Electronic Supplementary Material for CrystEngComm This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Martin Smith' _publ_contact_author_address ; Department of Chemistry Loughborough University Loughborough Leicestershire LE11 3TU UNITED KINGDOM ; _publ_contact_author_email M.B.SMITH@LBORO.AC.UK _publ_section_title ; Isomeric dinuclear gold(I) complexes with highly functionalised ditertiary phosphines: Self-assembly of dimers, rings and 1D polymeric chains ; loop_ _publ_author_name 'Martin Smith' 'Simon Coles' 'Sophie Dale' 'Thomas Gelbrich' 'M. Hursthouse' 'Mark E. Light' #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 223228' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H34 Au2 Cl2 N O0.50 P2' _chemical_formula_sum 'C34 H34 Au2 Cl2 N O0.50 P2' _chemical_formula_weight 991.40 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.7931(3) _cell_length_b 17.0401(5) _cell_length_c 19.8613(7) _cell_angle_alpha 90.00 _cell_angle_beta 102.479(1) _cell_angle_gamma 90.00 _cell_volume 3236.06(18) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 12312 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.035 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1884 _exptl_absorpt_coefficient_mu 9.348 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.257 _exptl_absorpt_correction_T_max 0.652 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius Kappa CCD Area detector' _diffrn_measurement_method '\f and \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9835 _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_sigmaI/netI 0.1003 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5681 _reflns_number_gt 3968 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; DENZO (Otwinowski and Minor, 1997), COLLECT (Hooft, 1998) ; _computing_cell_refinement ; DENZO (Otwinowski and MInor, 1997), COLLECT (Hooft, 1998) ; _computing_data_reduction ; DENZO (Otwinowski and MInor, 1997), COLLECT (Hooft, 1998), MAXUS (Mackay et al., 1998) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^)+(0.0373P)^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 5681 _refine_ls_number_parameters 385 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0789 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1006 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2936(9) 0.3210(6) 0.2653(4) 0.017(2) Uani 1 1 d . . . C2 C 0.1693(10) 0.3602(7) 0.2696(5) 0.031(3) Uani 1 1 d . . . H2 H 0.1251 0.3499 0.3068 0.037 Uiso 1 1 calc R . . C3 C 0.1114(10) 0.4147(7) 0.2186(5) 0.034(3) Uani 1 1 d . . . H3 H 0.0290 0.4427 0.2215 0.040 Uiso 1 1 calc R . . C4 C 0.1748(10) 0.4274(7) 0.1642(5) 0.033(3) Uani 1 1 d . . . H4 H 0.1374 0.4648 0.1297 0.040 Uiso 1 1 calc R . . C5 C 0.2927(10) 0.3855(6) 0.1600(5) 0.026(3) Uani 1 1 d . . . H5 H 0.3334 0.3932 0.1212 0.031 Uiso 1 1 calc R . . C6 C 0.3536(10) 0.3330(6) 0.2097(5) 0.022(2) Uani 1 1 d . . . H6 H 0.4359 0.3055 0.2058 0.027 Uiso 1 1 calc R . . C7 C 0.5201(9) 0.2116(6) 0.3171(5) 0.019(2) Uani 1 1 d . . . C8 C 0.5032(10) 0.1459(6) 0.2748(5) 0.028(3) Uani 1 1 d . . . H8 H 0.4125 0.1249 0.2576 0.033 Uiso 1 1 calc R . . C9 C 0.6189(10) 0.1111(7) 0.2578(5) 0.033(3) Uani 1 1 d . . . H9 H 0.6067 0.0656 0.2295 0.039 Uiso 1 1 calc R . . C10 C 0.7498(11) 0.1407(7) 0.2808(5) 0.029(3) Uani 1 1 d . . . H10 H 0.8280 0.1170 0.2677 0.035 Uiso 1 1 calc R . . C11 C 0.7673(10) 0.2050(7) 0.3230(5) 0.029(3) Uani 1 1 d . . . H11 H 0.8590 0.2244 0.3407 0.034 Uiso 1 1 calc R . . C12 C 0.6535(10) 0.2429(6) 0.3407(5) 0.025(2) Uani 1 1 d . . . H12 H 0.6667 0.2890 0.3682 0.030 Uiso 1 1 calc R . . C13 C 0.4290(9) 0.3266(6) 0.4067(4) 0.017(2) Uani 1 1 d . . . H13A H 0.4905 0.3654 0.3908 0.021 Uiso 1 1 calc R . . H13B H 0.3476 0.3553 0.4164 0.021 Uiso 1 1 calc R . . C14 C 0.6277(9) 0.3324(6) 0.5065(5) 0.018(2) Uani 1 1 d . . . C15 C 0.7403(10) 0.2881(7) 0.5426(5) 0.028(3) Uani 1 1 d . . . H15 H 0.7368 0.2324 0.5415 0.034 Uiso 1 1 calc R . . C16 C 0.8547(10) 0.3258(7) 0.5792(5) 0.028(3) Uani 1 1 d . . . H16 H 0.9295 0.2955 0.6049 0.033 Uiso 1 1 calc R . . C17 C 0.8665(10) 0.4086(8) 0.5803(5) 0.034(3) Uani 1 1 d . . . H17 H 0.9479 0.4338 0.6059 0.040 Uiso 1 1 calc R . . C18 C 0.7565(10) 0.4515(7) 0.5433(5) 0.026(3) Uani 1 1 d . . . H18 H 0.7617 0.5072 0.5427 0.032 Uiso 1 1 calc R . . C19 C 0.6369(10) 0.4132(6) 0.5065(5) 0.022(2) Uani 1 1 d . . . H19 H 0.5612 0.4432 0.4812 0.027 Uiso 1 1 calc R . . C20 C 0.4277(9) 0.2465(6) 0.5099(5) 0.020(2) Uani 1 1 d . . . H20A H 0.4962 0.2227 0.5484 0.024 Uiso 1 1 calc R . . H20B H 0.3819 0.2029 0.4806 0.024 Uiso 1 1 calc R . . C21 C 0.3799(9) 0.3682(6) 0.6080(5) 0.018(2) Uani 1 1 d . . . C22 C 0.5126(9) 0.3529(6) 0.6486(4) 0.019(2) Uani 1 1 d . . . H22 H 0.5559 0.3036 0.6452 0.023 Uiso 1 1 calc R . . C23 C 0.5812(10) 0.4092(7) 0.6937(5) 0.025(3) Uani 1 1 d . . . H23 H 0.6727 0.3994 0.7201 0.030 Uiso 1 1 calc R . . C24 C 0.5153(9) 0.4799(6) 0.7000(5) 0.024(3) Uani 1 1 d . . . H24 H 0.5611 0.5186 0.7313 0.029 Uiso 1 1 calc R . . C25 C 0.3847(9) 0.4941(6) 0.6612(5) 0.022(2) Uani 1 1 d . . . H25 H 0.3395 0.5424 0.6660 0.026 Uiso 1 1 calc R . . C26 C 0.3171(10) 0.4377(6) 0.6146(5) 0.022(2) Uani 1 1 d . . . H26 H 0.2266 0.4482 0.5874 0.027 Uiso 1 1 calc R . . C27 C 0.2366(9) 0.2171(6) 0.5947(4) 0.013(2) Uani 1 1 d . . . C28 C 0.2910(10) 0.2036(6) 0.6645(5) 0.024(2) Uani 1 1 d . . . H28 H 0.3561 0.2396 0.6903 0.028 Uiso 1 1 calc R . . C29 C 0.2506(10) 0.1377(7) 0.6970(5) 0.031(3) Uani 1 1 d . . . H29 H 0.2889 0.1287 0.7445 0.037 Uiso 1 1 calc R . . C30 C 0.1553(11) 0.0857(6) 0.6603(6) 0.030(3) Uani 1 1 d . . . H30 H 0.1278 0.0412 0.6830 0.036 Uiso 1 1 calc R . . C31 C 0.0995(10) 0.0972(6) 0.5914(5) 0.023(2) Uani 1 1 d . . . H31 H 0.0342 0.0607 0.5666 0.027 Uiso 1 1 calc R . . C32 C 0.1389(10) 0.1621(6) 0.5584(5) 0.024(2) Uani 1 1 d . . . H32 H 0.1001 0.1700 0.5108 0.029 Uiso 1 1 calc R . . N1 N 0.5045(7) 0.2916(5) 0.4696(4) 0.019(2) Uani 1 1 d . . . P1 P 0.3667(2) 0.25643(17) 0.33675(13) 0.0186(6) Uani 1 1 d . . . P2 P 0.2912(2) 0.29604(16) 0.54728(13) 0.0179(6) Uani 1 1 d . . . Cl1 Cl 0.0641(2) 0.07944(16) 0.38820(13) 0.0253(6) Uani 1 1 d . . . Cl2 Cl -0.0661(2) 0.39605(16) 0.38757(12) 0.0261(6) Uani 1 1 d . . . Au1 Au 0.21489(4) 0.16958(2) 0.361589(19) 0.01940(13) Uani 1 1 d . . . Au2 Au 0.11379(4) 0.34441(2) 0.468546(19) 0.01944(13) Uani 1 1 d . . . O1 O 0.0000 0.5000 0.0000 0.033(3) Uani 1 2 d SD . . C33 C -0.1871(12) 0.5529(10) 0.0477(6) 0.080(6) Uani 1 1 d D . . H33A H -0.2208 0.6022 0.0637 0.096 Uiso 0.50 1 d PR A 1 H33B H -0.1692 0.5149 0.0856 0.096 Uiso 0.50 1 d PR A 1 H33C H -0.2579 0.5319 0.0094 0.096 Uiso 0.50 1 d PR A 1 H33D H -0.2700 0.5320 0.0616 0.096 Uiso 0.50 1 d PR A 2 H33E H -0.2158 0.5920 0.0112 0.096 Uiso 0.50 1 d PR A 2 H33F H -0.1253 0.5776 0.0875 0.096 Uiso 0.50 1 d PR A 2 C34 C -0.0545(15) 0.5681(5) 0.0237(11) 0.043(7) Uani 0.50 1 d PD . . H34A H -0.0729 0.6073 -0.0140 0.051 Uiso 0.50 1 calc PR . . H34B H 0.0160 0.5905 0.0622 0.051 Uiso 0.50 1 calc PR . . C35 C 0.111(2) 0.5127(11) -0.0213(12) 0.042(7) Uani 0.50 1 d PD . . H35A H 0.1782 0.5379 0.0170 0.051 Uiso 0.50 1 calc PR . . H35B H 0.0879 0.5520 -0.0587 0.051 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.026(5) 0.014(6) 0.008(5) -0.004(4) 0.000(4) -0.003(4) C2 0.022(6) 0.049(9) 0.021(6) 0.005(6) 0.007(4) 0.013(5) C3 0.024(6) 0.056(9) 0.022(6) 0.024(6) 0.008(5) 0.022(6) C4 0.025(6) 0.046(8) 0.027(6) 0.015(6) 0.005(5) -0.001(5) C5 0.033(6) 0.030(7) 0.016(6) -0.001(5) 0.008(5) -0.003(5) C6 0.024(5) 0.031(7) 0.016(5) -0.006(5) 0.012(4) -0.009(5) C7 0.007(5) 0.036(7) 0.014(5) 0.006(5) 0.001(4) -0.004(4) C8 0.013(5) 0.031(7) 0.037(7) -0.003(6) 0.001(5) 0.000(5) C9 0.027(6) 0.033(8) 0.030(7) -0.010(6) -0.010(5) 0.001(5) C10 0.036(7) 0.039(8) 0.017(6) 0.000(6) 0.016(5) -0.004(5) C11 0.024(6) 0.050(8) 0.013(5) 0.011(6) 0.005(4) 0.006(5) C12 0.029(6) 0.014(6) 0.031(6) 0.002(5) 0.009(5) 0.000(5) C13 0.014(5) 0.023(6) 0.013(5) -0.004(5) 0.000(4) 0.003(4) C14 0.018(5) 0.020(7) 0.018(5) -0.011(5) 0.007(4) -0.003(4) C15 0.026(6) 0.026(7) 0.033(6) 0.003(5) 0.008(5) -0.005(5) C16 0.016(5) 0.048(9) 0.015(6) 0.007(5) -0.003(4) -0.001(5) C17 0.023(6) 0.056(10) 0.020(6) 0.003(6) -0.001(5) -0.013(6) C18 0.035(6) 0.025(7) 0.018(6) -0.002(5) 0.003(5) -0.012(5) C19 0.021(5) 0.028(7) 0.016(6) -0.006(5) 0.002(4) 0.000(5) C20 0.029(6) 0.015(6) 0.016(5) -0.007(5) 0.001(4) -0.004(5) C21 0.027(5) 0.018(6) 0.013(5) -0.004(5) 0.011(4) 0.003(5) C22 0.026(5) 0.025(7) 0.005(5) 0.004(4) 0.001(4) 0.004(5) C23 0.031(6) 0.037(8) 0.009(5) 0.002(5) 0.009(4) -0.005(5) C24 0.019(5) 0.031(7) 0.020(6) 0.000(5) -0.003(4) 0.001(5) C25 0.034(6) 0.015(6) 0.021(5) -0.003(5) 0.015(5) -0.008(5) C26 0.019(5) 0.030(7) 0.019(6) 0.004(5) 0.006(4) -0.005(5) C27 0.015(5) 0.014(6) 0.012(5) -0.005(4) 0.005(4) -0.003(4) C28 0.024(6) 0.027(7) 0.016(5) 0.000(5) -0.003(4) 0.000(5) C29 0.027(6) 0.042(8) 0.023(6) 0.003(6) 0.003(5) -0.005(5) C30 0.044(7) 0.015(7) 0.033(7) 0.006(5) 0.014(5) 0.001(5) C31 0.031(6) 0.009(6) 0.030(6) -0.002(5) 0.010(5) -0.007(5) C32 0.025(6) 0.021(7) 0.030(6) 0.004(5) 0.015(5) 0.006(5) N1 0.020(4) 0.024(5) 0.012(4) 0.002(4) -0.001(3) -0.005(4) P1 0.0163(13) 0.0223(17) 0.0174(14) 0.0006(12) 0.0041(10) 0.0012(11) P2 0.0193(13) 0.0205(17) 0.0133(13) -0.0020(12) 0.0021(10) -0.0027(11) Cl1 0.0251(13) 0.0261(17) 0.0239(14) 0.0018(12) 0.0036(10) -0.0063(11) Cl2 0.0209(13) 0.0322(18) 0.0222(14) 0.0022(12) -0.0018(10) 0.0023(12) Au1 0.0183(2) 0.0222(3) 0.0173(2) 0.00014(18) 0.00281(15) -0.00377(17) Au2 0.0173(2) 0.0239(3) 0.0157(2) 0.00106(18) 0.00051(15) -0.00296(17) O1 0.022(6) 0.039(8) 0.036(7) 0.004(6) 0.006(5) -0.009(5) C33 0.059(9) 0.159(19) 0.022(7) -0.001(10) 0.006(6) -0.015(11) C34 0.041(14) 0.038(17) 0.040(15) -0.006(13) -0.011(11) -0.008(13) C35 0.049(16) 0.027(16) 0.042(16) -0.013(13) -0.008(13) -0.017(13) _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 C2 1.408(13) . ? C1 C6 1.373(13) . ? C1 P1 1.815(9) . ? C2 C3 1.401(14) . ? C3 C4 1.374(14) . ? C4 C5 1.375(14) . ? C5 C6 1.369(14) . ? C7 C8 1.387(14) . ? C7 C12 1.395(13) . ? C7 P1 1.801(9) . ? C8 C9 1.384(14) . ? C9 C10 1.362(13) . ? C10 C11 1.367(15) . ? C11 C12 1.396(13) . ? C13 N1 1.437(11) . ? C13 P1 1.834(9) . ? C14 C15 1.399(13) . ? C14 C19 1.380(14) . ? C14 N1 1.447(11) . ? C15 C16 1.358(13) . ? C16 C17 1.416(16) . ? C17 C18 1.376(14) . ? C18 C19 1.401(13) . ? C20 N1 1.433(12) . ? C20 P2 1.866(9) . ? C21 C22 1.398(12) . ? C21 C26 1.353(14) . ? C21 P2 1.808(10) . ? C22 C23 1.383(13) . ? C23 C24 1.386(14) . ? C24 C25 1.363(12) . ? C25 C26 1.398(13) . ? C27 C28 1.394(12) . ? C27 C32 1.419(13) . ? C27 P2 1.788(10) . ? C28 C29 1.393(14) . ? C29 C30 1.375(14) . ? C30 C31 1.373(14) . ? C31 C32 1.382(13) . ? P1 Au1 2.228(3) . ? P2 Au2 2.229(2) . ? Cl1 Au1 2.271(2) . ? Cl2 Au2 2.289(2) . ? O1 C34 1.3997(10) . ? O1 C34 1.3997(10) 3_565 ? O1 C35 1.27(2) . ? O1 C35 1.27(2) 3_565 ? C33 C34 1.4997(10) . ? C35 C33 1.4997(10) 3_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 120.2(9) . . ? C2 C1 P1 116.1(7) . . ? C6 C1 P1 123.6(8) . . ? C1 C2 C3 119.4(9) . . ? C2 C3 C4 119.5(10) . . ? C3 C4 C5 119.6(10) . . ? C4 C5 C6 122.4(10) . . ? C1 C6 C5 118.8(10) . . ? C8 C7 C12 119.4(9) . . ? C8 C7 P1 118.5(7) . . ? C12 C7 P1 122.0(8) . . ? C7 C8 C9 119.8(9) . . ? C8 C9 C10 121.4(11) . . ? C9 C10 C11 119.1(10) . . ? C10 C11 C12 121.5(10) . . ? C7 C12 C11 118.7(10) . . ? N1 C13 P1 114.4(7) . . ? C15 C14 C19 119.6(9) . . ? C15 C14 N1 118.6(9) . . ? C19 C14 N1 121.8(9) . . ? C14 C15 C16 119.1(11) . . ? C15 C16 C17 122.4(10) . . ? C16 C17 C18 118.0(10) . . ? C17 C18 C19 120.0(10) . . ? C14 C19 C18 120.8(9) . . ? N1 C20 P2 119.2(7) . . ? C22 C21 C26 119.5(9) . . ? C22 C21 P2 120.7(8) . . ? C26 C21 P2 119.8(7) . . ? C21 C22 C23 120.4(10) . . ? C22 C23 C24 119.3(9) . . ? C23 C24 C25 120.1(10) . . ? C24 C25 C26 120.3(10) . . ? C21 C26 C25 120.4(9) . . ? C28 C27 C32 117.8(9) . . ? C28 C27 P2 123.7(7) . . ? C32 C27 P2 118.4(7) . . ? C27 C28 C29 120.5(9) . . ? C28 C29 C30 120.1(10) . . ? C29 C30 C31 121.0(10) . . ? C30 C31 C32 119.6(10) . . ? C27 C32 C31 121.0(9) . . ? C13 N1 C14 117.2(8) . . ? C13 N1 C20 118.3(7) . . ? C14 N1 C20 117.1(7) . . ? C1 P1 C7 107.1(4) . . ? C1 P1 C13 102.0(4) . . ? C1 P1 Au1 114.0(3) . . ? C7 P1 C13 106.5(4) . . ? C7 P1 Au1 113.2(4) . . ? C13 P1 Au1 113.2(3) . . ? C20 P2 C21 106.9(4) . . ? C20 P2 C27 101.0(4) . . ? C20 P2 Au2 113.9(3) . . ? C21 P2 C27 108.4(4) . . ? C21 P2 Au2 113.9(3) . . ? C27 P2 Au2 111.8(3) . . ? P1 Au1 Cl1 178.74(9) . . ? P2 Au2 Cl2 178.99(10) . . ? C34 O1 C34 180.0(16) . 