Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Raphael G. Raptis' 'Guang Yang' _publ_contact_author_name 'Raphael G. Raptis' _publ_contact_author_address ; Department of Chemistry University of Puerto Rico P.O.Box 23346 San Juan Puerto Rico UNITED STATES OF AMERICA ; _publ_contact_author_email raphael@adam.uprr.pr _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_section_title ; Oxidation of gold(I)-pyrazolates by aqua regia. X-ray structures of the first examples of trimeric Au(III)3 and Au(I)Au(III)2 pyrazolato complexes. ; data_Au(III)3 _database_code_CSD 191323 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H18 Au3 Cl9 N6' _chemical_formula_weight 1192.30 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' '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 Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.587(2) _cell_length_b 13.3340(19) _cell_length_c 14.971(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2912.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'deep red' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 15.921 _exptl_absorpt_correction_type 'semi-empirical' _exptl_absorpt_correction_T_min 0.155 _exptl_absorpt_correction_T_max 0.351 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5433 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 23.28 _reflns_number_total 1643 _reflns_number_gt 1182 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART-NT V5.0' _computing_cell_refinement 'BRUKER SMART-NT V5.0' _computing_data_reduction 'BRUKER SAINT-NT V5/6.0' _computing_structure_solution 'BRUKER SHELXTL-NT V5.1' _computing_structure_refinement 'BRUKER SHELXTL-NT V5.1' _computing_molecular_graphics 'BRUKER SHELXTL-NT V5.1' _computing_publication_material 'BRUKER SHELXTL-NT V5.1' _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^)+(0.0248P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1643 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0520 _refine_ls_wR_factor_gt 0.0476 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _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 0.06948(3) 0.09281(3) 0.65717(2) 0.05296(17) Uani 1 1 d . . . Au2 Au 0.0000 0.31645(4) 0.7500 0.0486(2) Uani 1 2 d S . . C1 C 0.0000 -0.1883(10) 0.7500 0.072(5) Uani 1 2 d S . . C2 C 0.0568(8) -0.1284(8) 0.7019(6) 0.062(3) Uani 1 1 d . . . C3 C 0.1337(8) -0.1546(7) 0.6404(6) 0.084(4) Uani 1 1 d . . . H3A H 0.1544 -0.0951 0.6103 0.126 Uiso 1 1 calc R . . H3B H 0.1127 -0.2025 0.5971 0.126 Uiso 1 1 calc R . . H3C H 0.1833 -0.1829 0.6741 0.126 Uiso 1 1 calc R . . C4 C 0.1782(8) 0.1622(8) 0.4637(7) 0.097(4) Uani 1 1 d . . . H4A H 0.2330 0.1375 0.4915 0.146 Uiso 1 1 calc R . . H4B H 0.1928 0.1887 0.4057 0.146 Uiso 1 1 calc R . . H4C H 0.1348 0.1085 0.4575 0.146 Uiso 1 1 calc R . . C5 C 0.1376(7) 0.2433(9) 0.5202(6) 0.061(3) Uani 1 1 d . . . C6 C 0.1394(7) 0.3444(9) 0.5090(6) 0.053(3) Uani 1 1 d . . . C7 C 0.0934(7) 0.3880(7) 0.5803(7) 0.051(3) Uani 1 1 d . . . C8 C 0.0748(6) 0.4937(7) 0.6023(6) 0.068(3) Uani 1 1 d . . . H8A H 0.0102 0.5028 0.6112 0.102 Uiso 1 1 calc R . . H8B H 0.0951 0.5357 0.5541 0.102 Uiso 1 1 calc R . . H8C H 0.1070 0.5115 0.6559 0.102 Uiso 1 1 calc R . . Cl1 Cl 0.2151(2) 0.0890(2) 0.71030(18) 0.0878(10) Uani 1 1 d . . . Cl2 Cl -0.06928(19) 0.0905(2) 0.59118(17) 0.0878(10) Uani 1 1 d . . . Cl3 Cl 0.1352(2) 0.3302(3) 0.82116(17) 0.0969(11) Uani 1 1 d . . . Cl4 Cl 0.0000 -0.3154(3) 0.7500 0.144(2) Uani 1 2 d S . . Cl5 Cl 0.1877(2) 0.4092(2) 0.42286(17) 0.0910(10) Uani 1 1 d . . . N1 N 0.0361(6) -0.0338(6) 0.7213(4) 0.061(3) Uani 1 1 d . . . N2 N 0.0955(5) 0.2230(6) 0.5973(5) 0.057(2) Uani 1 1 d . . . N3 N 0.0681(6) 0.3124(7) 0.6338(4) 0.054(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 0.0530(4) 0.0489(3) 0.0570(2) 0.0007(2) 0.0064(2) 0.0027(3) Au2 0.0459(5) 0.0499(4) 0.0501(3) 0.000 0.0008(3) 0.000 C1 0.124(17) 0.027(10) 0.064(9) 0.000 0.003(11) 0.000 C2 0.083(11) 0.046(8) 0.056(6) 0.007(6) 0.002(6) 0.007(7) C3 0.115(12) 0.059(7) 0.079(7) 0.008(6) 0.005(8) 0.032(8) C4 0.114(12) 0.076(8) 0.102(8) 0.003(7) 0.057(8) 0.017(8) C5 0.053(9) 0.064(8) 0.066(7) 0.006(7) 0.019(6) 0.014(7) C6 0.047(8) 0.057(8) 0.056(6) -0.001(6) 0.007(6) -0.009(6) C7 0.058(9) 0.033(7) 0.063(6) 0.000(6) -0.014(6) -0.011(6) C8 0.075(10) 0.053(7) 0.077(6) 0.001(6) 0.007(7) -0.013(7) Cl1 0.063(2) 0.107(2) 0.0938(19) 0.0052(18) -0.0067(17) 0.006(2) Cl2 0.070(3) 0.100(2) 0.0927(19) 0.0187(19) -0.0177(17) -0.011(2) Cl3 0.061(2) 0.146(3) 0.0834(17) -0.0146(19) -0.0172(18) -0.003(2) Cl4 0.229(8) 0.059(3) 0.145(4) 0.000 0.039(5) 0.000 Cl5 0.085(3) 0.102(2) 0.0864(18) 0.0248(19) 0.0296(17) -0.015(2) N1 0.087(9) 0.040(5) 0.056(5) -0.002(4) 0.009(4) 0.005(5) N2 0.067(7) 0.048(6) 0.056(5) 0.001(5) 0.019(5) -0.001(5) N3 0.059(7) 0.053(6) 0.050(4) -0.004(5) 0.001(4) -0.002(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 N2 1.990(7) . ? Au1 N1 2.002(8) . ? Au1 Cl2 2.253(3) . ? Au1 Cl1 2.268(3) . ? Au2 N3 2.005(7) 3_556 ? Au2 N3 2.005(7) . ? Au2 Cl3 2.249(3) . ? Au2 Cl3 2.249(3) 3_556 ? C1 C2 1.357(11) 3_556 ? C1 C2 1.357(11) . ? C1 Cl4 1.695(14) . ? C2 N1 1.328(11) . ? C2 C3 1.492(14) . ? C4 C5 1.495(13) . ? C5 N2 1.336(10) . ? C5 C6 1.359(12) . ? C6 C7 1.387(11) . ? C6 Cl5 1.705(9) . ? C7 N3 1.340(10) . ? C7 C8 1.472(11) . ? N1 N1 1.361(14) 3_556 ? N2 N3 1.371(9) . ? 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 N2 Au1 N1 176.2(3) . . ? N2 Au1 Cl2 89.2(2) . . ? N1 Au1 Cl2 88.9(2) . . ? N2 Au1 Cl1 90.0(2) . . ? N1 Au1 Cl1 92.3(2) . . ? Cl2 Au1 Cl1 174.14(10) . . ? N3 Au2 N3 176.9(5) 3_556 . ? N3 Au2 Cl3 91.5(2) 3_556 . ? N3 Au2 Cl3 88.8(2) . . ? N3 Au2 Cl3 88.8(2) 3_556 3_556 ? N3 Au2 Cl3 91.5(2) . 3_556 ? Cl3 Au2 Cl3 170.63(18) . 3_556 ? C2 C1 C2 107.9(14) 3_556 . ? C2 C1 Cl4 126.0(7) 3_556 . ? C2 C1 Cl4 126.0(7) . . ? N1 C2 C1 107.7(11) . . ? N1 C2 C3 121.8(9) . . ? C1 C2 C3 130.4(10) . . ? N2 C5 C6 108.4(9) . . ? N2 C5 C4 121.6(10) . . ? C6 C5 C4 129.9(10) . . ? C5 C6 C7 108.2(9) . . ? C5 C6 Cl5 127.1(9) . . ? C7 C6 Cl5 124.7(9) . . ? N3 C7 C6 106.1(8) . . ? N3 C7 C8 122.4(9) . . ? C6 C7 C8 131.5(10) . . ? C2 N1 N1 108.3(6) . 