 P1 C1 104.4(2) . . ? C111 P1 Au1 113.14(16) . . ? C211 P1 Au1 115.53(16) . . ? C1 P1 Au1 110.89(14) . . ? P1 C1 P1 110.3(3) 2 . ? P1 C1 H1 109(5) 2 . ? P1 C1 H1 112(5) . . ? C116 C111 C112 118.7(4) . . ? C116 C111 P1 123.7(4) . . ? C112 C111 P1 117.5(4) . . ? C113 C112 C111 120.9(5) . . ? C113 C112 H11A 119.5 . . ? C111 C112 H11A 119.5 . . ? C114 C113 C112 120.1(5) . . ? C114 C113 H11B 119.9 . . ? C112 C113 H11B 119.9 . . ? C113 C114 C115 120.1(5) . . ? C113 C114 H11C 120.0 . . ? C115 C114 H11C 120.0 . . ? C114 C115 C116 119.9(5) . . ? C114 C115 H11D 120.1 . . ? C116 C115 H11D 120.1 . . ? C111 C116 C115 120.4(5) . . ? C111 C116 H11E 119.8 . . ? C115 C116 H11E 119.8 . . ? C212 C211 C216 119.9(4) . . ? C212 C211 P1 121.5(4) . . ? C216 C211 P1 118.6(4) . . ? C213 C212 C211 120.0(5) . . ? C213 C212 H21A 120.0 . . ? C211 C212 H21A 120.0 . . ? C212 C213 C214 120.0(5) . . ? C212 C213 H21B 120.0 . . ? C214 C213 H21B 120.0 . . ? C215 C214 C213 120.3(5) . . ? C215 C214 H21C 119.8 . . ? C213 C214 H21C 119.8 . . ? C214 C215 C216 120.1(5) . . ? C214 C215 H21D 119.9 . . ? C216 C215 H21D 119.9 . . ? C211 C216 C215 119.6(5) . . ? C211 C216 H21E 120.2 . . ? C215 C216 H21E 120.2 . . ? 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 I1 Au1 P1 C111 -143.9(10) . . . . ? I1 Au1 P1 C211 94.3(10) . . . . ? I1 Au1 P1 C1 -24.3(11) . . . . ? C111 P1 C1 P1 85.13(17) . . . 2 ? C211 P1 C1 P1 -163.46(16) . . . 2 ? Au1 P1 C1 P1 -38.39(5) . . . 2 ? C211 P1 C111 C116 -82.3(4) . . . . ? C1 P1 C111 C116 28.4(5) . . . . ? Au1 P1 C111 C116 150.5(4) . . . . ? C211 P1 C111 C112 94.1(4) . . . . ? C1 P1 C111 C112 -155.2(4) . . . . ? Au1 P1 C111 C112 -33.1(4) . . . . ? C116 C111 C112 C113 -0.2(8) . . . . ? P1 C111 C112 C113 -176.8(5) . . . . ? C111 C112 C113 C114 0.0(9) . . . . ? C112 C113 C114 C115 -0.6(9) . . . . ? C113 C114 C115 C116 1.3(8) . . . . ? C112 C111 C116 C115 1.0(7) . . . . ? P1 C111 C116 C115 177.3(4) . . . . ? C114 C115 C116 C111 -1.5(8) . . . . ? C111 P1 C211 C212 52.0(4) . . . . ? C1 P1 C211 C212 -60.1(4) . . . . ? Au1 P1 C211 C212 177.8(3) . . . . ? C111 P1 C211 C216 -127.5(4) . . . . ? C1 P1 C211 C216 120.3(3) . . . . ? Au1 P1 C211 C216 -1.8(4) . . . . ? C216 C211 C212 C213 0.0(7) . . . . ? P1 C211 C212 C213 -179.6(4) . . . . ? C211 C212 C213 C214 -1.0(8) . . . . ? C212 C213 C214 C215 1.0(8) . . . . ? C213 C214 C215 C216 0.0(8) . . . . ? C212 C211 C216 C215 1.1(7) . . . . ? P1 C211 C216 C215 -179.3(4) . . . . ? C214 C215 C216 C211 -1.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.19 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.917 _refine_diff_density_min -1.925 _refine_diff_density_rms 0.186 #===END data_[(dppm)(AuBr)2Br22CH2Cl2] _database_code_depnum_ccdc_archive 'CCDC 232538' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(dppm)(AuBr)2Br22CH2Cl2]' _chemical_formula_sum 'C27 H26 Au2 Br4 Cl4 P2' _chemical_formula_weight 1267.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.1186(1) _cell_length_b 15.8399(1) _cell_length_c 19.7887(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.162(1) _cell_angle_gamma 90.00 _cell_volume 3465.00(5) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 85839 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour dark_red _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 2.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 13.490 _exptl_absorpt_correction_type DELABS _exptl_absorpt_correction_T_min 0.603 _exptl_absorpt_correction_T_max 0.881 _exptl_absorpt_process_details ? _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 DIP2020 HU' _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 85839 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_av_sigmaI/netI 0.045 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 26.49 _reflns_number_total 7114 _reflns_number_gt 6780 _reflns_threshold_expression >2sigma(I) _computing_data_collection XPRESS _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _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^)+(0.0120P)^2^+16.3378P] 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 7114 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0641 _refine_ls_wR_factor_gt 0.0632 _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_restrained_S_all 1.168 _refine_ls_shift/su_max 0.005 _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 -0.489042(16) 1.137884(12) 0.328866(9) 0.01779(6) Uani 1 1 d . . . Au2 Au -0.778632(16) 1.222679(11) 0.299667(9) 0.01862(6) Uani 1 1 d . . . P1 P -0.62006(10) 1.02520(8) 0.30627(6) 0.0157(2) Uani 1 1 d . . . P2 P -0.84728(11) 1.11159(8) 0.23682(6) 0.0168(2) Uani 1 1 d . . . Br1 Br -0.50844(5) 1.18331(4) 0.21081(3) 0.03725(14) Uani 1 1 d . . . Br2 Br -0.34035(5) 1.25089(3) 0.35561(3) 0.02875(12) Uani 1 1 d . . . Br3 Br -0.43772(5) 1.07959(4) 0.44153(3) 0.03185(13) Uani 1 1 d . . . Br4 Br -0.70388(5) 1.34013(3) 0.36880(3) 0.02676(12) Uani 1 1 d . . . C1 C -0.7243(4) 1.0358(3) 0.2288(2) 0.0189(10) Uani 1 1 d . . . H1A H -0.7599 0.9799 0.2166 0.023 Uiso 1 1 calc R . . H1B H -0.6782 1.0541 0.1913 0.023 Uiso 1 1 calc R . . C111 C -0.7161(4) 0.9991(3) 0.3716(2) 0.0186(10) Uani 1 1 d . . . C112 C -0.7390(4) 1.0535(4) 0.4234(2) 0.0230(11) Uani 1 1 d . . . H11A H -0.7004 1.1071 0.4276 0.028 Uiso 1 1 calc R . . C113 C -0.8185(5) 1.0293(4) 0.4688(3) 0.0320(13) Uani 1 1 d . . . H11B H -0.8336 1.0660 0.5049 0.038 Uiso 1 1 calc R . . C114 C -0.8766(5) 0.9515(4) 0.4621(3) 0.0331(13) Uani 1 1 d . . . H11C H -0.9308 0.9354 0.4938 0.040 Uiso 1 1 calc R . . C115 C -0.8559(5) 0.8981(4) 0.4102(3) 0.0286(12) Uani 1 1 d . . . H11D H -0.8962 0.8452 0.4055 0.034 Uiso 1 1 calc R . . C116 C -0.7755(4) 0.9219(3) 0.3642(3) 0.0238(11) Uani 1 1 d . . . H11E H -0.7614 0.8854 0.3278 0.029 Uiso 1 1 calc R . . C121 C -0.5285(4) 0.9338(3) 0.2941(3) 0.0195(10) Uani 1 1 d . . . C122 C -0.4914(5) 0.9162(4) 0.2308(3) 0.0277(12) Uani 1 1 d . . . H12A H -0.5171 0.9515 0.1932 0.033 Uiso 1 1 calc R . . C123 C -0.4176(5) 0.8478(4) 0.2220(3) 0.0320(13) Uani 1 1 d . . . H12B H -0.3923 0.8364 0.1786 0.038 Uiso 1 1 calc R . . C124 C -0.3803(5) 0.7958(3) 0.2767(3) 0.0299(12) Uani 1 1 d . . . H12C H -0.3299 0.7486 0.2708 0.036 Uiso 1 1 calc R . . C125 C -0.4169(5) 0.8131(3) 0.3399(3) 0.0309(12) Uani 1 1 d . . . H12D H -0.3911 0.7775 0.3773 0.037 Uiso 1 1 calc R . . C126 C -0.4908(4) 0.8819(3) 0.3494(3) 0.0238(11) Uani 1 1 d . . . H12E H -0.5154 0.8934 0.3929 0.029 Uiso 1 1 calc R . . C211 C -0.8969(4) 1.1386(3) 0.1491(2) 0.0198(10) Uani 1 1 d . . . C212 C -1.0022(5) 1.1052(4) 0.1141(3) 0.0279(12) Uani 1 1 d . . . H21A H -1.0495 1.0654 0.1356 0.034 Uiso 1 1 calc R . . C213 C -1.0372(5) 1.1307(4) 0.0476(3) 0.0316(13) Uani 1 1 d . . . H21B H -1.1084 1.1078 0.0236 0.038 Uiso 1 1 calc R . . C214 C -0.9693(5) 1.1892(4) 0.0161(3) 0.0303(12) Uani 1 1 d . . . H21C H -0.9940 1.2065 -0.0293 0.036 Uiso 1 1 calc R . . C215 C -0.8650(5) 1.2226(4) 0.0509(3) 0.0271(11) Uani 1 1 d . . . H21D H -0.8184 1.2628 0.0294 0.033 Uiso 1 1 calc R . . C216 C -0.8287(5) 1.1973(3) 0.1169(3) 0.0230(10) Uani 1 1 d . . . H21E H -0.7570 1.2200 0.1405 0.028 Uiso 1 1 calc R . . C221 C -0.9701(4) 1.0550(3) 0.2697(2) 0.0181(9) Uani 1 1 d . . . C222 C -1.0342(5) 1.0965(3) 0.3169(3) 0.0246(11) Uani 1 1 d . . . H22A H -1.0104 1.1515 0.3322 0.029 Uiso 1 1 calc R . . C223 C -1.1329(5) 1.0575(4) 0.3414(3) 0.0284(12) Uani 1 1 d . . . H22B H -1.1766 1.0856 0.3734 0.034 Uiso 1 1 calc R . . C224 C -1.1673(5) 0.9772(4) 0.3188(3) 0.0286(12) Uani 1 1 d . . . H22C H -1.2351 0.9508 0.3352 0.034 Uiso 1 1 calc R . . C225 C -1.1035(5) 0.9354(3) 0.2725(3) 0.0267(11) Uani 1 1 d . . . H22D H -1.1274 0.8804 0.2575 0.032 Uiso 1 1 calc R . . C226 C -1.0046(4) 0.9740(3) 0.2482(3) 0.0224(10) Uani 1 1 d . . . H22E H -0.9604 0.9450 0.2168 0.027 Uiso 1 1 calc R . . C2 C -0.0797(7) 0.6969(5) 0.4982(4) 0.058(2) Uani 1 1 d . . . H2A H -0.0586 0.6417 0.4791 0.069 Uiso 1 1 calc R . . H2B H -0.1395 0.6867 0.5310 0.069 Uiso 1 1 calc R . . Cl1 Cl -0.14378(19) 0.76146(15) 0.43302(11) 0.0667(6) Uani 1 1 d . . . Cl2 Cl 0.05151(16) 0.74301(11) 0.54109(8) 0.0451(4) Uani 1 1 d . . . C3 C 0.2595(8) 1.0541(5) -0.0356(6) 0.077(3) Uani 1 1 d . . . H3A H 0.2694 1.1149 -0.0453 0.092 Uiso 1 1 calc R . . H3B H 0.1729 1.0438 -0.0312 0.092 Uiso 1 1 calc R . . Cl3 Cl 0.3428(4) 1.02977(18) 0.03962(13) 0.1207(14) Uani 1 1 d . . . Cl4 Cl 0.30246(18) 0.99472(16) -0.10396(12) 