# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Peter Kunz' _publ_contact_author_email Peter.Kunz@uni-duesseldorf.de _publ_section_title ; Gold(I) complexes of water-soluble diphos-type ligands: Synthesis, anticancer activity, apoptosis and thioredoxin reductase inhibition. ; loop_ _publ_author_name P.Kunz C.Wetzel M.Kassack A.Hamacher P.Bohler W.Watjen ; R.Rubbiani ; I.Ott B.Spingler data_kp051008 _database_code_depnum_ccdc_archive 'CCDC 808833' #TrackingRef '- kp051008.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Au2 Cl2 N8 P2' _chemical_formula_weight 879.23 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' N N 0.0061 0.0033 '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' Cl Cl 0.1484 0.1585 '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 7.7649(2) _cell_length_b 9.3598(3) _cell_length_c 9.7306(3) _cell_angle_alpha 106.655(3) _cell_angle_beta 103.914(3) _cell_angle_gamma 100.648(3) _cell_volume 632.71(3) _cell_formula_units_Z 1 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 5168 _cell_measurement_theta_min 2.2930 _cell_measurement_theta_max 32.4652 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 410 _exptl_absorpt_coefficient_mu 11.941 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2646 _exptl_absorpt_correction_T_max 0.7158 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Xcalibur Ruby CCD' _diffrn_measurement_method '\o oscillation scan' _diffrn_detector_area_resol_mean 10.4498 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7398 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 30.51 _reflns_number_total 3836 _reflns_number_gt 3329 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis^Pro^ (Oxford, 2007)' _computing_cell_refinement 'CrysAlis^Pro^ (Oxford, 2007)' _computing_data_reduction 'CrysAlis^Pro^ (Oxford, 2007)' _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3836 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0708 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 0.38435(3) 0.02585(2) 0.821032(18) 0.02098(6) Uani 1 1 d . . . C4 C -0.0962(8) 0.0262(7) 0.7682(8) 0.0448(15) Uani 1 1 d . . . H4A H -0.0089 -0.0372 0.7684 0.067 Uiso 1 1 calc R . . H4B H -0.1140 0.0564 0.6784 0.067 Uiso 1 1 calc R . . H4C H -0.2146 -0.0338 0.7669 0.067 Uiso 1 1 calc R . . C5 C -0.1138(7) 0.2177(7) 1.0040(6) 0.0336(12) Uani 1 1 d . . . H5A H -0.2348 0.1693 0.9998 0.040 Uiso 1 1 calc R . . C2 C 0.1431(6) 0.2714(6) 0.9532(5) 0.0219(9) Uani 1 1 d . . . C11 C 0.2430(10) 0.3312(7) 0.4868(6) 0.0396(14) Uani 1 1 d . . . H11A H 0.2763 0.3454 0.4028 0.048 Uiso 1 1 calc R . . C10 C 0.5404(9) 0.2933(8) 0.6264(6) 0.0429(15) Uani 1 1 d . . . H10A H 0.5498 0.1984 0.6477 0.064 Uiso 1 1 calc R . . H10B H 0.6255 0.3834 0.7111 0.064 Uiso 1 1 calc R . . H10C H 0.5724 0.2897 0.5342 0.064 Uiso 1 1 calc R . . C6 C 0.0016(8) 0.3515(7) 1.1101(6) 0.0323(12) Uani 1 1 d . . . H6A H -0.0266 0.4127 1.1937 0.039 Uiso 1 1 calc R . . C8 C 0.2491(7) 0.2972(6) 0.6986(5) 0.0241(10) Uani 1 1 d . . . C12 C 0.0796(10) 0.3324(7) 0.5108(6) 0.0431(16) Uani 1 1 d . . . H12A H -0.0229 0.3454 0.4441 0.052 Uiso 1 1 calc R . . C1 C 0.5176(6) 0.4220(5) 0.9988(5) 0.0214(9) Uani 1 1 d . . . H1A H 0.5421 0.4182 1.1021 0.026 Uiso 1 1 calc R . . H1B H 0.6293 0.4141 0.9684 0.026 Uiso 1 1 calc R . . N3 N -0.0228(6) 0.1659(5) 0.9044(5) 0.0285(9) Uani 1 1 d . . . N7 N 0.1651(6) 0.3860(5) 1.0798(4) 0.0255(9) Uani 1 1 d . . . N13 N 0.0822(7) 0.3119(6) 0.6460(5) 0.0345(11) Uani 1 1 d . . . N9 N 0.3525(7) 0.3059(5) 0.6057(4) 0.0315(10) Uani 1 1 d . . . P1 P 0.32656(17) 0.25666(14) 0.87121(12) 0.0194(2) Uani 1 1 d . . . Cl1 Cl 0.4377(2) -0.21284(15) 0.75658(14) 0.0312(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 Au1 0.02011(9) 0.01849(10) 0.02298(9) 0.00490(6) 0.00807(6) 0.00400(6) C4 0.024(3) 0.031(3) 0.060(4) -0.004(3) 0.013(3) -0.006(2) C5 0.020(2) 0.043(3) 0.042(3) 0.018(3) 0.015(2) 0.008(2) C2 0.018(2) 0.022(2) 0.025(2) 0.0067(18) 0.0062(17) 0.0060(19) C11 0.060(4) 0.031(3) 0.021(2) 0.007(2) 0.007(2) 0.008(3) C10 0.038(3) 0.058(4) 0.029(3) 0.011(3) 0.017(2) 0.004(3) C6 0.027(3) 0.043(3) 0.033(3) 0.013(2) 0.016(2) 0.015(3) C8 0.028(3) 0.020(2) 0.019(2) 0.0028(18) 0.0047(18) 0.005(2) C12 0.059(4) 0.037(3) 0.026(3) 0.007(2) -0.001(3) 0.021(3) C1 0.018(2) 0.019(2) 0.024(2) 0.0064(18) 0.0028(17) 0.0022(18) N3 0.019(2) 0.026(2) 0.038(2) 0.0068(18) 0.0110(17) 0.0021(18) N7 0.024(2) 0.030(2) 0.0250(19) 0.0090(17) 0.0109(16) 0.0089(18) N13 0.037(3) 0.033(3) 0.028(2) 0.0055(19) 0.0008(19) 0.017(2) N9 0.039(3) 0.029(2) 0.0204(18) 0.0049(17) 0.0089(18) 0.002(2) P1 0.0181(6) 0.0172(6) 0.0205(5) 0.0037(4) 0.0065(4) 0.0034(5) Cl1 0.0454(8) 0.0254(6) 0.0308(6) 0.0123(5) 0.0181(5) 0.0158(6) _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 2.2284(12) . ? Au1 Cl1 2.2848(12) . ? C4 N3 1.470(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.355(8) . ? C5 N3 1.363(6) . ? C5 H5A 0.9500 . ? C2 N7 1.331(6) . ? C2 N3 1.352(6) . ? C2 P1 1.800(5) . ? C11 C12 1.346(9) . ? C11 N9 1.370(7) . ? C11 H11A 0.9500 . ? C10 N9 1.455(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C6 N7 1.373(7) . ? C6 H6A 0.9500 . ? C8 N13 1.322(6) . ? C8 N9 1.355(6) . ? C8 P1 1.814(5) . ? C12 N13 1.379(7) . ? C12 H12A 0.9500 . ? C1 C1 1.529(9) 2_667 ? C1 P1 1.817(5) . ? C1 H1A 0.9900 . ? C1 H1B 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 Cl1 177.04(4) . . ? N3 C4 H4A 109.5 . . ? N3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 N3 106.8(5) . . ? C6 C5 H5A 126.6 . . ? N3 C5 H5A 126.6 . . ? N7 C2 N3 112.3(4) . . ? N7 C2 P1 121.7(4) . . ? N3 C2 P1 125.8(4) . . ? C12 C11 N9 107.4(5) . . ? C12 C11 H11A 126.3 . . ? N9 C11 H11A 126.3 . . ? N9 C10 H10A 109.5 . . ? N9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5 C6 N7 110.4(4) . . ? C5 C6 H6A 124.8 . . ? N7 C6 H6A 124.8 . . ? N13 C8 N9 113.1(4) . . ? N13 C8 P1 123.5(4) . . ? N9 C8 P1 123.3(4) . . ? C11 C12 N13 110.3(5) . . ? C11 C12 H12A 124.9 . . ? N13 C12 H12A 124.9 . . ? C1 C1 P1 113.5(4) 2_667 . ? C1 C1 H1A 108.9 2_667 . ? P1 C1 H1A 108.9 . . ? C1 C1 H1B 108.9 2_667 . ? P1 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C2 N3 C5 106.3(4) . . ? C2 N3 C4 127.5(4) . . ? C5 N3 C4 126.1(5) . . ? C2 N7 C6 104.2(4) . . ? C8 N13 C12 104.0(5) . . ? C8 N9 C11 105.2(5) . . ? C8 N9 C10 128.2(4) . . ? C11 N9 C10 126.6(5) . . ? C2 P1 C8 104.1(2) . . ? C2 P1 C1 104.2(2) . . ? C8 P1 C1 106.5(2) . . ? C2 P1 Au1 114.24(17) . . ? C8 P1 Au1 110.52(16) . . ? C1 P1 Au1 116.32(15) . . ? 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 N3 C5 C6 N7 0.0(6) . . . . ? N9 C11 C12 N13 1.5(7) . . . . ? N7 C2 N3 C5 1.2(6) . . . . ? P1 C2 N3 C5 176.1(4) . . . . ? N7 C2 N3 C4 178.9(5) . . . . ? P1 C2 N3 C4 -6.3(8) . . . . ? C6 C5 N3 C2 -0.7(6) . . . . ? C6 C5 N3 C4 -178.4(5) . . . . ? N3 C2 N7 C6 -1.2(6) . . . . ? P1 C2 N7 C6 -176.3(4) . . . . ? C5 C6 N7 C2 0.7(6) . . . . ? N9 C8 N13 C12 -0.4(6) . . . . ? P1 C8 N13 C12 -176.5(4) . . . . ? C11 C12 N13 C8 -0.7(7) . . . . ? N13 C8 N9 C11 1.2(6) . . . . ? P1 C8 N9 C11 177.4(4) . . . . ? N13 C8 N9 C10 -179.4(5) . . . . ? P1 C8 N9 C10 -3.2(8) . . . . ? C12 C11 N9 C8 -1.6(6) . . . . ? C12 C11 N9 C10 179.0(6) . . . . ? N7 C2 P1 C8 -111.1(4) . . . . ? N3 C2 P1 C8 74.5(5) . . . . ? N7 C2 P1 C1 0.3(4) . . . . ? N3 C2 P1 C1 -174.1(4) . . . . ? N7 C2 P1 Au1 128.2(4) . . . . ? N3 C2 P1 Au1 -46.1(5) . . . . ? N13 C8 P1 C2 -7.8(5) . . . . ? N9 C8 P1 C2 176.4(4) . . . . ? N13 C8 P1 C1 -117.5(5) . . . . ? N9 C8 P1 C1 66.7(5) . . . . ? N13 C8 P1 Au1 115.3(4) . . . . ? N9 C8 P1 Au1 -60.5(5) . . . . ? C1 C1 P1 C2 -66.0(5) 2_667 . . . ? C1 C1 P1 C8 43.6(5) 2_667 . . . ? C1 C1 P1 Au1 167.3(4) 2_667 . . . ? Cl1 Au1 P1 C2 111.1(10) . . . . ? Cl1 Au1 P1 C8 -5.8(10) . . . . ? Cl1 Au1 P1 C1 -127.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.388 _refine_diff_density_min -1.278 _refine_diff_density_rms 0.257 data_kp061209 _database_code_depnum_ccdc_archive 'CCDC 808834' #TrackingRef 'web_deposit_cif_file_0_BernhardSpingler_1305802377.kp061209.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H48 Au F6 N8 P5' _chemical_formula_weight 1154.72 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' N N 0.0061 0.0033 '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' F F 0.0171 0.0103 '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 11.5666(2) _cell_length_b 12.5719(2) _cell_length_c 16.9038(4) _cell_angle_alpha 77.1249(18) _cell_angle_beta 81.4065(17) _cell_angle_gamma 80.7994(15) _cell_volume 2348.83(8) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 11693 _cell_measurement_theta_min 2.6079 _cell_measurement_theta_max 32.6843 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 3.368 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7495 _exptl_absorpt_correction_T_max 0.8771 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Xcalibur Ruby CCD' _diffrn_measurement_method '\o oscillation scan' _diffrn_detector_area_resol_mean 10.4498 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26468 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0902 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 30.51 _reflns_number_total 14316 _reflns_number_gt 9762 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis^Pro^ (Oxford, 2007)' _computing_cell_refinement 'CrysAlis^Pro^ (Oxford, 2007)' _computing_data_reduction 'CrysAlis^Pro^ (Oxford, 2007)' _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Only the major constituents of the disordered phenyl/methylimidazole groups could be anisotropically refined. The C54B-N46B bond distance had to be