3_556 ? C2 N1 Au1 129.9(6) . . ? N1 N1 Au1 119.4(3) 3_556 . ? C5 N2 N3 107.6(8) . . ? C5 N2 Au1 130.9(8) . . ? N3 N2 Au1 121.6(6) . . ? C7 N3 N2 109.7(7) . . ? C7 N3 Au2 129.4(7) . . ? N2 N3 Au2 120.9(6) . . ? _diffrn_measured_fraction_theta_max 0.782 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.782 _refine_diff_density_max 0.647 _refine_diff_density_min -0.900 _refine_diff_density_rms 0.130 #=============================================END data_Au(III)2Au(I) _database_code_CSD 191324 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H20 Au3 Cl9 N6' _chemical_formula_weight 1206.33 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' '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.7600(16) _cell_length_b 29.270(6) _cell_length_c 13.510(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.00(3) _cell_angle_gamma 90.00 _cell_volume 3038.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needles _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.637 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 15.258 _exptl_absorpt_correction_type 'semi-empirical' _exptl_absorpt_correction_T_min 0.091 _exptl_absorpt_correction_T_max 0.614 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14202 _diffrn_reflns_av_R_equivalents 0.0778 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 23.34 _reflns_number_total 4393 _reflns_number_gt 3528 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART-NT V5.0' _computing_cell_refinement 'BRUKER SMART-NT V5.0' _computing_data_reduction 'BRUKER SAINT-NT V5/6.0' _computing_structure_solution 'BRUKER SHELXTL-NT V5.1' _computing_structure_refinement 'BRUKER SHELXTL-NT V5.1' _computing_molecular_graphics 'BRUKER SHELXTL-NT V5.1' _computing_publication_material 'BRUKER SHELXTL-NT V5.1' _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^)+(0.0795P)^2^+5.2493P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4393 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1395 _refine_ls_wR_factor_gt 0.1259 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _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 0.25104(7) 0.082434(17) 0.81337(4) 0.0415(2) Uani 1 1 d . . . Au2 Au 0.22779(7) 0.138504(18) 0.58513(4) 0.0437(2) Uani 1 1 d . . . Au3 Au 0.23956(8) 0.023751(19) 0.59687(4) 0.0508(2) Uani 1 1 d . . . C1 C 0.266(2) 0.1693(6) 0.9837(11) 0.066(4) Uani 1 1 d . . . H1A H 0.2446 0.1373 0.9904 0.098 Uiso 1 1 calc R . . H1B H 0.1798 0.1865 1.0123 0.098 Uiso 1 1 calc R . . H1C H 0.3795 0.1767 1.0177 0.098 Uiso 1 1 calc R . . C2 C 0.2570(17) 0.1807(4) 0.8789(9) 0.039(3) Uani 1 1 d . . . C3 C 0.259(2) 0.2243(5) 0.8340(12) 0.058(4) Uani 1 1 d . . . C4 C 0.255(2) 0.2183(5) 0.7306(10) 0.052(4) Uani 1 1 d . . . C5 C 0.248(3) 0.2501(7) 0.6497(14) 0.088(6) Uani 1 1 d . . . H5A H 0.3583 0.2652 0.6524 0.132 Uiso 1 1 calc R . . H5B H 0.1588 0.2723 0.6552 0.132 Uiso 1 1 calc R . . H5C H 0.2223 0.2341 0.5874 0.132 Uiso 1 1 calc R . . C6 C 0.193(3) 0.1626(7) 0.3312(13) 0.089(6) Uani 1 1 d . . . H6A H 0.2552 0.1823 0.3806 0.134 Uiso 1 1 calc R . . H6B H 0.0727 0.1715 0.3196 0.134 Uiso 1 1 calc R . . H6C H 0.2421 0.1650 0.2700 0.134 Uiso 1 1 calc R . . C7 C 0.206(2) 0.1181(6) 0.3649(11) 0.059(4) Uani 1 1 d . . . C8 C 0.214(2) 0.0775(7) 0.3097(13) 0.072(5) Uani 1 1 d . . . C9 C 0.2221(19) 0.0384(6) 0.3737(12) 0.056(4) Uani 1 1 d . . . C10 C 0.241(2) -0.0097(6) 0.3534(14) 0.080(6) Uani 1 1 d . . . H10A H 0.2991 -0.0246 0.4120 0.120 Uiso 1 1 calc R . . H10B H 0.3076 -0.0134 0.2993 0.120 Uiso 1 1 calc R . . H10C H 0.1277 -0.0231 0.3355 0.120 Uiso 1 1 calc R . . C11 C 0.274(3) -0.0893(5) 0.6732(17) 0.089(7) Uani 1 1 d . . . H11A H 0.3639 -0.1112 0.6943 0.134 Uiso 1 1 calc R . . H11B H 0.2961 -0.0751 0.6122 0.134 Uiso 1 1 calc R . . H11C H 0.1634 -0.1046 0.6623 0.134 Uiso 1 1 calc R . . C12 C 0.271(2) -0.0548(5) 0.7499(13) 0.058(4) Uani 1 1 d . . . C13 C 0.272(2) -0.0584(6) 0.8508(13) 0.064(4) Uani 1 1 d . . . C14 C 0.267(2) -0.0150(6) 0.8946(12) 0.059(4) Uani 1 1 d . . . C15 C 0.261(2) -0.0008(6) 0.9956(11) 0.060(4) Uani 1 1 d . . . H15A H 0.3245 0.0273 1.0080 0.090 Uiso 1 1 calc R . . H15B H 0.3137 -0.0239 1.0406 0.090 Uiso 1 1 calc R . . H15C H 0.1428 0.0037 1.0060 0.090 Uiso 1 1 calc R . . C16 C 0.258(3) 0.3078(6) 0.2830(12) 0.079(5) Uani 1 1 d . . . H16A H 0.3467 0.3307 0.2770 0.095 Uiso 1 1 calc R . . H16B H 0.1461 0.3214 0.2599 0.095 Uiso 1 1 calc R . . Cl1 Cl -0.0235(5) 0.08237(13) 0.8547(4) 0.0661(11) Uani 1 1 d . . . Cl2 Cl 0.5331(5) 0.08277(13) 0.7882(4) 0.0641(11) Uani 1 1 d . . . Cl3 Cl -0.0565(5) 0.12511(16) 0.5944(3) 0.0716(12) Uani 1 1 d . . . Cl4 Cl 0.5061(6) 0.15515(19) 0.5652(3) 0.0828(14) Uani 1 1 d . . . Cl5 Cl 0.2639(8) 0.27528(16) 0.8955(4) 0.0986(18) Uani 1 1 d . . . Cl6 Cl 0.2101(11) 0.0751(3) 0.1822(4) 0.132(3) Uani 1 1 d . . . Cl7 Cl 0.2880(10) -0.10727(19) 0.9180(5) 0.120(2) Uani 1 1 d . . . Cl8 Cl 0.2903(9) 0.26231(19) 0.2059(4) 0.1024(17) Uani 1 1 d . . . Cl9 Cl 0.2662(10) 0.2934(2) 0.4067(4) 0.123(2) Uani 1 1 d . . . N1 N 0.2468(13) 0.1513(3) 0.8046(8) 0.040(3) Uani 1 1 d . . . N2 N 0.2482(15) 0.1731(4) 0.7168(8) 0.046(3) Uani 1 1 d . . . N3 N 0.2096(16) 0.1030(4) 0.4596(8) 0.049(3) Uani 1 1 d . . . N4 N 0.2222(16) 0.0565(4) 0.4667(8) 0.054(3) Uani 1 1 d . . . N5 N 0.2600(15) -0.0085(4) 0.7281(9) 0.050(3) Uani 1 1 d . . . N6 N 0.2536(14) 0.0146(3) 0.8159(8) 0.039(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 0.0574(4) 0.0282(3) 0.0404(3) -0.0006(2) 0.0117(2) 0.0013(2) Au2 0.0629(4) 0.0327(4) 0.0370(3) -0.0039(2) 0.0129(2) -0.0015(2) Au3 0.0707(4) 0.0341(4) 0.0487(4) -0.0059(3) 0.0123(3) 0.0024(3) C1 0.095(13) 0.049(10) 0.051(9) -0.010(8) 0.005(8) -0.008(9) C2 0.061(8) 0.025(7) 0.032(7) -0.009(6) 0.006(6) -0.012(6) C3 0.077(11) 0.033(9) 0.066(10) -0.011(8) 0.019(8) 0.004(7) C4 0.072(10) 0.039(9) 0.047(8) 0.010(7) 0.014(7) 0.004(7) C5 0.114(16) 0.090(15) 0.064(11) -0.001(11) 0.025(11) 0.005(12) C6 0.134(17) 0.077(15) 0.053(10) 0.000(10) 0.003(11) -0.007(12) C7 0.067(10) 0.060(11) 0.051(9) -0.004(8) 0.014(7) -0.013(8) C8 0.053(10) 0.113(17) 0.053(10) -0.016(10) 0.016(8) -0.005(9) C9 0.050(9) 0.056(10) 0.064(10) -0.024(9) 0.017(7) -0.007(7) C10 0.089(13) 0.061(12) 0.094(14) -0.039(10) 0.027(10) -0.014(10) C11 0.117(16) 0.008(8) 0.135(18) -0.005(9) -0.008(14) 0.016(8) C12 0.066(10) 0.026(8) 0.077(11) -0.023(8) -0.014(8) 0.006(7) C13 0.067(10) 0.055(11) 0.070(11) 0.018(9) 0.012(8) -0.001(8) C14 0.066(10) 