0.0697(6) 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 Au1 0.01775(9) 0.01879(10) 0.01681(10) 0.00063(7) 0.00185(7) -0.00312(7) Au2 0.02082(10) 0.01690(10) 0.01775(10) -0.00019(7) 0.00023(7) -0.00133(7) P1 0.0153(6) 0.0169(6) 0.0151(6) 0.0000(5) 0.0028(4) -0.0012(4) P2 0.0175(6) 0.0167(6) 0.0160(6) -0.0004(5) 0.0013(4) -0.0005(5) Br1 0.0375(3) 0.0491(4) 0.0249(3) 0.0098(2) 0.0024(2) -0.0143(3) Br2 0.0282(3) 0.0281(3) 0.0302(3) -0.0019(2) 0.0046(2) -0.0121(2) Br3 0.0335(3) 0.0360(3) 0.0243(3) 0.0057(2) -0.0046(2) -0.0069(2) Br4 0.0331(3) 0.0206(3) 0.0250(3) -0.0024(2) -0.0042(2) -0.0040(2) C1 0.017(2) 0.025(3) 0.015(2) -0.0018(19) 0.0028(18) 0.0000(18) C111 0.016(2) 0.021(2) 0.019(2) 0.0017(19) 0.0034(18) 0.0030(18) C112 0.020(2) 0.032(3) 0.017(2) 0.001(2) 0.0019(19) 0.003(2) C113 0.034(3) 0.041(3) 0.023(3) 0.001(2) 0.010(2) 0.011(3) C114 0.024(3) 0.043(3) 0.035(3) 0.015(3) 0.014(2) 0.009(2) C115 0.021(3) 0.031(3) 0.036(3) 0.009(2) 0.009(2) -0.001(2) C116 0.020(2) 0.026(3) 0.026(3) 0.005(2) 0.005(2) -0.001(2) C121 0.016(2) 0.017(2) 0.025(3) 0.000(2) 0.0030(19) 0.0006(18) C122 0.024(3) 0.032(3) 0.027(3) -0.005(2) 0.006(2) 0.003(2) C123 0.024(3) 0.038(3) 0.035(3) -0.012(3) 0.007(2) 0.002(2) C124 0.017(2) 0.023(3) 0.051(4) -0.011(3) 0.007(2) -0.001(2) C125 0.025(3) 0.023(3) 0.045(3) 0.008(2) 0.004(2) 0.002(2) C126 0.021(2) 0.026(3) 0.026(3) 0.003(2) 0.008(2) -0.002(2) C211 0.023(2) 0.017(2) 0.019(2) 0.0000(19) 0.0001(19) 0.0039(18) C212 0.029(3) 0.030(3) 0.024(3) 0.004(2) -0.004(2) -0.005(2) C213 0.034(3) 0.032(3) 0.027(3) 0.003(2) -0.008(2) -0.008(2) C214 0.034(3) 0.038(3) 0.018(3) 0.005(2) -0.003(2) -0.001(2) C215 0.028(3) 0.030(3) 0.023(3) 0.006(2) 0.004(2) -0.003(2) C216 0.022(2) 0.025(3) 0.022(2) 0.002(2) -0.001(2) -0.001(2) C221 0.015(2) 0.019(2) 0.020(2) 0.0027(19) -0.0001(18) 0.0016(18) C222 0.025(3) 0.023(3) 0.026(3) -0.004(2) 0.004(2) -0.001(2) C223 0.021(3) 0.037(3) 0.027(3) -0.004(2) 0.006(2) 0.003(2) C224 0.019(3) 0.034(3) 0.033(3) 0.004(2) 0.005(2) -0.003(2) C225 0.024(3) 0.025(3) 0.031(3) -0.001(2) 0.002(2) -0.005(2) C226 0.024(3) 0.020(3) 0.024(3) -0.003(2) 0.005(2) 0.0033(19) C2 0.050(4) 0.055(5) 0.068(5) 0.004(4) 0.003(4) -0.019(4) Cl1 0.0579(12) 0.0741(14) 0.0626(13) -0.0006(10) -0.0186(10) 0.0019(10) Cl2 0.0531(10) 0.0425(9) 0.0378(8) 0.0021(7) -0.0037(7) -0.0043(7) C3 0.057(5) 0.035(4) 0.142(9) 0.008(5) 0.026(6) 0.000(4) Cl3 0.233(4) 0.0755(18) 0.0653(15) 0.0266(13) 0.070(2) 0.075(2) Cl4 0.0469(11) 0.0845(16) 0.0767(14) 0.0213(12) 0.0020(10) -0.0085(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.3169(12) . ? Au1 Br3 2.4240(6) . ? Au1 Br1 2.4319(6) . ? Au1 Br2 2.4555(5) . ? Au2 P2 2.2409(12) . ? Au2 Br4 2.4040(5) . ? P1 C121 1.801(5) . ? P1 C111 1.812(5) . ? P1 C1 1.828(5) . ? P2 C221 1.812(5) . ? P2 C211 1.815(5) . ? P2 C1 1.839(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C111 C112 1.383(7) . ? C111 C116 1.390(7) . ? C112 C113 1.381(7) . ? C112 H11A 0.9500 . ? C113 C114 1.390(9) . ? C113 H11B 0.9500 . ? C114 C115 1.369(8) . ? C114 H11C 0.9500 . ? C115 C116 1.394(7) . ? C115 H11D 0.9500 . ? C116 H11E 0.9500 . ? C121 C122 1.388(7) . ? C121 C126 1.397(7) . ? C122 C123 1.382(8) . ? C122 H12A 0.9500 . ? C123 C124 1.387(9) . ? C123 H12B 0.9500 . ? C124 C125 1.382(8) . ? C124 H12C 0.9500 . ? C125 C126 1.389(7) . ? C125 H12D 0.9500 . ? C126 H12E 0.9500 . ? C211 C216 1.396(7) . ? C211 C212 1.399(7) . ? C212 C213 1.392(7) . ? C212 H21A 0.9500 . ? C213 C214 1.385(8) . ? C213 H21B 0.9500 . ? C214 C215 1.388(8) . ? C214 H21C 0.9500 . ? C215 C216 1.385(7) . ? C215 H21D 0.9500 . ? C216 H21E 0.9500 . ? C221 C226 1.394(7) . ? C221 C222 1.398(7) . ? C222 C223 1.392(7) . ? C222 H22A 0.9500 . ? C223 C224 1.387(8) . ? C223 H22B 0.9500 . ? C224 C225 1.385(8) . ? C224 H22C 0.9500 . ? C225 C226 1.388(7) . ? C225 H22D 0.9500 . ? C226 H22E 0.9500 . ? C2 Cl1 1.738(8) . ? C2 Cl2 1.765(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 Cl3 1.712(11) . ? C3 Cl4 1.755(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? 