restrained. ; _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^)+(0.0341P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14316 _refine_ls_number_parameters 616 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.0789 _refine_ls_wR_factor_gt 0.0743 _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_restrained_S_all 0.904 _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 -0.724318(12) -0.780169(11) -0.781765(9) 0.03274(5) Uani 1 1 d . . . C1 C -0.5776(3) -1.0342(3) -0.7618(2) 0.0359(8) Uani 1 1 d . . . H1A H -0.5575 -1.1107 -0.7320 0.043 Uiso 1 1 calc R . . H1B H -0.5861 -1.0363 -0.8188 0.043 Uiso 1 1 calc R . . C2 C -0.8159(3) -1.0663(3) -0.7236(3) 0.0454(10) Uani 1 1 d . . . C4 C -0.9910(5) -1.0071(5) -0.6329(4) 0.0892(17) Uani 1 1 d . . . H4C H -1.0699 -1.0294 -0.6160 0.134 Uiso 1 1 calc R . . H4B H -0.9981 -0.9293 -0.6603 0.134 Uiso 1 1 calc R . . H4A H -0.9495 -1.0175 -0.5848 0.134 Uiso 1 1 calc R . . C5 C -0.9714(5) -1.1551(4) -0.7151(4) 0.0830(18) Uani 1 1 d . . . H5 H -1.0474 -1.1783 -0.7011 0.100 Uiso 1 1 calc R . . C6 C -0.8818(5) -1.1927(4) -0.7653(4) 0.0750(16) Uani 1 1 d . . . H6 H -0.8843 -1.2503 -0.7927 0.090 Uiso 1 1 calc R . . C8 C -0.6973(3) -1.0098(3) -0.6061(2) 0.0401(9) Uani 1 1 d . . . C9 C -0.6814(4) -1.1219(4) -0.5668(3) 0.0692(14) Uani 1 1 d . . . H9 H -0.6850 -1.1767 -0.5967 0.083 Uiso 1 1 calc R . . C10 C -0.6615(5) -1.1523(5) -0.4895(4) 0.0886(18) Uani 1 1 d . . . H10 H -0.6503 -1.2278 -0.4635 0.106 Uiso 1 1 calc R . . C11 C -0.6577(4) -1.0693(5) -0.4474(3) 0.0750(15) Uani 1 1 d . . . H11 H -0.6451 -1.0898 -0.3914 0.090 Uiso 1 1 calc R . . C12 C -0.6711(5) -0.9619(5) -0.4824(3) 0.0700(14) Uani 1 1 d . . . H12 H -0.6667 -0.9082 -0.4517 0.084 Uiso 1 1 calc R . . C13 C -0.6912(4) -0.9301(4) -0.5630(3) 0.0564(12) Uani 1 1 d . . . H13 H -0.7007 -0.8544 -0.5886 0.068 Uiso 1 1 calc R . . C14 C -0.4803(3) -0.9671(3) -0.7610(2) 0.0338(8) Uani 1 1 d . . . H14A H -0.4056 -1.0005 -0.7879 0.041 Uiso 1 1 calc R . . H14B H -0.4692 -0.9692 -0.7037 0.041 Uiso 1 1 calc R . . C15 C -0.4538(3) -0.8338(3) -0.9178(2) 0.0391(9) Uani 1 1 d . . . C17 C -0.4725(4) -0.6355(4) -0.9794(3) 0.0659(13) Uani 1 1 d . . . H17A H -0.4119 -0.6132 -0.9540 0.099 Uiso 1 1 calc R . . H17B H -0.5493 -0.6238 -0.9469 0.099 Uiso 1 1 calc R . . H17C H -0.4759 -0.5915 -1.0349 0.099 Uiso 1 1 calc R . . C18 C -0.3977(4) -0.7908(4) -1.0526(3) 0.0545(11) Uani 1 1 d . . . H18 H -0.3788 -0.7517 -1.1067 0.065 Uiso 1 1 calc R . . C19 C -0.3861(4) -0.8991(4) -1.0249(3) 0.0535(11) Uani 1 1 d . . . H19 H -0.3577 -0.9509 -1.0589 0.064 Uiso 1 1 calc R . . C21 C -0.4061(3) -0.7584(3) -0.7788(2) 0.0373(8) Uani 1 1 d . . . C22 C -0.2872(3) -0.8048(3) -0.7814(3) 0.0477(10) Uani 1 1 d . . . H22 H -0.2614 -0.8675 -0.8052 0.057 Uiso 1 1 calc R . . C23 C -0.2084(4) -0.7606(4) -0.7500(3) 0.0592(12) Uani 1 1 d . . . H23 H -0.1277 -0.7914 -0.7525 0.071 Uiso 1 1 calc R . . C24 C -0.2474(4) -0.6703(4) -0.7147(3) 0.0567(11) Uani 1 1 d . . . H24 H -0.1933 -0.6403 -0.6915 0.068 Uiso 1 1 calc R . . C25 C -0.3621(4) -0.6237(4) -0.7126(3) 0.0522(11) Uani 1 1 d . . . H25 H -0.3871 -0.5610 -0.6887 0.063 Uiso 1 1 calc R . . C26 C -0.4429(4) -0.6672(3) -0.7453(3) 0.0480(10) Uani 1 1 d . . . H26 H -0.5228 -0.6341 -0.7444 0.058 Uiso 1 1 calc R . . C31 C -0.9480(3) -0.5927(3) -0.8506(2) 0.0367(8) Uani 1 1 d . . . H31A H -0.9837 -0.5423 -0.8970 0.044 Uiso 1 1 calc R . . H31B H -1.0126 -0.6230 -0.8110 0.044 Uiso 1 1 calc R . . C32 C -0.7903(3) -0.6325(3) -0.9864(2) 0.0350(8) Uani 1 1 d . . . C34 C -0.7099(4) -0.7974(3) -1.0492(3) 0.0562(12) Uani 1 1 d . . . H34A H -0.7825 -0.8224 -1.0573 0.084 Uiso 1 1 calc R . . H34B H -0.6843 -0.8379 -0.9968 0.084 Uiso 1 1 calc R . . H34C H -0.6481 -0.8108 -1.0936 0.084 Uiso 1 1 calc R . . C35 C -0.7039(4) -0.5956(3) -1.1128(3) 0.0491(10) Uani 1 1 d . . . H35 H -0.6649 -0.6017 -1.1655 0.059 Uiso 1 1 calc R . . C36 C -0.7437(3) -0.5023(3) -1.0847(3) 0.0448(9) Uani 1 1 d . . . H36 H -0.7350 -0.4304 -1.1156 0.054 Uiso 1 1 calc R . . C38 C -0.9539(3) -0.7825(3) -0.9161(2) 0.0379(9) Uani 1 1 d . . . C39 C -0.9545(3) -0.8917(3) -0.8839(3) 0.0489(10) Uani 1 1 d . . . H39 H -0.8995 -0.9290 -0.8473 0.059 Uiso 1 1 calc R . . C40 C -1.0348(4) -0.9491(4) -0.9042(3) 0.0649(13) Uani 1 1 d . . . H40 H -1.0367 -1.0249 -0.8804 0.078 Uiso 1 1 calc R . . C41 C -1.1117(4) -0.8951(4) -0.9592(3) 0.0627(13) Uani 1 1 d . . . H41 H -1.1655 -0.9345 -0.9745 0.075 Uiso 1 1 calc R . . C42 C -1.1117(4) -0.7854(4) -0.9921(3) 0.0604(12) Uani 1 1 d . . . H42 H -1.1663 -0.7489 -1.0294 0.072 Uiso 1 1 calc R . . C43 C -1.0333(3) -0.7277(3) -0.9716(3) 0.0472(10) Uani 1 1 d . . . H43 H -1.0329 -0.6516 -0.9947 0.057 Uiso 1 1 calc R . . C44 C -0.8811(3) -0.5279(3) -0.8094(3) 0.0435(10) Uani 1 1 d . . . H44A H -0.9367 -0.4695 -0.7881 0.052 Uiso 1 1 calc R . . H44B H -0.8206 -0.4924 -0.8500 0.052 Uiso 1 1 calc R . . C51 C -0.9296(3) -0.6384(4) -0.6442(3) 0.0550(12) Uani 1 1 d . . . C56 C -0.9572(4) -0.7419(4) -0.6091(3) 0.0788(15) Uani 0.60 1 d P A 1 H56 H -0.9171 -0.8062 -0.6266 0.095 Uiso 0.60 1 calc PR A 1 N46 N -0.6705(5) -0.5355(5) -0.6362(4) 0.0415(13) Uani 0.60 1 d P A 1 N50 N -0.6952(8) -0.4287(6) -0.7584(6) 0.059(2) Uani 0.60 1 d P A 1 C52 C -0.9966(7) -0.5360(7) -0.6207(5) 0.049(2) Uani 0.60 1 d P A 1 H52A H -0.9767 -0.4655 -0.6479 0.058 Uiso 0.60 1 calc PR A 1 C53 C -1.0867(6) -0.5470(7) -0.5595(5) 0.059(2) Uani 0.60 1 d P A 1 H53A H -1.1346 -0.4839 -0.5450 0.071 Uiso 0.60 1 calc PR A 1 C54 C -1.1077(16) -0.6503(14) -0.5190(12) 0.080(4) Uani 0.60 1 d P A 1 H54 H -1.1635 -0.6584 -0.4715 0.096 Uiso 0.60 1 calc PR A 1 C45 C -0.7215(8) -0.5190(7) -0.7059(6) 0.0367(18) Uani 0.60 1 d P A 1 C47 C -0.6709(8) -0.6294(7) -0.5687(5) 0.061(2) Uani 0.60 1 d P A 1 H47C H -0.6274 -0.6174 -0.5266 0.091 Uiso 0.60 1 calc PR A 1 H47B H -0.6331 -0.6958 -0.5883 0.091 Uiso 0.60 1 calc PR A 1 H47A H -0.7524 -0.6386 -0.5455 0.091 Uiso 0.60 1 calc PR A 1 C48 C -0.6074(8) -0.4437(8) -0.6461(7) 0.058(3) Uani 0.60 1 d P A 1 H48A H -0.5645 -0.4284 -0.6072 0.070 Uiso 0.60 1 calc PR A 1 C49 C -0.6201(10) -0.3856(8) -0.7182(8) 0.057(3) Uani 0.60 1 d P A 1 H49A H -0.5834 -0.3215 -0.7416 0.069 Uiso 0.60 1 calc PR A 1 N50B N -0.9572(4) -0.7419(4) -0.6091(3) 0.0788(15) Uani 0.40 1 d P A 2 C54B C -1.087(2) -0.645(2) -0.5417(15) 0.071(8) Uiso 0.40 1 d PD A 2 H54B H -1.1526 -0.6167 -0.5078 0.085 Uiso 0.40 1 calc PR A 2 N46B N -1.0060(9) -0.5868(9) -0.6014(7) 0.049(3) Uiso 0.40 1 d PD A 2 C47B C -1.0091(11) -0.4727(11) -0.6146(8) 0.067(4) Uiso 0.40 1 d P A 2 H47D H -1.0728 -0.4429 -0.5772 0.101 Uiso 0.40 1 calc PR A 2 H47E H -1.0233 -0.4399 -0.6712 0.101 Uiso 0.40 1 calc PR A 2 H47F H -0.9336 -0.4553 -0.6048 0.101 Uiso 0.40 1 calc PR A 2 C59 C -0.6399(10) -0.5323(10) -0.5612(9) 0.065(3) Uiso 0.40 1 d P A 2 H59A H -0.6254 -0.5586 -0.5059 0.078 Uiso 0.40 1 calc PR A 2 C58 C -0.7043(11) -0.5868(12) -0.5981(9) 0.048(3) Uiso 0.40 1 d P A 2 H58A H -0.7304 -0.6540 -0.5686 0.058 Uiso 0.40 1 calc PR A 2 C57 C -0.7319(13) -0.5459(11) -0.6770(9) 0.036(4) Uiso 0.40 1 d P A 2 C61 C -0.634(2) -0.399(2) -0.6840(15) 0.074(8) Uiso 0.40 1 d P A 2 H61A H -0.6134 -0.3289 -0.7118 0.089 Uiso 0.40 1 calc PR A 2 C60 C -0.5990(14) -0.4426(12) -0.6054(10) 0.066(4) Uiso 0.40 1 d P A 2 H60A H -0.5467 -0.4076 -0.5845 0.079 Uiso 0.40 1 calc PR A 2 C62 C -0.6940(16) -0.4517(16) -0.7212(10) 0.056(5) Uiso 0.40 1 d P A 2 H62A H -0.7096 -0.4243 -0.7761 0.067 Uiso 0.40 1 calc PR A 2 C55 C -1.0489(5) -0.7444(5) -0.5458(4) 0.0911(19) Uani 1 1 d . . . H55A H -1.0730 -0.8137 -0.5193 0.109 Uiso 1 1 calc R A 1 N3 N -0.9272(3) -1.0717(3) -0.6872(3) 0.0693(11) Uani 1 1 d . . . N7 N -0.7856(3) -1.1386(3) -0.7727(3) 0.0628(11) Uani 1 1 d . . . N16 N -0.4445(3) -0.7478(3) -0.9827(2) 0.0528(9) Uani 1 1 d . . . N20 N -0.4191(3) -0.9284(3) -0.9426(2) 0.0484(9) Uani 1 1 d . . . N33 N -0.7320(3) -0.6797(2) -1.0490(2) 0.0418(8) Uani 1 1 d . . . N37 N -0.7978(3) -0.5238(2) -1.0065(2) 0.0419(8) Uani 1 1 d . . . P1 P -0.71744(8) -0.97224(7) -0.71293(6) 0.0331(2) Uani 1 1 d . . . P2 P -0.51338(8) -0.82410(7) -0.81344(6) 0.0312(2) Uani 1 1 d . . . P31 P -0.85059(8) -0.70572(7) -0.88786(6) 0.0329(2) Uani 1 1 d . . . P32 P -0.81038(8) -0.62048(8) -0.72549(6) 0.0380(2) Uani 1 1 d . A . P41 P -0.29484(10) -0.27265(10) -0.67853(8) 0.0574(3) Uani 1 1 d . . . F41 F -0.3169(3) -0.3952(2) -0.6450(2) 0.1091(12) Uani 1 1 d . . . F42 F -0.1864(3) -0.3104(3) -0.7378(2) 0.1090(12) Uani 1 1 d . . . F43 F -0.3819(2) -0.2606(3) -0.74600(19) 0.0876(10) Uani 1 1 d . . . F44 F -0.2710(3) -0.1485(2) -0.7103(3) 0.1106(12) Uani 1 1 d . . . F45 F -0.4029(3) -0.2298(3) -0.6201(2) 0.1073(12) Uani 1 1 d . . . F46 F -0.2105(2) -0.2837(2) -0.61004(18) 0.0722(8) 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 0.03403(8) 0.03037(7) 0.03358(9) -0.00348(5) -0.01045(6) -0.00177(5) C1 0.041(2) 0.0313(18) 0.034(2) -0.0036(15) -0.0064(17) -0.0032(15) C2 0.039(2) 0.042(2) 0.053(3) 0.0069(19) -0.020(2) -0.0093(17) C4 0.069(4) 0.104(4) 0.087(5) -0.009(4) -0.002(3) -0.013(3) C5 0.080(4) 0.063(3) 0.113(5) 0.007(3) -0.048(4) -0.030(3) C6 0.075(4) 0.053(3) 0.110(5) -0.016(3) -0.037(4) -0.023(3) C8 0.0321(19) 0.051(2) 0.033(2) 0.0008(17) -0.0021(17) -0.0055(16) C9 0.066(3) 0.101(4) 0.034(3) 0.017(3) -0.019(2) -0.020(3) C10 0.096(4) 0.100(4) 0.061(4) 0.021(3) -0.022(3) -0.029(3) C11 0.074(4) 0.115(5) 0.042(3) -0.017(3) -0.011(3) -0.030(3) C12 0.084(4) 0.090(4) 0.046(3) -0.029(3) -0.013(3) -0.017(3) C13 0.059(3) 0.073(3) 0.038(3) -0.012(2) -0.011(2) -0.004(2) C14 0.0336(19) 0.0342(18) 0.032(2) -0.0021(15) -0.0088(16) -0.0013(14) C15 0.037(2) 0.050(2) 0.032(2) 0.0017(18) -0.0106(17) -0.0153(17) C17 0.076(3) 0.068(3) 