0.048(10) 0.063(10) -0.007(8) 0.012(8) -0.008(8) C15 0.067(10) 0.056(10) 0.058(9) 0.014(8) 0.013(8) -0.010(8) C16 0.113(15) 0.047(11) 0.075(11) 0.015(9) 0.011(10) -0.009(10) Cl1 0.065(2) 0.050(2) 0.089(3) 0.005(2) 0.029(2) 0.0026(18) Cl2 0.057(2) 0.049(2) 0.090(3) 0.000(2) 0.023(2) 0.0046(18) Cl3 0.064(2) 0.078(3) 0.076(3) -0.026(2) 0.020(2) -0.011(2) Cl4 0.073(3) 0.115(4) 0.066(3) -0.016(3) 0.026(2) -0.024(3) Cl5 0.170(5) 0.042(3) 0.089(3) -0.025(2) 0.037(3) -0.007(3) Cl6 0.189(7) 0.155(7) 0.057(3) -0.036(3) 0.041(4) -0.026(5) Cl7 0.180(6) 0.054(3) 0.125(5) 0.033(3) 0.020(4) 0.011(3) Cl8 0.153(5) 0.060(3) 0.094(4) 0.001(3) 0.018(3) -0.001(3) Cl9 0.199(7) 0.095(5) 0.080(4) 0.015(3) 0.037(4) -0.010(4) N1 0.049(7) 0.023(6) 0.050(7) 0.006(5) 0.013(5) 0.015(5) N2 0.064(7) 0.028(7) 0.046(6) -0.010(5) 0.013(5) -0.003(5) N3 0.076(8) 0.029(7) 0.047(7) -0.005(5) 0.023(6) -0.002(6) N4 0.078(9) 0.043(7) 0.042(7) -0.012(6) 0.018(6) 0.002(6) N5 0.069(8) 0.024(7) 0.053(7) 0.002(5) 0.001(6) 0.005(5) N6 0.061(7) 0.005(5) 0.050(7) 0.004(5) 0.012(5) 0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 N6 1.985(9) . ? Au1 N1 2.020(10) . ? Au1 Cl2 2.262(4) . ? Au1 Cl1 2.276(4) . ? Au1 Au3 3.3824(9) . ? Au1 Au2 3.4755(9) . ? Au2 N3 1.977(11) . ? Au2 N2 2.033(11) . ? Au2 Cl3 2.261(4) . ? Au2 Cl4 2.266(4) . ? Au2 Au3 3.3632(10) . ? Au3 N4 1.991(12) . ? Au3 N5 1.996(11) . ? C1 C2 1.446(19) . ? C2 N1 1.316(16) . ? C2 C3 1.41(2) . ? C3 C4 1.40(2) . ? C3 Cl5 1.707(15) . ? C4 N2 1.336(18) . ? C4 C5 1.43(2) . ? C6 C7 1.38(2) . ? C7 N3 1.351(18) . ? C7 C8 1.41(2) . ? C8 C9 1.43(2) . ? C8 Cl6 1.720(17) . ? C9 N4 1.364(17) . ? C9 C10 1.45(2) . ? C11 C12 1.45(2) . ? C12 C13 1.37(2) . ? C12 N5 1.385(18) . ? C13 C14 1.40(2) . ? C13 Cl7 1.691(17) . ? C14 N6 1.365(19) . ? C14 C15 1.43(2) . ? C16 Cl9 1.717(17) . ? C16 Cl8 1.728(18) . ? N1 N2 1.348(15) . ? N3 N4 1.366(17) . ? N5 N6 1.372(15) . ? 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 N6 Au1 N1 177.6(5) . . ? N6 Au1 Cl2 90.0(3) . . ? N1 Au1 Cl2 89.7(3) . . ? N6 Au1 Cl1 90.1(3) . . ? N1 Au1 Cl1 90.4(3) . . ? Cl2 Au1 Cl1 174.51(17) . . ? N6 Au1 Au3 60.4(3) . . ? N1 Au1 Au3 117.2(3) . . ? Cl2 Au1 Au3 77.39(12) . . ? Cl1 Au1 Au3 107.38(12) . . ? N6 Au1 Au2 119.1(3) . . ? N1 Au1 Au2 58.5(3) . . ? Cl2 Au1 Au2 78.25(12) . . ? Cl1 Au1 Au2 106.45(12) . . ? Au3 Au1 Au2 58.72(2) . . ? N3 Au2 N2 178.1(5) . . ? N3 Au2 Cl3 90.2(4) . . ? N2 Au2 Cl3 89.8(3) . . ? N3 Au2 Cl4 88.1(4) . . ? N2 Au2 Cl4 92.2(3) . . ? Cl3 Au2 Cl4 175.60(18) . . ? N3 Au2 Au3 60.9(3) . . ? N2 Au2 Au3 117.2(3) . . ? Cl3 Au2 Au3 81.06(12) . . ? Cl4 Au2 Au3 101.55(15) . . ? N3 Au2 Au1 120.1(3) . . ? N2 Au2 Au1 58.1(3) . . ? Cl3 Au2 Au1 78.44(12) . . ? Cl4 Au2 Au1 105.92(13) . . ? Au3 Au2 Au1 59.259(16) . . ? N4 Au3 N5 179.1(5) . . ? N4 Au3 Au2 58.6(3) . . ? N5 Au3 Au2 120.9(3) . . ? N4 Au3 Au1 120.6(3) . . ? N5 Au3 Au1 58.9(3) . . ? Au2 Au3 Au1 62.025(17) . . ? N1 C2 C3 105.4(11) . . ? N1 C2 C1 125.9(12) . . ? C3 C2 C1 128.8(13) . . ? C4 C3 C2 108.3(13) . . ? C4 C3 Cl5 126.2(12) . . ? C2 C3 Cl5 125.5(12) . . ? N2 C4 C3 105.0(12) . . ? N2 C4 C5 122.7(15) . . ? C3 C4 C5 132.2(16) . . ? N3 C7 C6 127.9(16) . . ? N3 C7 C8 103.2(15) . . ? C6 C7 C8 128.9(16) . . ? C7 C8 C9 110.9(14) . . ? C7 C8 Cl6 124.7(16) . . ? C9 C8 Cl6 124.4(14) . . ? N4 C9 C8 103.9(13) . . ? N4 C9 C10 124.5(16) . . ? C8 C9 C10 131.4(15) . . ? C13 C12 N5 106.2(13) . . ? C13 C12 C11 131.3(17) . . ? N5 C12 C11 122.5(16) . . ? C12 C13 C14 110.8(14) . . ? C12 C13 Cl7 126.3(15) . . ? C14 C13 Cl7 122.9(13) . . ? N6 C14 C13 104.5(13) . . ? N6 C14 C15 123.3(14) . . ? C13 C14 C15 132.1(15) . . ? Cl9 C16 Cl8 114.2(10) . . ? C2 N1 N2 110.8(10) . . ? C2 N1 Au1 127.5(9) . . ? N2 N1 Au1 121.4(8) . . ? C4 N2 N1 110.5(11) . . ? C4 N2 Au2 127.8(10) . . ? N1 N2 Au2 121.7(8) . . ? C7 N3 N4 112.6(11) . . ? C7 N3 Au2 129.0(10) . . ? N4 N3 Au2 117.9(8) . . ? C9 N4 N3 109.4(12) . . ? C9 N4 Au3 128.1(11) . . ? N3 N4 Au3 122.5(8) . . ? N6 N5 C12 107.9(11) . . ? N6 N5 Au3 121.7(8) . . ? C12 N5 Au3 130.2(10) . . ? C14 N6 N5 110.5(10) . . ? C14 N6 Au1 130.4(9) . . ? N5 N6 Au1 118.7(8) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.34 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.647 _refine_diff_density_min -1.847 _refine_diff_density_rms 0.307 #====================================END data_Au(III)Au(I)2 _database_code_CSD 191325 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H33 Au6 Cl11.30 N12' _chemical_formula_weight 2144.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Cl' 'Cl' 0.1484 0.1585 '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 12.686(3) _cell_length_b 13.792(3) _cell_length_c 16.634(3) _cell_angle_alpha 69.65(3) _cell_angle_beta 80.95(3) _cell_angle_gamma 67.60(3) _cell_volume 2521.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.824 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1926 _exptl_absorpt_coefficient_mu 18.025 _exptl_absorpt_correction_type 'semi-empirical' _exptl_absorpt_correction_T_min 0.330 _exptl_absorpt_correction_T_max 0.698 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11123 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 23.29 _reflns_number_total 7247 _reflns_number_gt 4672 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART-NT V5.0' _computing_cell_refinement 'BRUKER SMART-NT V5.0' _computing_data_reduction 'BRUKER SAINT-NT V5/6.0' _computing_structure_solution 'BRUKER SHELXTL-NT V5.1' _computing_structure_refinement 'BRUKER SHELXTL-NT V5.1' _computing_molecular_graphics 'BRUKER SHELXTL-NT V5.1' _computing_publication_material 'BRUKER SHELXTL-NT V5.1' _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^)+(0.0463P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7247 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0840 _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_restrained_S_all 0.920 _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 0.08910(5) 0.67724(4) 0.23485(4) 0.05213(18) Uani 1 1 d . . . Au2 Au 0.35715(5) 0.50888(5) 0.19766(4) 0.05725(19) Uani 1 1 d . . . Au3 Au 0.27717(5) 0.78010(5) 0.09727(4) 0.0620(2) Uani 1 1 d . . . Au4 Au 0.73325(5) 0.21997(5) 0.38995(4) 0.05615(18) Uani 1 1 d . . . Au5 Au 0.52661(5) 0.47382(5) 0.36361(4) 0.0618(2) Uani 1 1 d . . . Au6 Au 0.77203(5) 