3_565 ? C34 O1 C35 112.8(10) . . ? C34 O1 C35 112.8(10) 3_565 3_565 ? C34 O1 C35 67.2(10) 3_565 . ? C34 O1 C35 67.2(10) . 3_565 ? C35 O1 C35 180(3) . 3_565 ? O1 C34 C33 112.5(9) . . ? O1 C35 C33 121.1(16) . 3_565 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.894 _refine_diff_density_min -1.509 _refine_diff_density_rms 0.243 #== END data_6c _database_code_depnum_ccdc_archive 'CCDC 223264' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H29 Au2 Cl2 N O3 P2' _chemical_formula_weight 1014.35 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' 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' _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 10.5172(2) _cell_length_b 12.3110(3) _cell_length_c 13.3218(4) _cell_angle_alpha 72.659(1) _cell_angle_beta 84.320(2) _cell_angle_gamma 75.960(1) _cell_volume 1596.62(7) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 11238 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 26.00 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.110 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 9.481 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3305 _exptl_absorpt_correction_T_max 0.5176 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius Kappa CCD Area detector' _diffrn_measurement_method '\f and \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11238 _diffrn_reflns_av_R_equivalents 0.0810 _diffrn_reflns_av_sigmaI/netI 0.0716 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6130 _reflns_number_gt 5283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHEXTL and local programs' _computing_publication_material 'Bruker SHEXTL and local programs' _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^)+(0.0785P)^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 SHELXL _refine_ls_extinction_coef 0.0007(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6130 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1194 _refine_ls_wR_factor_gt 0.1145 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 0.19270(2) 0.36278(2) 0.380709(18) 0.01826(12) Uani 1 1 d . . . Au2 Au 0.34103(2) 0.36713(2) 0.151968(18) 0.01867(12) Uani 1 1 d . . . P1 P 0.00312(15) 0.45855(15) 0.30241(12) 0.0172(4) Uani 1 1 d . . . P2 P 0.26139(15) 0.23072(15) 0.11593(12) 0.0171(4) Uani 1 1 d . . . Cl1 Cl 0.37442(15) 0.25804(16) 0.47700(13) 0.0266(4) Uani 1 1 d . . . Cl2 Cl 0.43116(17) 0.50870(16) 0.18006(13) 0.0297(4) Uani 1 1 d . . . C7 C -0.1538(7) 0.0898(6) 0.3779(5) 0.0232(15) Uani 1 1 d . . . H7 H -0.1367 0.0357 0.4454 0.028 Uiso 1 1 calc R . . O1 O -0.1875(4) 0.4122(4) 0.0282(3) 0.0227(10) Uani 1 1 d . . . O2 O -0.3275(5) 0.3028(5) 0.0262(4) 0.0337(13) Uani 1 1 d . . . H2 H -0.3437 0.3507 -0.0334 0.050 Uiso 1 1 calc R . . O3 O 0.0387(4) 0.1506(4) 0.3853(3) 0.0233(10) Uani 1 1 d . . . H3 H 0.0843 0.1965 0.3491 0.035 Uiso 1 1 calc R . . N1 N 0.0117(5) 0.3034(5) 0.1858(4) 0.0151(11) Uani 1 1 d . . . C1 C -0.0147(6) 0.4280(6) 0.1787(5) 0.0165(13) Uani 1 1 d . . . H1A H -0.1052 0.4649 0.1544 0.020 Uiso 1 1 calc R . . H1B H 0.0459 0.4647 0.1249 0.020 Uiso 1 1 calc R . . C2 C 0.0845(6) 0.2745(6) 0.0935(5) 0.0177(14) Uani 1 1 d . . . H2A H 0.0661 0.3432 0.0310 0.021 Uiso 1 1 calc R . . H2B H 0.0550 0.2100 0.0796 0.021 Uiso 1 1 calc R . . C4 C -0.2037(6) 0.2465(6) 0.1779(5) 0.0200(14) Uani 1 1 d . . . C3 C -0.0891(6) 0.2399(6) 0.2293(5) 0.0188(13) Uani 1 1 d . . . C5 C -0.2913(6) 0.1791(7) 0.2263(5) 0.0249(15) Uani 1 1 d . . . H5 H -0.3697 0.1868 0.1924 0.030 Uiso 1 1 calc R . . C6 C -0.2653(7) 0.0992(6) 0.3255(6) 0.0267(16) Uani 1 1 d . . . H6 H -0.3247 0.0509 0.3574 0.032 Uiso 1 1 calc R . . C8 C -0.0679(6) 0.1601(6) 0.3306(5) 0.0176(13) Uani 1 1 d . . . C9 C -0.2360(6) 0.3301(6) 0.0707(5) 0.0196(14) Uani 1 1 d . . . C10 C -0.0213(6) 0.6174(6) 0.2624(5) 0.0224(15) Uani 1 1 d . . . C11 C 0.0659(7) 0.6686(7) 0.1869(5) 0.0232(15) Uani 1 1 d . . . H11 H 0.1339 0.6210 0.1563 0.028 Uiso 1 1 calc R . . C12 C 0.0530(7) 0.7880(7) 0.1570(6) 0.0326(17) Uani 1 1 d . . . H12 H 0.1108 0.8227 0.1048 0.039 Uiso 1 1 calc R . . C13 C -0.0442(7) 0.8569(7) 0.2032(6) 0.0329(18) Uani 1 1 d . . . H13 H -0.0532 0.9391 0.1827 0.040 Uiso 1 1 calc R . . C14 C -0.1291(7) 0.8057(7) 0.2798(6) 0.0293(16) Uani 1 1 d . . . H14 H -0.1946 0.8531 0.3126 0.035 Uiso 1 1 calc R . . C15 C -0.1185(6) 0.6875(6) 0.3081(5) 0.0207(14) Uani 1 1 d . . . H15 H -0.1779 0.6534 0.3591 0.025 Uiso 1 1 calc R . . C20 C -0.1387(6) 0.4303(6) 0.3851(5) 0.0184(14) Uani 1 1 d . . . C21 C -0.1259(7) 0.4013(6) 0.4948(5) 0.0219(15) Uani 1 1 d . . . H21 H -0.0433 0.3918 0.5233 0.026 Uiso 1 1 calc R . . C22 C -0.2357(6) 0.3864(6) 0.5616(5) 0.0212(14) Uani 1 1 d . . . H22 H -0.2286 0.3700 0.6354 0.025 Uiso 1 1 calc R . . C23 C -0.3540(7) 0.3957(6) 0.5201(6) 0.0274(16) Uani 1 1 d . . . H23 H -0.4280 0.3849 0.5658 0.033 Uiso 1 1 calc R . . C24 C -0.3664(6) 0.4205(6) 0.4120(5) 0.0244(15) Uani 1 1 d . . . H24 H -0.4481 0.4255 0.3843 0.029 Uiso 1 1 calc R . . C25 C -0.2596(6) 0.4379(6) 0.3453(5) 0.0192(14) Uani 1 1 d . . . H25 H -0.2683 0.4552 0.2715 0.023 Uiso 1 1 calc R . . C30 C 0.2819(6) 0.0971(6) 0.2225(5) 0.0187(14) Uani 1 1 d . . . C31 C 0.3667(6) 0.0825(6) 0.3036(5) 0.0200(14) Uani 1 1 d . . . H31 H 0.4134 0.1409 0.2994 0.024 Uiso 1 1 calc R . . C32 C 0.3822(7) -0.0152(6) 0.3883(5) 0.0237(15) Uani 1 1 d . . . H32 H 0.4402 -0.0245 0.4421 0.028 Uiso 1 1 calc R . . C33 C 0.3136(7) -0.1003(7) 0.3959(5) 0.0262(16) Uani 1 1 d . . . H33 H 0.3253 -0.1681 0.4545 0.031 Uiso 1 1 calc R . . C34 C 0.2272(6) -0.0868(6) 0.3174(5) 0.0220(14) Uani 1 1 d . . . H34 H 0.1789 -0.1444 0.3233 0.026 Uiso 1 1 calc R . . C35 C 0.2125(6) 0.0114(6) 0.2310(5) 0.0213(14) Uani 1 1 d . . . H35 H 0.1547 0.0203 0.1771 0.026 Uiso 1 1 calc R . . C40 C 0.3310(6) 0.1957(6) -0.0036(5) 0.0194(14) Uani 1 1 d . . . C41 C 0.3773(7) 0.2800(7) -0.0815(6) 0.0292(17) Uani 1 1 d . . . H41 H 0.3742 0.3535 -0.0707 0.035 Uiso 1 1 calc R . . C42 C 0.4294(8) 0.2582(8) -0.1771(6) 0.039(2) Uani 1 1 d . . . H42 H 0.4614 0.3165 -0.2307 0.046 Uiso 1 1 calc R . . C43 C 0.4333(7) 0.1502(7) -0.1919(6) 0.0296(17) Uani 1 1 d . . . H43 H 0.4675 0.1349 -0.2563 0.036 Uiso 1 1 calc R . . C44 C 0.3883(7) 0.0658(7) -0.1144(6) 0.0334(18) Uani 1 1 d . . . H44 H 0.3925 -0.0082 -0.1245 0.040 Uiso 1 1 calc R . . C45 C 0.3360(7) 0.0887(6) -0.0200(5) 0.0248(15) Uani 1 1 d . . . H45 H 0.3036 0.0304 0.0333 0.030 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01256(16) 0.02520(19) 0.01746(17) -0.00578(12) -0.00328(10) -0.00424(11) Au2 0.01496(17) 0.02375(19) 0.01827(17) -0.00324(12) -0.00259(10) -0.00873(12) P1 0.0131(8) 0.0229(10) 0.0160(8) -0.0057(7) -0.0036(6) -0.0032(7) P2 0.0124(8) 0.0232(9) 0.0158(8) -0.0044(7) -0.0014(6) -0.0054(7) Cl1 0.0175(8) 0.0319(10) 0.0292(9) -0.0059(7) -0.0100(6) -0.0029(7) Cl2 0.0333(9) 0.0337(10) 0.0255(8) -0.0013(7) -0.0100(7) -0.0194(8) C7 0.027(4) 0.026(4) 0.012(3) -0.002(3) 0.004(3) -0.005(3) O1 0.019(2) 0.031(3) 0.019(2) -0.002(2) -0.0027(18) -0.013(2) O2 0.033(3) 0.046(3) 0.028(3) -0.003(2) -0.013(2) -0.024(3) O3 0.021(2) 0.030(3) 0.014(2) 0.002(2) -0.0010(18) -0.007(2) N1 0.015(3) 0.018(3) 0.013(2) -0.002(2) 0.001(2) -0.008(2) C1 0.020(3) 0.016(3) 0.015(3) -0.006(3) 0.001(2) -0.006(3) C2 0.015(3) 0.025(4) 0.013(3) -0.004(3) -0.001(2) -0.007(3) C4 0.011(3) 0.029(4) 0.023(3) -0.015(3) 0.003(2) -0.003(3) C3 0.016(3) 0.023(4) 0.021(3) -0.011(3) 0.000(2) -0.004(3) C5 0.014(3) 0.035(4) 0.025(4) -0.007(3) 0.006(3) -0.009(3) C6 0.022(4) 0.029(4) 0.033(4) -0.009(3) 0.006(3) -0.014(3) C8 0.014(3) 0.023(4) 0.015(3) -0.009(3) 0.000(2) -0.001(3) C9 0.017(3) 0.031(4) 0.018(3) -0.017(3) 0.000(2) -0.006(3) C10 0.019(3) 0.028(4) 0.021(3) -0.005(3) -0.009(3) -0.007(3) C11 0.020(3) 0.032(4) 0.019(3) -0.008(3) 0.004(3) -0.010(3) C12 0.032(4) 0.035(5) 0.034(4) -0.005(3) -0.007(3) -0.017(3) C13 0.030(4) 0.027(4) 0.041(4) -0.004(4) -0.009(3) -0.010(3) C14 0.026(4) 0.029(4) 0.037(4) -0.014(3) -0.005(3) -0.006(3) C15 0.017(3) 0.023(4) 0.021(3) -0.007(3) -0.003(2) 0.001(3) C20 0.015(3) 0.023(4) 0.018(3) -0.001(3) 0.002(2) -0.012(3) C21 0.020(3) 0.029(4) 0.019(3) -0.006(3) -0.007(3) -0.008(3) C22 0.024(3) 0.018(4) 0.018(3) -0.002(3) 0.003(3) -0.004(3) C23 0.020(4) 0.026(4) 0.032(4) -0.003(3) 0.004(3) -0.005(3) C24 0.016(3) 0.027(4) 0.030(4) -0.006(3) -0.005(3) -0.007(3) C25 0.017(3) 0.024(4) 0.011(3) 0.000(3) -0.002(2) -0.001(3) C30 0.013(3) 0.023(4) 0.021(3) -0.009(3) 0.004(2) -0.003(3) C31 0.011(3) 0.028(4) 0.020(3) -0.004(3) 0.000(2) -0.004(3) C32 0.025(4) 0.029(4) 0.016(3) -0.007(3) -0.006(3) -0.001(3) C33 0.025(4) 0.027(4) 0.021(3) -0.005(3) 0.000(3) 0.001(3) C34 0.020(3) 0.021(4) 0.026(3) -0.001(3) -0.004(3) -0.011(3) C35 0.019(3) 0.025(4) 0.021(3) -0.005(3) -0.005(3) -0.006(3) C40 0.008(3) 0.032(4) 0.017(3) -0.006(3) 0.002(2) -0.004(3) C41 0.028(4) 0.038(5) 0.033(4) -0.020(4) 0.008(3) -0.019(3) C42 0.034(4) 0.063(6) 0.024(4) -0.011(4) 0.011(3) -0.027(4) C43 0.026(4) 0.041(5) 0.026(4) -0.019(3) 0.005(3) -0.006(3) C44 0.031(4) 0.043(5) 0.029(4) -0.022(4) -0.003(3) 0.000(4) C45 0.022(4) 0.026(4) 0.023(3) -0.005(3) -0.003(3) -0.001(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 2.2341(16) . ? Au1 Cl1 2.2944(15) . ? Au1 Au2 3.2748(3) . ? Au2 P2 2.2349(17) . ? Au2 Cl2 2.3102(17) . ? P1 C20 1.805(6) . ? P1 C10 1.827(7) . ? P1 C1 1.833(6) . ? P2 C30 1.807(7) . ? P2 C40 1.812(6) . ? P2 C2 1.835(6) . ? C7 C8 1.379(10) . ? C7 C6 1.387(10) . ? C7 H7 0.9500 . ? O1 C9 1.206(8) . ? O2 C9 1.334(8) . ? O2 H2 0.8400 . ? O3 C8 1.360(7) . ? O3 H3 0.8400 . ? N1 C3 1.443(8) . ? N1 C1 1.466(8) . ? N1 C2 1.472(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C4 C5 1.373(9) . ? C4 C3 1.418(9) . ? C4 C9 1.505(9) . ? C3 C8 1.414(9) . ? C5 C6 1.398(10) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C10 C15 1.386(9) . ? C10 C11 1.403(9) . ? C11 C12 1.379(11) . ? C11 H11 0.9500 . ? C12 C13 1.382(11) . ? C12 H12 0.9500 . ? C13 C14 1.395(11) . ? C13 H13 0.9500 . ? C14 C15 1.370(10) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C20 C25 1.398(9) . ? C20 C21 1.409(9) . ? C21 C22 1.400(9) . ? C21 H21 0.9500 . ? C22 C23 1.377(9) . ? C22 H22 0.9500 . ? C23 C24 1.393(10) . ? C23 H23 0.9500 . ? C24 C25 1.380(9) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C30 C35 1.394(9) . ? C30 C31 1.411(9) . ? C31 C32 1.371(9) . ? C31 H31 0.9500 . ? C32 C33 