0.057(3) -0.003(2) -0.021(3) -0.022(3) C18 0.054(3) 0.083(3) 0.033(3) -0.020(2) -0.010(2) -0.014(2) C19 0.051(3) 0.076(3) 0.040(3) -0.026(2) -0.004(2) -0.010(2) C21 0.043(2) 0.041(2) 0.029(2) -0.0018(16) -0.0085(17) -0.0129(16) C22 0.043(2) 0.058(2) 0.045(3) 0.001(2) -0.015(2) -0.0221(19) C23 0.048(3) 0.073(3) 0.055(3) -0.001(2) -0.011(2) -0.014(2) C24 0.063(3) 0.076(3) 0.036(3) -0.011(2) -0.005(2) -0.023(2) C25 0.056(3) 0.063(3) 0.047(3) -0.024(2) 0.001(2) -0.027(2) C26 0.046(2) 0.055(3) 0.048(3) -0.015(2) -0.004(2) -0.0147(19) C31 0.0305(18) 0.041(2) 0.036(2) -0.0051(16) -0.0073(17) 0.0019(15) C32 0.0283(18) 0.047(2) 0.030(2) -0.0044(16) -0.0086(16) -0.0055(15) C34 0.069(3) 0.047(2) 0.054(3) -0.018(2) -0.007(2) -0.004(2) C35 0.051(2) 0.056(3) 0.037(3) 0.0044(19) -0.011(2) -0.012(2) C36 0.048(2) 0.047(2) 0.034(2) 0.0063(18) -0.011(2) -0.0090(18) C38 0.0335(19) 0.046(2) 0.036(2) -0.0116(17) -0.0041(17) -0.0058(16) C39 0.046(2) 0.046(2) 0.058(3) -0.010(2) -0.017(2) -0.0082(18) C40 0.066(3) 0.054(3) 0.084(4) -0.017(3) -0.021(3) -0.018(2) C41 0.054(3) 0.071(3) 0.076(4) -0.031(3) -0.019(3) -0.015(2) C42 0.052(3) 0.078(3) 0.058(3) -0.020(3) -0.025(2) -0.001(2) C43 0.039(2) 0.057(2) 0.046(3) -0.007(2) -0.015(2) -0.0044(18) C44 0.050(2) 0.036(2) 0.046(3) -0.0130(18) -0.015(2) 0.0019(17) C51 0.035(2) 0.089(3) 0.039(3) -0.015(2) -0.012(2) 0.010(2) C56 0.056(3) 0.082(3) 0.070(4) 0.018(3) 0.014(3) 0.008(2) N46 0.043(3) 0.047(3) 0.041(4) -0.020(3) -0.010(3) -0.006(3) N50 0.077(5) 0.033(4) 0.074(6) -0.003(4) -0.030(5) -0.016(3) C52 0.065(5) 0.024(4) 0.057(5) -0.012(4) -0.006(4) -0.002(4) C53 0.052(4) 0.060(5) 0.066(6) -0.031(4) -0.001(4) 0.015(4) C54 0.071(9) 0.083(9) 0.067(11) 0.002(7) -0.001(7) 0.011(6) C45 0.041(4) 0.033(4) 0.035(5) -0.008(4) -0.009(4) 0.005(3) C47 0.083(6) 0.072(6) 0.035(5) -0.010(4) -0.022(4) -0.019(5) C48 0.056(5) 0.067(6) 0.063(7) -0.034(5) -0.030(5) 0.005(4) C49 0.062(6) 0.038(5) 0.080(10) -0.017(5) -0.010(6) -0.026(4) N50B 0.056(3) 0.082(3) 0.070(4) 0.018(3) 0.014(3) 0.008(2) C55 0.076(4) 0.078(4) 0.088(5) 0.015(3) 0.034(3) -0.001(3) N3 0.055(2) 0.073(3) 0.076(3) 0.008(2) -0.019(2) -0.019(2) N7 0.072(3) 0.043(2) 0.084(3) -0.016(2) -0.032(2) -0.0127(18) N16 0.052(2) 0.061(2) 0.048(3) -0.0059(18) -0.0129(18) -0.0167(17) N20 0.0472(19) 0.061(2) 0.045(2) -0.0241(18) -0.0073(17) -0.0076(16) N33 0.0471(19) 0.0415(18) 0.037(2) -0.0068(15) -0.0100(16) -0.0045(14) N37 0.0460(19) 0.0388(18) 0.038(2) -0.0001(14) -0.0122(16) -0.0022(14) P1 0.0325(5) 0.0337(5) 0.0318(6) -0.0003(4) -0.0074(4) -0.0061(4) P2 0.0304(5) 0.0336(5) 0.0300(6) -0.0029(4) -0.0069(4) -0.0071(4) P31 0.0321(5) 0.0349(5) 0.0327(6) -0.0053(4) -0.0110(4) -0.0024(4) P32 0.0381(5) 0.0400(5) 0.0387(6) -0.0147(4) -0.0097(5) 0.0011(4) P41 0.0549(7) 0.0617(7) 0.0617(9) -0.0243(6) -0.0226(6) 0.0057(6) F41 0.119(3) 0.0669(19) 0.158(4) -0.017(2) -0.063(3) -0.0271(18) F42 0.0675(19) 0.174(3) 0.088(3) -0.059(2) -0.0212(18) 0.032(2) F43 0.0644(18) 0.131(3) 0.080(2) -0.057(2) -0.0337(16) 0.0218(17) F44 0.110(3) 0.071(2) 0.148(4) 0.012(2) -0.068(2) -0.0049(17) F45 0.076(2) 0.165(3) 0.095(3) -0.079(2) -0.0154(19) 0.020(2) F46 0.0817(18) 0.0658(16) 0.078(2) -0.0144(15) -0.0441(16) -0.0039(14) _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 P31 2.4130(9) . ? Au1 P2 2.4197(9) . ? Au1 P32 2.4198(9) . ? Au1 P1 2.4301(9) . ? C1 C14 1.514(5) . ? C1 P1 1.841(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N7 1.336(5) . ? C2 N3 1.347(5) . ? C2 P1 1.821(4) . ? C4 N3 1.408(6) . ? C4 H4C 0.9800 . ? C4 H4B 0.9800 . ? C4 H4A 0.9800 . ? C5 C6 1.333(7) . ? C5 N3 1.430(6) . ? C5 H5 0.9500 . ? C6 N7 1.371(6) . ? C6 H6 0.9500 . ? C8 C13 1.379(5) . ? C8 C9 1.414(6) . ? C8 P1 1.803(4) . ? C9 C10 1.321(7) . ? C9 H9 0.9500 . ? C10 C11 1.397(7) . ? C10 H10 0.9500 . ? C11 C12 1.342(7) . ? C11 H11 0.9500 . ? C12 C13 1.376(6) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 P2 1.827(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N20 1.331(5) . ? C15 N16 1.363(5) . ? C15 P2 1.819(4) . ? C17 N16 1.409(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.328(6) . ? C18 N16 1.406(5) . ? C18 H18 0.9500 . ? C19 N20 1.370(5) . ? C19 H19 0.9500 . ? C21 C26 1.371(5) . ? C21 C22 1.404(5) . ? C21 P2 1.824(4) . ? C22 C23 1.364(6) . ? C22 H22 0.9500 . ? C23 C24 1.381(6) . ? C23 H23 0.9500 . ? C24 C25 1.361(6) . ? C24 H24 0.9500 . ? C25 C26 1.389(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C44 1.538(5) . ? C31 P31 1.832(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N37 1.325(4) . ? C32 N33 1.366(5) . ? C32 P31 1.812(4) . ? C34 N33 1.462(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.351(5) . ? C35 N33 1.372(5) . ? C35 H35 0.9500 . ? C36 N37 1.364(5) . ? C36 H36 0.9500 . ? C38 C39 1.361(5) . ? C38 C43 1.402(5) . ? C38 P31 1.825(4) . ? C39 C40 1.386(5) . ? C39 H39 0.9500 . ? C40 C41 1.374(6) . ? C40 H40 0.9500 . ? C41 C42 1.368(6) . ? C41 H41 0.9500 . ? C42 C43 1.374(6) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 P32 1.828(4) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C51 N46B 1.249(11) . ? C51 C56 1.370(6) . ? C51 C52 1.494(8) . ? C51 P32 1.799(5) . ? C56 C55 1.389(6) . ? C56 H56 0.9500 . ? N46 C45 1.356(10) . ? N46 C48 1.428(11) . ? N46 C47 1.447(10) . ? N50 C45 1.323(13) . ? N50 C49 1.414(13) . ? C52 C53 1.355(11) . ? C52 H52A 0.9500 . ? C53 C54 1.367(19) . ? C53 H53A 0.9500 . ? C54 C55 1.399(19) . ? C54 H54 0.9500 . ? C45 P32 1.872(9) . ? C47 H47C 0.9800 . ? C47 H47B 0.9800 . ? C47 H47A 0.9800 . ? C48 C49 1.290(18) . ? C48 H48A 0.9500 . ? C49 H49A 0.9500 . ? C54B C55 1.27(3) . ? C54B N46B 1.429(16) . ? C54B H54B 0.9500 . ? N46B C47B 1.397(14) . ? C47B H47D 0.9800 . ? C47B H47E 0.9800 . ? C47B H47F 0.9800 . ? C59 C60 1.321(19) . ? C59 C58 1.381(18) . ? C59 H59A 0.9500 . ? C58 C57 1.382(19) . ? C58 H58A 0.9500 . ? C57 C62 1.35(2) . ? C57 P32 1.793(16) . ? C61 C62 1.34(3) . ? C61 C60 1.41(3) . ? C61 H61A 0.9500 . ? C60 H60A 0.9500 . ? C62 H62A 0.9500 . ? C55 H55A 0.9500 . ? P41 F42 1.565(3) . ? P41 F41 1.567(3) . ? P41 F45 1.576(3) . ? P41 F44 1.587(3) . ? P41 F46 1.592(3) . ? P41 F43 1.598(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 P31 Au1 P2 121.54(3) . . ? P31 Au1 P32 85.44(3) . . ? P2 Au1 P32 122.04(3) . . ? P31 Au1 P1 120.26(3) . . ? P2 Au1 P1 84.94(3) . . ? P32 Au1 P1 127.30(4) . . ? C14 C1 P1 109.7(2) . . ? C14 C1 H1A 109.7 . . ? P1 C1 H1A 109.7 . . ? C14 C1 H1B 109.7 . . ? P1 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? N7 C2 N3 110.8(4) . . ? N7 C2 P1 122.6(3) . . ? N3 C2 P1 126.6(3) . . ? N3 C4 H4C 109.5 . . ? N3 C4 H4B 109.5 . . ? H4C C4 H4B 109.5 . . ? N3 C4 H4A 109.5 . . ? H4C C4 H4A 109.5 . . ? H4B C4 H4A 109.5 . . ? C6 C5 N3 104.3(5) . . ? C6 C5 H5 127.9 . . ? N3 C5 H5 127.9 . . ? C5 C6 N7 112.2(5) . . ? C5 C6 H6 123.9 . . ? N7 C6 H6 123.9 . . ? C13 C8 C9 119.4(4) . . ? C13 C8 P1 120.5(3) . . ? C9 C8 P1 120.1(3) . . ? C10 C9 C8 121.5(5) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C11 117.6(6) . . ? C9 C10 H10 121.2 . . ? C11 C10 H10 121.2 . . ? C12 C11 C10 122.9(5) . . ? C12 C11 H11 118.5 . . ? C10 C11 H11 118.5 . . ? C11 C12 C13 119.6(4) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C12 C13 C8 119.0(4) . . ? C12 C13 H13 120.5 . . ? C8 C13 H13 120.5 . . ? C1 C14 P2 112.0(2) . . ? C1 C14 H14A 109.2 . . ? P2 C14 H14A 109.2 . . ? C1 C14 H14B 109.2 . . ? P2 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? N20 C15 N16 109.8(4) . . ? N20 C15 P2 124.0(3) . . ? N16 C15 P2 126.1(3) . . ? N16 C17 H17A 109.5 . . ? N16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 N16 103.8(4) . . ? C19 C18 H18 128.1 . . ? N16 C18 H18 128.1 . . ? C18 C19 N20 113.2(4) . . ? C18 C19 H19 123.4 . . ? N20 C19 H19 123.4 . . ? C26 C21 C22 119.7(4) . . ? C26 C21 P2 119.8(3) . . ? C22 C21 P2 120.3(3) . . ? C23 C22 C21 120.5(4) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 119.1(4) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C25 C24 C23 121.0(4) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 120.4(4) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C21 C26 C25 119.2(4) . . ? C21 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C44 C31 P31 111.7(2) . . ? C44 C31 H31A 109.3 . . ? P31 C31 H31A 109.3 . . ? C44 C31 H31B 109.3 . . ? P31 C31 H31B 109.3 . . ? H31A C31 H31B 107.9 . . ? N37 C32 N33 111.1(3) . . ? N37 C32 P31 123.1(3) . . ? N33 C32 P31 125.8(3) . . ? N33 C34 H34A 109.5 . . ? N33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 N33 105.3(4) . . ? C36 C35 H35 127.3 . . ? N33 C35 H35 127.3 . . ? C35 C36 N37 111.7(4) . . ? C35 C36 H36 124.1 . . ? N37 C36 H36 124.1 . . ? C39 C38 C43 119.9(4) . . ? C39 C38 P31 120.8(3) . . ? C43 C38 P31 119.3(3) . . ? C38 C39 C40 120.6(4) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C41 C40 C39 119.2(4) . . ? C41 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? C42 C41 C40 120.8(4) . . ? C42 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? C41 C42 C43 120.3(4) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C42 C43 C38 119.2(4) . . ? C42 C43 H43 120.4 . . ? C38 C43 H43 120.4 . . ? C31 C44 P32 110.0(3) . . ? C31 C44 H44A 109.7 . . ? P32 C44 H44A 109.7 . . ? C31 C44 H44B 109.7 . . ? P32 C44 H44B 109.7 . . ? H44A C44 H44B 108.2 . . ? N46B C51 C56 97.4(6) . . ? N46B C51 C52 26.3(5) . . ? C56 C51 C52 123.5(5) . . ? N46B C51 P32 142.7(6) . . ? C56 C51 P32 119.9(3) . . ? C52 C51 P32 116.5(5) . . ? C51 C56 C55 114.1(5) . . ? C51 C56 H56 123.0 . . ? C55 C56 H56 123.0 . . ? C45 N46 C48 105.0(7) . . ? C45 N46 C47 128.2(7) . . ? C48 N46 C47 126.7(7) . . ? C45 N50 C49 103.7(9) . . ? C53 C52 C51 117.8(7) . . ? C53 