0.44980(5) 0.24923(4) 0.0681(2) Uani 1 1 d . . . C1 C -0.0405(12) 0.5035(14) 0.3784(11) 0.085(5) Uani 1 1 d . . . H1A H -0.0755 0.4485 0.4011 0.128 Uiso 1 1 calc R . . H1B H -0.0810 0.5598 0.3293 0.128 Uiso 1 1 calc R . . H1C H -0.0427 0.5361 0.4215 0.128 Uiso 1 1 calc R . . C2 C 0.0830(12) 0.4500(12) 0.3521(9) 0.054(4) Uani 1 1 d . . . C3 C 0.1533(13) 0.3426(12) 0.3713(10) 0.066(4) Uani 1 1 d . . . C4 C 0.2569(11) 0.3450(12) 0.3241(10) 0.057(4) Uani 1 1 d . . . C5 C 0.3618(15) 0.2489(14) 0.3211(12) 0.088(6) Uani 1 1 d . . . H5A H 0.4262 0.2736 0.3120 0.106 Uiso 1 1 calc R . . H5B H 0.3695 0.1940 0.3774 0.106 Uiso 1 1 calc R . . C6 C 0.6258(15) 0.3962(13) 0.1050(12) 0.100(6) Uani 1 1 d . . . H6A H 0.6811 0.3744 0.1472 0.151 Uiso 1 1 calc R . . H6B H 0.6634 0.3745 0.0560 0.151 Uiso 1 1 calc R . . H6C H 0.5707 0.3609 0.1291 0.151 Uiso 1 1 calc R . . C7 C 0.5667(13) 0.5190(13) 0.0783(10) 0.066(5) Uani 1 1 d . . . C8 C 0.5988(13) 0.6047(14) 0.0172(12) 0.079(5) Uani 1 1 d . . . C9 C 0.5127(14) 0.7012(14) 0.0139(10) 0.072(5) Uani 1 1 d . . . C10 C 0.5075(17) 0.8106(16) -0.0398(12) 0.106(7) Uani 1 1 d . . . H10A H 0.5846 0.8106 -0.0547 0.127 Uiso 1 1 calc R . . H10B H 0.4706 0.8620 -0.0076 0.127 Uiso 1 1 calc R . . C11 C 0.1352(15) 1.0604(12) 0.0317(10) 0.088(6) Uani 1 1 d . . . H11A H 0.1515 1.0435 -0.0212 0.133 Uiso 1 1 calc R . . H11B H 0.2053 1.0467 0.0560 0.133 Uiso 1 1 calc R . . H11C H 0.0880 1.1367 0.0210 0.133 Uiso 1 1 calc R . . C12 C 0.0754(13) 0.9904(12) 0.0920(9) 0.065(5) Uani 1 1 d . . . C13 C -0.0346(13) 1.0174(12) 0.1287(10) 0.063(4) Uani 1 1 d . . . C14 C -0.0520(12) 0.9247(12) 0.1776(9) 0.055(4) Uani 1 1 d . . . C15 C -0.1550(14) 0.9034(14) 0.2310(11) 0.093(6) Uani 1 1 d . . . H15A H -0.2229 0.9657 0.2104 0.140 Uiso 1 1 calc R . . H15B H -0.1456 0.8927 0.2900 0.140 Uiso 1 1 calc R . . H15C H -0.1613 0.8385 0.2262 0.140 Uiso 1 1 calc R . . C16 C 0.9817(15) 0.0047(16) 0.3782(14) 0.116(8) Uani 1 1 d . . . H16A H 0.9111 -0.0064 0.3793 0.173 Uiso 1 1 calc R . . H16B H 0.9985 -0.0043 0.4352 0.173 Uiso 1 1 calc R . . H16C H 1.0420 -0.0485 0.3565 0.173 Uiso 1 1 calc R . . C17 C 0.9714(15) 0.1202(17) 0.3205(12) 0.082(5) Uani 1 1 d . . . C18 C 1.0498(15) 0.1561(18) 0.2624(14) 0.093(7) Uani 1 1 d . . . C19 C 0.9996(15) 0.2683(19) 0.2291(12) 0.088(6) Uani 1 1 d . . . C20 C 1.0445(18) 0.353(2) 0.1665(12) 0.119(8) Uani 1 1 d . . . H20A H 1.1272 0.3228 0.1635 0.143 Uiso 1 1 calc R . . H20B H 1.0218 0.4175 0.1854 0.143 Uiso 1 1 calc R . . C21 C 0.7551(18) 0.7119(17) 0.1181(16) 0.162(11) Uani 1 1 d . . . H21A H 0.8144 0.7134 0.1466 0.242 Uiso 1 1 calc R . . H21B H 0.7277 0.7798 0.0720 0.242 Uiso 1 1 calc R . . H21C H 0.7846 0.6510 0.0956 0.242 Uiso 1 1 calc R . . C22 C 0.6553(17) 0.6983(15) 0.1832(14) 0.092(6) Uani 1 1 d . . . C23 C 0.554(2) 0.7701(15) 0.2034(13) 0.100(7) Uani 1 1 d . . . C24 C 0.4836(15) 0.7168(13) 0.2650(11) 0.074(5) Uani 1 1 d . . . C25 C 0.3730(15) 0.7558(15) 0.3089(13) 0.110(7) Uani 1 1 d . . . H25A H 0.3245 0.7196 0.3032 0.165 Uiso 1 1 calc R . . H25B H 0.3376 0.8342 0.2836 0.165 Uiso 1 1 calc R . . H25C H 0.3847 0.7389 0.3686 0.165 Uiso 1 1 calc R . . C26 C 0.3069(14) 0.4208(16) 0.5050(11) 0.107(7) Uani 1 1 d . . . H26A H 0.2952 0.4249 0.5624 0.160 Uiso 1 1 calc R . . H26B H 0.2432 0.4099 0.4899 0.160 Uiso 1 1 calc R . . H26C H 0.3138 0.4884 0.4659 0.160 Uiso 1 1 calc R . . C27 C 0.4139(13) 0.3260(14) 0.5001(11) 0.072(5) Uani 1 1 d . . . C28 C 0.4421(13) 0.2118(15) 0.5433(11) 0.077(5) Uani 1 1 d . . . C29 C 0.5504(16) 0.1584(14) 0.5157(11) 0.081(5) Uani 1 1 d . . . C30 C 0.6279(17) 0.0357(13) 0.5420(13) 0.113(7) Uani 1 1 d . . . H30A H 0.6942 0.0263 0.5690 0.169 Uiso 1 1 calc R . . H30B H 0.6509 0.0123 0.4919 0.169 Uiso 1 1 calc R . . H30C H 0.5868 -0.0080 0.5814 0.169 Uiso 1 1 calc R . . Cl1 Cl 0.0696(4) 0.6496(3) 0.1115(3) 0.0805(13) Uani 1 1 d . . . Cl2 Cl 0.0992(4) 0.7041(4) 0.3602(3) 0.0860(13) Uani 1 1 d . . . Cl3 Cl 0.1253(4) 0.2337(4) 0.4399(3) 0.1025(17) Uani 1 1 d . . . Cl4 Cl 0.7231(4) 0.5803(5) -0.0421(4) 0.118(2) Uani 1 1 d . . . Cl5 Cl -0.1322(4) 1.1507(3) 0.1077(3) 0.1023(17) Uani 1 1 d . . . Cl6 Cl 0.6739(4) 0.1523(4) 0.3064(3) 0.0829(13) Uani 1 1 d . . . Cl7 Cl 0.7969(4) 0.2776(4) 0.4781(3) 0.0867(14) Uani 1 1 d . . . Cl8 Cl 0.3600(5) 0.1538(5) 0.6186(4) 0.138(2) Uani 1 1 d . . . Cl9 Cl 0.5001(7) 0.9149(4) 0.1590(5) 0.168(3) Uani 1 1 d . . . Cl10 Cl 1.1845(4) 0.0800(6) 0.2397(4) 0.144(3) Uani 1 1 d . . . Cl11 Cl 0.4396(15) 0.8531(11) -0.1267(10) 0.175(6) Uani 0.50 1 d P . . Cl12 Cl 0.374(2) 0.195(2) 0.2603(19) 0.107(9) Uani 0.20 1 d P . . Cl13 Cl 0.996(2) 0.3874(19) 0.0756(13) 0.311(11) Uani 0.60 1 d P . . N1 N 0.1392(9) 0.5155(8) 0.2935(7) 0.054(3) Uani 1 1 d . . . N2 N 0.2477(9) 0.4475(10) 0.2770(8) 0.063(4) Uani 1 1 d . . . N3 N 0.4631(10) 0.5690(11) 0.1115(7) 0.061(3) Uani 1 1 d . . . N4 N 0.4341(10) 0.6791(10) 0.0729(8) 0.063(4) Uani 1 1 d . . . N5 N 0.1220(10) 0.8792(9) 0.1210(7) 0.056(3) Uani 1 1 d . . . N6 N 0.0456(9) 0.8387(9) 0.1758(7) 0.053(3) Uani 1 1 d . . . N7 N 0.5876(11) 0.2378(10) 0.4580(7) 0.060(3) Uani 1 1 d . . . N8 N 0.5035(10) 0.3382(9) 0.4457(8) 0.062(3) Uani 1 1 d . . . N9 N 0.5526(11) 0.6075(9) 0.2837(8) 0.068(4) Uani 1 1 d . . . N10 N 0.6537(11) 0.5977(10) 0.2330(9) 0.073(4) Uani 1 1 d . . . N11 N 0.8915(10) 0.3032(11) 0.2651(8) 0.064(4) Uani 1 1 d . . . N12 N 0.8783(10) 0.2073(11) 0.3205(8) 0.063(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 Au1 0.0438(3) 0.0433(3) 0.0597(4) -0.0141(3) 0.0079(3) -0.0107(3) Au2 0.0436(4) 0.0478(4) 0.0698(4) -0.0136(3) 0.0125(3) -0.0148(3) Au3 0.0541(4) 0.0489(4) 0.0722(4) -0.0170(3) 0.0168(3) -0.0158(3) Au4 0.0445(4) 0.0479(4) 0.0682(4) -0.0179(3) 0.0063(3) -0.0113(3) Au5 0.0520(4) 0.0458(4) 0.0775(5) -0.0143(3) 0.0091(3) -0.0153(3) Au6 0.0570(4) 0.0665(4) 0.0802(5) -0.0198(4) 0.0132(3) -0.0302(3) C1 0.049(11) 0.107(14) 0.105(14) -0.045(12) 0.029(10) -0.035(10) C2 0.053(10) 0.060(10) 0.051(10) -0.011(8) 0.006(8) -0.030(8) C3 0.054(10) 0.049(10) 0.083(12) -0.003(9) -0.006(9) -0.019(8) C4 0.030(8) 0.053(10) 0.085(12) -0.017(9) 0.009(8) -0.020(7) C5 0.069(12) 0.069(12) 0.114(16) -0.015(12) 0.006(11) -0.026(10) C6 0.090(14) 0.064(12) 0.118(16) -0.031(11) -0.026(12) 0.015(10) C7 0.048(10) 0.066(11) 0.075(12) -0.033(10) -0.001(9) -0.002(8) C8 