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 Br3 88.00(3) . . ? P1 Au1 Br1 93.06(3) . . ? Br3 Au1 Br1 169.78(2) . . ? P1 Au1 Br2 176.38(3) . . ? Br3 Au1 Br2 89.592(19) . . ? Br1 Au1 Br2 88.83(2) . . ? P2 Au2 Br4 178.95(3) . . ? C121 P1 C111 107.3(2) . . ? C121 P1 C1 106.2(2) . . ? C111 P1 C1 104.5(2) . . ? C121 P1 Au1 106.98(16) . . ? C111 P1 Au1 116.42(17) . . ? C1 P1 Au1 114.84(17) . . ? C221 P2 C211 107.3(2) . . ? C221 P2 C1 107.7(2) . . ? C211 P2 C1 102.9(2) . . ? C221 P2 Au2 114.45(16) . . ? C211 P2 Au2 113.32(16) . . ? C1 P2 Au2 110.38(16) . . ? P1 C1 P2 113.5(3) . . ? P1 C1 H1A 108.9 . . ? P2 C1 H1A 108.9 . . ? P1 C1 H1B 108.9 . . ? P2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C112 C111 C116 120.3(5) . . ? C112 C111 P1 123.7(4) . . ? C116 C111 P1 115.8(4) . . ? C113 C112 C111 119.3(5) . . ? C113 C112 H11A 120.3 . . ? C111 C112 H11A 120.3 . . ? C112 C113 C114 120.5(5) . . ? C112 C113 H11B 119.7 . . ? C114 C113 H11B 119.7 . . ? C115 C114 C113 120.3(5) . . ? C115 C114 H11C 119.8 . . ? C113 C114 H11C 119.8 . . ? C114 C115 C116 119.6(5) . . ? C114 C115 H11D 120.2 . . ? C116 C115 H11D 120.2 . . ? C111 C116 C115 119.9(5) . . ? C111 C116 H11E 120.0 . . ? C115 C116 H11E 120.0 . . ? C122 C121 C126 119.7(5) . . ? C122 C121 P1 120.6(4) . . ? C126 C121 P1 119.7(4) . . ? C123 C122 C121 120.6(5) . . ? C123 C122 H12A 119.7 . . ? C121 C122 H12A 119.7 . . ? C122 C123 C124 119.9(5) . . ? C122 C123 H12B 120.0 . . ? C124 C123 H12B 120.0 . . ? C125 C124 C123 119.7(5) . . ? C125 C124 H12C 120.1 . . ? C123 C124 H12C 120.1 . . ? C124 C125 C126 120.9(5) . . ? C124 C125 H12D 119.6 . . ? C126 C125 H12D 119.6 . . ? C125 C126 C121 119.2(5) . . ? C125 C126 H12E 120.4 . . ? C121 C126 H12E 120.4 . . ? C216 C211 C212 119.5(5) . . ? C216 C211 P2 118.0(4) . . ? C212 C211 P2 122.5(4) . . ? C213 C212 C211 119.5(5) . . ? C213 C212 H21A 120.2 . . ? C211 C212 H21A 120.2 . . ? C214 C213 C212 120.6(5) . . ? C214 C213 H21B 119.7 . . ? C212 C213 H21B 119.7 . . ? C213 C214 C215 119.8(5) . . ? C213 C214 H21C 120.1 . . ? C215 C214 H21C 120.1 . . ? C216 C215 C214 120.1(5) . . ? C216 C215 H21D 119.9 . . ? C214 C215 H21D 119.9 . . ? C215 C216 C211 120.4(5) . . ? C215 C216 H21E 119.8 . . ? C211 C216 H21E 119.8 . . ? C226 C221 C222 119.7(4) . . ? C226 C221 P2 122.6(4) . . ? C222 C221 P2 117.7(4) . . ? C223 C222 C221 120.0(5) . . ? C223 C222 H22A 120.0 . . ? C221 C222 H22A 120.0 . . ? C224 C223 C222 119.7(5) . . ? C224 C223 H22B 120.2 . . ? C222 C223 H22B 120.2 . . ? C225 C224 C223 120.5(5) . . ? C225 C224 H22C 119.7 . . ? C223 C224 H22C 119.7 . . ? C224 C225 C226 120.0(5) . . ? C224 C225 H22D 120.0 . . ? C226 C225 H22D 120.0 . . ? C225 C226 C221 120.0(5) . . ? C225 C226 H22E 120.0 . . ? C221 C226 H22E 120.0 . . ? Cl1 C2 Cl2 111.4(4) . . ? Cl1 C2 H2A 109.3 . . ? Cl2 C2 H2A 109.3 . . ? Cl1 C2 H2B 109.3 . . ? Cl2 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? Cl3 C3 Cl4 112.5(5) . . ? Cl3 C3 H3A 109.1 . . ? Cl4 C3 H3A 109.1 . . ? Cl3 C3 H3B 109.1 . . ? Cl4 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? 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 Br3 Au1 P1 C121 -74.62(17) . . . . ? Br1 Au1 P1 C121 95.21(17) . . . . ? Br2 Au1 P1 C121 -26.3(6) . . . . ? Br3 Au1 P1 C111 45.29(17) . . . . ? Br1 Au1 P1 C111 -144.88(17) . . . . ? Br2 Au1 P1 C111 93.7(5) . . . . ? Br3 Au1 P1 C1 167.84(17) . . . . ? Br1 Au1 P1 C1 -22.33(17) . . . . ? Br2 Au1 P1 C1 -143.8(5) . . . . ? Br4 Au2 P2 C221 62.8(19) . . . . ? Br4 Au2 P2 C211 -174(24) . . . . ? Br4 Au2 P2 C1 -58.9(19) . . . . ? C121 P1 C1 P2 168.0(3) . . . . ? C111 P1 C1 P2 54.7(3) . . . . ? Au1 P1 C1 P2 -74.0(3) . . . . ? C221 P2 C1 P1 -87.8(3) . . . . ? C211 P2 C1 P1 159.0(3) . . . . ? Au2 P2 C1 P1 37.8(3) . . . . ? C121 P1 C111 C112 137.7(4) . . . . ? C1 P1 C111 C112 -109.9(4) . . . . ? Au1 P1 C111 C112 17.9(5) . . . . ? C121 P1 C111 C116 -47.5(4) . . . . ? C1 P1 C111 C116 65.0(4) . . . . ? Au1 P1 C111 C116 -167.2(3) . . . . ? C116 C111 C112 C113 2.0(7) . . . . ? P1 C111 C112 C113 176.7(4) . . . . ? C111 C112 C113 C114 -1.0(8) . . . . ? C112 C113 C114 C115 -0.3(8) . . . . ? C113 C114 C115 C116 0.5(8) . . . . ? C112 C111 C116 C115 -1.8(7) . . . . ? P1 C111 C116 C115 -176.9(4) . . . . ? C114 C115 C116 C111 0.6(8) . . . . ? C111 P1 C121 C122 148.6(4) . . . . ? C1 P1 C121 C122 37.3(5) . . . . ? Au1 