C52 H52A 121.1 . . ? C51 C52 H52A 121.1 . . ? C52 C53 C54 119.0(10) . . ? C52 C53 H53A 120.5 . . ? C54 C53 H53A 120.5 . . ? C53 C54 C55 121.6(14) . . ? C53 C54 H54 119.2 . . ? C55 C54 H54 119.2 . . ? N50 C45 N46 112.6(9) . . ? N50 C45 P32 125.2(7) . . ? N46 C45 P32 122.1(7) . . ? N46 C47 H47C 109.5 . . ? N46 C47 H47B 109.5 . . ? H47C C47 H47B 109.5 . . ? N46 C47 H47A 109.5 . . ? H47C C47 H47A 109.5 . . ? H47B C47 H47A 109.5 . . ? C49 C48 N46 106.7(7) . . ? C49 C48 H48A 126.6 . . ? N46 C48 H48A 126.6 . . ? C48 C49 N50 111.9(8) . . ? C48 C49 H49A 124.1 . . ? N50 C49 H49A 124.1 . . ? C55 C54B N46B 101.8(18) . . ? C55 C54B H54B 129.1 . . ? N46B C54B H54B 129.1 . . ? C51 N46B C47B 118.0(10) . . ? C51 N46B C54B 119.7(15) . . ? C47B N46B C54B 122.3(16) . . ? N46B C47B H47D 109.5 . . ? N46B C47B H47E 109.5 . . ? H47D C47B H47E 109.5 . . ? N46B C47B H47F 109.5 . . ? H47D C47B H47F 109.5 . . ? H47E C47B H47F 109.5 . . ? C60 C59 C58 117.7(15) . . ? C60 C59 H59A 121.1 . . ? C58 C59 H59A 121.1 . . ? C59 C58 C57 121.6(15) . . ? C59 C58 H58A 119.2 . . ? C57 C58 H58A 119.2 . . ? C62 C57 C58 120.6(15) . . ? C62 C57 P32 118.2(13) . . ? C58 C57 P32 121.1(11) . . ? C62 C61 C60 123(2) . . ? C62 C61 H61A 118.4 . . ? C60 C61 H61A 118.4 . . ? C59 C60 C61 119.3(17) . . ? C59 C60 H60A 120.3 . . ? C61 C60 H60A 120.3 . . ? C61 C62 C57 116.9(18) . . ? C61 C62 H62A 121.5 . . ? C57 C62 H62A 121.5 . . ? C54B C55 C56 106.8(9) . . ? C54B C55 C54 17.2(13) . . ? C56 C55 C54 123.4(9) . . ? C54B C55 H55A 134.7 . . ? C56 C55 H55A 118.3 . . ? C54 C55 H55A 118.3 . . ? C2 N3 C4 127.4(4) . . ? C2 N3 C5 107.1(4) . . ? C4 N3 C5 125.4(5) . . ? C2 N7 C6 105.6(4) . . ? C15 N16 C18 108.0(4) . . ? C15 N16 C17 125.6(4) . . ? C18 N16 C17 126.3(4) . . ? C15 N20 C19 105.1(4) . . ? C32 N33 C35 107.1(3) . . ? C32 N33 C34 126.2(3) . . ? C35 N33 C34 126.7(4) . . ? C32 N37 C36 104.7(3) . . ? C8 P1 C2 103.42(19) . . ? C8 P1 C1 102.46(17) . . ? C2 P1 C1 100.14(17) . . ? C8 P1 Au1 119.12(13) . . ? C2 P1 Au1 125.50(13) . . ? C1 P1 Au1 101.98(12) . . ? C15 P2 C21 104.28(17) . . ? C15 P2 C14 100.64(17) . . ? C21 P2 C14 101.64(16) . . ? C15 P2 Au1 118.77(12) . . ? C21 P2 Au1 123.18(12) . . ? C14 P2 Au1 104.61(11) . . ? C32 P31 C38 102.24(17) . . ? C32 P31 C31 100.17(17) . . ? C38 P31 C31 102.80(16) . . ? C32 P31 Au1 119.94(11) . . ? C38 P31 Au1 123.87(13) . . ? C31 P31 Au1 104.06(12) . . ? C57 P32 C51 95.6(5) . . ? C57 P32 C44 110.4(4) . . ? C51 P32 C44 103.36(19) . . ? C57 P32 C45 16.7(4) . . ? C51 P32 C45 108.2(3) . . ? C44 P32 C45 96.3(3) . . ? C57 P32 Au1 124.8(5) . . ? C51 P32 Au1 117.16(16) . . ? C44 P32 Au1 103.88(12) . . ? C45 P32 Au1 123.4(2) . . ? F42 P41 F41 90.5(2) . . ? F42 P41 F45 177.7(2) . . ? F41 P41 F45 91.8(2) . . ? F42 P41 F44 89.9(2) . . ? F41 P41 F44 178.4(2) . . ? F45 P41 F44 87.8(2) . . ? F42 P41 F46 89.86(17) . . ? F41 P41 F46 89.78(17) . . ? F45 P41 F46 90.04(16) . . ? F44 P41 F46 88.70(16) . . ? F42 P41 F43 91.41(16) . . ? F41 P41 F43 90.28(18) . . ? F45 P41 F43 88.69(16) . . ? F44 P41 F43 91.23(19) . . ? F46 P41 F43 178.73(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 C5 C6 N7 -1.3(6) . . . . ? C13 C8 C9 C10 0.5(7) . . . . ? P1 C8 C9 C10 177.2(4) . . . . ? C8 C9 C10 C11 0.5(8) . . . . ? C9 C10 C11 C12 -1.2(8) . . . . ? C10 C11 C12 C13 0.9(8) . . . . ? C11 C12 C13 C8 0.1(7) . . . . ? C9 C8 C13 C12 -0.8(6) . . . . ? P1 C8 C13 C12 -177.5(4) . . . . ? P1 C1 C14 P2 -58.3(3) . . . . ? N16 C18 C19 N20 -1.5(5) . . . . ? C26 C21 C22 C23 0.7(6) . . . . ? P2 C21 C22 C23 -175.1(3) . . . . ? C21 C22 C23 C24 0.9(7) . . . . ? C22 C23 C24 C25 -1.6(7) . . . . ? C23 C24 C25 C26 0.8(7) . . . . ? C22 C21 C26 C25 -1.5(6) . . . . ? P2 C21 C26 C25 174.4(3) . . . . ? C24 C25 C26 C21 0.8(7) . . . . ? N33 C35 C36 N37 -1.3(5) . . . . ? C43 C38 C39 C40 -1.4(6) . . . . ? P31 C38 C39 C40 178.6(3) . . . . ? C38 C39 C40 C41 1.9(7) . . . . ? C39 C40 C41 C42 -1.7(7) . . . . ? C40 C41 C42 C43 1.0(7) . . . . ? C41 C42 C43 C38 -0.4(7) . . . . ? C39 C38 C43 C42 0.6(6) . . . . ? P31 C38 C43 C42 -179.4(3) . . . . ? P31 C31 C44 P32 -57.1(3) . . . . ? N46B C51 C56 C55 -0.9(8) . . . . ? C52 C51 C56 C55 -3.9(8) . . . . ? P32 C51 C56 C55 178.5(4) . . . . ? N46B C51 C52 C53 -4.2(12) . . . . ? C56 C51 C52 C53 2.4(10) . . . . ? P32 C51 C52 C53 -179.8(6) . . . . ? C51 C52 C53 C54 3.9(15) . . . . ? C52 C53 C54 C55 -8(2) . . . . ? C49 N50 C45 N46 0.6(10) . . . . ? C49 N50 C45 P32 -175.4(7) . . . . ? C48 N46 C45 N50 1.3(9) . . . . ? C47 N46 C45 N50 -174.2(8) . . . . ? C48 N46 C45 P32 177.5(6) . . . . ? C47 N46 C45 P32 2.0(10) . . . . ? C45 N46 C48 C49 -2.9(9) . . . . ? C47 N46 C48 C49 172.7(8) . . . . ? N46 C48 C49 N50 3.4(11) . . . . ? C45 N50 C49 C48 -2.6(12) . . . . ? C56 C51 N46B C47B 178.2(10) . . . . ? C52 C51 N46B C47B -7.3(11) . . . . ? P32 C51 N46B C47B -0.9(16) . . . . ? C56 C51 N46B C54B -2.4(18) . . . . ? C52 C51 N46B C54B 172(3) . . . . ? P32 C51 N46B C54B 178.5(16) . . . . ? C55 C54B N46B C51 5(3) . . . . ? C55 C54B N46B C47B -175.7(14) . . . . ? C60 C59 C58 C57 -3.9(19) . . . . ? C59 C58 C57 C62 1(2) . . . . ? C59 C58 C57 P32 177.4(10) . . . . ? C58 C59 C60 C61 7(2) . . . . ? C62 C61 C60 C59 -9(3) . . . . ? C60 C61 C62 C57 6(3) . . . . ? C58 C57 C62 C61 -3(3) . . . . ? P32 C57 C62 C61 -178.7(15) . . . . ? N46B C54B C55 C56 -5(2) . . . . ? N46B C54B C55 C54 162(9) . . . . ? C51 C56 C55 C54B 4.0(17) . . . . ? C51 C56 C55 C54 -0.7(13) . . . . ? C53 C54 C55 C54B -8(6) . . . . ? C53 C54 C55 C56 7(2) . . . . ? N7 C2 N3 C4 -178.5(5) . . . . ? P1 C2 N3 C4 -0.5(7) . . . . ? N7 C2 N3 C5 0.3(5) . . . . ? P1 C2 N3 C5 178.3(3) . . . . ? C6 C5 N3 C2 0.6(5) . . . . ? C6 C5 N3 C4 179.4(5) . . . . ? N3 C2 N7 C6 -1.1(5) . . . . ? P1 C2 N7 C6 -179.2(3) . . . . ? C5 C6 N7 C2 1.5(6) . . . . ? N20 C15 N16 C18 -1.8(4) . . . . ? P2 C15 N16 C18 -178.0(3) . . . . ? N20 C15 N16 C17 -179.5(4) . . . . ? P2 C15 N16 C17 4.3(6) . . . . ? C19 C18 N16 C15 2.0(4) . . . . ? C19 C18 N16 C17 179.6(4) . . . . ? N16 C15 N20 C19 0.9(4) . . . . ? P2 C15 N20 C19 177.2(3) . . . . ? C18 C19 N20 C15 0.4(5) . . . . ? N37 C32 N33 C35 -1.6(4) . . . . ? P31 C32 N33 C35 178.6(3) . . . . ? N37 C32 N33 C34 -178.5(3) . . . . ? P31 C32 N33 C34 1.7(5) . . . . ? C36 C35 N33 C32 1.7(4) . . . . ? C36 C35 N33 C34 178.5(4) . . . . ? N33 C32 N37 C36 0.8(4) . . . . ? P31 C32 N37 C36 -179.4(3) . . . . ? C35 C36 N37 C32 0.3(4) . . . . ? C13 C8 P1 C2 -141.8(3) . . . . ? C9 C8 P1 C2 41.5(4) . . . . ? C13 C8 P1 C1 114.4(3) . . . . ? C9 C8 P1 C1 -62.3(3) . . . . ? C13 C8 P1 Au1 2.9(4) . . . . ? C9 C8 P1 Au1 -173.8(3) . . . . ? N7 C2 P1 C8 -119.1(4) . . . . ? N3 C2 P1 C8 63.1(4) . . . . ? N7 C2 P1 C1 -13.5(4) . . . . ? N3 C2 P1 C1 168.7(4) . . . . ? N7 C2 P1 Au1 99.2(3) . . . . ? N3 C2 P1 Au1 -78.6(4) . . . . ? C14 C1 P1 C8 -74.4(3) . . . . ? C14 C1 P1 C2 179.3(3) . . . . ? C14 C1 P1 Au1 49.4(3) . . . . ? P31 Au1 P1 C8 -145.37(13) . . . . ? P2 Au1 P1 C8 90.83(14) . . . . ? P32 Au1 P1 C8 -36.18(14) . . . . ? P31 Au1 P1 C2 -9.00(19) . . . . ? P2 Au1 P1 C2 -132.80(18) . . . . ? P32 Au1 P1 C2 100.19(18) . . . . ? P31 Au1 P1 C1 102.87(12) . . . . ? P2 Au1 P1 C1 -20.93(12) . . . . ? P32 Au1 P1 C1 -147.94(12) . . . . ? N20 C15 P2 C21 116.0(3) . . . . ? N16 C15 P2 C21 -68.3(4) . . . . ? N20 C15 P2 C14 10.9(4) . . . . ? N16 C15 P2 C14 -173.4(3) . . . . ? N20 C15 P2 Au1 -102.4(3) . . . . ? N16 C15 P2 Au1 73.3(3) . . . . ? C26 C21 P2 C15 127.9(3) . . . . ? C22 C21 P2 C15 -56.2(4) . . . . ? C26 C21 P2 C14 -127.8(3) . . . . ? C22 C21 P2 C14 48.1(3) . . . . ? C26 C21 P2 Au1 -11.5(4) . . . . ? C22 C21 P2 Au1 164.3(3) . . . . ? C1 C14 P2 C15 -87.8(3) . . . . ? C1 C14 P2 C21 165.0(3) . . . . ? C1 C14 P2 Au1 35.9(3) . . . . ? P31 Au1 P2 C15 -15.41(15) . . . . ? P32 Au1 P2 C15 -121.31(14) . . . . ? P1 Au1 P2 C15 107.22(14) . . . . ? P31 Au1 P2 C21 118.64(15) . . . . ? P32 Au1 P2 C21 12.75(16) . . . . ? P1 Au1 P2 C21 -118.72(15) . . . . ? P31 Au1 P2 C14 -126.56(12) . . . . ? P32 Au1 P2 C14 127.55(12) . . . . ? P1 Au1 P2 C14 -3.92(12) . . . . ? N37 C32 P31 C38 121.3(3) . . . . ? N33 C32 P31 C38 -58.9(3) . . . . ? N37 C32 P31 C31 15.7(3) . . . . ? N33 C32 P31 C31 -164.5(3) . . . . ? N37 C32 P31 Au1 -97.1(3) . . . . ? N33 C32 P31 Au1 82.6(3) . . . . ? C39 C38 P31 C32 131.9(3) . . . . ? C43 C38 P31 C32 -48.1(3) . . . . ? C39 C38 P31 C31 -124.6(3) . . . . ? C43 C38 P31 C31 55.4(3) . . . . ? C39 C38 P31 Au1 -7.6(4) . . . . ? C43 C38 P31 Au1 172.3(2) . . . . ? C44 C31 P31 C32 -84.7(3) . . . . ? C44 C31 P31 C38 170.1(3) . . . . ? C44 C31 P31 Au1 39.9(3) . . . . ? P2 Au1 P31 C32 -23.99(14) . . . . ? P32 Au1 P31 C32 101.13(14) . . . . ? P1 Au1 P31 C32 -127.78(13) . . . . ? P2 Au1 P31 C38 108.95(14) . . . . ? P32 Au1 P31 C38 -125.93(14) . . . . ? P1 Au1 P31 C38 5.16(15) . . . . ? P2 Au1 P31 C31 -134.75(12) . . . . ? P32 Au1 P31 C31 -9.62(13) . . . . ? P1 Au1 P31 C31 121.47(13) . . . . ? C62 C57 P32 C51 -131.7(13) . . . . ? C58 C57 P32 C51 52.1(12) . . . . ? C62 C57 P32 C44 -25.2(14) . . . . ? C58 C57 P32 C44 158.6(10) . . . . ? C62 C57 P32 C45 8.3(15) . . . . ? C58 C57 P32 C45 -168(3) . . . . ? C62 C57 P32 Au1 99.5(13) . . . . ? C58 C57 P32 Au1 -76.6(12) . . . . ? N46B C51 P32 C57 54.1(10) . . . . ? C56 C51 P32 C57 -125.0(6) . . . . ? C52 C51 P32 C57 57.2(6) . . . . ? N46B C51 P32 C44 -58.5(9) . . . . ? C56 C51 P32 C44 122.5(4) . . . . ? C52 C51 P32 C44 -55.3(4) . . . . ? N46B C51 P32 C45 42.9(10) . . . . ? C56 C51 P32 C45 -136.2(5) . . . . ? C52 C51 P32 C45 46.0(5) . . . . ? N46B C51 P32 Au1 -172.0(9) . . . . ? C56 C51 P32 Au1 9.0(4) . . . . ? C52 C51 P32 Au1 -168.9(4) . . . . ? C31 C44 P32 C57 179.9(5) . . . . ? C31 C44 P32 C51 -78.9(3) . . . . ? C31 C44 P32 C45 170.7(4) . . . . ? C31 C44 P32 Au1 44.0(3) . . . . ? N50 C45 P32 C57 -169(3) . . . . ? N46 C45 P32 C57 15.8(18) . . . . ? N50 C45 P32 C51 -126.2(7) . . . . ? N46 C45 P32 C51 58.1(6) . . . . ? N50 C45 P32 C44 -19.9(8) . . . . ? N46 C45 P32 C44 164.4(6) . . . . ? N50 C45 P32 Au1 91.4(7) . . . . ? N46 C45 P32 Au1 -84.3(7) . . . . ? P31 Au1 P32 C57 -142.9(5) . . . . ? P2 Au1 P32 C57 -18.2(5) . . . . ? P1 Au1 P32 C57 92.0(5) . . . . ? P31 Au1 P32 C51 97.88(15) . . . . ? P2 Au1 P32 C51 -137.44(15) . . . . ? P1 Au1 P32 C51 -27.20(16) . . . . ? P31 Au1 P32 C44 -15.34(14) . . . . ? P2 Au1 P32 C44 109.34(14) . . . . ? P1 Au1 P32 C44 -140.42(14) . . . . ? P31 Au1 P32 C45 -122.7(4) . . . . ? P2 Au1 P32 C45 1.9(4) . . . . ? P1 Au1 P32 C45 112.