0.052(11) 0.072(12) 0.103(14) -0.030(11) 0.037(10) -0.025(9) C9 0.063(11) 0.069(12) 0.076(12) -0.007(10) 0.031(9) -0.041(10) C10 0.102(16) 0.098(16) 0.103(16) -0.019(13) 0.033(13) -0.047(13) C11 0.111(15) 0.051(10) 0.070(12) 0.002(9) 0.028(10) -0.024(10) C12 0.068(11) 0.050(10) 0.063(11) -0.023(8) 0.018(9) -0.009(8) C13 0.061(11) 0.050(10) 0.065(11) -0.021(9) -0.011(9) -0.001(8) C14 0.044(9) 0.048(9) 0.066(11) -0.020(8) 0.009(8) -0.010(8) C15 0.062(12) 0.083(13) 0.106(15) -0.038(11) 0.032(10) -0.001(9) C16 0.070(14) 0.099(17) 0.17(2) -0.066(16) -0.025(14) 0.010(11) C17 0.055(12) 0.098(15) 0.102(15) -0.047(13) 0.002(11) -0.024(11) C18 0.046(12) 0.120(18) 0.138(19) -0.086(16) 0.018(12) -0.023(12) C19 0.059(12) 0.133(19) 0.090(14) -0.064(14) 0.031(11) -0.038(13) C20 0.109(18) 0.20(3) 0.067(14) -0.055(16) 0.035(13) -0.079(18) C21 0.099(18) 0.081(16) 0.25(3) 0.037(17) 0.008(18) -0.056(14) C22 0.084(15) 0.042(11) 0.142(19) -0.021(12) -0.024(13) -0.013(10) C23 0.17(2) 0.047(11) 0.096(15) 0.008(11) -0.038(15) -0.068(14) C24 0.091(14) 0.049(10) 0.073(12) 0.001(9) -0.022(10) -0.025(10) C25 0.061(12) 0.096(15) 0.157(19) -0.049(14) 0.033(12) -0.017(11) C26 0.069(13) 0.121(16) 0.101(15) -0.037(13) 0.053(11) -0.023(11) C27 0.048(10) 0.082(13) 0.078(12) -0.024(10) 0.018(9) -0.024(9) C28 0.047(11) 0.091(14) 0.080(13) -0.019(11) 0.018(9) -0.027(10) C29 0.084(14) 0.070(12) 0.094(14) -0.020(11) 0.002(11) -0.040(11) C30 0.119(17) 0.045(11) 0.148(19) 0.004(12) 0.000(14) -0.033(11) Cl1 0.095(3) 0.069(3) 0.070(3) -0.025(2) -0.004(2) -0.018(2) Cl2 0.100(4) 0.083(3) 0.078(3) -0.036(3) -0.005(3) -0.024(3) Cl3 0.084(3) 0.067(3) 0.130(4) 0.006(3) 0.015(3) -0.039(3) Cl4 0.078(4) 0.130(4) 0.146(5) -0.061(4) 0.060(3) -0.045(3) Cl5 0.103(4) 0.053(3) 0.106(4) -0.018(3) 0.003(3) 0.012(2) Cl6 0.066(3) 0.091(3) 0.108(4) -0.054(3) 0.005(2) -0.027(2) Cl7 0.071(3) 0.117(4) 0.093(3) -0.055(3) 0.010(2) -0.040(3) Cl8 0.134(5) 0.156(6) 0.122(5) -0.018(4) 0.054(4) -0.096(5) Cl9 0.212(8) 0.053(3) 0.197(7) 0.006(4) -0.008(6) -0.044(4) Cl10 0.053(3) 0.203(7) 0.180(6) -0.120(5) 0.019(3) -0.003(4) Cl11 0.244(19) 0.112(10) 0.169(14) -0.011(10) -0.047(13) -0.079(11) Cl12 0.083(18) 0.087(18) 0.14(2) -0.048(18) -0.019(16) -0.003(13) Cl13 0.38(3) 0.35(3) 0.24(2) -0.04(2) 0.00(2) -0.23(3) N1 0.047(8) 0.033(6) 0.066(8) 0.000(6) -0.012(6) -0.008(6) N2 0.027(7) 0.050(8) 0.101(10) -0.023(7) 0.025(6) -0.011(6) N3 0.045(8) 0.075(9) 0.059(8) -0.024(7) 0.020(6) -0.024(7) N4 0.048(8) 0.042(8) 0.082(10) -0.013(7) 0.015(7) -0.010(6) N5 0.066(9) 0.031(7) 0.059(8) -0.012(6) 0.000(7) -0.007(6) N6 0.043(7) 0.040(7) 0.071(9) -0.018(6) 0.004(6) -0.012(6) N7 0.072(9) 0.063(9) 0.057(8) -0.018(7) 0.021(7) -0.046(8) N8 0.041(7) 0.051(8) 0.084(10) -0.019(7) 0.018(7) -0.014(6) N9 0.068(10) 0.045(8) 0.083(10) -0.021(7) -0.002(8) -0.010(7) N10 0.069(9) 0.048(8) 0.094(10) -0.004(7) 0.008(8) -0.032(7) N11 0.044(8) 0.072(9) 0.069(9) -0.025(8) 0.009(7) -0.013(7) N12 0.036(7) 0.069(9) 0.085(10) -0.039(8) 0.021(7) -0.015(7) _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 N1 1.983(10) . ? Au1 N6 1.985(11) . ? Au1 Cl2 2.272(4) . ? Au1 Cl1 2.279(4) . ? Au2 N2 1.982(11) . ? Au2 N3 1.991(11) . ? Au2 Au3 3.3326(15) . ? Au3 N5 1.994(11) . ? Au3 N4 2.023(11) . ? Au4 N7 1.987(11) . ? Au4 N12 1.994(11) . ? Au4 Cl7 2.260(4) . ? Au4 Cl6 2.267(4) . ? Au5 N9 1.974(12) . ? Au5 N8 1.991(12) . ? Au5 Au6 3.3484(14) . ? Au6 N11 1.968(12) . ? Au6 N10 1.974(13) . ? C1 C2 1.522(19) . ? C2 C3 1.359(18) . ? C2 N1 1.391(16) . ? C3 C4 1.427(19) . ? C3 Cl3 1.665(15) . ? C4 N2 1.326(16) . ? C4 C5 1.49(2) . ? C5 Cl12 1.41(3) . ? C6 C7 1.50(2) . ? C7 N3 1.362(17) . ? C7 C8 1.41(2) . ? C8 C9 1.35(2) . ? C8 Cl4 1.706(15) . ? C9 N4 1.329(17) . ? C9 C10 1.44(2) . ? C10 Cl11 1.61(2) . ? C11 C12 1.470(19) . ? C12 N5 1.348(16) . ? C12 C13 1.40(2) . ? C13 C14 1.334(19) . ? C13 Cl5 1.729(14) . ? C14 N6 1.354(16) . ? C14 C15 1.53(2) . ? C16 C17 1.51(2) . ? C17 N12 1.33(2) . ? C17 C18 1.38(2) . ? C18 C19 1.37(3) . ? C18 Cl10 1.695(17) . ? C19 N11 1.382(19) . ? C19 C20 1.50(3) . ? C20 Cl13 1.57(2) . ? C21 C22 1.56(3) . ? C22 N10 1.35(2) . ? C22 C23 1.37(3) . ? C23 C24 1.44(3) . ? C23 Cl9 1.758(18) . ? C24 N9 1.375(18) . ? C24 C25 1.47(2) . ? C26 C27 1.50(2) . ? C27 N8 1.363(17) . ? C27 C28 1.41(2) . ? C28 C29 1.38(2) . ? C28 Cl8 1.680(16) . ? C29 N7 1.364(19) . ? C29 C30 1.54(2) . ? N1 N2 1.388(14) . ? N3 N4 1.351(15) . ? N5 N6 1.365(15) . ? N7 N8 1.358(15) . ? N9 N10 1.408(17) . ? N11 N12 1.379(15) . ? 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 N1 Au1 N6 177.6(5) . . ? N1 Au1 Cl2 89.9(3) . . ? N6 Au1 Cl2 89.7(3) . . ? N1 Au1 Cl1 89.6(3) . . ? N6 Au1 Cl1 90.9(3) . . ? Cl2 Au1 Cl1 176.92(17) . . ? N2 Au2 N3 176.0(5) . . ? N2 Au2 Au3 119.5(3) . . ? N3 Au2 Au3 60.6(4) . . ? N5 Au3 N4 179.6(5) . . ? N5 Au3 Au2 119.7(3) . . ? N4 Au3 Au2 60.2(3) . . ? N7 Au4 N12 178.2(5) . . ? N7 Au4 Cl7 89.6(4) . . ? N12 Au4 Cl7 89.7(4) . . ? N7 Au4 Cl6 90.5(4) . . ? N12 Au4 Cl6 90.3(4) . . ? Cl7 Au4 Cl6 176.77(18) . . ? N9 Au5 N8 178.7(5) . . ? N9 Au5 Au6 60.3(4) . . ? N8 Au5 Au6 119.0(3) . . ? N11 Au6 N10 179.2(5) . . ? N11 Au6 Au5 119.8(4) . . ? N10 Au6 Au5 60.8(4) . . ? C3 C2 N1 108.7(13) . . ? C3 C2 C1 131.7(14) . . ? N1 C2 C1 119.4(13) . . ? C2 C3 C4 105.1(13) . . ? C2 C3 Cl3 126.6(13) . . ? C4 C3 Cl3 128.1(12) . . ? N2 C4 C3 110.8(12) . . ? N2 C4 C5 121.8(12) . . ? C3 C4 C5 127.2(14) . . ? Cl12 C5 C4 120.0(17) . . ? N3 C7 C8 106.3(13) . . ? N3 C7 C6 122.8(16) . . ? C8 C7 C6 130.9(15) . . ? C9 C8 C7 107.6(13) . . ? C9 C8 Cl4 129.6(14) . . ? C7 C8 Cl4 122.7(13) . . ? N4 C9 C8 107.8(14) . . ? N4 C9 C10 124.9(16) . . ? C8 C9 C10 127.2(15) . . ? C9 C10 Cl11 113.2(16) . . ? N5 C12 C13 105.9(13) . . ? N5 C12 C11 123.0(14) . . ? C13 C12 C11 131.1(14) . . ? C14 C13 C12 109.1(13) . . ? C14 C13 Cl5 126.8(13) . . ? C12 C13 Cl5 123.9(13) . . ? C13 C14 N6 107.8(13) . . ? C13 C14 C15 132.3(13) . . ? N6 C14 C15 119.9(13) . . ? N12 C17 C18 108.2(18) . . ? N12 C17 C16 122.1(17) . . ? C18 C17 C16 129.6(18) . . ? C19 C18 C17 106.3(17) . . ? C19 C18 Cl10 125.7(17) . . ? C17 C18 Cl10 127.9(19) . . ? C18 C19 N11 110.1(18) . . ? C18 C19 C20 131.0(19) . . ? N11 C19 C20 118.9(19) . . ? C19 C20 Cl13 109.4(17) . . ? N10 C22 C23 104.0(18) . . ? N10 C22 C21 