1.384(11) . ? C32 H32 0.9500 . ? C33 C34 1.399(10) . ? C33 H33 0.9500 . ? C34 C35 1.388(9) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C40 C41 1.376(10) . ? C40 C45 1.386(10) . ? C41 C42 1.410(10) . ? C41 H41 0.9500 . ? C42 C43 1.392(11) . ? C42 H42 0.9500 . ? C43 C44 1.368(11) . ? C43 H43 0.9500 . ? C44 C45 1.401(10) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 173.92(6) . . ? P1 Au1 Au2 90.75(4) . . ? Cl1 Au1 Au2 94.94(4) . . ? P2 Au2 Cl2 176.54(6) . . ? P2 Au2 Au1 98.77(4) . . ? Cl2 Au2 Au1 84.68(5) . . ? C20 P1 C10 104.5(3) . . ? C20 P1 C1 107.3(3) . . ? C10 P1 C1 102.5(3) . . ? C20 P1 Au1 113.2(2) . . ? C10 P1 Au1 114.5(2) . . ? C1 P1 Au1 113.9(2) . . ? C30 P2 C40 108.5(3) . . ? C30 P2 C2 104.6(3) . . ? C40 P2 C2 103.5(3) . . ? C30 P2 Au2 112.5(2) . . ? C40 P2 Au2 113.6(2) . . ? C2 P2 Au2 113.4(2) . . ? C8 C7 C6 119.1(6) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C9 O2 H2 109.5 . . ? C8 O3 H3 109.5 . . ? C3 N1 C1 118.9(5) . . ? C3 N1 C2 115.1(5) . . ? C1 N1 C2 113.4(5) . . ? N1 C1 P1 114.3(4) . . ? N1 C1 H1A 108.7 . . ? P1 C1 H1A 108.7 . . ? N1 C1 H1B 108.7 . . ? P1 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? N1 C2 P2 110.6(4) . . ? N1 C2 H2A 109.5 . . ? P2 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? P2 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C5 C4 C3 120.8(6) . . ? C5 C4 C9 117.8(6) . . ? C3 C4 C9 121.4(6) . . ? C8 C3 C4 117.4(6) . . ? C8 C3 N1 116.5(5) . . ? C4 C3 N1 126.0(6) . . ? C4 C5 C6 120.0(6) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C7 C6 C5 120.7(6) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? O3 C8 C7 117.5(6) . . ? O3 C8 C3 120.7(5) . . ? C7 C8 C3 121.8(6) . . ? O1 C9 O2 122.8(6) . . ? O1 C9 C4 125.8(6) . . ? O2 C9 C4 111.4(6) . . ? C15 C10 C11 119.5(7) . . ? C15 C10 P1 122.0(5) . . ? C11 C10 P1 118.4(5) . . ? C12 C11 C10 120.1(7) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 119.9(7) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C12 C13 C14 120.0(7) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.3(7) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C10 120.2(7) . . ? C14 C15 H15 119.9 . . ? C10 C15 H15 119.9 . . ? C25 C20 C21 119.2(5) . . ? C25 C20 P1 123.1(5) . . ? C21 C20 P1 117.7(5) . . ? C22 C21 C20 119.7(6) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C23 C22 C21 119.9(6) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 120.8(6) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C23 119.8(6) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C20 120.6(6) . . ? C24 C25 H25 119.7 . . ? C20 C25 H25 119.7 . . ? C35 C30 C31 118.9(6) . . ? C35 C30 P2 123.0(5) . . ? C31 C30 P2 118.0(5) . . ? C32 C31 C30 120.5(6) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C33 120.3(6) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C32 C33 C34 120.2(7) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C35 C34 C33 119.6(6) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C30 120.5(6) . . ? C34 C35 H35 119.8 . . ? C30 C35 H35 119.8 . . ? C41 C40 C45 119.3(6) . . ? C41 C40 P2 118.3(6) . . ? C45 C40 P2 122.3(5) . . ? C40 C41 C42 120.5(7) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C43 C42 C41 119.2(7) . . ? C43 C42 H42 120.4 . . ? C41 C42 H42 120.4 . . ? C44 C43 C42 120.5(7) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C43 C44 C45 119.9(8) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C40 C45 C44 120.6(7) . . ? C40 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 Cl2 0.84 2.29 3.113(5) 168 2_565 O3 H3 N1 0.84 2.28 2.755(6) 117 . _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 2.926 _refine_diff_density_min -2.805 _refine_diff_density_rms 0.279 data_3a _database_code_depnum_ccdc_archive 'CCDC 289356' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H29 N O3 P2' _chemical_formula_weight 549.51 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' 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' _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 9.8874(2) _cell_length_b 11.2785(2) _cell_length_c 13.3023(3) _cell_angle_alpha 70.929(1) _cell_angle_beta 81.604(1) _cell_angle_gamma 87.168(1) _cell_volume 1386.96(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 10781 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.192 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9270 _exptl_absorpt_correction_T_max 0.9848 _exptl_absorpt_process_details 'SORTAV Blessing (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_decay_% negligible _diffrn_reflns_number 20070 _diffrn_reflns_av_R_equivalents 0.0826 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.46 _reflns_number_total 6246 _reflns_number_gt 4907 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL and local programs' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0835P)^2^+0.2187P] 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 SHELXL _refine_ls_extinction_coef 0.003(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6246 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1404 _refine_ls_wR_factor_gt 0.1293 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 C3 C 0.08066(18) 0.78549(16) 0.51077(13) 0.0187(4) Uani 1 1 d . . . C4 C 0.02227(19) 0.66523(16) 0.55148(14) 0.0217(4) Uani 1 1 d . . . H4 H -0.0115 0.6305 0.5039 0.026 Uiso 1 1 calc R . . C5 C 0.01301(19) 0.59666(16) 0.65901(14) 0.0213(4) Uani 1 1 d . . . C6 C 0.06431(19) 0.64375(16) 0.73197(14) 0.0214(4) Uani 1 1 d . . . C9 C 0.04447(19) 0.57623(17) 0.84614(15) 0.0240(4) Uani 1 1 d . . . C7 C 0.12597(19) 0.76237(16) 0.69038(14) 0.0219(4) Uani 1 1 d . . . H7 H 0.1628 0.7955 0.7377 0.026 Uiso 1 1 calc R . . C8 C 0.13496(19) 0.83235(16) 0.58358(14) 0.0206(4) Uani 1 1 d . . . H8 H 0.1776 0.9123 0.5583 0.025 Uiso 1 1 calc R . . C1 C 0.14549(18) 0.98287(15) 0.36340(14) 0.0195(4) Uani 1 1 d . . . H1A H 0.1133 1.0297 0.4137 0.023 Uiso 1 1 calc R . . H1B H 0.1150 1.0290 0.2933 0.023 Uiso 1 1 calc R . . C16 C 0.36082(18) 0.88881(16) 0.24970(14) 0.0212(4) Uani 1 1 d . . . C17 C 0.3707(2) 0.75871(17) 0.29316(16) 0.0263(4) Uani 1 1 d . . . H17 H 0.3788 0.7212 0.3672 0.032 Uiso 1 1 calc R . . C18 C 0.3686(2) 0.68334(18) 0.22868(17) 0.0326(5) Uani 1 1 d . . . H18 H 0.3725 0.5946 0.2591 0.039 Uiso 1 1 calc R . . C19 C 0.3609(2) 0.7377(2) 0.12069(17) 0.0357(5) Uani 1 1 d . . . H19 H 0.3584 0.6863 0.0770 0.043 Uiso 1 1 calc R . . C20 C 0.3568(2) 0.86696(19) 0.07550(16) 0.0325(5) Uani 1 1 d . . . H20 H 0.3544 0.9040 0.0006 0.039 Uiso 1 1 calc R . . C21 C 0.3561(2) 0.94248(17) 0.14001(15) 0.0260(4) Uani 1 1 d . . . H21 H 0.3523 1.0311 0.1090 0.031 Uiso 1 1 calc R . . C10 C 0.38246(18) 1.13567(16) 0.26153(13) 0.0201(4) Uani 1 1 d . . . C11 C 0.2939(2) 1.23724(16) 0.25130(14) 0.0235(4) Uani 1 1 d . . . H11 H 0.2013 1.2238 0.2837 0.028 Uiso 1 1 calc R . . C12 C 0.3400(2) 1.35913(17) 0.19362(16) 0.0294(4) Uani 1 1 d . . . H12 H 0.2788 1.4281 0.1868 0.035 Uiso 1 1 calc R . . C13 C 0.4740(2) 1.37898(18) 0.14676(16) 0.0330(5) Uani 1 1 d . . . H13 H 0.5050 1.4618 0.1075 0.040 Uiso 1 1 calc R . . C14 C 0.5639(2) 1.2792(2) 0.15643(16) 0.0325(5) Uani 1 1 d . . . H14 H 0.6565 1.2936 0.1242 0.039 Uiso 1 1 calc R . . C15 C 0.5186(2) 1.15797(18) 0.21333(15) 0.0272(4) Uani 1 1 d . . . H15 H 0.5804 1.0896 0.2196 0.033 Uiso 1 1 calc R . . C2 C 0.03423(18) 0.81433(16) 0.32491(14) 0.0212(4) Uani 1 1 d . . . H2A H 0.0242 0.7220 0.3536 0.025 Uiso 1 1 calc R . . H2B H 0.1024 0.8348 0.2594 0.025 Uiso 1 1 calc R . . C22 C -0.25515(19) 0.78340(17) 0.39336(15) 0.0249(4) Uani 1 1 d . . . C23 C -0.3535(2) 0.8363(2) 0.45172(15) 0.0284(4) Uani 1 1 d . . . H23 H -0.3561 0.9247 0.4360 0.034 Uiso 1 1 calc R . . C24 C -0.4480(2) 0.7624(2) 0.53248(16) 0.0355(5) Uani 1 1 d . . . H24 H -0.5156 0.8002 0.5708 0.043 Uiso 1 1 calc R . . C25 C -0.4437(2) 0.6338(2) 0.55699(17) 0.0407(6) Uani 1 1 d . . . H25 H -0.5073 0.5827 0.6131 0.049 Uiso 1 1 calc R . . C26 C -0.3466(2) 0.5794(2) 0.49979(18) 0.0391(5) Uani 1 1 d . . . H26 H -0.3442 0.4907 0.5168 0.047 Uiso 1 1 calc R . . C27 C -0.2535(2) 0.65206(18) 0.41851(17) 0.0321(5) Uani 1 1 d . . . H27 H -0.1879 0.6135 0.3793 0.039 Uiso 1 1 calc R . . C28 C -0.1427(2) 0.83248(16) 0.17335(15) 0.0251(4) Uani 1 1 d . . . C29 C -0.2594(2) 0.7777(2) 0.15979(18) 0.0336(5) Uani 1 1 d . . . H29 H -0.3362 0.7612 0.2143 0.040 Uiso 1 1 calc R . . C30 C -0.2644(2) 0.7470(2) 0.06703(19) 0.0413(6) Uani 1 1 d . . . H30 H -0.3443 0.7095 0.0590 0.050 Uiso 1 1 calc R . . C31 C -0.1547(3) 0.7706(2) -0.01261(18) 0.0400(5) Uani 1 1 d . . . H31 H -0.1581 0.7483 -0.0751 0.048 Uiso 1 1 calc R . . C32 C -0.0390(3) 0.8269(2) -0.00181(16) 0.0377(5) Uani 1 1 d . . . H32 H 0.0365 0.8446 -0.0575 0.045 Uiso 1 1 calc R . . C33 C -0.0334(2) 0.85757(19) 0.09030(15) 0.0326(5) Uani 1 1 d . . . H33 H 0.0464 0.8964 0.0970 0.039 Uiso 1 1 calc R . . N1 N 0.08466(15) 0.85790(13) 0.40466(11) 0.0195(3) Uani 1 1 d . . . O3 O -0.04780(15) 0.48253(12) 0.69092(10) 0.0301(3) Uani 1 1 d . . . H3 H -0.0564 0.4522 0.7582 0.045 Uiso 1 1 calc R . . O1 O -0.02890(15) 0.48076(12) 0.88677(10) 0.0292(3) Uani 1 1 d . . . O2 O 0.10647(15) 0.62328(14) 0.90594(10) 0.0322(3) Uani 1 1 d . . . H2 H 0.0719 0.5929 0.9705 0.048 Uiso 1 1 calc R . . P1 P 0.33735(5) 0.97527(4) 0.34614(3) 0.01891(14) Uani 1 1 d . . . P2 P -0.13435(5) 0.88661(4) 0.28817(4) 0.02293(15) 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 C3 0.0209(9) 0.0169(8) 0.0180(8) -0.0061(6) -0.0016(7) 0.0008(7) C4 0.0273(10) 0.0195(8) 0.0201(9) -0.0088(7) -0.0026(7) -0.0030(7) C5 0.0241(9) 0.0149(8) 0.0235(9) -0.0054(7) -0.0004(7) -0.0016(7) C6 0.0236(9) 0.0202(9) 0.0185(8) -0.0040(7) -0.0018(7) -0.0007(7) C9 0.0247(10) 0.0226(9) 0.0233(9) -0.0052(7) -0.0038(7) -0.0011(7) C7 0.0244(9) 0.0224(9) 0.0202(9) -0.0082(7) -0.0033(7) -0.0028(7) C8 0.0262(9) 0.0161(8) 0.0193(8) -0.0050(7) -0.0026(7) -0.0032(7) C1 0.0227(9) 0.0151(8) 0.0198(8) -0.0046(7) -0.0018(7) -0.0031(7) C16 0.0215(9) 0.0186(8) 0.0232(9) -0.0068(7) -0.0018(7) -0.0008(7) C17 0.0300(10) 0.0205(9) 0.0276(10) -0.0061(7) -0.0056(8) 0.0008(7) C18 0.0424(12) 0.0191(9) 0.0372(11) -0.0098(8) -0.0069(9) 0.0022(8) C19 0.0458(13) 0.0322(11) 0.0358(11) -0.0214(9) -0.0033(10) 0.0015(10) C20 0.0416(12) 0.0325(11) 0.0233(9) -0.0104(8) -0.0005(9) -0.0014(9) C21 0.0316(10) 0.0210(9) 0.0242(9) -0.0068(7) -0.0004(8) -0.0015(8) C10 0.0243(9) 0.0198(8) 0.0175(8) -0.0062(7) -0.0058(7) -0.0028(7) C11 0.0278(10) 0.0201(9) 0.0251(9) -0.0081(7) -0.0083(8) -0.0027(7) C12 0.0411(12) 0.0182(9) 0.0309(10) -0.0063(8) -0.0142(9) -0.0029(8) C13 0.0499(13) 0.0231(10) 0.0250(10) -0.0022(8) -0.0107(9) -0.0140(9) C14 0.0331(11) 0.0361(11) 0.0259(10) -0.0059(9) -0.0006(8) -0.0149(9) C15 0.0270(10) 0.0291(10) 0.0252(9) -0.0077(8) -0.0035(8) -0.0037(8) C2 0.0251(9) 0.0195(8) 0.0199(8) -0.0066(7) -0.0049(7) -0.0027(7) C22 0.0261(10) 0.0235(9) 0.0270(9) -0.0076(7) -0.0106(8) -0.0015(7) C23 0.0281(10) 0.0357(11) 0.0257(10) -0.0118(8) -0.0118(8) -0.0010(8) C24 0.0315(11) 0.0557(14) 0.0220(10) -0.0142(9) -0.0071(8) -0.0033(10) C25 0.0323(12) 0.0574(15) 0.0247(10) 0.0012(10) -0.0087(9) -0.0144(10) C26 0.0385(13) 0.0306(11) 0.0406(12) 0.0046(9) -0.0151(10) -0.0125(9) C27 0.0297(11) 0.0251(10) 0.0395(11) -0.0060(9) -0.0078(9) -0.0029(8) C28 0.0335(11) 0.0186(9) 0.0237(9) -0.0033(7) -0.0136(8) -0.0004(8) C29 0.0285(11) 0.0376(11) 0.0403(12) -0.0173(9) -0.0126(9) 0.0020(9) C30 0.0396(13) 0.0445(13) 0.0527(14) -0.0248(11) -0.0279(11) 0.0056(10) C31 0.0540(15) 0.0414(12) 