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.848 _refine_diff_density_min -1.169 _refine_diff_density_rms 0.112 # Attachment '- kp270609.cif' data_kp270609 _database_code_depnum_ccdc_archive 'CCDC 808835' #TrackingRef '- kp270609.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23.50 H26 Au2 Cl3 N4 O0.50 P2' _chemical_formula_weight 934.71 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' O O 0.0106 0.0060 '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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.94880(13) _cell_length_b 12.37340(13) _cell_length_c 11.42410(14) _cell_angle_alpha 90.00 _cell_angle_beta 97.4074(11) _cell_angle_gamma 90.00 _cell_volume 1534.75(3) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 26106 _cell_measurement_theta_min 2.7528 _cell_measurement_theta_max 32.7485 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.023 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 9.935 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2292 _exptl_absorpt_correction_T_max 0.8261 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Xcalibur Ruby CCD' _diffrn_measurement_method '\o oscillation scan' _diffrn_detector_area_resol_mean 10.4498 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46544 _diffrn_reflns_av_R_equivalents 0.0674 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 30.51 _reflns_number_total 9360 _reflns_number_gt 8417 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis^Pro^ (Oxford, 2007)' _computing_cell_refinement 'CrysAlis^Pro^ (Oxford, 2007)' _computing_data_reduction 'CrysAlis^Pro^ (Oxford, 2007)' _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The C-C and the C-O distances of the partial occupied and disordered ethanol molecule had to be restrained. Furthermore, only the chlorine atoms of all the partial occupied and disordered solvent molecules could be anisotropically refined. The structure was refined as a racemic twin in a ratio of 56:44. ; _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^)+(0.0427P)^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 constr _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 0.00(6) _refine_ls_number_reflns 9360 _refine_ls_number_parameters 330 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0777 _refine_ls_wR_factor_gt 0.0766 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 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 0.443888(19) 0.797584(17) 0.53992(2) 0.02269(5) Uani 1 1 d . . . Au2 Au 0.56514(2) 0.748620(18) 0.31287(2) 0.02682(6) Uani 1 1 d . . . C1 C 0.2813(7) 0.9409(6) 0.3182(7) 0.0327(15) Uani 1 1 d . . . H1A H 0.2436 0.9268 0.2361 0.039 Uiso 1 1 calc R . . H1B H 0.2289 0.9945 0.3526 0.039 Uiso 1 1 calc R . . C2 C 0.2752(7) 0.7112(6) 0.2906(7) 0.0345(15) Uani 1 1 d . . . C4 C 0.3026(8) 0.5526(6) 0.4315(8) 0.045(2) Uani 1 1 d . . . H4C H 0.3614 0.4928 0.4326 0.067 Uiso 1 1 calc R . . H4B H 0.2229 0.5248 0.4486 0.067 Uiso 1 1 calc R . . H4A H 0.3335 0.6060 0.4914 0.067 Uiso 1 1 calc R . . C5 C 0.2864(9) 0.5552(8) 0.2040(9) 0.057(3) Uani 1 1 d . . . H5 H 0.2938 0.4800 0.1896 0.069 Uiso 1 1 calc R . . C6 C 0.2731(10) 0.6347(8) 0.1221(9) 0.060(3) Uani 1 1 d . . . H6 H 0.2703 0.6239 0.0395 0.072 Uiso 1 1 calc R . . C8 C 0.1323(6) 0.8109(6) 0.4590(8) 0.0382(17) Uani 1 1 d . . . C9 C 0.0409(7) 0.7366(7) 0.4116(10) 0.055(2) Uani 1 1 d . . . H9 H 0.0541 0.6880 0.3501 0.067 Uiso 1 1 calc R . . C10 C -0.0678(8) 0.7386(10) 0.4593(13) 0.078(4) Uani 1 1 d . . . H10 H -0.1322 0.6913 0.4281 0.094 Uiso 1 1 calc R . . C11 C -0.0868(9) 0.8043(11) 0.5478(14) 0.087(5) Uani 1 1 d . . . H11 H -0.1626 0.7999 0.5797 0.104 Uiso 1 1 calc R . . C12 C 0.0045(10) 0.8817(9) 0.5966(12) 0.078(4) Uani 1 1 d . . . H12 H -0.0105 0.9308 0.6571 0.094 Uiso 1 1 calc R . . C13 C 0.1135(8) 0.8803(7) 0.5505(10) 0.056(3) Uani 1 1 d . . . H13 H 0.1778 0.9277 0.5818 0.067 Uiso 1 1 calc R . . C14 C 0.4068(6) 0.9898(5) 0.3149(7) 0.0311(14) Uani 1 1 d . . . H14A H 0.4437 1.0031 0.3974 0.037 Uiso 1 1 calc R . . H14B H 0.3953 1.0611 0.2757 0.037 Uiso 1 1 calc R . . C15 C 0.4568(8) 0.9266(5) 0.0898(6) 0.0378(17) Uani 1 1 d . . . C17 C 0.5834(11) 0.7866(12) 0.0052(9) 0.078(4) Uani 1 1 d . . . H17C H 0.6155 0.7788 -0.0706 0.118 Uiso 1 1 calc R . . H17B H 0.5433 0.7192 0.0241 0.118 Uiso 1 1 calc R . . H17A H 0.6515 0.8027 0.0672 0.118 Uiso 1 1 calc R . . C18 C 0.4437(14) 0.9135(9) -0.1028(9) 0.079(4) Uani 1 1 d . . . H18 H 0.4574 0.8957 -0.1809 0.094 Uiso 1 1 calc R . . C19 C 0.3611(14) 0.9913(9) -0.0670(8) 0.081(4) Uani 1 1 d . . . H19 H 0.3059 1.0331 -0.1199 0.098 Uiso 1 1 calc R . . C21 C 0.6541(7) 1.0000(6) 0.2577(6) 0.0316(14) Uani 1 1 d . . . C22 C 0.6425(9) 1.1071(7) 0.2194(8) 0.046(2) Uani 1 1 d . . . H22 H 0.5648 1.1355 0.1869 0.056 Uiso 1 1 calc R . . C23 C 0.7494(9) 1.1720(7) 0.2303(9) 0.055(2) Uani 1 1 d . . . H23 H 0.7447 1.2452 0.2050 0.067 Uiso 1 1 calc R . . C24 C 0.8592(9) 1.1292(9) 0.2772(10) 0.058(3) Uani 1 1 d . . . H24 H 0.9306 1.1736 0.2862 0.070 Uiso 1 1 calc R . . C25 C 0.8689(10) 1.0245(10) 0.3112(13) 0.076(4) Uani 1 1 d . . . H25 H 0.9471 0.9957 0.3412 0.091 Uiso 1 1 calc R . . C26 C 0.7660(9) 0.9591(8) 0.3029(10) 0.060(3) Uani 1 1 d . . . H26 H 0.7731 0.8860 0.3284 0.071 Uiso 1 1 calc R . . C71A C -0.0684(16) 0.6825(16) -0.0092(11) 0.071(5) Uiso 0.35 1 d PD A 1 H71A H -0.0113 0.7429 -0.0187 0.085 Uiso 0.35 1 calc PR A 1 H71B H -0.0169 0.6165 -0.0068 0.085 Uiso 0.35 1 calc PR A 1 O71A O -0.1395(16) 0.6761(16) -0.1217(13) 0.056(5) Uiso 0.35 1 d PD A 1 C72A C -0.0935(18) 0.6945(17) 0.1197(13) 0.072(5) Uiso 0.35 1 d PD A 1 H72A H -0.1437 0.6337 0.1406 0.087 Uiso 0.35 1 calc PR A 1 H72B H -0.1377 0.7623 0.1285 0.087 Uiso 0.35 1 calc PR A 1 H72C H -0.0152 0.6953 0.1719 0.087 Uiso 0.35 1 calc PR A 1 C71B C -0.0684(16) 0.6825(16) -0.0092(11) 0.071(5) Uiso 0.25 1 d PD B 2 H71C H 0.0223 0.6874 -0.0051 0.085 Uiso 0.35 1 calc PR B 2 H71D H -0.0892 0.6062 -0.0293 0.085 Uiso 0.35 1 calc PR B 2 C72B C -0.0935(18) 0.6945(17) 0.1197(13) 0.072(5) Uiso 0.25 1 d P B 2 H72D H -0.1437 0.6337 0.1406 0.087 Uiso 0.25 1 calc PR B 2 H72E H -0.1377 0.7623 0.1285 0.087 Uiso 0.25 1 calc PR B 2 H72F H -0.0152 0.6953 0.1719 0.087 Uiso 0.25 1 calc PR B 2 O71B O -0.1140(17) 0.7414(18) -0.1130(15) 0.037(4) Uiso 0.25 1 d PD B 2 C73 C -0.003(2) 0.797(2) 0.014(2) 0.063(6) Uiso 0.40 1 d P C 3 H73A H -0.0510 0.7289 0.0075 0.076 Uiso 0.40 1 calc PR C 3 H73B H 0.0844 0.7787 0.0397 0.076 Uiso 0.40 1 calc PR C 3 Cl73 Cl -0.015(2) 0.857(2) -0.1175(11) 0.272(16) Uani 0.40 1 d P C 3 Cl74 Cl -0.0543(8) 0.8771(12) 0.1105(9) 0.131(5) Uani 0.40 1 d P C 3 P1 P 0.28031(14) 0.81502(13) 0.40253(16) 0.0272(3) Uani 1 1 d . . . P2 P 0.51779(17) 0.91424(13) 0.24220(16) 0.0281(3) Uani 1 1 d . . . Cl1 Cl 0.61353(14) 0.78104(13) 0.67968(14) 0.0312(3) Uani 1 1 d . . . Cl2 Cl 0.62444(17) 0.57910(13) 0.38010(16) 0.0343(4) Uani 1 1 d . . . N3 N 0.2872(6) 0.6046(5) 0.3123(6) 0.0352(14) Uani 1 1 d . . . N20 N 0.3706(10) 0.9984(7) 0.0515(7) 0.069(3) Uani 1 1 d . . . N16 N 0.4979(7) 0.8710(6) -0.0023(6) 0.0410(15) Uani 1 1 d . . . N7 N 0.2643(6) 0.7323(6) 0.1747(6) 0.0454(16) 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 0.02195(9) 0.02231(9) 0.02447(11) 0.00065(10) 0.00549(7) -0.00086(9) Au2 0.03492(12) 0.02067(10) 0.02618(12) 0.00199(10) 0.00889(9) 0.00285(10) C1 0.037(4) 0.027(3) 0.034(4) -0.001(3) 0.002(3) 0.009(3) C2 0.036(4) 0.030(3) 0.035(4) -0.004(3) -0.007(3) 0.001(3) C4 0.041(4) 0.025(3) 0.066(6) 0.010(4) -0.004(4) -0.001(3) C5 0.059(6) 0.043(5) 0.064(6) -0.017(4) -0.017(5) 0.014(4) C6 0.089(7) 0.048(5) 0.039(5) -0.016(4) -0.012(5) 0.012(5) C8 0.018(3) 0.036(4) 0.061(5) 0.003(4) 0.006(3) 0.004(3) C9 0.021(3) 0.041(4) 0.103(8) 0.016(5) 0.004(4) -0.003(3) C10 0.024(4) 0.058(6) 0.147(12) 0.029(8) -0.009(5) -0.001(4) C11 0.038(5) 0.063(7) 0.168(14) 0.052(9) 0.045(6) 0.021(5) C12 0.055(6) 0.058(6) 0.131(11) 0.026(7) 0.049(7) 0.020(5) C13 0.035(4) 0.040(4) 0.098(8) -0.004(5) 0.027(5) 0.007(4) C14 0.037(4) 0.022(3) 0.036(4) -0.002(3) 0.011(3) -0.004(3) C15 0.070(5) 0.022(3) 0.022(3) -0.002(3) 0.007(3) -0.004(3) C17 0.088(7) 0.105(10) 0.042(5) -0.028(7) 0.007(5) 0.018(8) C18 0.155(12) 0.057(6) 0.025(4) -0.005(4) 0.015(6) -0.027(7) C19 0.159(13) 0.050(5) 0.028(5) 0.009(4) -0.015(6) 0.027(7) C21 0.042(4) 0.030(3) 0.026(3) -0.003(3) 0.015(3) -0.002(3) C22 0.060(5) 0.034(4) 0.047(5) 0.005(4) 0.014(4) -0.006(4) C23 0.058(5) 0.039(4) 0.068(7) 0.004(4) 0.004(5) -0.012(4) C24 0.046(5) 0.056(5) 0.077(7) -0.003(5) 0.021(5) -0.009(4) C25 0.045(5) 0.068(7) 0.121(11) 0.017(7) 0.032(6) -0.003(5) C26 0.051(5) 0.043(5) 0.089(8) 0.016(5) 0.025(5) 0.006(4) Cl73 0.39(3) 0.35(3) 0.069(7) 0.016(11) 0.028(11) 0.30(3) Cl74 0.079(6) 0.224(14) 0.087(6) -0.073(8) -0.004(5) 0.048(7) P1 0.0214(7) 0.0231(8) 0.0362(9) 0.0017(7) 0.0006(6) 0.0009(6) P2 0.0418(9) 0.0202(7) 0.0231(8) 