121.8(17) . . ? C23 C22 C21 134.2(18) . . ? C22 C23 C24 113.9(17) . . ? C22 C23 Cl9 127.7(18) . . ? C24 C23 Cl9 118.4(19) . . ? N9 C24 C23 101.5(17) . . ? N9 C24 C25 123.5(16) . . ? C23 C24 C25 134.8(17) . . ? N8 C27 C28 106.7(13) . . ? N8 C27 C26 123.1(15) . . ? C28 C27 C26 130.1(14) . . ? C29 C28 C27 107.7(14) . . ? C29 C28 Cl8 126.8(15) . . ? C27 C28 Cl8 125.4(13) . . ? N7 C29 C28 107.0(15) . . ? N7 C29 C30 121.2(16) . . ? C28 C29 C30 131.7(17) . . ? N2 N1 C2 108.5(11) . . ? N2 N1 Au1 120.1(9) . . ? C2 N1 Au1 131.4(10) . . ? C4 N2 N1 106.8(10) . . ? C4 N2 Au2 131.8(9) . . ? N1 N2 Au2 121.4(9) . . ? N4 N3 C7 107.6(12) . . ? N4 N3 Au2 120.2(9) . . ? C7 N3 Au2 132.2(11) . . ? C9 N4 N3 110.6(12) . . ? C9 N4 Au3 129.8(11) . . ? N3 N4 Au3 118.9(9) . . ? C12 N5 N6 108.8(12) . . ? C12 N5 Au3 129.4(10) . . ? N6 N5 Au3 121.8(8) . . ? C14 N6 N5 108.3(11) . . ? C14 N6 Au1 132.1(10) . . ? N5 N6 Au1 119.7(8) . . ? N8 N7 C29 109.6(13) . . ? N8 N7 Au4 121.3(9) . . ? C29 N7 Au4 128.9(12) . . ? N7 N8 C27 108.8(12) . . ? N7 N8 Au5 120.7(9) . . ? C27 N8 Au5 130.4(11) . . ? C24 N9 N10 109.8(13) . . ? C24 N9 Au5 130.2(12) . . ? N10 N9 Au5 120.0(9) . . ? C22 N10 N9 110.8(14) . . ? C22 N10 Au6 130.2(12) . . ? N9 N10 Au6 118.8(9) . . ? N12 N11 C19 104.2(13) . . ? N12 N11 Au6 122.9(9) . . ? C19 N11 Au6 132.9(14) . . ? C17 N12 N11 111.1(13) . . ? C17 N12 Au4 130.9(13) . . ? N11 N12 Au4 117.9(9) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.231 _refine_diff_density_min -0.900 _refine_diff_density_rms 0.181 #============================================END data_Au(I)Au(III)2Cl4(dmpz)3 _database_code_CSD 191326 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H21 Au3 Cl4 N6' _chemical_formula_weight 1018.08 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' '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 7.6249(15) _cell_length_b 12.505(3) _cell_length_c 13.495(3) _cell_angle_alpha 73.88(3) _cell_angle_beta 86.39(3) _cell_angle_gamma 85.21(3) _cell_volume 1230.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description priam _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.747 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 18.283 _exptl_absorpt_correction_type 'semi-empirical' _exptl_absorpt_correction_T_min 0.173 _exptl_absorpt_correction_T_max 0.398 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6314 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 23.31 _reflns_number_total 3544 _reflns_number_gt 2670 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART-NT V5.0' _computing_cell_refinement 'BRUKER SMART-NT V5.0' _computing_data_reduction 'BRUKER SAINT-NT V5/6.0' _computing_structure_solution 'BRUKER SHELXTL-NT V5.1' _computing_structure_refinement 'BRUKER SHELXTL-NT V5.1' _computing_molecular_graphics 'BRUKER SHELXTL-NT V5.1' _computing_publication_material 'BRUKER SHELXTL-NT V5.1' _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^)+(0.0714P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3544 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.0993 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.015 _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 0.25294(7) 0.37188(5) 0.78587(4) 0.0589(2) Uani 1 1 d . . . Au2 Au 0.24911(8) 0.10020(5) 0.91936(4) 0.0679(2) Uani 1 1 d . . . Au3 Au 0.23206(8) 0.16768(5) 0.66044(4) 0.0643(2) Uani 1 1 d . . . C1 C 0.258(3) 0.5180(14) 0.9685(14) 0.105(6) Uani 1 1 d . . . H1A H 0.3767 0.5396 0.9661 0.158 Uiso 1 1 calc R . . H1B H 0.1867 0.5496 1.0158 0.158 Uiso 1 1 calc R . . H1C H 0.2115 0.5447 0.9009 0.158 Uiso 1 1 calc R . . C2 C 0.258(2) 0.3906(16) 1.0046(12) 0.083(5) Uani 1 1 d . . . C3 C 0.267(2) 0.3156(18) 1.1054(12) 0.091(5) Uani 1 1 d . . . H3 H 0.2709 0.3350 1.1669 0.110 Uiso 1 1 calc R . . C4 C 0.270(2) 0.2111(16) 1.0954(12) 0.087(5) Uani 1 1 d . . . C5 C 0.270(3) 0.1017(15) 1.1744(12) 0.107(7) Uani 1 1 d . . . H5A H 0.3649 0.0949 1.2197 0.160 Uiso 1 1 calc R . . H5B H 0.2846 0.0428 1.1410 0.160 Uiso 1 1 calc R . . H5C H 0.1600 0.0966 1.2137 0.160 Uiso 1 1 calc R . . C6 C 0.237(2) -0.1836(15) 0.9937(13) 0.100(6) Uani 1 1 d . . . H6A H 0.3567 -0.2050 1.0127 0.150 Uiso 1 1 calc R . . H6B H 0.1703 -0.2486 1.0111 0.150 Uiso 1 1 calc R . . H6C H 0.1867 -0.1318 1.0302 0.150 Uiso 1 1 calc R . . C7 C 0.233(2) -0.1303(14) 0.8813(14) 0.082(5) Uani 1 1 d . . . C8 C 0.216(3) -0.1739(18) 0.7973(18) 0.111(7) Uani 1 1 d . . . H8 H 0.2078 -0.2485 0.8001 0.133 Uiso 1 1 calc R . . C9 C 0.215(3) -0.0838(17) 0.7085(15) 0.102(6) Uani 1 1 d . . . C10 C 0.199(4) -0.0807(19) 0.5981(15) 0.157(11) Uani 1 1 d . . . H10A H 0.0775 -0.0687 0.5812 0.236 Uiso 1 1 calc R . . H10B H 0.2464 -0.1504 0.5872 0.236 Uiso 1 1 calc R . . H10C H 0.2637 -0.0211 0.5548 0.236 Uiso 1 1 calc R . . C11 C 0.223(3) 0.3087(17) 0.4045(13) 0.116(7) Uani 1 1 d . . . H11A H 0.2202 0.3574 0.3357 0.174 Uiso 1 1 calc R . . H11B H 0.1178 0.2695 0.4203 0.174 Uiso 1 1 calc R . . H11C H 0.3238 0.2560 0.4095 0.174 Uiso 1 1 calc R . . C12 C 0.237(2) 0.3765(15) 0.4801(11) 0.077(5) Uani 1 1 d . . . C13 C 0.243(2) 0.4880(15) 0.4646(12) 0.081(5) Uani 1 1 d . . . H13 H 0.2410 0.5417 0.4011 0.097 Uiso 1 1 calc R . . C14 C 0.2525(19) 0.5079(13) 0.5606(11) 0.072(5) Uani 1 1 d . . . C15 C 0.269(2) 0.6154(13) 0.5890(13) 0.092(6) Uani 1 1 d . . . H15A H 0.1655 0.6315 0.6278 0.139 Uiso 1 1 calc R . . H15B H 0.2826 0.6753 0.5272 0.139 Uiso 1 1 calc R . . H15C H 0.3706 0.6077 0.6299 0.139 Uiso 1 1 calc R . . Cl1 Cl 0.5454(7) 0.3419(9) 0.7788(4) 0.220(5) Uani 1 1 d . . . Cl2 Cl -0.0370(6) 0.4190(6) 0.7944(3) 0.131(2) Uani 1 1 d . . . Cl3 Cl 0.5216(7) 0.1399(6) 0.6266(7) 0.192(4) Uani 1 1 d . . . Cl4 Cl -0.0609(7) 0.1868(4) 0.6797(6) 0.153(3) Uani 1 1 d . . . N1 N 0.2587(16) 0.2175(11) 0.9913(8) 0.069(3) Uani 1 1 d . . . N2 N 0.2568(16) 0.3280(11) 0.9393(7) 0.068(3) Uani 1 1 d . . . N3 N 0.2373(16) -0.0161(10) 0.8489(10) 0.076(4) Uani 1 1 d . . . N4 N 0.2239(18) 0.0094(11) 0.7395(10) 0.080(4) Uani 1 1 d . . . N5 N 0.2398(14) 0.3297(10) 0.5830(8) 0.061(3) Uani 1 1 d . . . N6 N 0.2511(14) 0.4094(9) 0.6313(8) 0.055(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 0.0570(4) 0.0643(4) 0.0442(3) 0.0052(2) -0.0069(2) -0.0060(3) Au2 0.0678(4) 0.0673(4) 0.0553(3) 0.0067(3) -0.0074(3) -0.0050(3) Au3 0.0631(4) 0.0670(4) 