# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1264 data_phpcf2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety PhP(CF=CF2)2 _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C10 H5 F6 P' _chemical_formula_weight 270.11 _chemical_melting_point ? _chemical_compound_source ? 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' 'F' 'F' 0.0171 0.0103 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.486(2) _cell_length_b 26.719(7) _cell_length_c 10.717(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.22(3) _cell_angle_gamma 90.00 _cell_volume 2143.5(9) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 44 _cell_measurement_theta_min 15 _cell_measurement_theta_max 16 _exptl_crystal_description cylinder _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method ? _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.312 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 ; Stoe Stadi-4 diffractometer with Oxford Cryosystems variable temperature device. ; _diffrn_measurement_method 'Omega-theta with learnt-profile (Clegg)' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 8581 _diffrn_reflns_av_R_equivalents 0.0601 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3768 _reflns_number_observed 2664 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution SHELXTL _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 16 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+1.0490P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens 'Calculated positions' _refine_ls_hydrogen_treatment Riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3752 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_obs 0.0419 _refine_ls_wR_factor_all 0.1048 _refine_ls_wR_factor_obs 0.0899 _refine_ls_goodness_of_fit_all 1.020 _refine_ls_goodness_of_fit_obs 1.057 _refine_ls_restrained_S_all 1.035 _refine_ls_restrained_S_obs 1.057 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group P1 P 0.49532(10) 0.59168(3) 0.90051(7) 0.0265(2) Uani 1 d . . C1 C 0.4143(4) 0.65491(11) 0.9334(3) 0.0239(6) Uani 1 d . . C2 C 0.2965(4) 0.67978(12) 0.8536(3) 0.0313(7) Uani 1 d . . H2 H 0.2630(4) 0.66477(12) 0.7767(3) 0.038 Uiso 1 calc R . C3 C 0.2282(4) 0.72587(13) 0.8853(3) 0.0370(8) Uani 1 d . . H3 H 0.1491(4) 0.74254(13) 0.8296(3) 0.044 Uiso 1 calc R . C4 C 0.2738(4) 0.74806(12) 0.9971(3) 0.0335(7) Uani 1 d . . H4 H 0.2276(4) 0.78007(12) 1.0181(3) 0.040 Uiso 1 calc R . C5 C 0.3876(4) 0.72323(12) 1.0784(3) 0.0296(7) Uani 1 d . . H5 H 0.4165(4) 0.73798(12) 1.1566(3) 0.036 Uiso 1 calc R . C6 C 0.4596(4) 0.67719(11) 1.0472(3) 0.0262(6) Uani 1 d . . H6 H 0.5394(4) 0.66081(11) 1.1029(3) 0.031 Uiso 1 calc R . C1A C 0.7306(4) 0.59952(11) 0.9341(3) 0.0263(6) Uani 1 d . . F1A F 0.8198(2) 0.64029(7) 0.8928(2) 0.0365(4) Uani 1 d . . C2A C 0.8267(4) 0.56636(12) 0.9959(3) 0.0334(7) Uani 1 d . . F2A F 1.0002(2) 0.57051(8) 1.0165(2) 0.0484(5) Uani 1 d . . F3A F 0.7644(3) 0.52473(7) 1.0434(2) 0.0469(5) Uani 1 d . . C1B C 0.5067(4) 0.59309(12) 0.7322(3) 0.0294(7) Uani 1 d . . F1B F 0.5962(3) 0.63013(7) 0.6717(2) 0.0428(5) Uani 1 d . . C2B C 0.4324(4) 0.55930(13) 0.6595(3) 0.0361(8) Uani 1 d . . F2B F 0.4420(3) 0.55946(8) 0.5364(2) 0.0525(6) Uani 1 d . . F3B F 0.3381(3) 0.52106(8) 0.6992(2) 0.0554(6) Uani 1 d . . P1' P 0.99438(10) 0.59352(3) 0.33920(7) 0.0253(2) Uani 1 d . . C1' C 0.9124(4) 0.65643(11) 0.3027(2) 0.0240(6) Uani 1 d . . C2' C 0.9568(4) 0.67807(11) 0.1891(3) 0.0266(6) Uani 1 d . . H2' H 1.0350(4) 0.66110(11) 0.1338(3) 0.032 Uiso 1 calc R . C3' C 0.8878(4) 0.72410(13) 0.1565(3) 0.0322(7) Uani 1 d . . H3' H 0.9183(4) 0.73854(13) 0.0784(3) 0.039 Uiso 1 calc R . C4' C 0.7743(4) 0.74956(12) 0.2363(3) 