0.0329(11) -0.0171(10) -0.0246(11) 0.0109(11) C32 0.0534(14) 0.0350(12) 0.0233(10) -0.0057(9) -0.0094(10) -0.0014(10) C33 0.0434(12) 0.0291(10) 0.0248(10) -0.0041(8) -0.0110(9) -0.0070(9) N1 0.0258(8) 0.0162(7) 0.0165(7) -0.0040(6) -0.0041(6) -0.0048(6) O3 0.0463(9) 0.0188(7) 0.0238(7) -0.0036(5) -0.0039(6) -0.0111(6) O1 0.0364(8) 0.0252(7) 0.0225(7) -0.0016(5) -0.0043(6) -0.0083(6) O2 0.0363(8) 0.0392(8) 0.0191(6) -0.0044(6) -0.0046(6) -0.0146(6) P1 0.0219(3) 0.0164(2) 0.0179(2) -0.00406(17) -0.00436(18) -0.00081(17) P2 0.0273(3) 0.0175(2) 0.0246(3) -0.00573(19) -0.0072(2) -0.00223(19) _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 C3 N1 1.376(2) . ? C3 C4 1.404(2) . ? C3 C8 1.421(2) . ? C4 C5 1.378(2) . ? C4 H4 0.9500 . ? C5 O3 1.358(2) . ? C5 C6 1.410(2) . ? C6 C7 1.402(2) . ? C6 C9 1.448(2) . ? C9 O1 1.249(2) . ? C9 O2 1.319(2) . ? C7 C8 1.374(2) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C1 N1 1.460(2) . ? C1 P1 1.8784(18) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C16 C21 1.392(3) . ? C16 C17 1.394(2) . ? C16 P1 1.8327(18) . ? C17 C18 1.394(3) . ? C17 H17 0.9500 . ? C18 C19 1.377(3) . ? C18 H18 0.9500 . ? C19 C20 1.384(3) . ? C19 H19 0.9500 . ? C20 C21 1.392(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C10 C11 1.390(3) . ? C10 C15 1.401(3) . ? C10 P1 1.8278(18) . ? C11 C12 1.399(3) . ? C11 H11 0.9500 . ? C12 C13 1.375(3) . ? C12 H12 0.9500 . ? C13 C14 1.383(3) . ? C13 H13 0.9500 . ? C14 C15 1.389(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C2 N1 1.461(2) . ? C2 P2 1.8774(18) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C22 C23 1.389(3) . ? C22 C27 1.408(3) . ? C22 P2 1.823(2) . ? C23 C24 1.386(3) . ? C23 H23 0.9500 . ? C24 C25 1.378(3) . ? C24 H24 0.9500 . ? C25 C26 1.382(4) . ? C25 H25 0.9500 . ? C26 C27 1.376(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.395(3) . ? C28 C29 1.396(3) . ? C28 P2 1.8341(19) . ? C29 C30 1.394(3) . ? C29 H29 0.9500 . ? C30 C31 1.371(3) . ? C30 H30 0.9500 . ? C31 C32 1.382(3) . ? C31 H31 0.9500 . ? C32 C33 1.387(3) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? O3 H3 0.8400 . ? O2 H2 0.8400 . ? 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 C3 C4 122.15(15) . . ? N1 C3 C8 120.13(15) . . ? C4 C3 C8 117.72(15) . . ? C5 C4 C3 121.32(16) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? O3 C5 C4 116.91(15) . . ? O3 C5 C6 121.94(15) . . ? C4 C5 C6 121.16(16) . . ? C7 C6 C5 117.27(16) . . ? C7 C6 C9 121.54(16) . . ? C5 C6 C9 121.02(16) . . ? O1 C9 O2 121.45(16) . . ? O1 C9 C6 122.66(16) . . ? O2 C9 C6 115.88(16) . . ? C8 C7 C6 122.28(16) . . ? C8 C7 H7 118.9 . . ? C6 C7 H7 118.9 . . ? C7 C8 C3 120.21(16) . . ? C7 C8 H8 119.9 . . ? C3 C8 H8 119.9 . . ? N1 C1 P1 111.68(12) . . ? N1 C1 H1A 109.3 . . ? P1 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? P1 C1 H1B 109.3 . . ? H1A C1 H1B 107.9 . . ? C21 C16 C17 118.99(17) . . ? C21 C16 P1 124.65(14) . . ? C17 C16 P1 116.05(14) . . ? C18 C17 C16 120.40(18) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 119.86(18) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 120.40(18) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C21 119.91(19) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C16 120.35(17) . . ? C20 C21 H21 119.8 . . ? C16 C21 H21 119.8 . . ? C11 C10 C15 118.67(17) . . ? C11 C10 P1 123.86(14) . . ? C15 C10 P1 117.15(14) . . ? C10 C11 C12 120.52(18) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 119.89(19) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 120.49(18) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 119.8(2) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C10 120.58(19) . . ? C14 C15 H15 119.7 . . ? C10 C15 H15 119.7 . . ? N1 C2 P2 112.71(12) . . ? N1 C2 H2A 109.0 . . ? P2 C2 H2A 109.0 . . ? N1 C2 H2B 109.0 . . ? P2 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C23 C22 C27 118.22(18) . . ? C23 C22 P2 118.74(14) . . ? C27 C22 P2 123.04(15) . . ? C24 C23 C22 121.2(2) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C25 C24 C23 119.8(2) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 119.9(2) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C27 C26 C25 120.8(2) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C26 C27 C22 120.1(2) . . ? C26 C27 H27 119.9 . . ? C22 C27 H27 119.9 . . ? C33 C28 C29 117.78(18) . . ? C33 C28 P2 119.07(14) . . ? C29 C28 P2 122.84(16) . . ? C30 C29 C28 120.7(2) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C31 C30 C29 120.4(2) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 119.9(2) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C33 119.9(2) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C28 121.26(19) . . ? C32 C33 H33 119.4 . . ? C28 C33 H33 119.4 . . ? C3 N1 C1 121.60(14) . . ? C3 N1 C2 123.00(14) . . ? C1 N1 C2 115.35(13) . . ? C5 O3 H3 109.5 . . ? C9 O2 H2 109.5 . . ? C10 P1 C16 102.75(8) . . ? C10 P1 C1 101.53(8) . . ? C16 P1 C1 97.88(8) . . ? C22 P2 C28 102.71(8) . . ? C22 P2 C2 101.95(8) . . ? C28 P2 C2 98.38(8) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O1 0.84 1.80 2.6316(18) 170 2_567 O3 H3 O1 0.84 1.90 2.6326(19) 145 . _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.445 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.068 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 289357' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H39 Au2 Cl2 N O3 P2' _chemical_formula_weight 1072.47 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' 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' _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 11.2658(10) _cell_length_b 11.6465(2) _cell_length_c 14.4950(2) _cell_angle_alpha 85.708(1) _cell_angle_beta 74.044(1) _cell_angle_gamma 86.088(1) _cell_volume 1821.19(17) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 26211 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 26.00 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.956 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1028 _exptl_absorpt_coefficient_mu 8.318 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3684 _exptl_absorpt_correction_T_max 0.5558 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius Kappa CCD Area detector' _diffrn_measurement_method '\f and \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26211 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7097 _reflns_number_gt 6446 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; DENZO (Otwinowski and Minor, 1997), COLLECT (Hooft, 1998) ; _computing_cell_refinement ; DENZO (Otwinowski and MInor, 1997), COLLECT (Hooft, 1998) ; _computing_data_reduction ; DENZO (Otwinowski and MInor, 1997), COLLECT (Hooft, 1998), MAXUS (Mackay et al., 1998) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0534P)^2^+0.1240P] 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 SHELXL _refine_ls_extinction_coef 0.00184(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7097 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0819 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 0.018764(13) 0.230691(13) 0.355625(10) 0.01739(8) Uani 1 1 d . . . Au2 Au 0.349732(13) 0.631936(12) 0.060415(10) 0.01768(8) Uani 1 1 d . . . P1 P 0.21411(8) 0.26152(8) 0.27299(7) 0.0151(2) Uani 1 1 d . . . P2 P 0.30129(9) 0.69822(8) 0.20753(7) 0.0161(2) Uani 1 1 d . . . Cl1 Cl -0.18079(9) 0.19282(11) 0.43859(8) 0.0328(3) Uani 1 1 d . . . Cl2 Cl 0.40030(9) 0.56058(9) -0.09021(7) 0.0257(2) Uani 1 1 d . . . O1 O -0.3726(3) 0.5456(3) 0.5233(2) 0.0274(7) Uani 1 1 d . . . O2 O -0.3980(2) 0.4940(3) 0.3838(2) 0.0257(6) Uani 1 1 d . . . H2 H -0.4718 0.4911 0.4170 0.039 Uiso 1 1 calc R . . N1 N 0.1896(3) 0.4976(3) 0.2892(2) 0.0178(7) Uani 1 1 d . . . C1 C 0.2416(3) 0.4108(3) 0.2200(3) 0.0166(8) Uani 1 1 d . . . H1A H 0.3317 0.4198 0.1947 0.020 Uiso 1 1 calc R . . H1B H 0.2045 0.4236 0.1653 0.020 Uiso 1 1 calc R . . C2 C 0.2744(4) 0.5794(3) 0.3026(3) 0.0182(8) Uani 1 1 d . . . H2A H 0.3543 0.5383 0.3025 0.022 Uiso 1 1 calc R . . H2B H 0.2403 0.6124 0.3661 0.022 Uiso 1 1 calc R . . C3 C 0.0609(3) 0.5210(3) 0.3175(3) 0.0157(8) Uani 1 1 d . . . C4 C -0.0162(4) 0.4794(3) 0.2669(3) 0.0203(8) Uani 1 1 d . . . H4 H 0.0199 0.4455 0.2074 0.024 Uiso 1 1 calc R . . C5 C -0.1431(4) 0.4871(3) 0.3023(3) 0.0198(8) Uani 1 1 d . . . H5 H -0.1933 0.4594 0.2666 0.024 Uiso 1 1 calc R . . C6 C -0.1983(3) 0.5353(3) 0.3900(3) 0.0173(8) Uani 1 1 d . . . C7 C -0.1230(3) 0.5846(3) 0.4370(3) 0.0190(8) Uani 1 1 d . . . H7 H -0.1598 0.6223 0.4947 0.023 Uiso 1 1 calc R . . C8 C 0.0047(4) 0.5793(3) 0.4007(3) 0.0201(8) Uani 1 1 d . . . H8 H 0.0542 0.6154 0.4325 0.024 Uiso 1 1 calc R . . C9 C -0.3306(4) 0.5256(3) 0.4362(3) 0.0190(8) Uani 1 1 d . . . C10 C 0.3241(3) 0.2260(4) 0.3437(3) 0.0190(8) Uani 1 1 d . . . C11 C 0.2866(4) 0.1529(4) 0.4251(3) 0.0233(9) Uani 1 1 d . . . H11 H 0.2052 0.1259 0.4434 0.028 Uiso 1 1 calc R . . C12 C 0.3683(4) 0.1190(4) 0.4800(3) 0.0338(11) Uani 1 1 d . . . H12 H 0.3429 0.0679 0.5352 0.041 Uiso 1 1 calc R . . C13 C 0.4869(4) 0.1599(4) 0.4542(3) 0.0305(10) Uani 1 1 d . . . H13 H 0.5419 0.1378 0.4924 0.037 Uiso 1 1 calc R . . C14 C 0.5247(4) 0.2331(4) 0.3724(3) 0.0264(10) Uani 1 1 d . . . H14 H 0.6058 0.2607 0.3543 0.032 Uiso 1 1 calc R . . C15 C 0.4432(3) 0.2657(3) 0.3173(3) 0.0200(8) Uani 1 1 d . . . H15 H 0.4690 0.3154 0.2612 0.024 Uiso 1 1 calc R . . C20 C 0.2657(3) 0.1804(3) 0.1661(3) 0.0163(8) Uani 1 1 d . . . C21 C 0.3821(4) 0.1956(4) 0.1025(3) 0.0248(9) Uani 1 1 d . . . H21 H 0.4374 0.2453 0.1168 0.030 Uiso 1 1 calc R . . C22 C 0.4169(4) 0.1375(4) 0.0177(3) 0.0286(10) Uani 1 1 d . . . H22 H 0.4958 0.1483 -0.0261 0.034 Uiso 1 1 calc R . . C23 C 0.3376(4) 0.0645(4) -0.0029(3) 0.0289(10) Uani 1 1 d . . . H23 H 0.3624 0.0247 -0.0605 0.035 Uiso 1 1 calc R . . C24 C 0.2213(4) 0.0488(4) 0.0606(3) 0.0261(9) Uani 1 1 d . . . H24 H 0.1664 -0.0009 0.0460 0.031 Uiso 1 1 calc R . . C25 C 0.1864(4) 0.1055(3) 0.1443(3) 0.0198(8) Uani 1 1 d . . . H25 H 0.1076 0.0937 0.1880 0.024 Uiso 1 1 calc R . . C30 C 0.4220(3) 0.7763(3) 0.2329(3) 0.0174(8) Uani 1 1 d . . . C31 C 0.4121(4) 0.8962(3) 0.2393(3) 0.0208(8) Uani 1 1 d . . . H31 H 0.3407 0.9389 0.2304 0.025 Uiso 1 1 calc R . . C32 C 0.5055(4) 0.9519(4) 0.2585(3) 0.0251(9) Uani 1 1 d . . . H32 H 0.4983 1.0333 0.2627 0.030 Uiso 1 1 calc R . . C33 C 0.6097(4) 0.8913(4) 0.2717(4) 0.0289(10) Uani 1 1 d . . . H33 H 0.6735 0.9307 0.2854 0.035 Uiso 1 1 calc R . . C34 C 0.6211(4) 0.7731(4) 0.2649(3) 0.0280(10) Uani 1 1 d . . . H34 H 0.6926 0.7311 0.2744 0.034 Uiso 1 1 calc R . . C35 C 0.5282(4) 0.7156(3) 0.2443(3) 0.0233(9) Uani 1 1 d . . . H35 H 0.5373 0.6347 0.2380 0.028 Uiso 1 1 calc R . . C40 C 0.1599(3) 0.7893(3) 0.2403(3) 0.0184(8) Uani 1 1 d . . . C41 C 0.1279(4) 0.8410(3) 0.3277(3) 0.0191(8) Uani 1 1 d . . . H41 H 0.1806 0.8302 0.3691 0.023 Uiso 1 1 calc R . . C42 C 0.0182(4) 0.9092(3) 0.3546(3) 0.0237(9) Uani 1 1 d . . . H42 H -0.0034 0.9459 0.4138 0.028 Uiso 1 1 calc R . . C45 C 0.0825(4) 0.8026(3) 0.1803(3) 0.0234(9) Uani 1 1 d . . . H45 H 0.1045 0.7664 0.1209 0.028 Uiso 1 1 calc R . . C43 C -0.0582(4) 0.9225(4) 0.2945(4) 0.0312(10) Uani 1 1 d . . . H43 H -0.1327 0.9687 0.3128 0.037 Uiso 1 1 calc R . . C44 C -0.0284(4) 0.8695(4) 0.2073(3) 0.0282(10) Uani 1 1 d . . . H44 H -0.0824 0.8786 0.1668 0.034 Uiso 1 1 calc R . . O3 O 0.9557(3) 0.2464(3) 0.0374(2) 0.0324(7) Uani 1 1 d . . . C100 C 0.7774(5) 0.1510(4) 0.1306(4) 0.0405(12) Uani 1 1 d . . . H10A H 0.7148 