P1 C121 C122 -85.8(4) . . . . ? C111 P1 C121 C126 -33.6(5) . . . . ? C1 P1 C121 C126 -144.9(4) . . . . ? Au1 P1 C121 C126 92.0(4) . . . . ? C126 C121 C122 C123 -0.1(8) . . . . ? P1 C121 C122 C123 177.7(4) . . . . ? C121 C122 C123 C124 0.4(8) . . . . ? C122 C123 C124 C125 -0.4(8) . . . . ? C123 C124 C125 C126 0.1(8) . . . . ? C124 C125 C126 C121 0.1(8) . . . . ? C122 C121 C126 C125 -0.1(7) . . . . ? P1 C121 C126 C125 -177.9(4) . . . . ? C221 P2 C211 C216 166.9(4) . . . . ? C1 P2 C211 C216 -79.6(4) . . . . ? Au2 P2 C211 C216 39.6(4) . . . . ? C221 P2 C211 C212 -10.8(5) . . . . ? C1 P2 C211 C212 102.7(5) . . . . ? Au2 P2 C211 C212 -138.1(4) . . . . ? C216 C211 C212 C213 0.2(8) . . . . ? P2 C211 C212 C213 177.9(4) . . . . ? C211 C212 C213 C214 -0.5(9) . . . . ? C212 C213 C214 C215 0.3(9) . . . . ? C213 C214 C215 C216 0.2(9) . . . . ? C214 C215 C216 C211 -0.4(8) . . . . ? C212 C211 C216 C215 0.2(8) . . . . ? P2 C211 C216 C215 -177.6(4) . . . . ? C211 P2 C221 C226 69.6(4) . . . . ? C1 P2 C221 C226 -40.6(5) . . . . ? Au2 P2 C221 C226 -163.8(4) . . . . ? C211 P2 C221 C222 -108.2(4) . . . . ? C1 P2 C221 C222 141.6(4) . . . . ? Au2 P2 C221 C222 18.4(4) . . . . ? C226 C221 C222 C223 -0.8(8) . . . . ? P2 C221 C222 C223 177.0(4) . . . . ? C221 C222 C223 C224 0.0(8) . . . . ? C222 C223 C224 C225 0.6(8) . . . . ? C223 C224 C225 C226 -0.3(8) . . . . ? C224 C225 C226 C221 -0.6(8) . . . . ? C222 C221 C226 C225 1.2(7) . . . . ? P2 C221 C226 C225 -176.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.49 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.064 _refine_diff_density_min -1.094 _refine_diff_density_rms 0.143 #===END data_[[(dppbe)AuI2]+I3-] _database_code_depnum_ccdc_archive 'CCDC 232539' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[[(dppbe)AuI2]+I3-]' _chemical_formula_sum 'C30 H24 Au I5 P2' _chemical_formula_weight 1277.90 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' I I -0.4742 1.8119 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.80500(1) _cell_length_b 14.3361(2) _cell_length_c 24.5570(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.442(1) _cell_angle_gamma 90.00 _cell_volume 3383.27(7) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 76016 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 9.024 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_absorpt_correction_T_min 0.5320 _exptl_absorpt_correction_T_max 0.8540 _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 76016 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 25.43 _reflns_number_total 6208 _reflns_number_gt 6092 _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^)+(0.0340P)^2^+19.9189P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _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 6208 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.161 _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 0.03079(2) 0.191583(15) 0.159362(9) 0.01630(7) Uani 1 1 d . . . I1 I -0.09642(4) 0.03765(3) 0.118423(18) 0.02827(11) Uani 1 1 d . . . I4 I -0.35577(4) -0.37382(3) 0.093348(15) 0.02104(10) Uani 1 1 d . . . I5 I -0.38492(5) -0.57809(3) 0.089367(18) 0.03077(11) Uani 1 1 d . . . I3 I -0.33118(5) -0.17355(3) 0.096687(19) 0.03027(11) Uani 1 1 d . . . I2 I -0.02706(5) 0.15478(3) 0.257774(17) 0.02921(11) Uani 1 1 d . . . P1 P 0.15374(15) 0.32551(10) 0.19297(6) 0.0166(3) Uani 1 1 d . . . P2 P 0.08970(15) 0.22889(10) 0.07443(6) 0.0158(3) Uani 1 1 d . . . C11 C 0.2393(6) 0.1642(4) 0.0645(2) 0.0185(11) Uani 1 1 d . . . C32 C 0.1674(6) 0.3927(4) 0.1321(2) 0.0191(12) Uani 1 1 d . . . C21 C -0.0484(6) 0.2176(4) 0.0145(2) 0.0176(11) Uani 1 1 d . . . C41 C 0.3262(6) 0.2935(4) 0.2279(2) 0.0191(12) Uani 1 1 d . . . C51 C 0.0725(6) 0.4006(4) 0.2355(2) 0.0217(12) Uani 1 1 d . . . C31 C 0.1379(6) 0.3507(4) 0.0796(2) 0.0165(11) Uani 1 1 d . . . C23 C -0.2873(7) 0.2428(5) -0.0279(3) 0.0269(14) Uani 1 1 d . . . H23 H -0.3781 0.2632 -0.0254 0.032 Uiso 1 1 calc R . . C12 C 0.2271(6) 0.0706(4) 0.0483(2) 0.0217(12) Uani 1 1 d . . . H12 H 0.1384 0.0414 0.0400 0.026 Uiso 1 1 calc R . . C16 C 0.3708(6) 0.2071(4) 0.0760(3) 0.0232(13) Uani 1 1 d . . . H16 H 0.3793 0.2711 0.0863 0.028 Uiso 1 1 calc R . . C26 C -0.0210(7) 0.1848(5) -0.0361(3) 0.0248(13) Uani 1 1 d . . . H26 H 0.0700 0.1652 -0.0388 0.030 Uiso 1 1 calc R . . C13 C 0.3473(7) 0.0205(4) 0.0446(3) 0.0258(13) Uani 1 1 d . . . H13 H 0.3402 -0.0431 0.0334 0.031 Uiso 1 1 calc R . . C24 C -0.2613(7) 0.2097(5) -0.0777(3) 0.0261(13) Uani 1 1 d . . . H24 H -0.3350 0.2064 -0.1093 0.031 Uiso 1 1 calc R . . C25 C -0.1294(7) 0.1814(5) -0.0821(3) 0.0280(14) Uani 1 1 d . . . H25 H -0.1127 0.1595 -0.1166 0.034 Uiso 1 1 calc R . . C15 C 0.4881(6) 0.1553(5) 0.0723(3) 0.0251(13) Uani 1 1 d . . . H15 H 0.5774 0.1837 0.0803 0.030 Uiso 1 1 calc R . . C14 C 0.4753(6) 0.0626(5) 0.0568(3) 0.0253(13) Uani 1 1 d . . . H14 H 0.5562 0.0275 0.0547 0.030 Uiso 1 1 calc R . . C22 C -0.1806(6) 0.2462(4) 0.0185(3) 0.0215(12) Uani 1 1 d . . . H22 H -0.1983 0.2681 0.0529 0.026 Uiso 1 1 calc R . . C35 C 0.1979(7) 0.4934(5) 0.0384(3) 0.0304(15) Uani 1 1 d . . . H35 H 0.2092 0.5280 0.0066 0.037 Uiso 1 1 calc R . . C33 C 0.2109(7) 0.4860(5) 0.1373(3) 0.0298(14) Uani 1 1 d . . . H33 H 0.2302 0.5152 0.1728 0.036 Uiso 1 1 calc R . . C34 C 0.2255(8) 0.5349(5) 0.0901(3) 0.0336(16) Uani 1 1 d . . . H34 H 0.2550 0.5982 0.0933 0.040 Uiso 1 1 calc R . . C44 C 0.5918(7) 0.2363(6) 0.2776(3) 0.0357(17) Uani 1 1 d . . . H44 H 0.6828 0.2162 0.2944 0.043 Uiso 1 1 calc R . . C36 C 0.1539(7) 0.4017(5) 0.0326(3) 0.0254(13) Uani 1 1 d . . . H36 H 0.1346 0.3734 -0.0031 0.030 Uiso 1 1 calc R . . C52 C 0.1526(7) 0.4494(5) 0.2804(3) 0.0291(14) Uani 1 1 d . . . H52 H 0.2499 0.4389 0.2911 0.035 Uiso 1 1 calc R . . C56 C -0.0695(7) 0.4166(5) 0.2204(3) 0.0318(15) Uani 1 1 d . . . H56 H -0.1231 0.3840 0.1898 0.038 Uiso 1 1 calc R . . C53 C 0.0867(9) 0.5126(5) 0.3083(3) 0.0383(17) Uani 1 1 d . . . H53 H 0.1398 0.5474 0.3381 0.046 Uiso 1 1 calc R . . C42 C 0.4404(7) 0.3222(5) 0.2064(3) 0.0321(15) Uani 1 1 d . . . H42 H 0.4277 0.3614 0.1746 0.039 Uiso 1 1 calc R . . C46 C 0.3457(7) 0.2381(5) 0.2746(3) 0.0321(15) Uani 1 1 d . . . H46 H 0.2681 0.2202 0.2900 0.038 Uiso 1 1 calc R . . C55 C -0.1325(8) 0.4789(5) 0.2493(3) 0.0364(16) Uani 1 1 d . . . H55 H -0.2297 0.4896 0.2385 0.044 Uiso 1 1 calc R . . C54 C -0.0565(8) 0.5265(5) 0.2939(3) 0.0353(16) Uani 1 1 d . . . H54 H -0.1013 0.5684 0.3146 0.042 Uiso 1 1 calc R . . C45 C 0.4795(7) 0.2080(6) 0.2996(3) 0.0377(17) Uani 1 1 d . . . H45 H 0.4927 0.1686 0.3313 0.045 Uiso 1 1 calc R . . C43 C 0.5735(7) 0.2930(6) 0.2319(3) 0.0367(17) Uani 1 1 d . . . H43 H 0.6518 0.3126 0.2174 0.044 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 0.01612(12) 0.01596(12) 0.01735(12) -0.00060(8) 0.00461(9) -0.00201(8) I1 0.0299(2) 0.0214(2) 0.0353(2) -0.00681(16) 0.01067(18) -0.00990(17) I4 0.02119(19) 0.0220(2) 0.01974(19) -0.00081(14) 0.00354(14) -0.00089(15) I5 0.0344(2) 0.0233(2) 0.0370(2) -0.00257(17) 0.01273(19) -0.00264(18) I3 0.0272(2) 0.0229(2) 0.0389(2) 0.00373(17) 0.00233(18) -0.00229(17) I2 0.0327(2) 0.0341(2) 0.0232(2) 0.00303(17) 0.01116(17) -0.00788(18) P1 0.0176(7) 0.0165(7) 0.0154(7) -0.0021(5) 0.0028(5) -0.0026(6) P2 0.0165(7) 0.0177(7) 0.0138(7) -0.0013(5) 0.0046(5) -0.0005(6) C11 0.020(3) 0.020(3) 0.015(3) 0.000(2) 0.005(2) 0.001(2) C32 0.018(3) 0.019(3) 0.021(3) 0.000(2) 0.004(2) -0.002(2) C21 0.018(3) 0.016(3) 0.018(3) 0.000(2) 0.003(2) -0.002(2) C41 0.015(3) 0.023(3) 0.018(3) -0.004(2) -0.002(2) 0.002(2) C51 0.027(3) 0.019(3) 0.019(3) -0.001(2) 0.005(2) 0.000(2) C31 0.018(3) 0.013(3) 0.019(3) 0.002(2) 0.007(2) 0.005(2) C23 0.020(3) 0.027(3) 0.032(3) 0.004(3) 0.001(3) 0.004(3) C12 0.021(3) 0.021(3) 0.023(3) -0.001(2) 0.006(2) -0.001(2) C16 0.022(3) 0.019(3) 0.029(3) -0.001(2) 0.007(3) 0.001(2) C26 0.022(3) 0.032(4) 0.020(3) -0.004(2) 0.004(2) 0.005(3) C13 0.033(3) 0.022(3) 0.024(3) 0.000(2) 0.011(3) 0.005(3) C24 0.028(3) 0.025(3) 0.021(3) 0.003(2) -0.007(3) -0.004(3) C25 0.033(4) 0.029(3) 0.020(3) -0.004(2) 0.001(3) -0.002(3) C15 0.015(3) 0.031(3) 0.030(3) 0.002(3) 0.006(2) 0.001(3) C14 0.022(3) 0.029(3) 0.026(3) 0.006(3) 0.009(2) 0.010(3) C22 0.020(3) 0.021(3) 0.024(3) 0.001(2) 0.006(2) 0.001(2) C35 0.037(4) 0.022(3) 0.035(4) 0.009(3) 0.016(3) 0.006(3) C33 0.043(4) 0.019(3) 0.029(3) -0.005(3) 0.011(3) -0.008(3) C34 0.046(4) 0.016(3) 0.041(4) 