0.0336(7) Uani 1 d . . H4' H 0.7293(4) 0.78166(12) 0.2147(3) 0.040 Uiso 1 calc R . C5' C 0.7278(4) 0.72730(13) 0.3484(3) 0.0367(8) Uani 1 d . . H5' H 0.6482(4) 0.74414(13) 0.4030(3) 0.044 Uiso 1 calc R . C6' C 0.7947(4) 0.68136(12) 0.3820(3) 0.0323(7) Uani 1 d . . H6' H 0.7609(4) 0.66659(12) 0.4590(3) 0.039 Uiso 1 calc R . C1A' C 1.0061(4) 0.59612(11) 0.5075(3) 0.0260(6) Uani 1 d . . F1A' F 1.1001(2) 0.63332(7) 0.5659(2) 0.0397(5) Uani 1 d . . C2A' C 0.9337(4) 0.56312(12) 0.5816(3) 0.0310(7) Uani 1 d . . F2A' F 0.9462(3) 0.56359(8) 0.7043(2) 0.0441(5) Uani 1 d . . F3A' F 0.8367(2) 0.52469(7) 0.5440(2) 0.0421(5) Uani 1 d . . C1B' C 1.2296(4) 0.60199(11) 0.3071(3) 0.0273(7) Uani 1 d . . F1B' F 1.3151(2) 0.64408(7) 0.3440(2) 0.0364(4) Uani 1 d . . C2B' C 1.3287(4) 0.56877(12) 0.2486(3) 0.0315(7) Uani 1 d . . F2B' F 1.5008(2) 0.57400(7) 0.2268(2) 0.0454(5) Uani 1 d . . F3B' F 1.2701(3) 0.52595(7) 0.2054(2) 0.0443(5) Uani 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 P1 0.0283(4) 0.0248(4) 0.0264(4) 0.0014(3) -0.0026(3) -0.0009(3) C1 0.0188(14) 0.027(2) 0.0262(14) 0.0029(12) 0.0019(11) -0.0007(12) C2 0.028(2) 0.037(2) 0.029(2) 0.0017(13) -0.0057(12) 0.0048(14) C3 0.030(2) 0.043(2) 0.038(2) 0.011(2) -0.0015(14) 0.0113(15) C4 0.030(2) 0.031(2) 0.040(2) 0.0021(14) 0.0096(14) 0.0048(13) C5 0.023(2) 0.034(2) 0.031(2) -0.0006(13) 0.0040(12) -0.0001(13) C6 0.0221(15) 0.031(2) 0.0251(15) 0.0047(12) -0.0004(11) -0.0004(12) C1A 0.028(2) 0.026(2) 0.0251(14) -0.0053(12) -0.0006(12) 0.0029(13) F1A 0.0283(9) 0.0360(11) 0.0451(10) 0.0021(8) -0.0037(8) -0.0032(8) C2A 0.040(2) 0.032(2) 0.028(2) -0.0082(14) -0.0023(13) 0.0106(15) F2A 0.0351(11) 0.0599(14) 0.0499(12) -0.0091(10) -0.0156(8) 0.0204(10) F3A 0.0626(13) 0.0377(12) 0.0402(11) 0.0079(9) -0.0065(9) 0.0149(10) C1B 0.029(2) 0.028(2) 0.031(2) 0.0004(13) -0.0031(12) 0.0015(13) F1B 0.0511(12) 0.0502(13) 0.0271(9) 0.0009(8) 0.0005(8) -0.0131(10) C2B 0.036(2) 0.037(2) 0.035(2) -0.0030(14) -0.0116(14) 0.007(2) F2B 0.0675(14) 0.0560(14) 0.0337(11) -0.0133(9) -0.0203(9) 0.0156(11) F3B 0.0659(14) 0.0362(12) 0.0638(14) -0.0038(10) -0.0278(11) -0.0115(10) P1' 0.0275(4) 0.0252(4) 0.0232(4) -0.0021(3) 0.0002(3) -0.0020(3) C1' 0.0205(14) 0.028(2) 0.0230(14) -0.0032(12) -0.0031(11) -0.0006(12) C2' 0.0225(15) 0.032(2) 0.0256(15) -0.0015(12) -0.0019(11) 0.0016(13) C3' 0.026(2) 0.040(2) 0.031(2) 0.0016(14) -0.0050(12) -0.0012(14) C4' 0.028(2) 0.030(2) 0.042(2) -0.0019(14) -0.0102(14) 0.0065(13) C5' 0.030(2) 0.047(2) 0.033(2) -0.0113(15) 0.0001(13) 0.013(2) C6' 0.029(2) 0.038(2) 0.029(2) 0.0000(14) 0.0005(12) 0.0034(14) C1A' 0.0279(15) 0.024(2) 0.0266(15) -0.0044(12) -0.0001(12) -0.0009(13) F1A' 0.0527(12) 0.0388(11) 0.0275(9) -0.0022(8) -0.0071(8) -0.0142(9) C2A' 0.033(2) 0.031(2) 0.029(2) 0.0009(13) 0.0045(13) 0.0035(14) F2A' 0.0561(12) 0.0496(13) 0.0265(10) 0.0066(8) 0.0080(8) 0.0062(10) F3A' 0.0429(11) 0.0358(11) 0.0476(11) 0.0033(9) 0.0103(9) -0.0100(9) C1B' 0.031(2) 0.027(2) 0.0239(15) 0.0034(12) -0.0008(12) -0.0001(13) F1B' 0.0291(9) 0.0344(10) 0.0458(11) -0.0030(8) 0.0026(8) -0.0047(8) C2B' 0.036(2) 0.027(2) 0.031(2) 0.0082(13) 0.0048(13) 0.0071(14) F2B' 0.0348(10) 0.0499(13) 0.0517(12) 0.0107(9) 0.0148(9) 0.0159(9) F3B' 0.0591(13) 0.0318(11) 0.0421(11) -0.0037(9) 0.0091(9) 0.0109(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 P1 C1B 1.807(3) . ? P1 C1A 1.809(3) . ? P1 C1 1.830(3) . ? C1 C2 1.394(4) . ? C1 C6 1.398(4) . ? C2 C3 1.376(5) . ? C3 C4 1.378(5) . ? C4 C5 1.386(4) . ? C5 C6 1.385(4) . ? C1A C2A 1.318(4) . ? C1A F1A 1.353(3) . ? C2A F3A 1.310(4) . ? C2A F2A 1.321(4) . ? C1B C2B 1.314(4) . ? C1B F1B 1.361(4) . ? C2B F3B 1.314(4) . ? C2B F2B 1.321(4) . ? P1' C1A' 1.807(3) . ? P1' C1B' 1.809(3) . ? P1' C1' 1.831(3) . ? C1' C2' 1.389(4) . ? C1' C6' 1.396(4) . ? C2' C3' 1.379(4) . ? C3' C4' 1.386(4) . ? C4' C5' 1.386(5) . ? C5' C6' 1.373(5) . ? C1A' C2A' 1.305(4) . ? C1A' F1A' 1.368(3) . ? C2A' F2A' 1.318(3) . ? C2A' F3A' 1.319(4) . ? C1B' C2B' 1.317(4) . ? C1B' F1B' 1.353(3) . ? C2B' F3B' 1.309(4) . ? C2B' F2B' 1.318(3) . ? 