0.0026(6) 0.0075(7) 0.0030(7) Cl1 0.0334(7) 0.0278(8) 0.0302(7) 0.0019(6) -0.0040(6) -0.0040(6) Cl2 0.0426(9) 0.0242(7) 0.0368(9) 0.0060(7) 0.0079(7) 0.0061(7) N3 0.034(3) 0.027(3) 0.042(4) -0.003(3) -0.006(3) -0.002(2) N20 0.122(8) 0.044(4) 0.036(4) 0.003(3) -0.009(5) 0.033(5) N16 0.058(4) 0.041(3) 0.023(3) -0.002(3) 0.005(3) 0.003(3) N7 0.054(4) 0.043(4) 0.036(3) -0.001(3) -0.008(3) 0.003(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 2.2345(17) . ? Au1 Cl1 2.2970(15) . ? Au1 Au2 3.1218(3) . ? Au2 P2 2.2388(16) . ? Au2 Cl2 2.2984(16) . ? C1 C14 1.506(10) . ? C1 P1 1.832(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N7 1.339(10) . ? C2 N3 1.346(9) . ? C2 P1 1.808(7) . ? C4 N3 1.496(11) . ? C4 H4C 0.9800 . ? C4 H4B 0.9800 . ? C4 H4A 0.9800 . ? C5 C6 1.353(14) . ? C5 N3 1.379(11) . ? C5 H5 0.9500 . ? C6 N7 1.358(11) . ? C6 H6 0.9500 . ? C8 C13 1.388(12) . ? C8 C9 1.415(12) . ? C8 P1 1.820(7) . ? C9 C10 1.372(14) . ? C9 H9 0.9500 . ? C10 C11 1.33(2) . ? C10 H10 0.9500 . ? C11 C12 1.443(19) . ? C11 H11 0.9500 . ? C12 C13 1.366(12) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 P2 1.817(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N20 1.328(12) . ? C15 N16 1.380(10) . ? C15 P2 1.789(8) . ? C17 N16 1.398(14) . ? C17 H17C 0.9800 . ? C17 H17B 0.9800 . ? C17 H17A 0.9800 . ? C18 N16 1.331(13) . ? C18 C19 1.417(17) . ? C18 H18 0.9500 . ? C19 N20 1.348(12) . ? C19 H19 0.9500 . ? C21 C26 1.364(13) . ? C21 C22 1.397(11) . ? C21 P2 1.821(7) . ? C22 C23 1.412(12) . ? C22 H22 0.9500 . ? C23 C24 1.359(14) . ? C23 H23 0.9500 . ? C24 C25 1.353(16) . ? C24 H24 0.9500 . ? C25 C26 1.380(14) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C71A O71A 1.416(9) . ? C71A C72A 1.540(9) . ? C71A H71A 0.9900 . ? C71A H71B 0.9900 . ? C72A H72A 0.9800 . ? C72A H72B 0.9800 . ? C72A H72C 0.9800 . ? C73 Cl74 1.64(3) . ? C73 Cl73 1.66(3) . ? C73 H73A 0.9900 . ? C73 H73B 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 Cl1 179.25(7) . . ? P1 Au1 Au2 79.82(5) . . ? Cl1 Au1 Au2 99.66(4) . . ? P2 Au2 Cl2 176.54(7) . . ? P2 Au2 Au1 91.06(5) . . ? Cl2 Au2 Au1 91.81(5) . . ? C14 C1 P1 114.9(5) . . ? C14 C1 H1A 108.5 . . ? P1 C1 H1A 108.5 . . ? C14 C1 H1B 108.5 . . ? P1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? N7 C2 N3 111.6(7) . . ? N7 C2 P1 123.4(6) . . ? N3 C2 P1 124.9(6) . . ? N3 C4 H4C 109.5 . . ? N3 C4 H4B 109.5 . . ? H4C C4 H4B 109.5 . . ? N3 C4 H4A 109.5 . . ? H4C C4 H4A 109.5 . . ? H4B C4 H4A 109.5 . . ? C6 C5 N3 106.6(8) . . ? C6 C5 H5 126.7 . . ? N3 C5 H5 126.7 . . ? C5 C6 N7 110.4(8) . . ? C5 C6 H6 124.8 . . ? N7 C6 H6 124.8 . . ? C13 C8 C9 121.6(7) . . ? C13 C8 P1 118.4(6) . . ? C9 C8 P1 120.1(7) . . ? C10 C9 C8 116.3(11) . . ? C10 C9 H9 121.8 . . ? C8 C9 H9 121.8 . . ? C11 C10 C9 122.7(11) . . ? C11 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? C10 C11 C12 121.9(9) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C13 C12 C11 116.0(11) . . ? C13 C12 H12 122.0 . . ? C11 C12 H12 122.0 . . ? C12 C13 C8 121.4(10) . . ? C12 C13 H13 119.3 . . ? C8 C13 H13 119.3 . . ? C1 C14 P2 118.1(5) . . ? C1 C14 H14A 107.8 . . ? P2 C14 H14A 107.8 . . ? C1 C14 H14B 107.8 . . ? P2 C14 H14B 107.8 . . ? H14A C14 H14B 107.1 . . ? N20 C15 N16 111.7(7) . . ? N20 C15 P2 122.6(6) . . ? N16 C15 P2 125.6(6) . . ? N16 C17 H17C 109.5 . . ? N16 C17 H17B 109.5 . . ? H17C C17 H17B 109.5 . . ? N16 C17 H17A 109.5 . . ? H17C C17 H17A 109.5 . . ? H17B C17 H17A 109.5 . . ? N16 C18 C19 104.5(8) . . ? N16 C18 H18 127.8 . . ? C19 C18 H18 127.8 . . ? N20 C19 C18 111.4(9) . . ? N20 C19 H19 124.3 . . ? C18 C19 H19 124.3 . . ? C26 C21 C22 120.8(8) . . ? C26 C21 P2 120.4(6) . . ? C22 C21 P2 118.8(6) . . ? C21 C22 C23 118.1(8) . . ? C21 C22 H22 121.0 . . ? C23 C22 H22 121.0 . . ? C24 C23 C22 119.6(9) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C25 C24 C23 121.3(9) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C24 C25 C26 120.6(11) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C21 C26 C25 119.6(9) . . ? C21 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? O71A C71A C72A 136.8(17) . . ? O71A C71A H71A 103.0 . . ? C72A C71A H71A 102.9 . . ? O71A C71A H71B 102.9 . . ? C72A C71A H71B 103.0 . . ? H71A C71A H71B 105.1 . . ? C71A C72A H72A 109.5 . . ? C71A C72A H72B 109.5 . . ? H72A C72A H72B 109.5 . . ? C71A C72A H72C 109.5 . . ? H72A C72A H72C 109.5 . . ? H72B C72A H72C 109.5 . . ? Cl74 C73 Cl73 109.9(18) . . ? Cl74 C73 H73A 109.7 . . ? Cl73 C73 H73A 109.7 . . ? Cl74 C73 H73B 109.7 . . ? Cl73 C73 H73B 109.7 . . ? H73A C73 H73B 108.2 . . ? C2 P1 C8 106.4(4) . . ? C2 P1 C1 103.5(4) . . ? C8 P1 C1 106.0(3) . . ? C2 P1 Au1 112.2(2) . . ? C8 P1 Au1 114.7(3) . . ? C1 P1 Au1 113.1(2) . . ? C15 P2 C14 102.3(4) . . ? C15 P2 C21 104.1(4) . . ? C14 P2 C21 104.1(3) . . ? C15 P2 Au2 118.0(2) . . ? C14 P2 Au2 116.3(2) . . ? C21 P2 Au2 110.4(2) . . ? C2 N3 C5 106.2(7) . . ? C2 N3 C4 125.9(7) . . ? C5 N3 C4 127.8(7) . . ? C15 N20 C19 104.3(9) . . ? C18 N16 C15 107.9(8) . . ? C18 N16 C17 124.6(8) . . ? C15 N16 C17 127.4(7) . . ? C2 N7 C6 105.2(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 P1 Au1 Au2 P2 61.75(6) . . . . ? Cl1 Au1 Au2 P2 -117.69(6) . . . . ? P1 Au1 Au2 Cl2 -120.19(6) . . . . ? Cl1 Au1 Au2 Cl2 60.37(6) . . . . ? N3 C5 C6 N7 -0.5(12) . . . . ? C13 C8 C9 C10 1.3(14) . . . . ? P1 C8 C9 C10 179.9(7) . . . . ? C8 C9 C10 C11 -1.8(16) . . . . ? C9 C10 C11 C12 2.8(18) . . . . ? C10 C11 C12 C13 -3.0(17) . . . . ? C11 C12 C13 C8 2.5(16) . . . . ? C9 C8 C13 C12 -1.8(14) . . . . ? P1 C8 C13 C12 179.6(8) . . . . ? P1 C1 C14 P2 64.4(7) . . . . ? N16 C18 C19 N20 3.0(14) . . . . ? C26 C21 C22 C23 -0.8(13) . . . . ? P2 C21 C22 C23 -179.0(7) . . . . ? C21 C22 C23 C24 -0.1(14) . . . . ? C22 C23 C24 C25 1.6(17) . . . . ? C23 C24 C25 C26 -2(2) . . . . ? C22 C21 C26 C25 0.3(16) . . . . ? P2 C21 C26 C25 178.4(9) . . . . ? C24 C25 C26 C21 1(2) . . . . ? N7 C2 P1 C8 106.7(7) . . . . ? N3 C2 P1 C8 -76.4(7) . . . . ? N7 C2 P1 C1 -4.8(7) . . . . ? N3 C2 P1 C1 172.0(6) . . . . ? N7 C2 P1 Au1 -127.1(6) . . . . ? N3 C2 P1 Au1 49.7(7) . . . . ? C13 C8 P1 C2 177.4(7) . . . . ? C9 C8 P1 C2 -1.2(8) . . . . ? C13 C8 P1 C1 -72.8(7) . . . . ? C9 C8 P1 C1 108.6(7) . . . . ? C13 C8 P1 Au1 52.7(7) . . . . ? C9 C8 P1 Au1 -125.9(6) . . . . ? C14 C1 P1 C2 -97.5(6) . . . . ? C14 C1 P1 C8 150.7(5) . . . . ? C14 C1 P1 Au1 24.2(6) . . . . ? Cl1 Au1 P1 C2 88(5) . . . . ? Au2 Au1 P1 C2 41.7(3) . . . . ? Cl1 Au1 P1 C8 -150(5) . . . . ? Au2 Au1 P1 C8 163.2(3) . . . . ? Cl1 Au1 P1 C1 -28(5) . . . . ? Au2 Au1 P1 C1 -75.0(3) . . . . ? N20 C15 P2 C14 14.7(9) . . . . ? N16 C15 P2 C14 -170.6(7) . . . . ? N20 C15 P2 C21 -93.5(9) . . . . ? N16 C15 P2 C21 81.2(7) . . . . ? N20 C15 P2 Au2 143.7(7) . . . . ? N16 C15 P2 Au2 -41.6(8) . . . . ? C1 C14 P2 C15 71.8(6) . . . . ? C1 C14 P2 C21 180.0(6) . . . . ? C1 C14 P2 Au2 -58.3(6) . . . . ? C26 C21 P2 C15 -125.1(8) . . . . ? C22 C21 P2 C15 53.1(7) . . . . ? C26 C21 P2 C14 128.0(7) . . . . ? C22 C21 P2 C14 -53.8(7) . . . . ? C26 C21 P2 Au2 2.5(8) . . . . ? C22 C21 P2 Au2 -179.4(5) . . . . ? Cl2 Au2 P2 C15 77.9(12) . . . . ? Au1 Au2 P2 C15 -136.2(3) . . . . ? Cl2 Au2 P2 C14 -160.0(11) . . . . ? Au1 Au2 P2 C14 -14.1(3) . . . . ? Cl2 Au2 P2 C21 -41.6(12) . . . . ? Au1 Au2 P2 C21 104.3(2) . . . . ? N7 C2 N3 C5 1.3(9) . . . . ? P1 C2 N3 C5 -175.9(6) . . . . ? N7 C2 N3 C4 179.3(7) . . . . ? P1 C2 N3 C4 2.2(11) . . . . ? C6 C5 N3 C2 -0.4(10) . . . . ? C6 C5 N3 C4 -178.4(8) . . . . ? N16 C15 N20 C19 -2.7(12) . . . . ? P2 C15 N20 C19 172.7(8) . . . . ? C18 C19 N20 C15 -0.2(14) . . . . ? C19 C18 N16 C15 -4.5(12) . . . . ? C19 C18 N16 C17 177.0(11) . . . . ? N20 C15 N16 C18 4.7(11) . . . . ? P2 C15 N16 C18 -170.5(7) . . . . ? N20 C15 N16 C17 -176.8(11) . . . . ? P2 C15 N16 C17 8.0(14) . . . . ? N3 C2 N7 C6 -1.6(10) . . . . ? P1 C2 N7 C6 175.6(7) . . . . ? C5 C6 N7 C2 1.3(11) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.418 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.174 # Attachment '- kp290510.cif' data_kp290510 _database_code_depnum_ccdc_archive 'CCDC 808836' #TrackingRef '- kp290510.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H26 Au2 Cl2 N4 O3 P2 S4' _chemical_formula_weight 1145.56 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' S S 0.1246 0.1234 '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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 8.0992(3) _cell_length_b 9.9494(3) _cell_length_c 11.4694(4) _cell_angle_alpha 94.260(3) _cell_angle_beta 93.131(3) _cell_angle_gamma 97.282(3) _cell_volume 912.32(5) _cell_formula_units_Z 1 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 8189 _cell_measurement_theta_min 2.5354 _cell_measurement_theta_max 34.8315 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.085 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 8.532 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3943 _exptl_absorpt_correction_T_max 0.7265 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Xcalibur Ruby CCD' _diffrn_measurement_method '\o oscillation scan' _diffrn_detector_area_resol_mean 10.4498 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15195 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0492 _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 -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 33.14 _reflns_number_total 6962 _reflns_number_gt 5537 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis^Pro^ (Oxford, 2007)' _computing_cell_refinement 'CrysAlis^Pro^ (Oxford, 2007)' _computing_data_reduction 'CrysAlis^Pro^ (Oxford, 2007)' _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6962 