0.1486 0.1928 0.061 Uiso 1 1 calc R . . H10B H 0.8235 0.0763 0.1218 0.061 Uiso 1 1 calc R . . H10C H 0.7369 0.1676 0.0789 0.061 Uiso 1 1 calc R . . C101 C 0.8646(4) 0.2433(4) 0.1278(3) 0.0347(11) Uani 1 1 d . . . H10D H 0.8185 0.3189 0.1370 0.042 Uiso 1 1 calc R . . H10E H 0.9050 0.2274 0.1803 0.042 Uiso 1 1 calc R . . C102 C 1.0405(5) 0.3354(4) 0.0299(3) 0.0332(11) Uani 1 1 d . . . H10F H 1.0817 0.3228 0.0823 0.040 Uiso 1 1 calc R . . H10G H 0.9948 0.4114 0.0368 0.040 Uiso 1 1 calc R . . C103 C 1.1350(5) 0.3344(5) -0.0649(4) 0.0435(13) Uani 1 1 d . . . H10H H 1.1925 0.3953 -0.0695 0.065 Uiso 1 1 calc R . . H10I H 1.0939 0.3479 -0.1165 0.065 Uiso 1 1 calc R . . H10J H 1.1806 0.2594 -0.0711 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01396(11) 0.02323(12) 0.01289(11) -0.00198(7) -0.00001(7) -0.00051(7) Au2 0.01976(11) 0.01940(12) 0.01272(11) -0.00284(7) -0.00189(7) -0.00129(7) P1 0.0149(5) 0.0157(5) 0.0123(5) -0.0027(4) 0.0003(4) 0.0009(4) P2 0.0168(5) 0.0171(5) 0.0137(5) -0.0030(4) -0.0029(4) -0.0001(4) Cl1 0.0160(5) 0.0566(7) 0.0222(6) 0.0050(5) -0.0003(4) -0.0058(4) Cl2 0.0287(5) 0.0314(6) 0.0154(5) -0.0072(4) -0.0018(4) -0.0015(4) O1 0.0224(15) 0.0392(18) 0.0171(16) -0.0109(13) 0.0017(12) 0.0030(13) O2 0.0180(14) 0.0393(18) 0.0174(15) -0.0059(13) -0.0001(12) 0.0002(12) N1 0.0152(16) 0.0166(17) 0.0194(18) -0.0067(13) 0.0002(13) 0.0007(12) C1 0.0148(19) 0.0156(19) 0.017(2) -0.0017(15) -0.0010(15) 0.0021(14) C2 0.0157(19) 0.022(2) 0.017(2) -0.0011(16) -0.0041(15) 0.0000(14) C3 0.0181(19) 0.0131(18) 0.0135(19) 0.0005(14) -0.0012(15) 0.0016(14) C4 0.021(2) 0.023(2) 0.016(2) -0.0055(16) -0.0037(16) 0.0029(15) C5 0.019(2) 0.026(2) 0.014(2) -0.0031(16) -0.0049(16) 0.0044(16) C6 0.021(2) 0.0129(19) 0.016(2) -0.0018(15) -0.0046(16) 0.0055(14) C7 0.020(2) 0.017(2) 0.016(2) -0.0069(16) 0.0018(16) 0.0039(15) C8 0.022(2) 0.021(2) 0.017(2) -0.0026(16) -0.0038(17) -0.0028(16) C9 0.020(2) 0.020(2) 0.016(2) -0.0019(16) -0.0035(17) 0.0026(15) C10 0.0152(19) 0.030(2) 0.0134(19) -0.0091(17) -0.0058(15) 0.0071(16) C11 0.019(2) 0.035(2) 0.013(2) -0.0002(17) 0.0006(16) 0.0009(17) C12 0.036(3) 0.045(3) 0.017(2) 0.008(2) -0.005(2) 0.002(2) C13 0.027(2) 0.045(3) 0.023(2) -0.006(2) -0.0132(19) 0.0084(19) C14 0.023(2) 0.027(2) 0.031(2) -0.0106(19) -0.0081(19) 0.0018(18) C15 0.0167(19) 0.024(2) 0.018(2) -0.0027(17) -0.0020(16) -0.0001(15) C20 0.0202(19) 0.0141(19) 0.0118(19) -0.0018(14) -0.0003(15) 0.0038(14) C21 0.023(2) 0.028(2) 0.022(2) -0.0064(18) -0.0011(18) -0.0035(17) C22 0.026(2) 0.036(3) 0.019(2) -0.0030(19) 0.0038(18) -0.0029(18) C23 0.041(3) 0.026(2) 0.018(2) -0.0048(18) -0.0038(19) -0.0041(19) C24 0.030(2) 0.028(2) 0.021(2) -0.0086(18) -0.0061(19) -0.0035(18) C25 0.021(2) 0.023(2) 0.015(2) -0.0034(16) -0.0050(16) -0.0026(16) C30 0.0168(18) 0.022(2) 0.0131(19) -0.0026(15) -0.0028(15) -0.0012(15) C31 0.0172(19) 0.023(2) 0.021(2) -0.0044(17) -0.0028(16) 0.0011(15) C32 0.026(2) 0.022(2) 0.025(2) -0.0065(17) -0.0012(18) -0.0008(17) C33 0.022(2) 0.037(3) 0.032(3) -0.007(2) -0.011(2) -0.0072(18) C34 0.017(2) 0.037(3) 0.028(2) 0.004(2) -0.0056(18) 0.0011(17) C35 0.024(2) 0.018(2) 0.027(2) 0.0011(17) -0.0069(18) 0.0007(16) C40 0.0172(19) 0.0156(19) 0.020(2) 0.0006(16) -0.0005(16) -0.0024(14) C41 0.019(2) 0.023(2) 0.014(2) -0.0021(16) -0.0013(16) -0.0049(16) C42 0.023(2) 0.021(2) 0.024(2) -0.0054(17) 0.0020(17) -0.0025(16) C45 0.022(2) 0.027(2) 0.023(2) -0.0020(18) -0.0074(17) -0.0053(16) C43 0.016(2) 0.028(2) 0.046(3) -0.008(2) -0.001(2) 0.0029(17) C44 0.023(2) 0.027(2) 0.041(3) -0.007(2) -0.017(2) 0.0011(17) O3 0.0432(19) 0.0323(18) 0.0230(17) -0.0072(14) -0.0092(15) -0.0029(14) C100 0.043(3) 0.044(3) 0.031(3) -0.004(2) -0.003(2) 0.000(2) C101 0.040(3) 0.041(3) 0.025(2) -0.013(2) -0.009(2) 0.009(2) C102 0.047(3) 0.026(2) 0.033(3) -0.003(2) -0.023(2) 0.001(2) C103 0.049(3) 0.040(3) 0.046(3) 0.001(2) -0.019(3) -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.2363(10) . ? Au1 Cl1 2.2944(10) . ? Au2 P2 2.2338(10) . ? Au2 Cl2 2.3033(10) . ? P1 C20 1.811(4) . ? P1 C10 1.823(4) . ? P1 C1 1.858(4) . ? P2 C30 1.817(4) . ? P2 C40 1.821(4) . ? P2 C2 1.857(4) . ? O1 C9 1.255(5) . ? O2 C9 1.298(5) . ? O2 H2 0.8400 . ? N1 C3 1.407(5) . ? N1 C2 1.453(5) . ? N1 C1 1.456(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.401(5) . ? C3 C4 1.409(5) . ? C4 C5 1.379(5) . ? C4 H4 0.9500 . ? C5 C6 1.394(5) . ? C5 H5 0.9500 . ? C6 C7 1.399(5) . ? C6 C9 1.465(5) . ? C7 C8 1.388(5) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C10 C11 1.386(6) . ? C10 C15 1.391(5) . ? C11 C12 1.394(6) . ? C11 H11 0.9500 . ? C12 C13 1.392(6) . ? C12 H12 0.9500 . ? C13 C14 1.391(6) . ? C13 H13 0.9500 . ? C14 C15 1.392(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C20 C21 1.394(6) . ? C20 C25 1.400(5) . ? C21 C22 1.395(6) . ? C21 H21 0.9500 . ? C22 C23 1.377(6) . ? C22 H22 0.9500 . ? C23 C24 1.393(6) . ? C23 H23 0.9500 . ? C24 C25 1.373(6) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C30 C35 1.392(5) . ? C30 C31 1.402(5) . ? C31 C32 1.374(5) . ? C31 H31 0.9500 . ? C32 C33 1.380(6) . ? C32 H32 0.9500 . ? C33 C34 1.382(6) . ? C33 H33 0.9500 . ? C34 C35 1.389(6) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C40 C45 1.386(5) . ? C40 C41 1.389(6) . ? C41 C42 1.399(5) . ? C41 H41 0.9500 . ? C42 C43 1.378(6) . ? C42 H42 0.9500 . ? C45 C44 1.402(6) . ? C45 H45 0.9500 . ? C43 C44 1.396(7) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? O3 C101 1.425(5) . ? O3 C102 1.435(5) . ? C100 C101 1.496(7) . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? C100 H10C 0.9800 . ? C101 H10D 0.9900 . ? C101 H10E 0.9900 . ? C102 C103 1.490(7) . ? C102 H10F 0.9900 . ? C102 H10G 0.9900 . ? C103 H10H 0.9800 . ? C103 H10I 0.9800 . ? C103 H10J 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 178.05(4) . . ? P2 Au2 Cl2 179.05(4) . . ? C20 P1 C10 106.96(17) . . ? C20 P1 C1 100.68(17) . . ? C10 P1 C1 107.21(18) . . ? C20 P1 Au1 113.00(13) . . ? C10 P1 Au1 113.06(14) . . ? C1 P1 Au1 114.92(12) . . ? C30 P2 C40 106.65(18) . . ? C30 P2 C2 103.20(17) . . ? C40 P2 C2 103.40(18) . . ? C30 P2 Au2 114.58(13) . . ? C40 P2 Au2 115.80(13) . . ? C2 P2 Au2 111.89(13) . . ? C9 O2 H2 109.5 . . ? C3 N1 C2 121.2(3) . . ? C3 N1 C1 119.6(3) . . ? C2 N1 C1 116.6(3) . . ? N1 C1 P1 112.6(3) . . ? N1 C1 H1A 109.1 . . ? P1 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? P1 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? N1 C2 P2 112.3(3) . . ? N1 C2 H2A 109.1 . . ? P2 C2 H2A 109.1 . . ? N1 C2 H2B 109.1 . . ? P2 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? C8 C3 N1 120.9(3) . . ? C8 C3 C4 117.9(3) . . ? N1 C3 C4 121.1(3) . . ? C5 C4 C3 121.2(4) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 120.5(4) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C7 118.6(3) . . ? C5 C6 C9 120.8(3) . . ? C7 C6 C9 120.5(3) . . ? C8 C7 C6 121.0(4) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C3 120.4(4) . . ? C7 C8 H8 119.8 . . ? C3 C8 H8 119.8 . . ? O1 C9 O2 123.5(4) . . ? O1 C9 C6 119.3(3) . . ? O2 C9 C6 117.2(3) . . ? C11 C10 C15 119.8(3) . . ? C11 C10 P1 117.3(3) . . ? C15 C10 P1 122.9(3) . . ? C10 C11 C12 119.9(4) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C13 120.2(4) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 119.9(4) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 119.7(4) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C10 C15 C14 120.4(4) . . ? C10 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C21 C20 C25 119.3(4) . . ? C21 C20 P1 120.6(3) . . ? C25 C20 P1 120.0(3) . . ? C20 C21 C22 119.5(4) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C23 C22 C21 120.5(4) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 120.2(4) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C25 C24 C23 119.8(4) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C20 120.7(4) . . ? C24 C25 H25 119.6 . . ? C20 C25 H25 119.6 . . ? C35 C30 C31 119.1(3) . . ? C35 C30 P2 119.1(3) . . ? C31 C30 P2 121.8(3) . . ? C32 C31 C30 120.0(4) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.8(4) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C32 C33 C34 119.8(4) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C33 C34 C35 120.1(4) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C30 C35 C34 120.2(4) . . ? C30 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C45 C40 C41 120.5(4) . . ? C45 C40 P2 120.0(3) . . ? C41 C40 P2 119.5(3) . . ? C40 C41 C42 120.0(4) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C43 C42 C41 119.3(4) . . ? C43 C42 H42 120.4 . . ? C41 C42 H42 120.4 . . ? C40 C45 C44 119.9(4) . . ? C40 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C42 C43 C44 121.4(4) . . ? C42 C43 H43 119.3 . . ? C44 C43 H43 119.3 . . ? C43 C44 C45 118.9(4) . . ? C43 C44 H44 120.6 . . ? C45 C44 H44 120.6 . . ? C101 O3 C102 111.8(3) . . ? C101 C100 H10A 109.5 . . ? C101 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C101 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? O3 C101 C100 109.4(4) . . ? O3 C101 H10D 109.8 . . ? C100 C101 H10D 109.8 . . ? O3 C101 H10E 109.8 . . ? C100 C101 H10E 109.8 . . ? H10D C101 H10E 108.2 . . ? O3 C102 C103 109.9(4) . . ? O3 C102 H10F 109.7 . . ? C103 C102 H10F 109.7 . . ? O3 C102 H10G 109.7 . . ? C103 C102 H10G 109.7 . . ? H10F C102 H10G 108.2 . . ? C102 C103 H10H 109.5 . . ? C102 C103 H10I 109.5 . . ? H10H C103 H10I 109.5 . . ? C102 C103 H10J 109.5 . . ? H10H C103 H10J 109.5 . . ? H10I C103 H10J 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O1 0.84 1.79 2.619(4) 167 2_466 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.545 _refine_diff_density_min -2.546 _refine_diff_density_rms 0.187 #===END data_6a _database_code_depnum_ccdc_archive 'CCDC 289358' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H39 Au2 Cl2 N O4 P2' _chemical_formula_weight 1088.47 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' 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' _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 11.288(2) _cell_length_b 11.664(2) _cell_length_c 14.665(3) _cell_angle_alpha 83.41(3) _cell_angle_beta 73.92(3) _cell_angle_gamma 85.81(3) _cell_volume 1841.