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 C1B P1 C1A 98.45(14) . . ? C1B P1 C1 100.93(14) . . ? C1A P1 C1 100.26(13) . . ? C2 C1 C6 118.9(3) . . ? C2 C1 P1 122.1(2) . . ? C6 C1 P1 118.8(2) . . ? C3 C2 C1 120.7(3) . . ? C2 C3 C4 120.6(3) . . ? C3 C4 C5 119.4(3) . . ? C6 C5 C4 120.8(3) . . ? C5 C6 C1 119.7(3) . . ? C2A C1A F1A 115.9(3) . . ? C2A C1A P1 123.5(3) . . ? F1A C1A P1 120.6(2) . . ? F3A C2A C1A 124.9(3) . . ? F3A C2A F2A 110.9(3) . . ? C1A C2A F2A 124.2(3) . . ? C2B C1B F1B 115.2(3) . . ? C2B C1B P1 123.8(3) . . ? F1B C1B P1 121.0(2) . . ? F3B C2B C1B 124.7(3) . . ? F3B C2B F2B 110.9(3) . . ? C1B C2B F2B 124.4(3) . . ? C1A' P1' C1B' 98.13(13) . . ? C1A' P1' C1' 101.12(13) . . ? C1B' P1' C1' 99.80(13) . . ? C2' C1' C6' 119.3(3) . . ? C2' C1' P1' 119.2(2) . . ? C6' C1' P1' 121.3(2) . . ? C3' C2' C1' 120.2(3) . . ? C2' C3' C4' 120.7(3) . . ? C5' C4' C3' 118.7(3) . . ? C6' C5' C4' 121.2(3) . . ? C5' C6' C1' 119.8(3) . . ? C2A' C1A' F1A' 115.3(3) . . ? C2A' C1A' P1' 124.2(2) . . ? F1A' C1A' P1' 120.5(2) . . ? C1A' C2A' F2A' 124.9(3) . . ? C1A' C2A' F3A' 124.7(3) . . ? F2A' C2A' F3A' 110.4(2) . . ? C2B' C1B' F1B' 115.6(3) . . ? C2B' C1B' P1' 123.8(3) . . ? F1B' C1B' P1' 120.6(2) . . ? F3B' C2B' C1B' 124.7(3) . . ? F3B' C2B' F2B' 110.9(3) . . ? C1B' C2B' F2B' 124.5(3) . . ? _refine_diff_density_max 0.347 _refine_diff_density_min -0.237 _refine_diff_density_rms 0.060 #=END data_cal2b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H20 Cl2 F6 P2 Pt' _chemical_formula_weight 798.37 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' 'F' 'F' 0.0171 0.0103 '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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 2(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 11.083(3) _cell_length_b 15.162(2) _cell_length_c 16.668(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.231(14) _cell_angle_gamma 90.00 _cell_volume 2756.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 146(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.924 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 5.459 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 146(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4843 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0802 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4843 _reflns_number_gt 3382 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4843 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1396 _refine_ls_wR_factor_gt 0.1156 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.916 _refine_ls_shift/su_max 0.117 _refine_ls_shift/su_mean 0.014 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.08546(4) 0.13423(2) 0.18546(2) 0.02184(15) Uani 1 1 d . . . Cl1 Cl 0.2375(3) 0.17895(19) 0.11551(17) 0.0358(7) Uani 1 1 d . . . Cl2 Cl -0.0236(3) 0.26081(18) 0.13508(17) 0.0357(7) Uani 1 1 d . . . P1 P -0.0711(3) 0.10443(17) 0.24893(16) 0.0225(6) Uani 1 1 d . . . P2 P 0.1948(3) 0.01579(17) 0.23216(16) 0.0225(6) Uani 1 1 d . . . F1 F -0.3127(6) 0.1388(5) 0.2140(4) 0.0408(16) Uani 1 1 d . . . F2 F -0.3470(7) 0.1037(6) 0.0566(4) 0.058(2) Uani 1 1 d . . . F3 F -0.1582(7) 0.0717(6) 0.0595(4) 0.062(2) Uani 1 1 d . . . F4 F 0.3121(7) -0.0257(5) 0.1108(4) 0.051(2) Uani 1 1 d . . . F5 F 0.5385(7) -0.0063(5) 