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0893 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 C1 C 0.5263(5) 0.4920(4) 0.5638(3) 0.0266(7) Uani 1 1 d . . . H1A H 0.5662 0.4027 0.5699 0.032 Uiso 1 1 calc R . . H1B H 0.4290 0.4952 0.6121 0.032 Uiso 1 1 calc R . . C2 C 0.5856(5) 0.7766(4) 0.6320(3) 0.0263(7) Uani 1 1 d . . . C4 C 0.5148(5) 1.0058(4) 0.6635(4) 0.0282(8) Uani 1 1 d . . . C5 C 0.4915(6) 1.1413(4) 0.6849(4) 0.0357(9) Uani 1 1 d . . . H5 H 0.5823 1.2122 0.6875 0.043 Uiso 1 1 calc R . . C6 C 0.3305(6) 1.1692(4) 0.7023(4) 0.0375(10) Uani 1 1 d . . . H6 H 0.3106 1.2608 0.7172 0.045 Uiso 1 1 calc R . . C7 C 0.1959(6) 1.0634(5) 0.6982(5) 0.0432(11) Uani 1 1 d . . . H7 H 0.0864 1.0847 0.7090 0.052 Uiso 1 1 calc R . . C8 C 0.2215(6) 0.9312(5) 0.6790(4) 0.0392(10) Uani 1 1 d . . . H8 H 0.1306 0.8605 0.6772 0.047 Uiso 1 1 calc R . . C9 C 0.3822(5) 0.9003(4) 0.6619(4) 0.0280(8) Uani 1 1 d . . . N10 N 0.4273(4) 0.7698(3) 0.6448(3) 0.0283(7) Uani 1 1 d . . . C11 C 0.7237(5) 0.5899(4) 0.7699(4) 0.0289(8) Uani 1 1 d . . . C13 C 0.8059(7) 0.5825(5) 0.9752(4) 0.0440(12) Uani 1 1 d . . . C14 C 0.8588(9) 0.5894(7) 1.0931(5) 0.0611(16) Uani 1 1 d . . . H14 H 0.9327 0.6655 1.1275 0.073 Uiso 1 1 calc R . . C15 C 0.8044(9) 0.4872(8) 1.1583(5) 0.066(2) Uani 1 1 d . . . H15 H 0.8382 0.4916 1.2393 0.080 Uiso 1 1 calc R . . C16 C 0.7011(10) 0.3778(8) 1.1072(5) 0.075(2) Uani 1 1 d . . . H16 H 0.6656 0.3052 1.1532 0.090 Uiso 1 1 calc R . . C17 C 0.6464(10) 0.3692(7) 0.9907(5) 0.0674(18) Uani 1 1 d . . . H17 H 0.5734 0.2924 0.9566 0.081 Uiso 1 1 calc R . . C18 C 0.7008(7) 0.4761(5) 0.9238(4) 0.0433(11) Uani 1 1 d . . . N19 N 0.6524(5) 0.4780(4) 0.8090(3) 0.0384(8) Uani 1 1 d . . . P1 P 0.69070(13) 0.62647(10) 0.61852(9) 0.02523(19) Uani 1 1 d . . . S3 S 0.69785(13) 0.93837(10) 0.63633(11) 0.0339(2) Uani 1 1 d . . . S12 S 0.84879(19) 0.70093(14) 0.87114(12) 0.0516(3) Uani 1 1 d . . . Cl1 Cl 1.11459(15) 0.69676(13) 0.38500(12) 0.0465(3) Uani 1 1 d . . . Au1 Au 0.908758(18) 0.658135(15) 0.510703(14) 0.02951(6) Uani 1 1 d . . . O20 O 0.5000 0.0000 1.0000 0.093(3) Uani 1 2 d S . . O21 O 0.1730(10) -0.0807(8) 1.0632(8) 0.165(4) 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 C1 0.0300(19) 0.0196(16) 0.0307(19) 0.0020(14) 0.0041(15) 0.0039(14) C2 0.0289(19) 0.0227(16) 0.0279(18) 0.0035(14) 0.0043(15) 0.0044(14) C4 0.0301(19) 0.0221(16) 0.034(2) 0.0047(15) 0.0065(16) 0.0057(14) C5 0.042(2) 0.0231(18) 0.043(2) 0.0049(17) 0.0082(19) 0.0048(17) C6 0.044(2) 0.0264(19) 0.046(3) 0.0046(18) 0.011(2) 0.0127(18) C7 0.036(2) 0.036(2) 0.061(3) 0.003(2) 0.011(2) 0.0141(19) C8 0.031(2) 0.031(2) 0.056(3) 0.001(2) 0.008(2) 0.0040(17) C9 0.0287(19) 0.0232(17) 0.033(2) 0.0045(15) 0.0043(15) 0.0066(14) N10 0.0279(16) 0.0221(14) 0.0349(17) 0.0032(13) 0.0035(13) 0.0023(12) C11 0.0293(19) 0.0270(18) 0.033(2) 0.0031(15) 0.0045(15) 0.0106(15) C13 0.055(3) 0.049(3) 0.035(2) 0.003(2) 0.003(2) 0.032(2) C14 0.074(4) 0.072(4) 0.041(3) -0.006(3) -0.009(3) 0.035(3) C15 0.088(5) 0.094(5) 0.030(3) 0.008(3) 0.013(3) 0.056(4) C16 0.095(5) 0.097(6) 0.041(3) 0.023(3) 0.022(3) 0.029(5) C17 0.097(5) 0.069(4) 0.037(3) 0.021(3) 0.009(3) 0.003(4) C18 0.053(3) 0.041(2) 0.040(2) 0.008(2) 0.013(2) 0.016(2) N19 0.042(2) 0.0315(18) 0.042(2) -0.0013(16) 0.0054(17) 0.0082(16) P1 0.0263(5) 0.0210(4) 0.0293(5) 0.0031(4) 0.0048(4) 0.0048(4) S3 0.0273(5) 0.0231(4) 0.0528(6) 0.0067(4) 0.0104(4) 0.0030(4) S12 0.0614(8) 0.0418(7) 0.0481(7) 0.0038(6) -0.0147(6) 0.0016(6) Cl1 0.0356(6) 0.0508(7) 0.0591(7) 0.0158(6) 0.0214(5) 0.0144(5) Au1 0.02571(8) 0.02862(8) 0.03521(9) 0.00382(6) 0.00564(6) 0.00521(5) O20 0.157(7) 0.055(3) 0.047(3) 0.036(3) -0.037(4) -0.066(4) O21 0.142(6) 0.107(5) 0.221(9) -0.095(6) -0.116(6) 0.039(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 C1 C1 1.527(8) 2_666 ? C1 P1 1.813(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N10 1.293(5) . ? C2 S3 1.741(4) . ? C2 P1 1.812(4) . ? C4 C5 1.390(5) . ? C4 C9 1.402(6) . ? C4 S3 1.737(4) . ? C5 C6 1.389(6) . ? C5 H5 0.9500 . ? C6 C7 1.412(7) . ? C6 H6 0.9500 . ? C7 C8 1.361(6) . ? C7 H7 0.9500 . ? C8 C9 1.395(6) . ? C8 H8 0.9500 . ? C9 N10 1.396(5) . ? C11 N19 1.309(5) . ? C11 S12 1.730(4) . ? C11 P1 1.813(4) . ? C13 C18 1.348(8) . ? C13 C14 1.389(7) . ? C13 S12 1.756(5) . ? C14 C15 1.350(10) . ? C14 H14 0.9500 . ? C15 C16 1.360(11) . ? C15 H15 0.9500 . ? C16 C17 1.378(9) . ? C16 H16 0.9500 . ? C17 C18 1.398(8) . ? C17 H17 0.9500 . ? C18 N19 1.355(6) . ? P1 Au1 2.2143(10) . ? Cl1 Au1 2.2777(11) . ? 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 C1 C1 P1 110.5(3) 2_666 . ? C1 C1 H1A 109.6 2_666 . ? P1 C1 H1A 109.6 . . ? C1 C1 H1B 109.6 2_666 . ? P1 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? N10 C2 S3 116.9(3) . . ? N10 C2 P1 122.3(3) . . ? S3 C2 P1 120.7(2) . . ? C5 C4 C9 121.6(4) . . ? C5 C4 S3 128.7(3) . . ? C9 C4 S3 109.7(3) . . ? C6 C5 C4 117.5(4) . . ? C6 C5 H5 121.2 . . ? C4 C5 H5 121.2 . . ? C5 C6 C7 121.0(4) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C8 C7 C6 120.7(4) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 119.5(4) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C8 C9 N10 125.7(4) . . ? C8 C9 C4 119.6(4) . . ? N10 C9 C4 114.7(3) . . ? C2 N10 C9 110.1(3) . . ? N19 C11 S12 116.2(3) . . ? N19 C11 P1 121.7(3) . . ? S12 C11 P1 122.2(2) . . ? C18 C13 C14 121.7(6) . . ? C18 C13 S12 108.5(4) . . ? C14 C13 S12 129.8(5) . . ? C15 C14 C13 119.5(7) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 119.5(6) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C17 121.9(7) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C16 C17 C18 118.5(7) . . ? C16 C17 H17 120.8 . . ? C18 C17 H17 120.8 . . ? C13 C18 N19 118.2(5) . . ? C13 C18 C17 118.9(5) . . ? N19 C18 C17 122.9(6) . . ? C11 N19 C18 109.1(4) . . ? C2 P1 C11 102.35(18) . . ? C2 P1 C1 103.87(19) . . ? C11 P1 C1 102.00(19) . . ? C2 P1 Au1 111.39(13) . . ? C11 P1 Au1 118.94(14) . . ? C1 P1 Au1 116.35(13) . . ? C4 S3 C2 88.51(19) . . ? C11 S12 C13 88.0(2) . . ? P1 Au1 Cl1 174.05(4) . . ? 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 C9 C4 C5 C6 -1.4(7) . . . . ? S3 C4 C5 C6 178.9(4) . . . . ? C4 C5 C6 C7 -0.1(7) . . . . ? C5 C6 C7 C8 1.1(8) . . . . ? C6 C7 C8 C9 -0.7(8) . . . . ? C7 C8 C9 N10 178.0(5) . . . . ? C7 C8 C9 C4 -0.7(7) . . . . ? C5 C4 C9 C8 1.8(7) . . . . ? S3 C4 C9 C8 -178.5(4) . . . . ? C5 C4 C9 N10 -177.1(4) . . . . ? S3 C4 C9 N10 2.7(5) . . . . ? S3 C2 N10 C9 -1.1(5) . . . . ? P1 C2 N10 C9 175.5(3) . . . . ? C8 C9 N10 C2 -179.8(4) . . . . ? C4 C9 N10 C2 -1.1(5) . . . . ? C18 C13 C14 C15 0.1(8) . . . . ? S12 C13 C14 C15 177.5(4) . . . . ? C13 C14 C15 C16 1.2(9) . . . . ? C14 C15 C16 C17 -1.5(11) . . . . ? C15 C16 C17 C18 0.6(11) . . . . ? C14 C13 C18 N19 178.7(4) . . . . ? S12 C13 C18 N19 0.9(6) . . . . ? C14 C13 C18 C17 -1.1(8) . . . . ? S12 C13 C18 C17 -178.9(5) . . . . ? C16 C17 C18 C13 0.7(10) . . . . ? C16 C17 C18 N19 -179.1(6) . . . . ? S12 C11 N19 C18 -1.7(5) . . . . ? P1 C11 N19 C18 179.0(3) . . . . ? C13 C18 N19 C11 0.5(6) . . . . ? C17 C18 N19 C11 -179.7(5) . . . . ? N10 C2 P1 C11 -81.7(4) . . . . ? S3 C2 P1 C11 94.7(3) . . . . ? N10 C2 P1 C1 24.1(4) . . . . ? S3 C2 P1 C1 -159.4(2) . . . . ? N10 C2 P1 Au1 150.1(3) . . . . ? S3 C2 P1 Au1 -33.4(3) . . . . ? N19 C11 P1 C2 115.8(4) . . . . ? S12 C11 P1 C2 -63.5(3) . . . . ? N19 C11 P1 C1 8.5(4) . . . . ? S12 C11 P1 C1 -170.8(2) . . . . ? N19 C11 P1 Au1 -121.0(3) . . . . ? S12 C11 P1 Au1 59.7(3) . . . . ? C1 C1 P1 C2 71.5(4) 2_666 . . . ? C1 C1 P1 C11 177.6(3) 2_666 . . . ? C1 C1 P1 Au1 -51.3(4) 2_666 . . . ? C5 C4 S3 C2 177.1(4) . . . . ? C9 C4 S3 C2 -2.6(3) . . . . ? N10 C2 S3 C4 2.2(3) . . . . ? P1 C2 S3 C4 -174.4(3) . . . . ? N19 C11 S12 C13 1.9(3) . . . . ? P1 C11 S12 C13 -178.8(3) . . . . ? C18 C13 S12 C11 -1.5(4) . . . . ? C14 C13 S12 C11 -179.1(5) . . . . ? C2 P1 Au1 Cl1 -54.9(4) . . . . ? C11 P1 Au1 Cl1 -173.5(4) . . . . ? C1 P1 Au1 Cl1 63.9(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 33.14 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.173 _refine_diff_density_min -0.800 _refine_diff_density_rms 0.182 # Attachment '- kp301108.cif' data_kp301108 _database_code_depnum_ccdc_archive 'CCDC 808837' #TrackingRef '- kp301108.