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 32842 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.965 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1046 _exptl_absorpt_coefficient_mu 8.230 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2065 _exptl_absorpt_correction_T_max 0.7343 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_decay_% negligible _diffrn_reflns_number 28458 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.44 _reflns_number_total 8249 _reflns_number_gt 7368 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHEXTL and local programs' _computing_publication_material 'Bruker SHEXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0198P)^2^+4.6428P] 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 SHELXL _refine_ls_extinction_coef 0.00166(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8249 _refine_ls_number_parameters 452 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.008 _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 0.2244(4) 0.4361(4) 0.2032(3) 0.0202(8) Uani 1 1 d . B . H1A H 0.2566 0.4086 0.1392 0.024 Uiso 1 1 calc R . . H1B H 0.1453 0.4798 0.2053 0.024 Uiso 1 1 calc R . . C2 C 0.2613(4) 0.5983(4) 0.2851(3) 0.0211(8) Uani 1 1 d . B . H2A H 0.2997 0.5851 0.3387 0.025 Uiso 1 1 calc R . . H2B H 0.1715 0.5881 0.3117 0.025 Uiso 1 1 calc R . . C3 C 0.4391(4) 0.4901(4) 0.1871(3) 0.0198(8) Uani 1 1 d . B . C4 C 0.5181(4) 0.5323(4) 0.2335(3) 0.0230(9) Uani 1 1 d . . . H4 H 0.4844 0.5674 0.2910 0.028 Uiso 1 1 calc R A 1 C5 C 0.6445(4) 0.5227(4) 0.1957(3) 0.0236(9) Uani 1 1 d . B 1 H5 H 0.6964 0.5520 0.2279 0.028 Uiso 1 1 calc R B 1 O3' O 0.7147(6) 0.5560(6) 0.2467(5) 0.0369(16) Uani 0.50 1 d P C 2 C6 C 0.6978(4) 0.4717(4) 0.1125(3) 0.0230(9) Uani 1 1 d . . . C7 C 0.6175(4) 0.4221(4) 0.0706(3) 0.0234(9) Uani 1 1 d . B 1 H7 H 0.6515 0.3817 0.0160 0.028 Uiso 1 1 calc R B 1 O3 O 0.6606(5) 0.3658(5) -0.0064(4) 0.0232(13) Uani 0.50 1 d P D 2 C8 C 0.4913(4) 0.4309(4) 0.1071(3) 0.0226(9) Uani 1 1 d . . . H8 H 0.4397 0.3964 0.0776 0.027 Uiso 1 1 calc R B 1 C9 C 0.8294(4) 0.4763(4) 0.0659(3) 0.0238(9) Uani 1 1 d . B . C10 C 0.0766(4) 0.2347(4) 0.2688(3) 0.0194(8) Uani 1 1 d . B . C11 C 0.0873(4) 0.1166(4) 0.2590(3) 0.0251(9) Uani 1 1 d . . . H11 H 0.1590 0.0727 0.2662 0.030 Uiso 1 1 calc R . . C12 C -0.0072(4) 0.0633(4) 0.2387(3) 0.0295(10) Uani 1 1 d . . . H12 H 0.0001 -0.0171 0.2318 0.035 Uiso 1 1 calc R . . C13 C -0.1121(4) 0.1272(4) 0.2285(3) 0.0294(10) Uani 1 1 d . . . H13 H -0.1759 0.0907 0.2135 0.035 Uiso 1 1 calc R . . C14 C -0.1240(4) 0.2436(4) 0.2401(4) 0.0323(11) Uani 1 1 d . . . H14 H -0.1966 0.2867 0.2338 0.039 Uiso 1 1 calc R . . C15 C -0.0312(4) 0.2981(4) 0.2608(3) 0.0281(10) Uani 1 1 d . . . H15 H -0.0404 0.3780 0.2696 0.034 Uiso 1 1 calc R . . C16 C 0.3373(4) 0.2201(3) 0.2613(3) 0.0198(8) Uani 1 1 d . B . C17 C 0.3692(4) 0.1731(4) 0.1737(3) 0.0227(9) Uani 1 1 d . . . H17 H 0.3159 0.1861 0.1332 0.027 Uiso 1 1 calc R . . C18 C 0.4784(4) 0.1075(4) 0.1459(3) 0.0280(10) Uani 1 1 d . . . H18 H 0.4996 0.0743 0.0869 0.034 Uiso 1 1 calc R . . C19 C 0.5564(4) 0.0908(4) 0.2052(4) 0.0333(11) Uani 1 1 d . . . H19 H 0.6311 0.0459 0.1865 0.040 Uiso 1 1 calc R . . C20 C 0.5263(4) 0.1391(4) 0.2913(4) 0.0317(10) Uani 1 1 d . . . H20 H 0.5811 0.1280 0.3308 0.038 Uiso 1 1 calc R . . C21 C 0.4164(4) 0.2034(4) 0.3201(3) 0.0245(9) Uani 1 1 d . . . H21 H 0.3953 0.2357 0.3794 0.029 Uiso 1 1 calc R . . C22 C 0.1773(3) 0.7833(3) 0.1586(3) 0.0163(8) Uani 1 1 d . B . C23 C 0.2116(4) 0.8561(4) 0.0761(3) 0.0288(10) Uani 1 1 d . . . H23 H 0.2918 0.8859 0.0568 0.035 Uiso 1 1 calc R . . C24 C 0.1305(5) 0.8867(5) 0.0206(4) 0.0389(12) Uani 1 1 d . . . H24 H 0.1558 0.9363 -0.0367 0.047 Uiso 1 1 calc R . . C25 C 0.0129(4) 0.8452(4) 0.0486(3) 0.0335(11) Uani 1 1 d . . . H25 H -0.0422 0.8657 0.0102 0.040 Uiso 1 1 calc R . . C26 C -0.0245(4) 0.7734(4) 0.1328(3) 0.0253(9) Uani 1 1 d . . . H26 H -0.1054 0.7450 0.1521 0.030 Uiso 1 1 calc R . . C27 C 0.0559(4) 0.7432(4) 0.1886(3) 0.0222(9) Uani 1 1 d . . . H27 H 0.0297 0.6957 0.2470 0.027 Uiso 1 1 calc R . . C28 C -0.2340(4) 0.1735(4) 0.6648(3) 0.0212(8) Uani 1 1 d . . . C29 C -0.1180(4) 0.1915(4) 0.6007(3) 0.0263(9) Uani 1 1 d . . . H29 H -0.0635 0.2415 0.6140 0.032 Uiso 1 1 calc R . . C30 C -0.0822(4) 0.1366(4) 0.5177(3) 0.0317(11) Uani 1 1 d . . . H30 H -0.0029 0.1484 0.4749 0.038 Uiso 1 1 calc R . . C31 C -0.1615(5) 0.0647(4) 0.4970(3) 0.0321(11) Uani 1 1 d . . . H31 H -0.1371 0.0280 0.4397 0.039 Uiso 1 1 calc R . . C32 C -0.2768(4) 0.0464(4) 0.5604(3) 0.0294(10) Uani 1 1 d . . . H32 H -0.3313 -0.0028 0.5462 0.035 Uiso 1 1 calc R . . C33 C -0.3128(4) 0.0996(4) 0.6441(3) 0.0244(9) Uani 1 1 d . . . H33 H -0.3913 0.0856 0.6876 0.029 Uiso 1 1 calc R . . C34 C 0.5335(5) 0.3312(5) 0.5300(4) 0.0448(13) Uani 1 1 d . . . H34A H 0.5736 0.3181 0.5826 0.054 Uiso 1 1 calc R . . H34B H 0.4853 0.4057 0.5360 0.054 Uiso 1 1 calc R . . C35 C 0.6302(5) 0.3361(5) 0.4357(4) 0.0502(14) Uani 1 1 d . . . H35A H 0.6793 0.2631 0.4308 0.075 Uiso 1 1 calc R . . H35B H 0.6842 0.3998 0.4311 0.075 Uiso 1 1 calc R . . H35C H 0.5901 0.3485 0.3838 0.075 Uiso 1 1 calc R . . C36 C 0.3622(5) 0.2317(5) 0.6259(4) 0.0389(12) Uani 1 1 d . . . H36A H 0.3155 0.3065 0.6354 0.047 Uiso 1 1 calc R . . H36B H 0.4025 0.2130 0.6781 0.047 Uiso 1 1 calc R . . C37 C 0.2761(5) 0.1391(5) 0.6281(4) 0.0460(13) Uani 1 1 d . . . H37A H 0.2332 0.1600 0.5784 0.069 Uiso 1 1 calc R . . H37B H 0.2154 0.1312 0.6906 0.069 Uiso 1 1 calc R . . H37C H 0.3231 0.0657 0.6166 0.069 Uiso 1 1 calc R . . N1 N 0.3119(3) 0.5120(3) 0.2187(3) 0.0215(7) Uani 1 1 d . . . O2 O 0.8972(3) 0.5199(3) 0.1088(2) 0.0339(8) Uani 1 1 d . . . H2 H 0.9687 0.5269 0.0722 0.051 Uiso 1 1 calc R B . O1 O 0.8722(3) 0.4412(3) -0.0157(2) 0.0357(8) Uani 1 1 d . . . O4 O 0.4532(3) 0.2400(3) 0.5366(2) 0.0368(8) Uani 1 1 d . . . P1 P 0.19692(9) 0.30966(9) 0.29499(7) 0.0181(2) Uani 1 1 d . . . P2 P 0.28627(9) 0.74951(9) 0.22978(7) 0.0183(2) Uani 1 1 d . . . Cl1 Cl 0.09921(10) 0.43561(10) 0.58938(7) 0.0281(2) Uani 1 1 d . . . Cl2 Cl 0.67803(10) 0.82792(12) 0.06208(8) 0.0364(3) Uani 1 1 d . . . Au1 Au 0.149215(13) 0.368471(13) 0.441028(11) 0.01945(6) Uani 1 1 d . B . Au2 Au 0.480297(13) 0.784855(14) 0.146534(11) 0.02143(6) Uani 1 1 d . B . H3' H 0.811(10) 0.558(9) 0.204(7) 0.032 Uiso 0.50 1 d P E 3 H3 H 0.751(10) 0.377(9) -0.026(7) 0.032 Uiso 0.50 1 d P F 3 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 0.0170(19) 0.020(2) 0.024(2) -0.0018(16) -0.0060(16) -0.0014(16) C2 0.018(2) 0.022(2) 0.022(2) -0.0012(16) -0.0040(16) -0.0017(16) C3 0.0160(19) 0.019(2) 0.021(2) 0.0034(16) -0.0021(15) -0.0003(15) C4 0.019(2) 0.029(2) 0.020(2) -0.0025(17) -0.0052(16) 0.0045(17) C5 0.018(2) 0.032(2) 0.024(2) -0.0027(17) -0.0091(17) -0.0038(17) O3' 0.027(3) 0.047(4) 0.041(4) -0.017(3) -0.012(3) 0.002(3) C6 0.020(2) 0.021(2) 0.026(2) 0.0019(17) -0.0055(17) 0.0011(16) C7 0.023(2) 0.020(2) 0.024(2) -0.0027(17) -0.0009(17) 0.0000(17) O3 0.018(3) 0.027(3) 0.023(3) -0.012(2) 0.001(2) -0.001(2) C8 0.019(2) 0.022(2) 0.025(2) -0.0002(17) -0.0042(16) -0.0033(16) C9 0.022(2) 0.020(2) 0.029(2) 0.0040(17) -0.0087(18) 0.0025(17) C10 0.0161(19) 0.023(2) 0.019(2) -0.0021(16) -0.0038(15) -0.0044(16) C11 0.020(2) 0.023(2) 0.031(2) -0.0062(18) -0.0053(17) 0.0013(17) C12 0.016(2) 0.030(3) 0.043(3) -0.010(2) -0.0036(18) -0.0042(18) C13 0.024(2) 0.034(3) 0.033(3) -0.004(2) -0.0096(19) -0.0083(19) C14 0.021(2) 0.035(3) 0.043(3) 0.002(2) -0.014(2) -0.0017(19) C15 0.022(2) 0.023(2) 0.040(3) 0.0017(19) -0.0104(19) -0.0032(18) C16 0.0166(19) 0.017(2) 0.026(2) -0.0008(16) -0.0050(16) -0.0046(15) C17 0.019(2) 0.026(2) 0.023(2) -0.0033(17) -0.0058(16) -0.0016(17) C18 0.022(2) 0.025(2) 0.034(3) -0.0063(19) -0.0008(18) -0.0038(18) C19 0.014(2) 0.029(3) 0.055(3) -0.007(2) -0.005(2) -0.0016(18) C20 0.023(2) 0.032(3) 0.045(3) -0.007(2) -0.017(2) 0.0006(19) C21 0.023(2) 0.026(2) 0.027(2) -0.0042(17) -0.0091(17) -0.0047(17) C22 0.0110(17) 0.020(2) 0.019(2) -0.0031(15) -0.0060(15) 0.0030(15) C23 0.018(2) 0.035(3) 0.027(2) 0.0070(19) -0.0004(17) -0.0019(18) C24 0.031(3) 0.053(3) 0.028(3) 0.009(2) -0.007(2) 0.005(2) C25 0.030(2) 0.040(3) 0.033(3) -0.001(2) -0.017(2) 0.006(2) C26 0.021(2) 0.024(2) 0.033(2) -0.0059(18) -0.0099(18) 0.0016(17) C27 0.020(2) 0.020(2) 0.026(2) -0.0008(16) -0.0060(17) -0.0020(16) C28 0.021(2) 0.020(2) 0.022(2) -0.0019(16) -0.0049(16) -0.0011(16) C29 0.026(2) 0.025(2) 0.028(2) -0.0049(18) -0.0040(18) -0.0048(18) C30 0.026(2) 0.035(3) 0.029(3) -0.006(2) 0.0036(19) -0.006(2) C31 0.040(3) 0.030(3) 0.025(2) -0.0080(19) -0.003(2) -0.005(2) C32 0.035(3) 0.030(3) 0.026(2) -0.0070(19) -0.0089(19) -0.010(2) C33 0.025(2) 0.022(2) 0.027(2) -0.0001(17) -0.0066(17) -0.0064(17) C34 0.055(3) 0.037(3) 0.050(3) -0.006(2) -0.027(3) -0.003(3) C35 0.046(3) 0.045(3) 0.062(4) 0.003(3) -0.020(3) -0.008(3) C36 0.041(3) 0.041(3) 0.038(3) -0.010(2) -0.015(2) 0.006(2) C37 0.049(3) 0.041(3) 0.045(3) -0.007(2) -0.007(3) 0.000(3) N1 0.0159(16) 0.0185(18) 0.0284(19) -0.0015(14) -0.0037(14) -0.0011(14) O2 0.0170(15) 0.050(2) 0.0334(19) -0.0006(15) -0.0052(13) -0.0077(15) O1 0.0244(16) 0.039(2) 0.038(2) -0.0098(15) 0.0036(14) -0.0048(14) O4 0.044(2) 0.035(2) 0.037(2) -0.0076(15) -0.0178(16) -0.0049(16) P1 0.0160(5) 0.0180(5) 0.0211(5) -0.0022(4) -0.0060(4) -0.0014(4) P2 0.0151(5) 0.0191(5) 0.0199(5) -0.0015(4) -0.0029(4) -0.0022(4) Cl1 0.0297(5) 0.0325(6) 0.0219(5) -0.0065(4) -0.0043(4) -0.0043(4) Cl2 0.0166(5) 0.0589(8) 0.0307(6) 0.0015(5) -0.0018(4) -0.0099(5) Au1 0.01910(9) 0.01934(10) 0.01964(10) -0.00148(6) -0.00429(6) -0.00355(6) Au2 0.01448(9) 0.02722(10) 0.02138(10) -0.00040(7) -0.00296(6) -0.00368(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 C1 N1 1.452(5) . ? C1 P1 1.861(4) . ? C2 N1 1.456(5) . ? C2 P2 1.862(4) . ? C3 C8 1.394(6) . ? C3 N1 1.395(5) . ? C3 C4 1.407(6) . ? C4 C5 1.382(6) . ? C5 C6 1.382(6) . ? C6 C7 1.414(6) . ? C6 C9 1.455(6) . ? C7 C8 1.376(6) . ? C9 O1 1.264(5) . ? C9 O2 1.280(5) . ? C10 C11 1.394(6) . ? C10 C15 1.403(6) . ? C10 P1 1.816(4) . ? C11 C12 1.388(6) . ? C12 C13 1.387(6) . ? C13 C14 1.380(7) . ? C14 C15 1.383(6) . ? C16 C21 1.393(6) . ? C16 C17 1.398(6) . ? C16 P1 1.814(4) . ? C17 C18 1.389(6) . ? C18 C19 1.388(7) . ? C19 C20 1.388(7) . ? C20 C21 1.388(6) . ? C22 C23 1.374(6) . ? C22 C27 1.415(6) . ? C22 P2 1.818(4) . ? C23 C24 1.387(7) . ? C24 C25 1.383(7) . ? C25 C26 1.390(7) . ? C26 C27 1.385(6) . ? C28 C33 1.395(6) . ? C28 C29 1.398(6) . ? C28 P2 1.812(4) 2_566 ? C29 C30 1.386(6) . ? C30 C31 1.383(7) . ? C31 C32 1.389(7) . ? C32 C33 1.385(6) . ? C34 O4 1.425(6) . ? C34 C35 1.504(8) . ? C36 O4 1.421(6) . ? C36 C37 1.497(8) . ? P1 Au1 2.2341(12) . ? P2 C28 1.812(4) 2_566 ? P2 Au2 2.2345(13) . ? Cl1 Au1 2.3045(12) . ? Cl2 Au2 2.2931(13) . ? 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 C1 P1 111.4(3) . . ? N1 C2 P2 113.5(3) . . ? C8 C3 N1 121.4(4) . . ? C8 C3 C4 118.5(4) . . ? N1 C3 C4 120.1(4) . . ? C5 C4 C3 120.1(4) . . ? C6 C5 C4 122.1(4) . . ? C5 C6 C7 117.0(4) . . ? C5 C6 C9 121.7(4) . . ? C7 C6 C9 121.1(4) . . ? C8 C7 C6 121.7(4) . . ? C7 C8 C3 120.3(4) . . ? O1 C9 O2 122.3(4) . . ? O1 C9 C6 119.8(4) . . ? O2 C9 C6 117.9(4) . . ? C11 C10 C15 119.7(4) . . ? C11 C10 P1 122.0(3) . . ? C15 C10 P1 118.3(3) . . ? C12 C11 C10 119.8(4) . . ? C13 C12 C11 120.2(4) . . ? C14 C13 C12 120.1(4) . . ? C13 C14 C15 120.6(4) . . ? C14 C15 C10 119.6(4) . . ? C21 C16 C17 120.1(4) . . ? C21 C16 P1 120.1(3) . . ? C17 C16 P1 119.8(3) . . ? C18 C17 C16 120.2(4) . . ? C17 C18 C19 119.2(4) . . ? C20 C19 C18 120.8(4) . . ? C19 C20 C21 120.2(4) . . ? C20 C21 C16 119.5(4) . . ? C23 C22 C27 119.1(4) . . ? C23 C22 P2 118.7(3) . . ? C27 C22 P2 122.1(3) . . ? C22 C23 C24 120.8(4) . . ? C25 C24 C23 120.2(5) . . ? C24 C25 C26 119.9(4) . . ? C27 C26 C25 120.0(4) . . ? C26 C27 C22 119.9(4) . . ? C33 C28 C29 119.1(4) . . ? C33 C28 P2 119.8(3) . 2_566 ? C29 C28 P2 121.0(3) . 