0.1845(5) 0.060(2) Uani 1 1 d . . . F6 F 0.4913(7) 0.0376(5) 0.2978(5) 0.0477(19) Uani 1 1 d . . . C1 C -0.0891(10) -0.0016(6) 0.2955(6) 0.022(2) Uani 1 1 d . . . C2 C -0.0273(11) -0.0187(7) 0.3745(6) 0.026(2) Uani 1 1 d . . . H2 H 0.0234 0.0254 0.4037 0.031 Uiso 1 1 calc R . . C3 C -0.0394(12) -0.0992(8) 0.4103(7) 0.038(3) Uani 1 1 d . . . H3 H 0.0044 -0.1114 0.4635 0.046 Uiso 1 1 calc R . . C4 C -0.1152(13) -0.1618(8) 0.3685(8) 0.044(3) Uani 1 1 d . . . H4 H -0.1247 -0.2169 0.3937 0.053 Uiso 1 1 calc R . . C5 C -0.1781(12) -0.1461(7) 0.2903(8) 0.041(3) Uani 1 1 d . . . H5 H -0.2302 -0.1900 0.2619 0.049 Uiso 1 1 calc R . . C6 C -0.1639(10) -0.0658(7) 0.2542(7) 0.030(3) Uani 1 1 d . . . H6 H -0.2061 -0.0546 0.2004 0.036 Uiso 1 1 calc R . . C7 C -0.0836(10) 0.1828(6) 0.3292(6) 0.025(2) Uani 1 1 d . . . C8 C -0.0084(11) 0.2538(7) 0.3419(6) 0.032(3) Uani 1 1 d . . . H8 H 0.0500 0.2639 0.3076 0.039 Uiso 1 1 calc R . . C9 C -0.0170(13) 0.3124(7) 0.4057(7) 0.039(3) Uani 1 1 d . . . H9 H 0.0372 0.3613 0.4150 0.047 Uiso 1 1 calc R . . C10 C -0.1013(12) 0.3001(7) 0.4543(7) 0.037(3) Uani 1 1 d . . . H10 H -0.1062 0.3406 0.4971 0.045 Uiso 1 1 calc R . . C11 C -0.1808(11) 0.2283(7) 0.4417(7) 0.034(3) Uani 1 1 d . . . H11 H -0.2407 0.2199 0.4753 0.041 Uiso 1 1 calc R . . C12 C -0.1713(11) 0.1688(7) 0.3792(7) 0.030(3) Uani 1 1 d . . . H12 H -0.2240 0.1190 0.3706 0.036 Uiso 1 1 calc R . . C13 C -0.2141(12) 0.1175(6) 0.1804(6) 0.031(3) Uani 1 1 d . . . C14 C -0.2399(11) 0.0984(9) 0.1026(7) 0.039(3) Uani 1 1 d . . . C15 C 0.1169(9) -0.0861(7) 0.1980(6) 0.025(2) Uani 1 1 d . . . C16 C 0.0562(11) -0.0873(8) 0.1172(7) 0.035(3) Uani 1 1 d . . . H16 H 0.0529 -0.0351 0.0855 0.042 Uiso 1 1 calc R . . C17 C 0.0006(13) -0.1633(9) 0.0823(8) 0.047(3) Uani 1 1 d . . . H17 H -0.0409 -0.1632 0.0273 0.056 Uiso 1 1 calc R . . C18 C 0.0064(12) -0.2386(9) 0.1282(9) 0.049(4) Uani 1 1 d . . . H18 H -0.0260 -0.2922 0.1039 0.059 Uiso 1 1 calc R . . C19 C 0.0600(13) -0.2368(8) 0.2107(9) 0.050(4) Uani 1 1 d . . . H19 H 0.0567 -0.2878 0.2433 0.060 Uiso 1 1 calc R . . C20 C 0.1180(12) -0.1612(8) 0.2453(7) 0.040(3) Uani 1 1 d . . . H20 H 0.1578 -0.1610 0.3007 0.048 Uiso 1 1 calc R . . C21 C 0.2506(10) 0.0173(7) 0.3400(6) 0.025(2) Uani 1 1 d . . . C22 C 0.3098(11) -0.0543(8) 0.3839(8) 0.038(3) Uani 1 1 d . . . H22 H 0.3225 -0.1077 0.3566 0.046 Uiso 1 1 calc R . . C23 C 0.3494(13) -0.0464(9) 0.4672(8) 0.048(4) Uani 1 1 d . . . H23 H 0.3860 -0.0955 0.4976 0.058 Uiso 1 1 calc R . . C24 C 0.3364(13) 0.0308(10) 0.5056(8) 0.050(4) Uani 1 1 d . . . H24 H 0.3618 0.0343 0.5630 0.060 Uiso 1 1 calc R . . C25 C 0.2875(12) 0.1039(9) 0.4635(8) 0.044(3) Uani 1 1 d . . . H25 H 0.2846 0.1588 0.4905 0.053 Uiso 1 1 calc R . . C26 C 0.2429(10) 0.0960(8) 0.3820(6) 0.030(2) Uani 1 1 d . . . H26 H 0.2055 0.1457 0.3531 0.036 Uiso 1 1 calc R . . C27 C 0.3341(12) 0.0013(7) 0.1896(8) 0.036(3) Uani 1 1 d . . . C28 C 0.4478(10) 0.0108(7) 0.2233(8) 0.033(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0220(2) 0.0218(2) 0.0217(2) 0.00067(17) 0.00394(14) -0.0002(2) Cl1 0.0365(18) 0.0389(16) 0.0345(14) 0.0063(12) 0.0130(13) -0.0047(13) Cl2 0.0416(18) 0.0298(14) 0.0352(14) 0.0097(11) 0.0056(13) 0.0054(13) P1 0.0237(15) 0.0191(12) 0.0242(12) -0.0008(10) 0.0030(11) 0.0019(11) P2 0.0194(15) 0.0226(13) 0.0235(12) -0.0039(10) -0.0019(11) 0.0005(11) F1 0.023(4) 0.058(4) 0.040(4) -0.011(3) 0.002(3) 0.006(3) F2 0.039(5) 0.087(6) 0.040(4) 0.003(4) -0.014(4) 0.003(4) F3 0.049(5) 0.111(7) 0.025(4) -0.018(4) 0.001(3) 0.007(5) F4 0.034(4) 0.073(5) 0.051(4) -0.028(4) 0.018(3) -0.002(4) F5 0.034(5) 0.054(5) 0.098(7) -0.030(4) 0.023(4) -0.009(4) F6 0.036(5) 0.048(4) 