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H32 Au2 Cl2 N8 P2' _chemical_formula_weight 1079.45 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' N N 0.0061 0.0033 '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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6754(7) _cell_length_b 11.3757(7) _cell_length_c 12.1339(7) _cell_angle_alpha 103.894(5) _cell_angle_beta 108.377(6) _cell_angle_gamma 108.128(6) _cell_volume 1116.59(12) _cell_formula_units_Z 1 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 2952 _cell_measurement_theta_min 2.2036 _cell_measurement_theta_max 30.8585 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 514 _exptl_absorpt_coefficient_mu 6.783 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6921 _exptl_absorpt_correction_T_max 0.8763 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Xcalibur Ruby CCD' _diffrn_measurement_method '\o oscillation scan' _diffrn_detector_area_resol_mean 10.4498 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10910 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.1829 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.10 _reflns_number_total 4930 _reflns_number_gt 2820 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis^Pro^ (Oxford, 2007)' _computing_cell_refinement 'CrysAlis^Pro^ (Oxford, 2007)' _computing_data_reduction 'CrysAlis^Pro^ (Oxford, 2007)' _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. As the refinement of the disordered solvents turned out to be impossible, the squeeze procedure was applied. ; _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^)+(0.0673P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4930 _refine_ls_number_parameters 219 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1065 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1498 _refine_ls_wR_factor_gt 0.1401 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _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 0.41929(7) -0.03210(5) 0.13611(5) 0.03289(19) Uani 1 1 d . . . P1 P 0.1761(4) -0.0576(3) 0.1188(3) 0.0265(8) Uani 1 1 d . . . Cl1 Cl 0.6710(5) -0.0007(4) 0.1545(3) 0.0552(10) Uani 1 1 d . . . C1 C 0.0877(14) 0.0188(10) 0.0169(10) 0.027(3) Uani 1 1 d . . . H1A H 0.1465 0.1170 0.0591 0.032 Uiso 1 1 calc R . . H1B H 0.1022 -0.0076 -0.0611 0.032 Uiso 1 1 calc R . . C2 C 0.1641(15) 0.0175(10) 0.2636(10) 0.027(3) Uani 1 1 d . . . C4 C 0.2737(19) -0.1160(14) 0.3804(12) 0.047(4) Uani 1 1 d . . . H4C H 0.3345 -0.0971 0.4690 0.071 Uiso 1 1 calc R . . H4B H 0.3431 -0.1168 0.3366 0.071 Uiso 1 1 calc R . . H4A H 0.1819 -0.2033 0.3428 0.071 Uiso 1 1 calc R . . C5 C 0.1906(15) 0.0721(10) 0.4564(10) 0.029(3) Uani 1 1 d . . . C6 C 0.2168(17) 0.0826(12) 0.5804(11) 0.041(4) Uani 1 1 d . . . H6 H 0.2562 0.0280 0.6171 0.049 Uiso 1 1 calc R . . C7 C 0.1809(17) 0.1778(13) 0.6439(12) 0.046(4) Uani 1 1 d . . . H7 H 0.1988 0.1908 0.7284 0.055 Uiso 1 1 calc R . . C8 C 0.1211(18) 0.2541(13) 0.5912(12) 0.047(4) Uani 1 1 d . . . H8 H 0.0995 0.3192 0.6397 0.057 Uiso 1 1 calc R . . C9 C 0.0909(17) 0.2386(11) 0.4672(11) 0.040(3) Uani 1 1 d . . . H9 H 0.0464 0.2908 0.4304 0.047 Uiso 1 1 calc R . . C10 C 0.1269(16) 0.1460(11) 0.3987(11) 0.033(3) Uani 1 1 d . . . C12 C 0.0245(15) -0.2280(10) 0.0575(10) 0.027(3) Uani 1 1 d . . . C14 C 0.0629(18) -0.3087(12) -0.1426(11) 0.038(3) Uani 1 1 d . . . H14A H 0.1774 -0.2495 -0.0951 0.057 Uiso 1 1 calc R . . H14B H 0.0113 -0.2706 -0.1986 0.057 Uiso 1 1 calc R . . H14C H 0.0498 -0.3965 -0.1922 0.057 Uiso 1 1 calc R . . C15 C -0.1407(15) -0.4327(10) -0.0717(10) 0.028(3) Uani 1 1 d . . . C16 C -0.2315(18) -0.5551(12) -0.1701(12) 0.044(4) Uani 1 1 d . . . H16 H -0.2093 -0.5767 -0.2414 0.052 Uiso 1 1 calc R . . C17 C -0.3577(19) -0.6454(13) -0.1587(12) 0.049(4) Uani 1 1 d . . . H17 H -0.4243 -0.7305 -0.2240 0.058 Uiso 1 1 calc R . . C18 C -0.3865(17) -0.6127(12) -0.0551(13) 0.046(4) Uani 1 1 d . . . H18 H -0.4725 -0.6763 -0.0497 0.055 Uiso 1 1 calc R . . C19 C -0.2953(17) -0.4911(12) 0.0416(12) 0.040(3) Uani 1 1 d . . . H19 H -0.3173 -0.4700 0.1130 0.048 Uiso 1 1 calc R . . C20 C -0.1708(15) -0.4002(11) 0.0323(10) 0.027(3) Uani 1 1 d . . . N3 N 0.2152(13) -0.0112(9) 0.3694(8) 0.032(3) Uani 1 1 d . . . N11 N 0.1108(13) 0.1097(8) 0.2766(8) 0.030(3) Uani 1 1 d . . . N13 N -0.0115(13) -0.3228(8) -0.0559(8) 0.028(2) Uani 1 1 d . . . N21 N -0.0648(13) -0.2702(8) 0.1148(8) 0.026(2) 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 0.0319(4) 0.0409(3) 0.0323(3) 0.0176(2) 0.0176(2) 0.0160(2) P1 0.028(2) 0.0294(16) 0.0203(15) 0.0072(12) 0.0111(14) 0.0112(15) Cl1 0.037(3) 0.090(3) 0.063(2) 0.049(2) 0.031(2) 0.032(2) C1 0.033(8) 0.023(6) 0.026(6) 0.011(5) 0.016(6) 0.009(6) C2 0.018(8) 0.026(6) 0.029(6) 0.007(5) 0.013(5) 0.000(5) C4 0.062(12) 0.075(9) 0.044(8) 0.029(7) 0.040(8) 0.054(9) C5 0.023(8) 0.029(6) 0.020(6) 0.002(5) 0.011(5) -0.002(6) C6 0.037(10) 0.043(7) 0.023(6) 0.008(5) 0.005(6) 0.002(7) C7 0.027(10) 0.060(9) 0.026(7) 0.006(6) 0.007(6) 0.001(7) C8 0.049(11) 0.043(8) 0.031(7) -0.004(6) 0.019(7) 0.008(7) C9 0.039(10) 0.037(7) 0.033(7) 0.005(5) 0.014(6) 0.012(7) C10 0.026(9) 0.025(6) 0.032(7) 0.000(5) 0.013(6) 0.001(6) C12 0.024(8) 0.031(6) 0.026(6) 0.007(5) 0.009(6) 0.013(6) C14 0.057(11) 0.043(7) 0.032(7) 0.016(5) 0.033(7) 0.027(7) C15 0.034(9) 0.014(6) 0.031(6) 0.005(5) 0.008(6) 0.009(6) C16 0.050(11) 0.045(8) 0.041(8) 0.015(6) 0.019(7) 0.026(8) C17 0.058(12) 0.035(8) 0.044(8) 0.005(6) 0.017(8) 0.021(8) C18 0.030(10) 0.039(8) 0.069(10) 0.022(7) 0.019(8) 0.015(7) C19 0.040(10) 0.041(7) 0.045(8) 0.015(6) 0.028(7) 0.017(7) C20 0.033(9) 0.032(6) 0.029(6) 0.015(5) 0.020(6) 0.018(6) N3 0.035(8) 0.036(5) 0.024(5) 0.009(4) 0.015(5) 0.012(5) N11 0.038(8) 0.025(5) 0.025(5) 0.005(4) 0.015(5) 0.009(5) N13 0.040(8) 0.028(5) 0.018(5) 0.002(4) 0.014(5) 0.018(5) N21 0.037(7) 0.026(5) 0.027(5) 0.009(4) 0.026(5) 0.015(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.213(4) . ? Au1 Cl1 2.277(4) . ? P1 C2 1.816(11) . ? P1 C12 1.821(11) . ? P1 C1 1.823(11) . ? C1 C1 1.50(2) 2 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N11 1.304(14) . ? C2 N3 1.379(14) . ? C4 N3 1.487(15) . ? C4 H4C 0.9800 . ? C4 H4B 0.9800 . ? C4 H4A 0.9800 . ? C5 N3 1.373(14) . ? C5 C10 1.381(16) . ? C5 C6 1.413(16) . ? C6 C7 1.374(19) . ? C6 H6 0.9500 . ? C7 C8 1.358(19) . ? C7 H7 0.9500 . ? C8 C9 1.395(17) . ? C8 H8 0.9500 . ? C9 C10 1.383(16) . ? C9 H9 0.9500 . ? C10 N11 1.382(14) . ? C12 N21 1.319(14) . ? C12 N13 1.389(13) . ? C14 N13 1.461(14) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C20 1.374(16) . ? C15 C16 1.384(15) . ? C15 N13 1.388(14) . ? C16 C17 1.400(19) . ? C16 H16 0.9500 . ? C17 C18 1.362(19) . ? C17 H17 0.9500 . ? C18 C19 1.370(17) . ? C18 H18 0.9500 . ? C19 C20 1.378(17) . ? C19 H19 0.9500 . ? C20 N21 1.393(14) . ? 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 178.62(13) . . ? C2 P1 C12 102.5(5) . . ? C2 P1 C1 103.2(5) . . ? C12 P1 C1 104.3(5) . . ? C2 P1 Au1 115.5(4) . . ? C12 P1 Au1 116.8(4) . . ? C1 P1 Au1 112.8(4) . . ? C1 C1 P1 114.1(9) 2 . ? C1 C1 H1A 108.7 2 . ? P1 C1 H1A 108.7 . . ? C1 C1 H1B 108.7 2 . ? P1 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? N11 C2 N3 114.1(10) . . ? N11 C2 P1 121.1(8) . . ? N3 C2 P1 124.7(9) . . ? N3 C4 H4C 109.5 . . ? N3 C4 H4B 109.5 . . ? H4C C4 H4B 109.5 . . ? N3 C4 H4A 109.5 . . ? H4C C4 H4A 109.5 . . ? H4B C4 H4A 109.5 . . ? N3 C5 C10 106.7(9) . . ? N3 C5 C6 129.4(11) . . ? C10 C5 C6 123.8(11) . . ? C7 C6 C5 115.0(12) . . ? C7 C6 H6 122.5 . . ? C5 C6 H6 122.5 . . ? C8 C7 C6 122.8(12) . . ? C8 C7 H7 118.6 . . ? C6 C7 H7 118.6 . . ? C7 C8 C9 121.1(12) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C10 C9 C8 118.8(12) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C5 C10 N11 110.1(10) . . ? C5 C10 C9 118.3(11) . . ? N11 C10 C9 131.6(12) . . ? N21 C12 N13 114.5(10) . . ? N21 C12 P1 122.7(8) . . ? N13 C12 P1 122.8(9) . . ? N13 C14 H14A 109.5 . . ? N13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 122.6(12) . . ? C20 C15 N13 107.3(9) . . ? C16 C15 N13 130.1(12) . . ? C15 C16 C17 116.3(13) . . ? C15 C16 H16 121.9 . . ? C17 C16 H16 121.9 . . ? C18 C17 C16 120.9(12) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 122.1(14) . . ? C17 C18 H18 119.0 . . ? C19 C18 H18 119.0 . . ? C18 C19 C20 118.2(12) . . ? C18 C19 H19 120.9 . . ? C20 C19 H19 120.9 . . ? C15 C20 C19 120.1(11) . . ? C15 C20 N21 110.6(10) . . ? C19 C20 N21 129.3(11) . . ? C5 N3 C2 104.8(9) . . ? C5 N3 C4 129.0(9) . . ? C2 N3 C4 126.1(9) . . ? C2 N11 C10 104.3(9) . . ? C15 N13 C12 103.9(9) . . ? C15 N13 C14 127.6(9) . . ? C12 N13 C14 128.4(10) . . ? C12 N21 C20 103.6(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 Cl1 Au1 P1 C2 -74(5) . . . . ? Cl1 Au1 P1 C12 165(5) . . . . ? Cl1 Au1 P1 C1 44(5) . . . . ? C2 P1 C1 C1 -65.9(11) . . . 2 ? C12 P1 C1 C1 41.0(12) . . . 2 ? Au1 P1 C1 C1 168.8(9) . . . 2 ? C12 P1 C2 N11 -112.2(10) . . . . ? C1 P1 C2 N11 -4.0(11) . . . . ? Au1 P1 C2 N11 119.6(9) . . . . ? C12 P1 C2 N3 70.8(11) . . . . ? C1 P1 C2 N3 179.1(10) . . . . ? Au1 P1 C2 N3 -57.3(11) . . . . ? N3 C5 C6 C7 179.5(12) . . . . ? C10 C5 C6 C7 -3.0(19) . . . . ? C5 C6 C7 C8 2(2) . . . . ? C6 C7 C8 C9 1(2) . . . . ? C7 C8 C9 C10 -2(2) . . . . ? N3 C5 C10 N11 0.2(14) . . . . ? C6 C5 C10 N11 -177.8(11) . . . . ? N3 C5 C10 C9 -180.0(11) . . . . ? C6 C5 C10 C9 2.0(19) . . . . ? C8 C9 C10 C5 0.4(19) . . . . ? C8 C9 C10 N11 -179.8(13) . . . . ? C2 P1 C12 N21 1.2(11) . . . . ? C1 P1 C12 N21 -106.1(10) . . . . ? Au1 P1 C12 N21 128.6(9) . . . . ? C2 P1 C12 N13 178.4(9) . . . . ? C1 P1 C12 N13 71.0(10) . . . . ? Au1 P1 C12 N13 -54.3(10) . . . . ? C20 C15 C16 C17 0.3(18) . . . . ? N13 C15 C16 C17 -178.7(12) . . . . ? C15 C16 C17 C18 -1(2) . . . . ? C16 C17 C18 C19 1(2) . . . . ? C17 C18 C19 C20 0(2) . . . . ? C16 C15 C20 C19 0.1(18) . . . . ? N13 C15 C20 C19 179.2(11) . . . . ? C16 C15 C20 N21 -178.3(11) . . . . ? N13 C15 C20 N21 0.8(13) . . . . ? C18 C19 C20 C15 -0.1(18) . . . . ? C18 C19 C20 N21 177.9(11) . . . . ? C10 C5 N3 C2 -0.1(13) . . . . ? C6 C5 N3 C2 177.7(12) . . . . ? C10 C5 N3 C4 -176.6(12) . . . . ? C6 C5 N3 C4 1(2) . . . . ? N11 C2 N3 C5 0.0(14) . . . . ? P1 C2 N3 C5 177.2(9) . . . . ? N11 C2 N3 C4 176.7(12) . . . . ? P1 C2 N3 C4 -6.2(18) . . . . ? N3 C2 N11 C10 0.1(14) . . . . ? P1 C2 N11 C10 -177.2(8) . . . . ? C5 C10 N11 C2 -0.2(14) . . . . ? C9 C10 N11 C2 180.0(14) . . . . ? C20 C15 N13 C12 -1.9(12) . . . . ? C16 C15 N13 C12 177.2(12) . . . . ? C20 C15 N13 C14 -179.0(11) . . . . ? C16 C15 N13 C14 0(2) . . . . ? N21 C12 N13 C15 2.5(13) . . . . ? P1 C12 N13 C15 -174.9(8) . . . . ? N21 C12 N13 C14 179.5(11) . . . . ? P1 C12 N13 C14 2.2(17) . . . . ? N13 C12 N21 C20 -2.0(13) . . . . ? P1 C12 N21 C20 175.4(8) . . . . ? C15 C20 N21 C12 0.6(13) . . . . ? C19 C20 N21 C12 -177.6(13) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.064 _refine_diff_density_min -0.875 _refine_diff_density_rms 0.187 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.051 0.500 0.500 329 125 ' ' _platon_squeeze_details ; ;