0.0547(3) -0.0015(3) -0.0096(2) -0.0046(3) C1 0.148(19) 0.080(13) 0.096(13) -0.029(11) -0.007(12) -0.040(12) C2 0.070(11) 0.113(14) 0.054(9) -0.001(9) 0.002(7) -0.006(10) C3 0.098(14) 0.121(16) 0.048(8) -0.007(9) -0.007(8) -0.023(11) C4 0.098(14) 0.091(13) 0.061(9) -0.002(9) -0.001(8) -0.005(10) C5 0.124(16) 0.117(15) 0.054(9) 0.017(10) -0.004(9) -0.001(12) C6 0.102(14) 0.080(12) 0.093(12) 0.021(10) -0.014(10) -0.013(10) C7 0.060(10) 0.069(11) 0.095(12) 0.017(10) -0.017(8) -0.004(8) C8 0.109(17) 0.088(14) 0.131(17) -0.022(14) -0.007(13) -0.007(12) C9 0.124(17) 0.075(12) 0.098(14) -0.006(11) -0.035(11) 0.004(11) C10 0.29(4) 0.117(18) 0.078(13) -0.036(13) -0.015(17) -0.03(2) C11 0.17(2) 0.110(15) 0.063(10) -0.011(10) -0.020(11) 0.002(14) C12 0.068(11) 0.094(13) 0.060(9) -0.002(9) -0.018(7) -0.001(9) C13 0.069(11) 0.090(13) 0.066(10) 0.006(9) 0.003(8) -0.007(9) C14 0.055(9) 0.075(11) 0.070(9) 0.004(9) 0.002(7) 0.011(8) C15 0.111(15) 0.068(11) 0.081(11) 0.010(9) -0.012(9) -0.008(10) Cl1 0.058(3) 0.464(14) 0.064(3) 0.044(5) -0.008(2) 0.008(5) Cl2 0.071(3) 0.227(6) 0.068(2) -0.006(3) -0.004(2) 0.031(4) Cl3 0.078(4) 0.153(5) 0.250(8) 0.086(6) 0.028(4) 0.023(4) Cl4 0.063(3) 0.093(4) 0.256(8) 0.029(4) 0.002(4) -0.008(3) N1 0.077(9) 0.083(9) 0.039(6) -0.003(6) -0.006(5) -0.013(7) N2 0.075(9) 0.088(9) 0.028(5) 0.010(6) -0.012(5) -0.008(7) N3 0.073(9) 0.067(8) 0.073(8) 0.008(6) -0.010(6) -0.010(6) N4 0.089(10) 0.062(8) 0.079(9) -0.002(7) -0.009(7) 0.000(7) N5 0.057(7) 0.057(7) 0.052(6) 0.018(6) -0.012(5) -0.010(5) N6 0.059(7) 0.054(7) 0.043(6) 0.004(5) -0.007(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 N2 1.990(10) . ? Au1 N6 2.008(10) . ? Au1 Cl1 2.230(5) . ? Au1 Cl2 2.244(4) . ? Au1 Au2 3.3762(13) . ? Au2 N3 1.956(15) . ? Au2 N1 1.980(13) . ? Au2 Au3 3.3675(11) . ? Au3 N4 1.975(13) . ? Au3 N5 2.010(11) . ? Au3 Cl4 2.233(5) . ? Au3 Cl3 2.244(5) . ? C1 C2 1.53(2) . ? C2 N2 1.33(2) . ? C2 C3 1.42(2) . ? C3 C4 1.35(3) . ? C4 N1 1.39(2) . ? C4 C5 1.48(2) . ? C6 C7 1.48(2) . ? C7 N3 1.38(2) . ? C7 C8 1.40(3) . ? C8 C9 1.40(3) . ? C9 N4 1.35(2) . ? C9 C10 1.49(3) . ? C11 C12 1.51(3) . ? C12 N5 1.349(17) . ? C12 C13 1.35(2) . ? C13 C14 1.39(2) . ? C14 N6 1.332(17) . ? C14 C15 1.51(2) . ? N1 N2 1.364(16) . ? N3 N4 1.430(18) . ? N5 N6 1.344(16) . ? 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 N2 Au1 N6 177.6(5) . . ? N2 Au1 Cl1 89.2(4) . . ? N6 Au1 Cl1 90.1(3) . . ? N2 Au1 Cl2 90.2(4) . . ? N6 Au1 Cl2 90.7(3) . . ? Cl1 Au1 Cl2 174.3(4) . . ? N2 Au1 Au2 60.0(4) . . ? N6 Au1 Au2 117.6(3) . . ? Cl1 Au1 Au2 85.7(3) . . ? Cl2 Au1 Au2 98.89(18) . . ? N3 Au2 N1 179.4(5) . . ? N3 Au2 Au3 59.6(3) . . ? N1 Au2 Au3 120.6(3) . . ? N3 Au2 Au1 121.2(3) . . ? N1 Au2 Au1 59.1(3) . . ? Au3 Au2 Au1 61.57(3) . . ? N4 Au3 N5 178.7(6) . . ? N4 Au3 Cl4 88.9(4) . . ? N5 Au3 Cl4 90.9(3) . . ? N4 Au3 Cl3 90.0(4) . . ? N5 Au3 Cl3 90.3(3) . . ? Cl4 Au3 Cl3 173.5(4) . . ? N4 Au3 Au2 61.3(4) . . ? N5 Au3 Au2 117.5(4) . . ? Cl4 Au3 Au2 88.0(2) . . ? Cl3 Au3 Au2 97.0(2) . . ? N2 C2 C3 106.5(17) . . ? N2 C2 C1 122.7(13) . . ? C3 C2 C1 130.7(19) . . ? C4 C3 C2 107.5(17) . . ? C3 C4 N1 108.6(14) . . ? C3 C4 C5 130.8(16) . . ? N1 C4 C5 120.4(18) . . ? N3 C7 C8 110.8(15) . . ? N3 C7 C6 117.1(18) . . ? C8 C7 C6 132.0(18) . . ? C9 C8 C7 106.9(19) . . ? N4 C9 C8 107.1(18) . . ? N4 C9 C10 122.6(17) . . ? C8 C9 C10 130(2) . . ? N5 C12 C13 106.8(16) . . ? N5 C12 C11 122.3(16) . . ? C13 C12 C11 130.8(15) . . ? C12 C13 C14 107.8(14) . . ? N6 C14 C13 107.1(15) . . ? N6 C14 C15 122.2(14) . . ? C13 C14 C15 130.6(14) . . ? N2 N1 C4 106.5(13) . . ? N2 N1 Au2 122.0(8) . . ? C4 N1 Au2 131.5(12) . . ? C2 N2 N1 110.8(10) . . ? C2 N2 Au1 130.3(10) . . ? N1 N2 Au1 118.9(10) . . ? C7 N3 N4 103.5(14) . . ? C7 N3 Au2 134.3(12) . . ? N4 N3 Au2 122.1(9) . . ? C9 N4 N3 111.6(13) . . ? C9 N4 Au3 131.4(12) . . ? N3 N4 Au3 116.9(11) . . ? N6 N5 C12 109.6(12) . . ? N6 N5 Au3 122.1(8) . . ? C12 N5 Au3 128.3(13) . . ? C14 N6 N5 108.6(11) . . ? C14 N6 Au1 130.2(11) . . ? N5 N6 Au1 121.2(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.31 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.397 _refine_diff_density_min -1.159 _refine_diff_density_rms 0.209 #================================================END data_Au(I)2Au(III)Cl2(dmpz)3 _database_code_CSD 191327 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H20 Au3 Cl2.22 N6' _chemical_formula_weight 954.06 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' '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 Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 23.920(5) _cell_length_b 11.800(2) _cell_length_c 7.7400(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2184.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.901 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1707 _exptl_absorpt_coefficient_mu 20.380 _exptl_absorpt_correction_type 'semi-empirical' _exptl_absorpt_correction_T_min 0.106 _exptl_absorpt_correction_T_max 0.393 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10747 _diffrn_reflns_av_R_equivalents 0.0910 _diffrn_reflns_av_sigmaI/netI 0.0487 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 23.28 _reflns_number_total 2898 _reflns_number_gt 2672 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART-NT V5.0' _computing_cell_refinement 'BRUKER SMART-NT V5.0' _computing_data_reduction 'BRUKER SAINT-NT V5/6.0' _computing_structure_solution 'BRUKER SHELXTL-NT V5.1' _computing_structure_refinement 'BRUKER SHELXTL-NT V5.1' _computing_molecular_graphics 'BRUKER SHELXTL-NT V5.1' _computing_publication_material 'BRUKER SHELXTL-NT V5.1' _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^)+(0.0669P)^2^+8.6277P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 2898 _refine_ls_number_parameters 250 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 0.57446(3) 0.14719(6) 0.84119(11) 0.0577(2) Uani 1 1 d . . . Au2 Au 0.71158(3) 0.21935(7) 0.86514(11) 0.0642(3) Uani 1 1 d . . . Au3 Au 0.61584(3) 0.41834(6) 0.92486(13) 0.0619(3) Uani 1 1 d . . . C1 C 0.7798(10) -0.020(2) 0.754(4) 0.096(9) Uani 1 1 d . . . H1A H 0.7903 -0.0311 0.6360 0.144 Uiso 1 1 calc R . . H1B H 0.7972 -0.0766 0.8251 0.144 Uiso 1 1 calc R . . H1C H 0.7917 0.0540 0.7915 0.144 Uiso 1 1 calc R . . C2 C 0.7184(9) -0.0288(19) 