0.055(5) -0.006(3) -0.004(4) -0.007(3) C1 0.024(6) 0.014(5) 0.029(5) 0.005(4) 0.007(5) -0.001(4) C2 0.031(7) 0.023(5) 0.026(5) -0.008(4) 0.012(5) 0.001(5) C3 0.045(8) 0.033(6) 0.037(6) 0.012(5) 0.006(6) -0.004(6) C4 0.060(10) 0.031(6) 0.040(7) 0.009(5) 0.005(6) -0.011(6) C5 0.040(8) 0.028(7) 0.053(7) -0.012(5) 0.002(6) -0.012(6) C6 0.024(6) 0.028(6) 0.037(6) 0.008(5) 0.001(5) -0.004(5) C7 0.029(6) 0.017(5) 0.026(5) 0.010(4) 0.001(5) -0.004(5) C8 0.041(8) 0.029(6) 0.029(6) 0.001(5) 0.010(5) 0.004(5) C9 0.059(9) 0.022(6) 0.035(6) -0.007(5) 0.006(6) -0.009(6) C10 0.050(9) 0.031(6) 0.034(6) -0.004(5) 0.019(6) -0.003(6) C11 0.039(8) 0.036(6) 0.033(6) -0.005(5) 0.018(5) 0.001(6) C12 0.032(7) 0.023(5) 0.036(6) -0.004(5) 0.006(5) 0.003(5) C13 0.051(8) 0.014(5) 0.027(5) -0.003(4) 0.005(5) 0.015(5) C14 0.026(7) 0.049(7) 0.039(7) 0.004(6) 0.002(5) 0.006(6) C15 0.016(6) 0.023(5) 0.033(6) -0.012(4) -0.002(5) 0.006(4) C16 0.032(7) 0.046(7) 0.027(6) -0.010(5) 0.005(5) -0.006(6) C17 0.048(9) 0.045(7) 0.043(7) -0.011(6) -0.006(6) -0.005(7) C18 0.035(8) 0.044(8) 0.064(9) -0.025(7) -0.002(7) -0.005(6) C19 0.055(10) 0.021(6) 0.067(9) -0.002(6) -0.007(7) -0.008(6) C20 0.046(8) 0.037(7) 0.031(6) 0.006(5) -0.006(6) 0.001(6) C21 0.016(6) 0.033(6) 0.023(5) -0.001(4) -0.001(4) 0.003(5) C22 0.026(7) 0.033(6) 0.051(7) 0.004(5) -0.006(6) 0.002(5) C23 0.047(9) 0.049(8) 0.044(7) 0.023(6) -0.007(6) -0.010(7) C24 0.046(9) 0.065(10) 0.037(7) 0.007(7) 0.000(6) -0.021(7) C25 0.036(8) 0.053(8) 0.044(7) -0.014(6) 0.008(6) -0.005(6) C26 0.017(6) 0.044(6) 0.028(5) -0.006(5) 0.000(4) -0.002(5) C27 0.037(8) 0.020(5) 0.051(7) 0.003(5) 0.012(6) 0.005(5) C28 0.009(6) 0.024(6) 0.064(8) -0.007(5) 0.004(5) 0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P2 2.228(3) . ? Pt1 P1 2.233(3) . ? Pt1 Cl1 2.315(3) . ? Pt1 Cl2 2.343(3) . ? P1 C13 1.792(12) . ? P1 C1 1.811(10) . ? P1 C7 1.813(11) . ? P2 C21 1.795(10) . ? P2 C15 1.812(10) . ? P2 C27 1.823(13) . ? F1 C13 1.354(13) . ? F2 C14 1.296(13) . ? F3 C14 1.315(14) . ? F4 C27 1.356(14) . ? F5 C28 1.315(14) . ? F6 C28 1.314(14) . ? C1 C6 1.381(15) . ? C1 C2 1.397(14) . ? C2 C3 1.376(15) . ? C3 C4 1.372(18) . ? C4 C5 1.385(17) . ? C5 C6 1.379(15) . ? C7 C8 1.355(15) . ? C7 C12 1.405(15) . ? C8 C9 1.402(15) . ? C9 C10 1.354(17) . ? C10 C11 1.393(16) . ? C11 C12 1.396(15) . ? C13 C14 1.309(16) . ? C15 C20 1.383(16) . ? C15 C16 1.395(15) . ? C16 C17 1.384(17) . ? C17 C18 1.369(19) . ? C18 C19 1.397(19) . ? C19 C20 1.388(17) . ? C21 C26 1.394(15) . ? C21 C22 1.405(15) . ? C22 C23 1.385(17) . ? C23 C24 1.35(2) . ? C24 C25 1.371(19) . ? C25 C26 1.365(16) . ? C27 C28 1.293(17) . ? 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 P2 Pt1 P1 95.25(10) . . ? P2 Pt1 Cl1 90.73(11) . . ? P1 Pt1 Cl1 173.99(10) . . ? P2 Pt1 Cl2 178.09(11) . . ? P1 Pt1 Cl2 86.59(10) . . ? Cl1 Pt1 Cl2 87.42(11) . . ? C13 P1 C1 102.7(5) . . ? C13 P1 C7 102.9(5) . . ? C1 P1 C7 103.7(4) . . ? C13 P1 Pt1 110.4(4) . . ? C1 P1 Pt1 122.4(4) . . ? C7 P1 Pt1 112.6(4) . . ? C21 P2 C15 112.7(5) . . ? C21 P2 C27 103.1(5) . . ? C15 P2 C27 99.5(5) . . ? C21 P2 Pt1 114.1(4) . . ? C15 P2 Pt1 112.2(3) . . ? C27 P2 Pt1 114.0(4) . . ? C6 C1 C2 119.3(9) . . ? C6 C1 P1 121.0(8) . . ? C2 C1 P1 119.7(8) . . ? C3 C2 C1 120.3(10) . . ? C4 C3 C2 119.4(11) . . ? C3 C4 C5 121.4(11) . . ? C6 C5 C4 119.0(11) . . ? C5 C6 C1 120.7(10) . . ? C8 C7 C12 119.9(10) . . ? C8 C7 P1 120.7(8) . . ? C12 C7 P1 119.4(8) . . ? C7 C8 C9 120.0(11) . . ? C10 C9 C8 120.9(11) . . ? C9 C10 C11 120.2(11) . . ? C10 C11 C12 119.2(11) . . ? C11 C12 C7 119.8(11) . . ? C14 C13 F1 114.4(11) . . ? C14 C13 P1 128.3(10) . . ? F1 C13 P1 116.7(7) . . ? F2 C14 C13 126.0(12) . . ? F2 C14 F3 110.1(10) . . ? C13 