2_566 ? C30 C29 C28 120.2(4) . . ? C31 C30 C29 120.3(4) . . ? C30 C31 C32 119.7(4) . . ? C33 C32 C31 120.4(4) . . ? C32 C33 C28 120.2(4) . . ? O4 C34 C35 109.8(5) . . ? O4 C36 C37 109.5(4) . . ? C3 N1 C1 121.9(3) . . ? C3 N1 C2 120.6(3) . . ? C1 N1 C2 116.4(3) . . ? C36 O4 C34 111.1(4) . . ? C16 P1 C10 106.49(19) . . ? C16 P1 C1 103.56(19) . . ? C10 P1 C1 104.01(19) . . ? C16 P1 Au1 116.21(14) . . ? C10 P1 Au1 115.05(13) . . ? C1 P1 Au1 110.25(14) . . ? C28 P2 C22 108.17(19) 2_566 . ? C28 P2 C2 100.04(19) 2_566 . ? C22 P2 C2 107.04(19) . . ? C28 P2 Au2 113.25(14) 2_566 . ? C22 P2 Au2 112.48(13) . . ? C2 P2 Au2 114.92(14) . . ? P1 Au1 Cl1 178.01(4) . . ? P2 Au2 Cl2 177.96(4) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.696 _refine_diff_density_min -2.074 _refine_diff_density_rms 0.150 #===END data_6b _database_code_depnum_ccdc_archive 'CCDC 289359' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H29 Au2 Cl2 N O3 P2, 0.32(C H4 O)' _chemical_formula_sum 'C33.32 H30.28 Au2 Cl2 N O3.32 P2' _chemical_formula_weight 1024.60 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.0711(2) _cell_length_b 17.7756(4) _cell_length_c 19.7048(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.616(1) _cell_angle_gamma 90.00 _cell_volume 3455.30(14) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 23906 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 26.00 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.961 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1943 _exptl_absorpt_coefficient_mu 8.763 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3532 _exptl_absorpt_correction_T_max 0.6684 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius Kappa CCD Area detector' _diffrn_measurement_method '\f and \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23906 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_sigmaI/netI 0.0804 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6733 _reflns_number_gt 4875 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHEXTL and local programs' _computing_publication_material 'Bruker SHEXTL and local programs' _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^)+(0.0209P)^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 6733 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0688 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.19782(2) 0.180250(16) 0.364999(14) 0.02397(9) Uani 1 1 d . . . Au2 Au 0.10444(2) 0.309412(16) 0.470677(13) 0.02292(9) Uani 1 1 d . . . Cl1 Cl 0.04422(17) 0.09207(11) 0.38314(9) 0.0358(5) Uani 1 1 d . . . Cl2 Cl -0.08138(15) 0.35575(11) 0.39390(9) 0.0287(4) Uani 1 1 d . . . P1 P 0.35728(16) 0.25935(11) 0.34504(9) 0.0224(4) Uani 1 1 d . . . P2 P 0.28236(16) 0.27331(11) 0.55061(9) 0.0212(4) Uani 1 1 d . . . O1 O 0.7621(4) 0.5260(3) 0.5591(2) 0.0310(12) Uani 1 1 d . . . O2 O 0.9731(4) 0.4823(3) 0.6004(3) 0.0357(13) Uani 1 1 d . . . H2 H 0.9897 0.5285 0.6062 0.04(3) Uiso 1 1 calc R . . O3 O 0.5742(4) 0.4300(3) 0.5073(2) 0.0269(12) Uani 1 1 d . . . H3 H 0.6082 0.4724 0.5185 0.004(17) Uiso 1 1 calc R . . N1 N 0.4983(5) 0.2811(3) 0.4804(3) 0.0216(14) Uani 1 1 d . . . C1 C 0.4292(6) 0.3202(4) 0.4189(3) 0.0235(17) Uani 1 1 d . . . H1A H 0.4939 0.3555 0.4041 0.028 Uiso 1 1 calc R . . H1B H 0.3551 0.3505 0.4312 0.028 Uiso 1 1 calc R . . C2 C 0.4232(6) 0.2296(4) 0.5162(3) 0.0243(17) Uani 1 1 d . . . H2A H 0.4874 0.2063 0.5553 0.029 Uiso 1 1 calc R . . H2B H 0.3854 0.1888 0.4838 0.029 Uiso 1 1 calc R . . C3 C 0.6310(6) 0.3011(4) 0.5142(3) 0.0204(16) Uani 1 1 d . . . C4 C 0.6687(6) 0.3759(4) 0.5277(3) 0.0217(17) Uani 1 1 d . . . C5 C 0.8024(6) 0.3935(4) 0.5606(3) 0.0228(17) Uani 1 1 d . . . C6 C 0.8934(6) 0.3358(4) 0.5838(3) 0.0254(18) Uani 1 1 d . . . H6 H 0.9826 0.3475 0.6077 0.030 Uiso 1 1 calc R . . C7 C 0.8550(6) 0.2618(4) 0.5725(4) 0.0283(18) Uani 1 1 d . . . H7 H 0.9166 0.2225 0.5895 0.034 Uiso 1 1 calc R . . C8 C 0.7260(7) 0.2451(4) 0.5360(3) 0.0259(17) Uani 1 1 d . . . H8 H 0.7019 0.1941 0.5257 0.031 Uiso 1 1 calc R . . C9 C 0.8400(6) 0.4727(4) 0.5731(3) 0.0249(17) Uani 1 1 d . . . C10 C 0.2922(6) 0.3268(4) 0.2763(3) 0.0211(16) Uani 1 1 d . . . C11 C 0.1665(8) 0.3592(6) 0.2756(4) 0.062(3) Uani 1 1 d . . . H11 H 0.1137 0.3431 0.3078 0.074 Uiso 1 1 calc R . . C12 C 0.1190(9) 0.4141(7) 0.2287(5) 0.083(4) Uani 1 1 d . . . H12 H 0.0324 0.4355 0.2281 0.100 Uiso 1 1 calc R . . C13 C 0.1951(8) 0.4392(5) 0.1818(4) 0.048(2) Uani 1 1 d . . . H13 H 0.1623 0.4782 0.1498 0.058 Uiso 1 1 calc R . . C14 C 0.3170(7) 0.4069(4) 0.1827(4) 0.0321(19) Uani 1 1 d . . . H14 H 0.3684 0.4223 0.1496 0.039 Uiso 1 1 calc R . . C15 C 0.3689(7) 0.3519(4) 0.2305(4) 0.0274(18) Uani 1 1 d . . . H15 H 0.4567 0.3317 0.2316 0.033 Uiso 1 1 calc R . . C20 C 0.4993(6) 0.2113(4) 0.3206(3) 0.0238(17) Uani 1 1 d . . . C21 C 0.4728(7) 0.1486(5) 0.2781(4) 0.036(2) Uani 1 1 d . . . H21 H 0.3823 0.1312 0.2637 0.043 Uiso 1 1 calc R . . C22 C 0.5786(7) 0.1112(5) 0.2566(4) 0.041(2) Uani 1 1 d . . . H22 H 0.5595 0.0705 0.2248 0.049 Uiso 1 1 calc R . . C23 C 0.7096(7) 0.1326(4) 0.2809(3) 0.0271(18) Uani 1 1 d . . . H23 H 0.7818 0.1051 0.2682 0.033 Uiso 1 1 calc R . . C24 C 0.7371(7) 0.1943(4) 0.3237(4) 0.0320(19) Uani 1 1 d . . . H24 H 0.8282 0.2097 0.3402 0.038 Uiso 1 1 calc R . . C25 C 0.6308(7) 0.2340(4) 0.3429(4) 0.0312(19) Uani 1 1 d . . . H25 H 0.6499 0.2772 0.3716 0.037 Uiso 1 1 calc R . . C30 C 0.3608(6) 0.3493(4) 0.6059(3) 0.0214(16) Uani 1 1 d . . . C31 C 0.4867(6) 0.3406(4) 0.6492(3) 0.0246(17) Uani 1 1 d . . . H31 H 0.5309 0.2931 0.6527 0.030 Uiso 1 1 calc R . . C32 C 0.5478(7) 0.4008(5) 0.6872(3) 0.033(2) Uani 1 1 d . . . H32 H 0.6345 0.3953 0.7166 0.040 Uiso 1 1 calc R . . C33 C 0.4815(7) 0.4692(5) 0.6821(4) 0.034(2) Uani 1 1 d . . . H33 H 0.5237 0.5107 0.7082 0.041 Uiso 1 1 calc R . . C34 C 0.3566(7) 0.4784(5) 0.6404(3) 0.0316(19) Uani 1 1 d . . . H34 H 0.3127 0.5260 0.6372 0.038 Uiso 1 1 calc R . . C35 C 0.2950(7) 0.4175(4) 0.6028(3) 0.0253(17) Uani 1 1 d . . . H35 H 0.2069 0.4229 0.5749 0.030 Uiso 1 1 calc R . . C40 C 0.2380(6) 0.1985(4) 0.6039(3) 0.0228(17) Uani 1 1 d . . . C41 C 0.2772(8) 0.1964(5) 0.6753(4) 0.040(2) Uani 1 1 d . . . H41 H 0.3263 0.2372 0.6995 0.048 Uiso 1 1 calc R . . C42 C 0.2442(8) 0.1336(5) 0.7121(4) 0.042(2) Uani 1 1 d . . . H42 H 0.2722 0.1318 0.7610 0.051 Uiso 1 1 calc R . . C43 C 0.1722(7) 0.0753(5) 0.6777(4) 0.036(2) Uani 1 1 d . . . H43 H 0.1513 0.0328 0.7028 0.043 Uiso 1 1 calc R . . C44 C 0.1295(8) 0.0780(5) 0.6064(4) 0.044(2) Uani 1 1 d . . . H44 H 0.0778 0.0377 0.5828 0.052 Uiso 1 1 calc R . . C45 C 0.1618(7) 0.1390(5) 0.5695(4) 0.037(2) Uani 1 1 d . . . H45 H 0.1321 0.1406 0.5206 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.02351(15) 0.0251(2) 0.02293(17) -0.00135(13) 0.00369(11) -0.00729(12) Au2 0.02133(14) 0.0254(2) 0.02073(16) 0.00257(13) 0.00119(11) -0.00385(11) Cl1 0.0353(10) 0.0362(14) 0.0356(11) 0.0002(10) 0.0059(8) -0.0166(8) Cl2 0.0229(8) 0.0293(12) 0.0305(10) 0.0032(9) -0.0024(7) -0.0043(7) P1 0.0222(9) 0.0232(12) 0.0218(10) 0.0006(9) 0.0042(7) -0.0038(8) P2 0.0227(9) 0.0209(12) 0.0197(10) 0.0023(9) 0.0035(7) -0.0040(7) O1 0.032(3) 0.019(3) 0.039(3) 0.001(3) 0.000(2) 0.000(2) O2 0.022(3) 0.028(4) 0.052(4) 0.004(3) -0.004(2) -0.006(2) O3 0.021(2) 0.022(3) 0.037(3) -0.003(3) 0.005(2) 0.000(2) N1 0.018(3) 0.021(4) 0.025(3) 0.007(3) 0.003(2) -0.005(2) C1 0.028(4) 0.019(5) 0.026(4) 0.008(3) 0.011(3) -0.001(3) C2 0.028(4) 0.028(5) 0.016(4) 0.000(3) 0.004(3) -0.004(3) C3 0.023(3) 0.018(5) 0.022(4) 0.005(3) 0.012(3) 0.000(3) C4 0.029(4) 0.024(5) 0.015(4) 0.001(3) 0.010(3) 0.009(3) C5 0.018(3) 0.019(5) 0.032(4) 0.002(3) 0.006(3) -0.004(3) C6 0.021(4) 0.030(5) 0.023(4) 0.006(4) 0.001(3) 0.002(3) C7 0.028(4) 0.023(5) 0.033(5) 0.006(4) 0.005(3) 0.010(3) C8 0.035(4) 0.014(4) 0.027(4) 0.001(3) 0.005(3) 0.001(3) C9 0.025(4) 0.020(5) 0.026(4) 0.007(3) -0.003(3) -0.008(3) C10 0.024(4) 0.020(5) 0.017(4) -0.001(3) -0.001(3) -0.002(3) C11 0.045(5) 0.098(9) 0.051(6) 0.050(6) 0.030(4) 0.025(5) C12 0.048(6) 0.125(11) 0.086(8) 0.066(8) 0.037(5) 0.050(6) C13 0.049(5) 0.049(7) 0.049(6) 0.023(5) 0.017(4) 0.010(4) C14 0.031(4) 0.036(6) 0.030(4) 0.003(4) 0.008(3) -0.009(4) C15 0.022(4) 0.029(5) 0.030(4) 0.000(4) 0.002(3) 0.001(3) C20 0.031(4) 0.015(4) 0.023(4) -0.003(3) 0.001(3) 0.000(3) C21 0.024(4) 0.040(6) 0.042(5) -0.003(4) 0.003(3) 0.001(4) C22 0.044(5) 0.045(6) 0.030(5) -0.015(4) -0.001(4) 0.006(4) C23 0.029(4) 0.026(5) 0.027(4) -0.001(4) 0.007(3) 0.008(3) C24 0.026(4) 0.029(5) 0.039(5) -0.003(4) 0.003(3) -0.004(3) C25 0.034(4) 0.025(5) 0.036(5) -0.006(4) 0.012(3) -0.005(3) C30 0.029(4) 0.019(5) 0.018(4) -0.001(3) 0.009(3) -0.002(3) C31 0.030(4) 0.026(5) 0.019(4) -0.002(4) 0.009(3) 0.004(3) C32 0.029(4) 0.052(6) 0.017(4) -0.001(4) 0.003(3) -0.005(4) C33 0.039(5) 0.038(6) 0.028(5) -0.014(4) 0.012(3) -0.019(4) C34 0.046(5) 0.028(5) 0.019(4) 0.000(4) 0.003(3) -0.003(4) C35 0.031(4) 0.024(5) 0.021(4) 0.001(4) 0.005(3) -0.005(3) C40 0.016(3) 0.029(5) 0.024(4) 0.006(4) 0.005(3) 0.000(3) C41 0.058(5) 0.034(6) 0.026(5) -0.007(4) 0.003(4) -0.017(4) C42 0.053(5) 0.044(6) 0.028(5) 0.005(4) 0.004(4) -0.017(4) C43 0.043(4) 0.027(5) 0.042(5) 0.017(4) 0.021(4) 0.002(4) C44 0.049(5) 0.042(6) 0.043(5) -0.004(5) 0.018(4) -0.023(4) C45 0.053(5) 0.030(6) 0.031(5) 0.006(4) 0.012(4) -0.017(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.2282(18) . ? Au1 Cl1 2.2805(18) . ? Au1 Au2 3.3587(4) . ? Au2 P2 2.2286(17) . ? Au2 Cl2 2.3086(16) . ? P1 C20 1.813(7) . ? P1 C10 1.828(7) . ? P1 C1 1.841(7) . ? P2 C40 1.805(7) . ? P2 C30 1.814(7) . ? P2 C2 1.861(7) . ? O1 C9 1.226(8) . ? O2 C9 1.350(7) . ? O2 H2 0.8400 . ? O3 C4 1.355(8) . ? O3 H3 0.8400 . ? N1 C3 1.413(8) . ? N1 C1 1.446(8) . ? N1 C2 1.458(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.387(9) . ? C3 C4 1.395(9) . ? C4 C5 1.406(9) . ? C5 C6 1.390(9) . ? C5 C9 1.466(9) . ? C6 C7 1.376(10) . ? C6 H6 0.9500 . ? C7 C8 1.385(9) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C10 C15 1.376(9) . ? C10 C11 1.388(10) . ? C11 C12 1.363(12) . ? C11 H11 0.9500 . ? C12 C13 1.388(12) . ? C12 H12 0.9500 . ? C13 C14 1.353(10) . ? C13 H13 0.9500 . ? C14 C15 1.385(10) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C20 C25 1.370(9) . ? C20 C21 1.386(10) . ? C21 C22 1.394(10) . ? C21 H21 0.9500 . ? C22 C23 1.364(9) . ? C22 H22 0.9500 . ? C23 C24 1.377(10) . ? C23 H23 0.9500 . ? C24 C25 1.396(10) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C30 C35 1.378(9) . ? C30 C31 1.387(9) . ? C31 C32 1.378(10) . ? C31 H31 0.9500 . ? C32 C33 1.380(11) . ? C32 H32 0.9500 . ? C33 C34 1.367(9) . ? C33 H33 0.9500 . ? C34 C35 1.385(10) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C40 C41 1.384(9) . ? C40 C45 1.400(10) . ? C41 C42 1.406(11) . ? C41 H41 0.9500 . ? C42 C43 1.364(10) . ? C42 H42 0.9500 . ? C43 C44 1.386(10) . ? C43 H43 0.9500 . ? C44 C45 1.380(10) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 175.68(7) . . ? P1 Au1 Au2 88.84(5) . . ? Cl1 Au1 Au2 95.12(5) . . ? P2 Au2 Cl2 175.02(7) . . ? P2 Au2 Au1 87.46(5) . . ? Cl2 Au2 Au1 97.40(5) . . ? C20 P1 C10 107.2(3) . . ? C20 P1 C1 106.3(3) . . ? C10 P1 C1 103.1(3) . . ? C20 P1 Au1 112.6(2) . . ? C10 P1 Au1 112.4(2) . . ? C1 P1 Au1 114.5(2) . . ? C40 P2 C30 109.1(3) . . ? C40 P2 C2 101.6(3) . . ? C30 P2 C2 104.9(3) . . ? C40 P2 Au2 111.4(2) . . ? C30 P2 Au2 113.6(2) . . ? C2 P2 Au2 115.2(2) . . ? C9 O2 H2 109.5 . . ? C4 O3 H3 109.5 . . ? C3 N1 C1 121.6(5) . . ? C3 N1 C2 117.5(5) . . ? C1 N1 C2 119.9(5) . . ? N1 C1 P1 115.3(5) . . ? N1 C1 H1A 108.5 . . ? P1 C1 H1A 108.5 . . ? N1 C1 H1B 108.5 . . ? P1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? N1 C2 P2 115.0(5) . . ? N1 C2 H2A 108.5 . . ? P2 C2 H2A 108.5 . . ? N1 C2 H2B 108.5 . . ? P2 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? C8 C3 C4 118.7(6) . . ? C8 C3 N1 119.6(6) . . ? C4 C3 N1 121.7(6) . . ? O3 C4 C3 118.1(6) . . ? O3 C4 C5 122.0(7) . . ? C3 C4 C5 119.9(6) . . ? C6 C5 C4 119.7(7) . . ? C6 C5 C9 121.4(6) . . ? C4 C5 C9 118.8(6) . . ? C7 C6 C5 120.4(6) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 119.5(6) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C7 C8 C3 121.6(7) . . ? C7 C8 H8 119.2 . . ? C3 C8 H8 119.2 . . ? O1 C9 O2 122.1(7) . . ? O1 C9 C5 124.9(6) . . ? O2 C9 C5 113.0(6) . . ? C15 