0.771(3) 0.071(6) Uani 1 1 d . . . C3 C 0.6819(11) -0.1222(19) 0.746(3) 0.078(7) Uani 1 1 d . . . H3 H 0.6923 -0.1948 0.7123 0.094 Uiso 1 1 calc R . . C4 C 0.6268(11) -0.0850(19) 0.783(3) 0.078(7) Uani 1 1 d . . . C5 C 0.5736(9) -0.144(2) 0.788(4) 0.094(10) Uani 1 1 d . . . H5A H 0.5593 -0.1433 0.9037 0.142 Uiso 1 1 calc R . . H5B H 0.5786 -0.2205 0.7500 0.142 Uiso 1 1 calc R . . H5C H 0.5476 -0.1061 0.7127 0.142 Uiso 1 1 calc R . . C6 C 0.4314(10) 0.163(2) 0.807(4) 0.091(8) Uani 1 1 d . . . H6A H 0.3956 0.1647 0.8631 0.136 Uiso 1 1 calc R . . H6B H 0.4529 0.1009 0.8523 0.136 Uiso 1 1 calc R . . H6C H 0.4263 0.1531 0.6852 0.136 Uiso 1 1 calc R . . C7 C 0.4615(8) 0.2720(18) 0.841(4) 0.071(6) Uani 1 1 d . . . C8 C 0.4450(8) 0.380(2) 0.842(4) 0.081(6) Uani 1 1 d . . . H8 H 0.4084 0.4042 0.8267 0.097 Uiso 1 1 calc R . . C9 C 0.4912(8) 0.4501(18) 0.871(3) 0.073(6) Uani 1 1 d . . . C10 C 0.4990(10) 0.5763(17) 0.878(4) 0.086(8) Uani 1 1 d . . . H10A H 0.4920 0.6023 0.9940 0.129 Uiso 1 1 calc R . . H10B H 0.4734 0.6123 0.8004 0.129 Uiso 1 1 calc R . . H10C H 0.5366 0.5949 0.8460 0.129 Uiso 1 1 calc R . . C11 C 0.6899(11) 0.6516(17) 1.078(3) 0.078(7) Uani 1 1 d . . . H11A H 0.6518 0.6452 1.0405 0.117 Uiso 1 1 calc R . . H11B H 0.7066 0.7175 1.0275 0.117 Uiso 1 1 calc R . . H11C H 0.6908 0.6583 1.2021 0.117 Uiso 1 1 calc R . . C12 C 0.7217(9) 0.548(2) 1.025(3) 0.068(6) Uani 1 1 d . . . C13 C 0.7784(10) 0.5278(18) 1.022(3) 0.068(6) Uani 1 1 d . . . C14 C 0.7856(9) 0.420(2) 0.965(3) 0.075(7) Uani 1 1 d . . . C15 C 0.8395(10) 0.352(2) 0.935(5) 0.099(8) Uani 1 1 d . . . H15A H 0.8304 0.2771 0.8973 0.149 Uiso 1 1 calc R . . H15B H 0.8605 0.3486 1.0406 0.149 Uiso 1 1 calc R . . H15C H 0.8615 0.3894 0.8479 0.149 Uiso 1 1 calc R . . Cl1 Cl 0.5606(3) 0.1412(5) 0.5519(8) 0.0804(17) Uani 1 1 d . . . Cl2 Cl 0.5842(3) 0.1438(6) 1.1317(8) 0.0811(17) Uani 1 1 d . . . Cl3 Cl 0.8295(10) 0.614(2) 1.078(4) 0.073(7) Uani 0.22 1 d P . . N1 N 0.6323(7) 0.0309(16) 0.818(3) 0.070(5) Uani 1 1 d . . . N2 N 0.6854(7) 0.0621(14) 0.808(2) 0.066(5) Uani 1 1 d . . . N3 N 0.7365(6) 0.3755(12) 0.928(3) 0.061(4) Uani 1 1 d . . . N4 N 0.6961(7) 0.4555(13) 0.965(2) 0.061(4) Uani 1 1 d . . . N5 N 0.5359(6) 0.3791(14) 0.878(2) 0.063(4) Uani 1 1 d . . . N6 N 0.5176(6) 0.2726(13) 0.864(3) 0.066(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 Au1 0.0555(4) 0.0580(4) 0.0597(5) 0.0021(4) -0.0008(4) -0.0029(3) Au2 0.0542(4) 0.0597(4) 0.0786(6) 0.0040(4) -0.0006(4) 0.0015(3) Au3 0.0483(4) 0.0614(4) 0.0762(5) -0.0009(4) -0.0039(4) -0.0007(3) C1 0.077(16) 0.098(19) 0.11(2) -0.002(17) 0.017(15) 0.023(15) C2 0.065(13) 0.060(13) 0.087(16) 0.016(12) 0.001(11) 0.016(11) C3 0.101(18) 0.049(12) 0.084(17) 0.001(11) 0.003(14) 0.004(13) C4 0.102(19) 0.062(14) 0.068(15) 0.001(11) -0.001(13) -0.009(12) C5 0.070(15) 0.066(14) 0.15(3) 0.010(15) 0.024(15) -0.022(12) C6 0.080(15) 0.095(18) 0.10(2) 0.018(15) 0.001(13) -0.046(14) C7 0.051(10) 0.071(13) 0.091(16) 0.005(14) -0.004(12) -0.006(9) C8 0.042(10) 0.091(15) 0.111(18) 0.008(17) 0.004(13) -0.002(11) C9 0.055(11) 0.072(12) 0.091(18) 0.003(13) -0.016(12) 0.013(10) C10 0.070(13) 0.068(13) 0.12(2) -0.016(15) -0.019(15) 0.027(10) C11 0.081(16) 0.055(14) 0.097(18) -0.009(12) 0.007(13) 0.011(11) C12 0.057(13) 0.082(15) 0.064(14) 0.005(12) 0.011(10) -0.011(11) C13 0.081(16) 0.048(12) 0.076(15) 0.007(10) 0.010(12) -0.017(10) C14 0.061(13) 0.095(18) 0.070(15) 0.024(14) -0.003(11) -0.006(11) C15 0.077(16) 0.097(18) 0.12(2) -0.005(19) 0.009(16) 0.010(13) Cl1 0.095(4) 0.083(4) 0.064(3) 0.005(3) -0.006(3) -0.001(3) Cl2 0.085(4) 0.099(4) 0.060(3) 0.003(3) -0.004(3) 0.006(3) Cl3 0.056(13) 0.076(16) 0.088(18) -0.018(14) 0.006(12) -0.021(12) N1 0.056(9) 0.084(12) 0.070(12) -0.003(10) -0.004(9) 0.001(9) N2 0.067(11) 0.058(9) 0.074(12) 0.000(9) 0.006(9) 0.002(8) N3 0.051(9) 0.054(8) 0.079(11) 0.001(10) -0.018(8) -0.006(7) N4 0.050(8) 0.053(9) 0.081(13) 0.004(9) -0.005(8) -0.006(8) N5 0.044(8) 0.063(9) 0.082(13) -0.004(9) -0.003(8) 0.004(7) N6 0.050(8) 0.058(9) 0.090(12) -0.004(9) -0.004(9) -0.006(7) _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 N1 1.956(18) . ? Au1 N6 2.017(15) . ? Au1 Cl2 2.261(6) . ? Au1 Cl1 2.265(6) . ? Au2 N3 1.997(15) . ? Au2 N2 2.008(17) . ? Au2 Au3 3.3123(11) . ? Au3 N4 1.993(16) . ? Au3 N5 1.999(14) . ? C1 C2 1.48(3) . ? C2 N2 1.36(3) . ? C2 C3 1.42(3) . ? C3 C4 1.42(4) . ? C4 N1 1.40(3) . ? C4 C5 1.45(3) . ? C6 C7 1.50(3) . ? C7 C8 1.33(3) . ? C7 N6 1.35(2) . ? C8 C9 1.40(3) . ? C9 N5 1.36(2) . ? C9 C10 1.50(3) . ? C11 C12 1.50(3) . ? C12 N4 1.34(3) . ? C12 C13 1.38(3) . ? C13 C14 1.36(3) . ? C13 Cl3 1.65(3) . ? C14 N3 1.32(3) . ? C14 C15 1.53(3) . ? N1 N2 1.33(2) . ? N3 N4 1.38(2) . ? N5 N6 1.34(2) . ? 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 N1 Au1 N6 177.4(7) . . ? N1 Au1 Cl2 90.3(6) . . ? N6 Au1 Cl2 89.8(6) . . ? N1 Au1 Cl1 89.5(6) . . ? N6 Au1 Cl1 90.6(6) . . ? Cl2 Au1 Cl1 176.2(2) . . ? N3 Au2 N2 178.5(8) . . ? N3 Au2 Au3 61.2(4) . . ? N2 Au2 Au3 118.1(5) . . ? N4 Au3 N5 178.4(7) . . ? N4 Au3 Au2 60.8(5) . . ? N5 Au3 Au2 118.1(4) . . ? N2 C2 C3 106.5(19) . . ? N2 C2 C1 123(2) . . ? C3 C2 C1 131(2) . . ? C2 C3 C4 108(2) . . ? N1 C4 C3 105(2) . . ? N1 C4 C5 123(2) . . ? C3 C4 C5 132(2) . . ? C8 C7 N6 106.7(17) . . ? C8 C7 C6 133(2) . . ? N6 C7 C6 120(2) . . ? C7 C8 C9 109.6(18) . . ? N5 C9 C8 105.1(18) . . ? N5 C9 C10 120.7(18) . . ? C8 C9 C10 133.9(19) . . ? N4 C12 C13 108(2) . . ? N4 C12 C11 122(2) . . ? C13 C12 C11 130(2) . . ? C14 C13 C12 107(2) . . ? C14 C13 Cl3 125(2) . . ? C12 C13 Cl3 128(2) . . ? N3 C14 C13 109(2) . . ? N3 C14 C15 121(2) . . ? C13 C14 C15 130(2) . . ? N2 N1 C4 110.5(19) . . ? N2 N1 Au1 119.2(14) . . ? C4 N1 Au1 129.5(16) . . ? N1 N2 C2 110.4(17) . . ? N1 N2 Au2 122.9(14) . . ? C2 N2 Au2 126.4(15) . . ? C14 N3 N4 108.0(17) . . ? C14 N3 Au2 133.2(15) . . ? N4 N3 Au2 118.2(11) . . ? C12 N4 N3 108.1(16) . . ? C12 N4 Au3 132.5(15) . . ? N3 N4 Au3 119.4(11) . . ? N6 N5 C9 108.6(15) . . ? N6 N5 Au3 123.1(11) . . ? C9 N5 Au3 128.1(14) . . ? N5 N6 C7 109.9(15) . . ? N5 N6 Au1 118.5(11) . . ? C7 N6 Au1 130.7(14) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.713 _refine_diff_density_min -0.968 _refine_diff_density_rms 0.176 #===============================================END