C14 F3 124.0(11) . . ? C20 C15 C16 119.6(10) . . ? C20 C15 P2 124.6(8) . . ? C16 C15 P2 115.8(9) . . ? C17 C16 C15 121.3(12) . . ? C18 C17 C16 119.0(12) . . ? C17 C18 C19 120.2(12) . . ? C20 C19 C18 120.7(12) . . ? C15 C20 C19 119.0(11) . . ? C26 C21 C22 117.7(10) . . ? C26 C21 P2 118.3(8) . . ? C22 C21 P2 123.8(9) . . ? C23 C22 C21 119.3(12) . . ? C24 C23 C22 120.6(12) . . ? C23 C24 C25 121.5(12) . . ? C26 C25 C24 118.6(13) . . ? C25 C26 C21 122.1(12) . . ? C28 C27 F4 116.6(11) . . ? C28 C27 P2 130.2(10) . . ? F4 C27 P2 113.2(9) . . ? C27 C28 F6 127.6(11) . . ? C27 C28 F5 122.4(12) . . ? F6 C28 F5 110.0(10) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.179 _refine_diff_density_min -1.431 _refine_diff_density_rms 0.198 #=END data_kal4b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28.50 H21 Au2 Cl3 F6 P2' _chemical_formula_weight 1039.68 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' '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'C 2/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 20.1903(14) _cell_length_b 9.8220(15) _cell_length_c 31.974(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.493(9) _cell_angle_gamma 90.00 _cell_volume 6165.7(12) _cell_formula_units_Z 8 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3880 _exptl_absorpt_coefficient_mu 9.926 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5591 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5591 _reflns_number_gt 4519 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0420P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5591 _refine_ls_number_parameters 375 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0823 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.082 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.173238(15) 0.87198(3) 0.146564(10) 0.02583(10) Uani 1 1 d . . . Au2 Au 0.272197(16) 0.91598(3) 0.082999(10) 0.02701(10) Uani 1 1 d . . . Cl1 Cl 0.22626(11) 1.0724(2) 0.17069(7) 0.0377(5) Uani 1 1 d . . . Cl2 Cl 0.17761(11) 1.0016(2) 0.03727(7) 0.0420(6) Uani 1 1 d . . . Cl3 Cl 0.02554(18) 0.9540(4) 0.21139(12) 0.0922(11) Uani 1 1 d . . . P1 P 0.12070(10) 0.6766(2) 0.12611(6) 0.0240(4) Uani 1 1 d . . . P2 P 0.36465(10) 0.8264(2) 0.12548(6) 0.0244(4) Uani 1 1 d . . . F1 F 0.0681(3) 0.4666(5) 0.15982(16) 0.0494(14) Uani 1 1 d . . . F2 F 0.1054(3) 0.5314(6) 0.24099(17) 0.0630(17) Uani 1 1 d . . . F3 F 0.1561(3) 0.7130(6) 0.22887(16) 0.0528(14) Uani 1 1 d . . . F4 F 0.4586(3) 0.8981(5) 0.19595(16) 0.0472(14) Uani 1 1 d . . . F5 F 0.4465(3) 1.1631(6) 0.1873(2) 0.075(2) Uani 1 1 d . . . F6 F 0.3678(3) 1.1493(5) 0.1292(2) 0.0633(17) Uani 1 1 d . . . C1 C 0.1654(4) 0.5603(8) 0.0989(3) 0.0267(18) Uani 1 1 d . . . C2 C 0.1849(4) 0.6109(9) 0.0630(3) 0.034(2) Uani 1 1 d . . . H2 H 0.1744 0.7003 0.0544 0.040 Uiso 1 1 calc R . . C3 C 0.2195(4) 0.5305(11) 0.0403(3) 0.042(2) Uani 1 1 d . . . H3 H 0.2327 0.5649 0.0164 0.050 Uiso 1 1 calc R . . C4 C 0.2345(5) 0.3960(10) 0.0535(3) 0.048(3) Uani 1 1 d . . . H4 H 0.2578 0.3406 0.0382 0.058 Uiso 1 1 calc R . . C5 C 0.2154(4) 0.3449(9) 0.0886(3) 0.040(2) Uani 1 1 d . . . H5 H 0.2252 0.2551 0.0971 0.048 Uiso 1 1 calc R . . C6 C 0.1814(4) 0.4285(9) 0.1112(3) 0.037(2) Uani 1 1 d . . . H6 H 0.1689 0.3945 0.1354 0.045 Uiso 1 1 calc R . . C7 C 0.0374(4) 0.6928(8) 0.0903(3) 0.0267(18) Uani 1 1 d . . . C8 C 0.0070(4) 0.5838(9) 0.0652(3) 0.036(2) Uani 1 1 d . . . H8 H 0.0292 0.5004 0.0667 0.043 Uiso 1 1 calc R . . C9 C -0.0564(4) 0.6012(9) 0.0381(3) 0.036(2) Uani 1 1 d . . . H9 H -0.0770 0.5291 0.0211 0.044 Uiso 1 1 calc R . . C10 C -0.0891(4) 0.7234(10) 0.0361(3) 0.041(2) Uani 1 1 d . . . H10 H -0.1316 0.7341 0.0175 0.049 