0.003(3) 0.015(3) -0.006(3) C44 0.023(3) 0.054(5) 0.028(4) -0.004(3) -0.001(3) 0.007(3) C36 0.028(3) 0.029(3) 0.021(3) 0.003(2) 0.010(3) -0.002(3) C52 0.027(3) 0.036(4) 0.023(3) -0.001(3) 0.004(3) 0.002(3) C56 0.028(3) 0.034(4) 0.032(4) -0.010(3) 0.002(3) -0.002(3) C53 0.054(5) 0.039(4) 0.020(3) -0.012(3) 0.003(3) 0.004(4) C42 0.024(3) 0.044(4) 0.028(4) 0.006(3) 0.004(3) -0.004(3) C46 0.025(3) 0.045(4) 0.027(3) 0.007(3) 0.007(3) 0.003(3) C55 0.031(4) 0.033(4) 0.046(4) -0.006(3) 0.011(3) 0.006(3) C54 0.040(4) 0.031(4) 0.039(4) -0.005(3) 0.018(3) 0.003(3) C45 0.029(4) 0.052(5) 0.029(4) 0.011(3) -0.002(3) 0.009(3) C43 0.017(3) 0.056(5) 0.036(4) 0.001(3) 0.002(3) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.3293(15) . ? Au1 P2 2.3340(14) . ? Au1 I1 2.6342(4) . ? Au1 I2 2.6428(4) . ? I4 I3 2.8811(6) . ? I4 I5 2.9420(6) . ? P1 C51 1.793(6) . ? P1 C41 1.797(6) . ? P1 C32 1.807(6) . ? P2 C11 1.793(6) . ? P2 C21 1.799(6) . ? P2 C31 1.807(6) . ? C11 C12 1.397(8) . ? C11 C16 1.406(9) . ? C32 C31 1.400(8) . ? C32 C33 1.401(9) . ? C21 C22 1.382(8) . ? C21 C26 1.402(8) . ? C41 C46 1.377(9) . ? C41 C42 1.391(9) . ? C51 C56 1.387(9) . ? C51 C52 1.406(9) . ? C31 C36 1.400(8) . ? C23 C24 1.383(10) . ? C23 C22 1.386(9) . ? C23 H23 0.9500 . ? C12 C13 1.399(9) . ? C12 H12 0.9500 . ? C16 C15 1.388(9) . ? C16 H16 0.9500 . ? C26 C25 1.390(9) . ? C26 H26 0.9500 . ? C13 C14 1.371(9) . ? C13 H13 0.9500 . ? C24 C25 1.380(10) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C15 C14 1.382(9) . ? C15 H15 0.9500 . ? C14 H14 0.9500 . ? C22 H22 0.9500 . ? C35 C34 1.378(10) . ? C35 C36 1.383(10) . ? C35 H35 0.9500 . ? C33 C34 1.388(9) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C44 C43 1.370(11) . ? C44 C45 1.380(10) . ? C44 H44 0.9500 . ? C36 H36 0.9500 . ? C52 C53 1.373(10) . ? C52 H52 0.9500 . ? C56 C55 1.362(10) . ? C56 H56 0.9500 . ? C53 C54 1.393(11) . ? C53 H53 0.9500 . ? C42 C43 1.395(10) . ? C42 H42 0.9500 . ? C46 C45 1.402(10) . ? C46 H46 0.9500 . ? C55 C54 1.378(11) . ? C55 H55 0.9500 . ? C54 H54 0.9500 . ? C45 H45 0.9500 . ? C43 H43 0.9500 . ? 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 P2 85.71(5) . . ? P1 Au1 I1 176.68(4) . . ? P2 Au1 I1 91.91(4) . . ? P1 Au1 I2 91.75(4) . . ? P2 Au1 I2 177.36(4) . . ? I1 Au1 I2 90.600(15) . . ? I3 I4 I5 179.23(2) . . ? C51 P1 C41 111.1(3) . . ? C51 P1 C32 106.0(3) . . ? C41 P1 C32 108.3(3) . . ? C51 P1 Au1 116.3(2) . . ? C41 P1 Au1 109.3(2) . . ? C32 P1 Au1 105.3(2) . . ? C11 P2 C21 110.2(3) . . ? C11 P2 C31 107.5(3) . . ? C21 P2 C31 106.8(3) . . ? C11 P2 Au1 110.95(19) . . ? C21 P2 Au1 115.55(19) . . ? C31 P2 Au1 105.47(18) . . ? C12 C11 C16 120.1(5) . . ? C12 C11 P2 120.6(5) . . ? C16 C11 P2 119.2(5) . . ? C31 C32 C33 120.0(6) . . ? C31 C32 P1 119.8(4) . . ? C33 C32 P1 120.2(5) . . ? C22 C21 C26 120.7(6) . . ? C22 C21 P2 118.6(4) . . ? C26 C21 P2 120.6(5) . . ? C46 C41 C42 119.8(6) . . ? C46 C41 P1 120.5(5) . . ? C42 C41 P1 119.7(5) . . ? C56 C51 C52 120.2(6) . . ? C56 C51 P1 118.8(5) . . ? C52 C51 P1 120.8(5) . . ? C36 C31 C32 119.8(6) . . ? C36 C31 P2 121.2(5) . . ? C32 C31 P2 118.9(4) . . ? C24 C23 C22 119.8(6) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C11 C12 C13 119.1(6) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? C15 C16 C11 119.4(6) . . ? C15 C16 H16 120.3 . . ? C11 C16 H16 120.3 . . ? C25 C26 C21 118.7(6) . . ? C25 C26 H26 120.6 . . ? C21 C26 H26 120.6 . . ? C14 C13 C12 120.4(6) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C25 C24 C23 120.6(6) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 120.3(6) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C14 C15 C16 120.1(6) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C13 C14 C15 120.9(6) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C21 C22 C23 119.8(6) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C34 C35 C36 120.4(6) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C34 C33 C32 119.0(6) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C35 C34 C33 121.1(6) . . ? C35 C34 H34 119.4 . . ? C33 C34 H34 119.4 . . ? C43 C44 C45 120.7(6) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C35 C36 C31 119.7(6) . . ? C35 C36 H36 120.2 . . ? C31 C36 H36 120.2 . . ? C53 C52 C51 118.4(6) . . ? C53 C52 H52 120.8 . . ? C51 C52 H52 120.8 . . ? C55 C56 C51 120.2(6) . . ? C55 C56 H56 119.9 . . ? C51 C56 H56 119.9 . . ? C52 C53 C54 121.2(7) . . ? C52 C53 H53 119.4 . . ? C54 C53 H53 119.4 . . ? C41 C42 C43 119.6(6) . . ? C41 C42 H42 120.2 . . ? C43 C42 H42 120.2 . . ? C41 C46 C45 120.4(6) . . ? C41 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C56 C55 C54 120.6(7) . . ? C56 C55 H55 119.7 . . ? C54 C55 H55 119.7 . . ? C55 C54 C53 119.4(6) . . ? C55 C54 H54 120.3 . . ? C53 C54 H54 120.3 . . ? C44 C45 C46 119.3(7) . . ? C44 C45 H45 120.4 . . ? C46 C45 H45 120.4 . . ? C44 C43 C42 120.3(7) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Au1 P1 C51 135.1(2) . . . . ? I1 Au1 P1 C51 179(95) . . . . ? I2 Au1 P1 C51 -45.6(2) . . . . ? P2 Au1 P1 C41 -98.2(2) . . . . ? I1 Au1 P1 C41 -53.9(7) . . . . ? I2 Au1 P1 C41 81.1(2) . . . . ? P2 Au1 P1 C32 18.0(2) . . . . ? I1 Au1 P1 C32 62.3(7) . . . . ? I2 Au1 P1 C32 -162.7(2) . . . . ? P1 Au1 P2 C11 97.5(2) . . . . ? I1 Au1 P2 C11 -80.2(2) . . . . ? I2 Au1 P2 C11 82.1(9) . . . . ? P1 Au1 P2 C21 -136.2(2) . . . . ? I1 Au1 P2 C21 46.1(2) . . . . ? I2 Au1 P2 C21 -151.6(8) . . . . ? P1 Au1 P2 C31 -18.55(19) . . . . ? I1 Au1 P2 C31 163.77(19) . . . . ? I2 Au1 P2 C31 -34.0(9) . . . . ? C21 P2 C11 C12 -51.5(5) . . . . ? C31 P2 C11 C12 -167.4(5) . . . . ? Au1 P2 C11 C12 77.7(5) . . . . ? C21 P2 C11 C16 132.0(5) . . . . ? C31 P2 C11 C16 16.0(5) . . . . ? Au1 P2 C11 C16 -98.8(5) . . . . ? C51 P1 C32 C31 -138.3(5) . . . . ? C41 P1 C32 C31 102.4(5) . . . . ? Au1 P1 C32 C31 -14.4(5) . . . . ? C51 P1 C32 C33 43.4(6) . . . . ? C41 P1 C32 C33 -75.9(6) . . . . ? Au1 P1 C32 C33 167.2(5) . . . . ? C11 P2 C21 C22 166.9(5) . . . . ? C31 P2 C21 C22 -76.7(5) . . . . ? Au1 P2 C21 C22 40.2(5) . . . . ? C11 P2 C21 C26 -16.2(6) . . . . ? C31 P2 C21 C26 100.2(5) . . . . ? Au1 P2 C21 C26 -142.9(5) . . . . ? C51 P1 C41 C46 66.8(6) . . . . ? C32 P1 C41 C46 -177.1(5) . . . . ? Au1 P1 C41 C46 -62.8(6) . . . . ? C51 P1 C41 C42 -115.6(5) . . . . ? C32 P1 C41 C42 0.5(6) . . . . ? Au1 P1 C41 C42 114.8(5) . . . . ? C41 P1 C51 C56 -166.8(5) . . . . ? C32 P1 C51 C56 75.7(6) . . . . ? Au1 P1 C51 C56 -40.9(6) . . . . ? C41 P1 C51 C52 19.1(6) . . . . ? C32 P1 C51 C52 -98.4(5) . . . . ? Au1 P1 C51 C52 144.9(5) . . . . ? C33 C32 C31 C36 0.9(9) . . . . ? P1 C32 C31 C36 -177.4(5) . . . . ? C33 C32 C31 P2 177.2(5) . . . . ? P1 C32 C31 P2 -1.2(7) . . . . ? C11 P2 C31 C36 73.9(5) . . . . ? C21 P2 C31 C36 -44.2(6) . . . . ? Au1 P2 C31 C36 -167.6(4) . . . . ? C11 P2 C31 C32 -102.3(5) . . . . ? C21 P2 C31 C32 139.6(5) . . . . ? Au1 P2 C31 C32 16.1(5) . . . . ? C16 C11 C12 C13 0.8(9) . . . . ? P2 C11 C12 C13 -175.7(5) . . . . ? C12 C11 C16 C15 -1.2(9) . . . . ? P2 C11 C16 C15 175.4(5) . . . . ? C22 C21 C26 C25 -0.1(9) . . . . ? P2 C21 C26 C25 -176.9(5) . . . . ? C11 C12 C13 C14 0.3(9) . . . . ? C22 C23 C24 C25 -1.1(10) . . . . ? C23 C24 C25 C26 0.8(10) . . . . ? C21 C26 C25 C24 -0.2(10) . . . . ? C11 C16 C15 C14 0.5(9) . . . . ? C12 C13 C14 C15 -1.0(9) . . . . ? C16 C15 C14 C13 0.6(10) . . . . ? C26 C21 C22 C23 -0.2(9) . . . . ? P2 C21 C22 C23 176.6(5) . . . . ? C24 C23 C22 C21 0.8(10) . . . . ? C31 C32 C33 C34 -0.7(10) . . . . ? P1 C32 C33 C34 177.6(5) . . . . ? C36 C35 C34 C33 0.5(11) . . . . ? C32 C33 C34 C35 0.0(11) . . . . ? C34 C35 C36 C31 -0.3(10) . . . . ? C32 C31 C36 C35 -0.4(9) . . . . ? P2 C31 C36 C35 -176.6(5) . . . . ? C56 C51 C52 C53 -0.1(10) . . . . ? P1 C51 C52 C53 174.0(5) . . . . ? C52 C51 C56 C55 -0.7(10) . . . . ? P1 C51 C56 C55 -174.8(6) . . . . ? C51 C52 C53 C54 1.8(11) . . . . ? C46 C41 C42 C43 1.2(11) . . . . ? P1 C41 C42 C43 -176.5(6) . . . . ? C42 C41 C46 C45 -2.1(11) . . . . ? P1 C41 C46 C45 175.6(6) . . . . ? C51 C56 C55 C54 -0.3(12) . . . . ? C56 C55 C54 C53 2.0(12) . . . . ? C52 C53 C54 C55 -2.8(12) . . . . ? C43 C44 C45 C46 -0.1(12) . . . . ? C41 C46 C45 C44 1.5(12) . . . . ? C45 C44 C43 C42 -0.7(12) . . . . ? C41 C42 C43 C44 0.2(12) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.43 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.338 _refine_diff_density_min -1.469 _refine_diff_density_rms 0.170