Uiso 1 1 calc R . . C11 C -0.0601(5) 0.8300(9) 0.0611(3) 0.042(2) Uani 1 1 d . . . H11 H -0.0829 0.9127 0.0598 0.051 Uiso 1 1 calc R . . C12 C 0.0035(4) 0.8141(9) 0.0883(3) 0.033(2) Uani 1 1 d . . . H12 H 0.0234 0.8864 0.1055 0.040 Uiso 1 1 calc R . . C13 C 0.1047(4) 0.5800(9) 0.1705(3) 0.033(2) Uani 1 1 d . . . C14 C 0.1215(4) 0.6071(9) 0.2112(3) 0.037(2) Uani 1 1 d . . . C15 C 0.3472(4) 0.6997(8) 0.1621(2) 0.0275(18) Uani 1 1 d . . . C16 C 0.3484(4) 0.5630(9) 0.1537(3) 0.037(2) Uani 1 1 d . . . H16 H 0.3616 0.5329 0.1293 0.044 Uiso 1 1 calc R . . C17 C 0.3302(5) 0.4698(10) 0.1814(3) 0.050(3) Uani 1 1 d . . . H17 H 0.3302 0.3773 0.1753 0.060 Uiso 1 1 calc R . . C18 C 0.3124(5) 0.5134(12) 0.2177(3) 0.053(3) Uani 1 1 d . . . H18 H 0.3013 0.4502 0.2366 0.064 Uiso 1 1 calc R . . C19 C 0.3107(5) 0.6482(12) 0.2264(3) 0.053(3) Uani 1 1 d . . . H19 H 0.2986 0.6769 0.2513 0.064 Uiso 1 1 calc R . . C20 C 0.3266(4) 0.7419(10) 0.1989(3) 0.038(2) Uani 1 1 d . . . H20 H 0.3238 0.8342 0.2046 0.045 Uiso 1 1 calc R . . C21 C 0.4251(4) 0.7545(8) 0.0976(3) 0.0255(18) Uani 1 1 d . . . C22 C 0.4897(4) 0.7178(8) 0.1206(3) 0.036(2) Uani 1 1 d . . . H22 H 0.5007 0.7236 0.1504 0.043 Uiso 1 1 calc R . . C23 C 0.5376(4) 0.6726(9) 0.0993(3) 0.039(2) Uani 1 1 d . . . H23 H 0.5806 0.6461 0.1147 0.047 Uiso 1 1 calc R . . C24 C 0.5215(5) 0.6672(10) 0.0560(3) 0.044(2) Uani 1 1 d . . . H24 H 0.5543 0.6415 0.0414 0.053 Uiso 1 1 calc R . . C25 C 0.4571(5) 0.6994(10) 0.0332(3) 0.047(3) Uani 1 1 d . . . H25 H 0.4457 0.6893 0.0035 0.056 Uiso 1 1 calc R . . C26 C 0.4089(4) 0.7465(8) 0.0540(3) 0.034(2) Uani 1 1 d . . . H26 H 0.3659 0.7725 0.0384 0.040 Uiso 1 1 calc R . . C27 C 0.4117(4) 0.9478(9) 0.1621(3) 0.0308(19) Uani 1 1 d . . . C28 C 0.4095(5) 1.0777(11) 0.1598(3) 0.049(3) Uani 1 1 d . . . C29 C 0.0000 1.0570(15) 0.2500 0.066(5) Uani 1 2 d S . . H29A H 0.0375 1.1149 0.2641 0.079 Uiso 0.50 1 calc PR . . H29B H -0.0375 1.1149 0.2359 0.079 Uiso 0.50 1 calc PR . . 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 0.02721(17) 0.02456(17) 0.02578(17) -0.00311(13) 0.00630(13) -0.00244(14) Au2 0.02661(17) 0.02927(18) 0.02592(17) 0.00403(14) 0.00770(13) 0.00796(14) Cl1 0.0458(13) 0.0333(12) 0.0361(12) -0.0106(10) 0.0137(10) -0.0112(10) Cl2 0.0375(12) 0.0511(14) 0.0347(12) 0.0072(11) 0.0033(10) 0.0217(11) Cl3 0.077(2) 0.094(3) 0.091(3) -0.024(2) -0.0100(19) 0.015(2) P1 0.0240(10) 0.0236(11) 0.0239(11) -0.0002(9) 0.0046(9) -0.0021(9) P2 0.0227(10) 0.0261(11) 0.0245(11) 0.0021(9) 0.0054(9) 0.0022(9) F1 0.056(3) 0.047(3) 0.046(3) 0.003(3) 0.013(3) -0.024(3) F2 0.074(4) 0.076(4) 0.040(3) 0.016(3) 0.017(3) -0.013(3) F3 0.063(4) 0.061(4) 0.031(3) -0.004(3) 0.003(3) -0.008(3) F4 0.042(3) 0.057(4) 0.038(3) -0.016(3) 0.001(2) -0.004(3) F5 0.080(4) 0.048(4) 0.098(5) -0.040(4) 0.021(4) -0.029(3) F6 0.075(4) 0.024(3) 0.097(5) -0.001(3) 0.032(4) -0.008(3) C1 0.024(4) 0.025(4) 0.031(4) -0.007(4) 0.005(3) -0.002(3) C2 0.038(5) 0.038(5) 0.027(4) 0.000(4) 0.012(4) 0.000(4) C3 0.041(5) 0.066(7) 0.021(4) -0.007(5) 0.010(4) 0.001(5) C4 0.038(5) 0.058(7) 0.047(6) -0.027(5) 0.006(5) 0.013(5) C5 0.044(5) 0.026(5) 0.048(6) -0.007(4) 0.009(5) 0.007(4) C6 0.038(5) 0.038(5) 0.035(5) 0.000(4) 0.008(4) -0.001(4) C7 0.023(4) 0.028(5) 0.031(5) 0.007(4) 0.010(4) 0.005(4) C8 0.034(5) 0.027(5) 0.044(5) 0.004(4) 0.003(4) 0.011(4) C9 0.029(5) 0.037(5) 0.035(5) -0.005(4) -0.008(4) -0.003(4) C10 0.030(5) 0.052(6) 0.037(5) 0.013(5) -0.002(4) 0.003(4) C11 0.040(5) 0.026(5) 0.057(6) 0.005(5) 0.004(5) 0.011(4) C12 0.033(5) 0.031(5) 0.031(5) -0.005(4) 0.000(4) 0.002(4) C13 0.029(4) 0.032(5) 0.040(5) 0.001(4) 0.012(4) 0.000(4) C14 0.039(5) 0.037(5) 0.037(5) 0.009(4) 0.009(4) -0.003(4) C15 0.022(4) 0.038(5) 0.021(4) 0.008(4) 0.001(3) 0.006(4) C16 0.034(5) 0.036(5) 0.041(5) 0.001(4) 0.009(4) -0.003(4) C17 0.056(6) 0.029(5) 0.058(7) 0.019(5) 0.001(5) 0.002(5) C18 0.043(6) 0.066(8) 0.049(7) 0.029(6) 0.009(5) -0.001(5) C19 0.049(6) 0.068(8) 0.046(6) 0.020(6) 0.018(5) 0.004(6) C20 0.032(5) 0.050(6) 0.030(5) 0.004(4) 0.006(4) 0.007(4) C21 0.026(4) 0.021(4) 0.031(4) 0.003(3) 0.009(4) 0.002(3) C22 0.033(5) 0.026(5) 0.043(5) -0.001(4) -0.002(4) -0.001(4) C23 0.026(5) 0.030(5) 0.061(6) 0.000(5) 0.010(4) 0.008(4) C24 0.039(5) 0.042(6) 0.058(7) 0.003(5) 0.026(5) 0.011(5) C25 0.059(6) 0.051(6) 0.037(5) 0.003(5) 0.025(5) 0.013(5) C26 0.040(5) 0.030(5) 0.033(5) 0.007(4) 0.012(4) 0.011(4) C27 0.030(5) 0.035(5) 0.031(5) -0.008(4) 0.015(4) 0.001(4) C28 0.045(6) 0.051(7) 0.051(6) -0.005(6) 0.016(5) -0.009(5) C29 0.068(11) 0.042(9) 0.079(12) 0.000 -0.001(9) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.216(2) . ? Au1 Cl1 2.288(2) . ? Au1 Au2 3.1945(5) . ? Au2 P2 2.218(2) . ? Au2 Cl2 2.278(2) . ? Cl3 C29 1.764(9) . ? P1 C13 1.799(9) . ? P1 C1 1.801(8) . ? P1 C7 1.808(8) . ? P2 C27 1.783(8) . ? P2 C15 1.799(8) . ? P2 C21 1.814(8) . ? F1 C13 1.336(9) . ? F2 C14 1.307(10) . ? F3 C14 1.306(10) . ? F4 C27 1.351(10) . ? F5 C28 1.315(11) . ? F6 C28 1.333(12) . ? C1 C6 1.369(11) . ? C1 C2 1.390(11) . ? C2 C3 1.370(12) . ? C3 C4 1.399(13) . ? C4 C5 1.365(13) . ? C5 C6 1.378(12) . ? C7 C12 1.368(11) . ? C7 C8 1.391(12) . ? C8 C9 1.379(11) . ? C9 C10 1.364(12) . ? C10 C11 1.364(12) . ? C11 C12 1.381(11) . ? C13 C14 1.294(12) . ? C15 C16 1.370(12) . ? C15 C20 1.399(11) . ? C16 C17 1.382(12) . ? C17 C18 1.360(14) . ? C18 C19 1.355(15) . ? C19 C20 1.361(12) . ? C21 C26 1.359(11) . ? C21 C22 1.386(10) . ? C22 C23 1.380(12) . ? C23 C24 1.349(13) . ? C24 C25 1.371(13) . ? C25 C26 1.380(11) . ? C27 C28 1.277(13) . ? C29 Cl3 1.764(9) 6_556 ? 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 Cl1 177.36(8) . . ? P1 Au1 Au2 104.87(5) . . ? Cl1 Au1 Au2 77.59(5) . . ? P2 Au2 Cl2 177.65(8) . . ? P2 Au2 Au1 96.81(5) . . ? Cl2 Au2 Au1 84.44(6) . . ? C13 P1 C1 104.4(4) . . ? C13 P1 C7 103.6(4) . . ? C1 P1 C7 104.3(4) . . ? C13 P1 Au1 112.7(3) . . ? C1 P1 Au1 115.6(3) . . ? C7 P1 Au1 114.9(3) . . ? C27 P2 C15 101.0(4) . . ? C27 P2 C21 105.5(4) . . ? C15 P2 C21 107.9(4) . . ? C27 P2 Au2 112.3(3) . . ? C15 P2 Au2 114.1(2) . . ? C21 P2 Au2 114.9(3) . . ? C6 C1 C2 118.9(8) . . ? C6 C1 P1 124.9(7) . . ? C2 C1 P1 116.2(6) . . ? C3 C2 C1 120.6(8) . . ? C2 C3 C4 119.0(9) . . ? C5 C4 C3 120.9(8) . . ? C4 C5 C6 118.9(9) . . ? C1 C6 C5 121.7(9) . . ? C12 C7 C8 119.7(7) . . ? C12 C7 P1 119.2(6) . . ? C8 C7 P1 121.1(6) . . ? C9 C8 C7 119.1(8) . . ? C10 C9 C8 120.4(8) . . ? C11 C10 C9 120.8(8) . . ? C10 C11 C12 119.4(8) . . ? C7 C12 C11 120.6(8) . . ? C14 C13 F1 115.4(8) . . ? C14 C13 P1 129.3(7) . . ? F1 C13 P1 115.3(6) . . ? C13 C14 F3 125.9(8) . . ? C13 C14 F2 124.4(8) . . ? F3 C14 F2 109.8(8) . . ? C16 C15 C20 118.5(8) . . ? C16 C15 P2 122.4(7) . . ? C20 C15 P2 119.0(7) . . ? C15 C16 C17 120.3(9) . . ? C18 C17 C16 120.0(10) . . ? C19 C18 C17 120.4(10) . . ? C18 C19 C20 120.5(10) . . ? C19 C20 C15 120.2(9) . . ? C26 C21 C22 120.0(8) . . ? C26 C21 P2 119.8(6) . . ? C22 C21 P2 119.9(6) . . ? C23 C22 C21 120.2(8) . . ? C24 C23 C22 119.4(8) . . ? C23 C24 C25 120.5(8) . . ? C24 C25 C26 120.7(9) . . ? C21 C26 C25 119.0(8) . . ? C28 C27 F4 114.5(8) . . ? C28 C27 P2 128.6(8) . . ? F4 C27 P2 116.8(6) . . ? C27 C28 F5 126.2(10) . . ? C27 C28 F6 125.2(9) . . ? F5 C28 F6 108.5(9) . . ? Cl3 C29 Cl3 110.0(8) 6_556 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.336 _refine_diff_density_min -1.126 _refine_diff_density_rms 0.176