C10 C11 119.4(7) . . ? C15 C10 P1 122.3(5) . . ? C11 C10 P1 118.0(5) . . ? C12 C11 C10 119.9(7) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 121.1(8) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C14 C13 C12 118.5(8) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C13 C14 C15 121.7(7) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C10 C15 C14 119.4(6) . . ? C10 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C25 C20 C21 119.1(6) . . ? C25 C20 P1 122.7(6) . . ? C21 C20 P1 118.2(5) . . ? C20 C21 C22 120.1(7) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 120.3(7) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 119.9(7) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C25 119.9(6) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C20 C25 C24 120.5(7) . . ? C20 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C35 C30 C31 119.8(6) . . ? C35 C30 P2 118.8(5) . . ? C31 C30 P2 121.4(5) . . ? C32 C31 C30 120.1(7) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 119.2(6) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C34 C33 C32 121.5(7) . . ? C34 C33 H33 119.3 . . ? C32 C33 H33 119.3 . . ? C33 C34 C35 119.1(7) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C30 C35 C34 120.3(6) . . ? C30 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C41 C40 C45 119.2(7) . . ? C41 C40 P2 124.0(6) . . ? C45 C40 P2 116.8(5) . . ? C40 C41 C42 119.8(7) . . ? C40 C41 H41 120.1 . . ? C42 C41 H41 120.1 . . ? C43 C42 C41 120.3(7) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 120.2(7) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C45 C44 C43 120.2(7) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C44 C45 C40 120.3(7) . . ? C44 C45 H45 119.9 . . ? C40 C45 H45 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Au1 Au2 Cl2 -81.29(6) . . . . ? P1 Au1 Au2 P2 -78.45(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 Cl2 0.84 2.26 3.072(6) 164 3_666 O3 H3 O1 0.84 1.86 2.599(7) 147 . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.119 _refine_diff_density_min -0.793 _refine_diff_density_rms 0.176 #== END data_6d _database_code_depnum_ccdc_archive 'CCDC 289360' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H29 Au2 Cl2 N O3 P2' _chemical_formula_weight 1014.35 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' 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' _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 14.4668(5) _cell_length_b 10.6327(4) _cell_length_c 20.9068(12) _cell_angle_alpha 90.00 _cell_angle_beta 95.0540(16) _cell_angle_gamma 90.00 _cell_volume 3203.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16743 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 25.05 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.103 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 9.451 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6494 _exptl_absorpt_correction_T_max 0.7647 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius Kappa CCD Area detector' _diffrn_measurement_method '\f and \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16743 _diffrn_reflns_av_R_equivalents 0.1041 _diffrn_reflns_av_sigmaI/netI 0.1608 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5555 _reflns_number_gt 2715 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHEXTL and local programs' _computing_publication_material 'Bruker SHEXTL and local programs' _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^)+(0.0001P)^2^+10.0000P] 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 5555 _refine_ls_number_parameters 346 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.1616 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.0987 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.155 _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 0.14847(4) 0.16901(4) 0.46915(4) 0.0489(2) Uani 1 1 d U . . Au2 Au 0.32117(4) 0.28264(5) 0.54879(4) 0.0615(3) Uani 1 1 d U . . P1 P 0.1358(3) 0.2948(3) 0.3830(2) 0.0411(12) Uani 1 1 d . . . P2 P 0.2444(3) 0.4561(3) 0.5736(2) 0.0420(12) Uani 1 1 d . . . Cl1 Cl 0.1422(3) 0.0328(3) 0.5546(2) 0.0753(15) Uani 1 1 d U . . Cl2 Cl 0.4136(3) 0.1137(3) 0.5326(3) 0.115(2) Uani 1 1 d U . . O1 O 0.0276(6) 0.6977(7) 0.4564(5) 0.046(3) Uani 1 1 d . . . O2 O 0.0525(6) 0.8728(7) 0.4012(5) 0.059(3) Uani 1 1 d . . . H2 H -0.0044 0.8843 0.4044 0.088 Uiso 1 1 calc R . . O3 O 0.3848(6) 0.9216(7) 0.3916(5) 0.063(3) Uani 1 1 d U . . H3 H 0.4406 0.8999 0.3922 0.095 Uiso 1 1 calc R . . N1 N 0.1672(7) 0.5073(8) 0.4516(6) 0.030(3) Uani 1 1 d U . . C1 C 0.1013(9) 0.4561(10) 0.4032(7) 0.038(4) Uani 1 1 d . . . H1A H 0.0985 0.5095 0.3643 0.046 Uiso 1 1 calc R . . H1B H 0.0388 0.4548 0.4191 0.046 Uiso 1 1 calc R . . C2 C 0.1453(9) 0.4968(10) 0.5173(7) 0.034(4) Uani 1 1 d U . . H2A H 0.0967 0.4319 0.5198 0.040 Uiso 1 1 calc R . . H2B H 0.1193 0.5779 0.5306 0.040 Uiso 1 1 calc R . . C3 C 0.2189(10) 0.6193(10) 0.4345(6) 0.030(4) Uani 1 1 d U . . C4 C 0.1811(9) 0.7377(10) 0.4229(7) 0.030(4) Uani 1 1 d . . . C5 C 0.2368(10) 0.8353(11) 0.4074(7) 0.050(5) Uani 1 1 d . . . H5 H 0.2104 0.9153 0.3969 0.060 Uiso 1 1 calc R . . C6 C 0.3309(10) 0.8178(12) 0.4071(7) 0.041(4) Uani 1 1 d U . . C7 C 0.3726(10) 0.7002(10) 0.4181(7) 0.042(4) Uani 1 1 d . . . H7 H 0.4374 0.6878 0.4169 0.050 Uiso 1 1 calc R . . C8 C 0.3133(10) 0.6029(10) 0.4308(6) 0.033(4) Uani 1 1 d . . . H8 H 0.3385 0.5209 0.4372 0.039 Uiso 1 1 calc R . . C9 C 0.0780(11) 0.7640(12) 0.4279(8) 0.046(5) Uani 1 1 d . . . C10 C 0.2355(9) 0.3074(10) 0.3393(7) 0.030(4) Uani 1 1 d U . . C11 C 0.2541(10) 0.4097(12) 0.3018(8) 0.047(5) Uani 1 1 d . . . H11 H 0.2170 0.4830 0.3041 0.056 Uiso 1 1 calc R . . C12 C 0.3242(11) 0.4101(14) 0.2610(8) 0.056(5) Uani 1 1 d . . . H12 H 0.3347 0.4824 0.2359 0.068 Uiso 1 1 calc R . . C13 C 0.3790(11) 0.3043(16) 0.2570(8) 0.059(5) Uani 1 1 d . . . H13 H 0.4278 0.3032 0.2294 0.071 Uiso 1 1 calc R . . C14 C 0.3621(10) 0.2012(14) 0.2933(9) 0.059(5) Uani 1 1 d . . . H14 H 0.3987 0.1278 0.2898 0.070 Uiso 1 1 calc R . . C15 C 0.2917(10) 0.2014(11) 0.3356(8) 0.049(5) Uani 1 1 d . . . H15 H 0.2825 0.1299 0.3615 0.058 Uiso 1 1 calc R . . C20 C 0.0431(11) 0.2395(12) 0.3273(10) 0.050(5) Uani 1 1 d . . . C21 C 0.0481(12) 0.2535(16) 0.2624(11) 0.081(7) Uani 1 1 d . . . H21 H 0.1018 0.2907 0.2473 0.097 Uiso 1 1 calc R . . C22 C -0.0245(17) 0.2141(19) 0.2178(11) 0.116(8) Uani 1 1 d U . . H22 H -0.0249 0.2305 0.1731 0.139 Uiso 1 1 calc R . . C23 C -0.0966(17) 0.1483(19) 0.2444(13) 0.112(8) Uani 1 1 d U . . H23 H -0.1418 0.1078 0.2157 0.134 Uiso 1 1 calc R . . C24 C -0.1055(13) 0.1393(15) 0.3064(11) 0.081(7) Uani 1 1 d . . . H24 H -0.1604 0.1068 0.3221 0.097 Uiso 1 1 calc R . . C25 C -0.0317(11) 0.1791(12) 0.3475(8) 0.051(5) Uani 1 1 d . . . H25 H -0.0332 0.1635 0.3922 0.062 Uiso 1 1 calc R . . C30 C 0.1899(9) 0.4364(13) 0.6487(5) 0.074(5) Uiso 1 1 d G . . C31 C 0.1950(9) 0.5399(10) 0.6895(7) 0.114(7) Uiso 1 1 d G . . H31 H 0.2234 0.6155 0.6769 0.137 Uiso 1 1 calc R . . C32 C 0.1586(10) 0.5329(11) 0.7487(6) 0.160(10) Uiso 1 1 d G . . H32 H 0.1621 0.6036 0.7766 0.191 Uiso 1 1 calc R . . C33 C 0.1170(9) 0.4223(15) 0.7672(5) 0.126(8) Uiso 1 1 d G . . H33 H 0.0921 0.4175 0.8077 0.151 Uiso 1 1 calc R . . C34 C 0.1119(9) 0.3189(11) 0.7264(7) 0.132(8) Uiso 1 1 d G . . H34 H 0.0835 0.2433 0.7390 0.159 Uiso 1 1 calc R . . C35 C 0.1483(10) 0.3259(10) 0.6672(6) 0.152(10) Uiso 1 1 d G . . H35 H 0.1448 0.2552 0.6393 0.182 Uiso 1 1 calc R . . C41 C 0.2862(11) 0.7107(13) 0.5780(7) 0.053(5) Uani 1 1 d . . . H41 H 0.2209 0.7236 0.5742 0.064 Uiso 1 1 calc R . . C40 C 0.3202(10) 0.5902(11) 0.5831(7) 0.033(4) Uani 1 1 d . . . C42 C 0.3437(11) 0.8126(14) 0.5784(8) 0.073(6) Uani 1 1 d . . . H42 H 0.3187 0.8951 0.5746 0.088 Uiso 1 1 calc R . . C43 C 0.4391(12) 0.7944(13) 0.5843(9) 0.085(7) Uani 1 1 d . . . H43 H 0.4795 0.8650 0.5861 0.102 Uiso 1 1 calc R . . C44 C 0.4756(10) 0.6747(13) 0.5874(7) 0.053(5) Uani 1 1 d U . . H44 H 0.5408 0.6622 0.5902 0.063 Uiso 1 1 calc R . . C45 C 0.4156(10) 0.5724(12) 0.5864(7) 0.041(4) Uani 1 1 d . . . H45 H 0.4401 0.4895 0.5879 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.0261(4) 0.0193(3) 0.1037(6) 0.0035(3) 0.0187(4) -0.0002(3) Au2 0.0204(4) 0.0228(3) 0.1418(8) 0.0073(4) 0.0097(4) 0.0004(3) P1 0.029(3) 0.0199(19) 0.076(4) -0.0129(19) 0.015(3) -0.0049(17) P2 0.022(3) 0.037(2) 0.070(4) 0.004(2) 0.014(2) 0.0059(18) Cl1 0.041(3) 0.043(2) 0.146(4) 0.045(2) 0.027(3) 0.0097(19) Cl2 0.035(3) 0.027(2) 0.283(6) -0.020(3) 0.008(4) 0.0082(19) O1 0.023(7) 0.020(5) 0.099(10) 0.014(5) 0.016(6) 0.009(4) O2 0.029(7) 0.034(6) 0.114(11) 0.023(6) 0.013(7) 0.011(5) O3 0.030(6) 0.033(5) 0.130(9) 0.013(5) 0.028(6) 0.002(4) N1 0.029(6) 0.013(5) 0.048(7) -0.007(5) 0.009(6) 0.000(4) C1 0.023(10) 0.028(8) 0.063(13) -0.022(7) 0.000(9) 0.000(6) C2 0.020(8) 0.029(7) 0.051(10) -0.017(6) -0.002(7) 0.008(6) C3 0.028(8) 0.016(6) 0.044(9) -0.001(6) 0.001(7) -0.008(6) C4 0.008(8) 0.017(7) 0.067(13) -0.005(7) 0.006(8) 0.002(6) C5 0.031(11) 0.026(8) 0.096(15) 0.017(8) 0.023(10) 0.006(7) C6 0.021(8) 0.042(8) 0.060(10) 0.008(7) 0.008(8) -0.011(7) C7 0.025(10) 0.021(8) 0.082(14) -0.003(7) 0.019(9) 0.004(7) C8 0.030(10) 0.014(7) 0.055(12) -0.002(6) 0.013(9) -0.002(6) C9 0.032(11) 0.018(9) 0.088(15) -0.004(8) 0.009(10) -0.006(7) C10 0.015(8) 0.023(7) 0.052(9) -0.007(6) 0.000(7) -0.008(6) C11 0.034(12) 0.041(9) 0.068(15) -0.005(8) 0.019(10) -0.001(7) C12 0.036(13) 0.063(11) 0.070(16) 0.018(9) 0.003(11) 0.003(9) C13 0.039(13) 0.088(14) 0.051(14) 0.000(10) 0.008(10) 0.000(11) C14 0.021(11) 0.054(11) 0.103(17) -0.023(10) 0.017(11) 0.000(8) C15 0.036(11) 0.025(8) 0.087(15) -0.021(8) 0.021(10) -0.006(7) C20 0.026(11) 0.044(9) 0.080(17) -0.010(10) 0.003(12) 0.001(7) C21 0.021(12) 0.125(15) 0.10(2) -0.059(14) 0.016(13) -0.041(10) C22 0.096(13) 0.148(12) 0.106(13) -0.018(11) 0.024(11) -0.023(11) C23 0.100(14) 0.124(12) 0.113(14) -0.024(11) 0.013(12) -0.033(10) C24 0.042(14) 0.082(13) 0.12(2) 0.000(13) 0.001(15) -0.029(10) C25 0.025(11) 0.052(10) 0.077(15) -0.010(9) 0.008(11) -0.012(8) C41 0.033(11) 0.048(10) 0.073(14) -0.030(9) -0.029(10) 0.006(9) C40 0.021(10) 0.032(8) 0.046(12) -0.015(7) 0.008(8) 0.008(7) C42 0.027(12) 0.061(11) 0.124(18) -0.055(10) -0.040(12) 0.018(9) C43 0.044(13) 0.036(10) 0.17(2) -0.040(10) -0.007(13) -0.003(9) C44 0.027(9) 0.050(8) 0.079(11) -0.025(7) -0.017(8) 0.004(7) C45 0.024(10) 0.040(9) 0.060(13) -0.025(8) 0.009(9) 0.003(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 P1 2.238(4) . ? Au1 Cl1 2.309(4) . ? Au1 Au2 3.1210(10) . ? Au2 P2 2.238(3) . ? Au2 Cl2 2.283(4) . ? P1 C10 1.779(13) . ? P1 C20 1.796(17) . ? P1 C1 1.845(11) . ? P2 C40 1.799(13) . ? P2 C2 1.825(13) . ? P2 C30 1.830(10) . ? O1 C9 1.209(14) . ? O2 C9 1.323(15) . ? O2 H2 0.8400 . ? O3 C6 1.405(13) . ? O3 H3 0.8400 . ? N1 C1 1.436(15) . ? N1 C2 1.441(14) . ? N1 C3 1.467(14) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.386(16) . ? C3 C4 1.385(15) . ? C4 C5 1.371(15) . ? C4 C9 1.529(17) . ? C5 C6 1.374(17) . ? C5 H5 0.9500 . ? C6 C7 1.399(16) . ? C7 C8 1.384(15) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C10 C11 1.381(16) . ? C10 C15 1.396(15) . ? C11 C12 1.382(18) . ? C11 H11 0.9500 . ? C12 C13 1.383(18) . ? C12 H12 0.9500 . ? C13 C14 1.367(18) . ? C13 H13 0.9500 . ? C14 C15 1.406(18) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C20 C25 1.358(18) . ? C20 C21 1.37(2) . ? C21 C22 1.40(2) . ? C21 H21 0.9500 . ? C22 C23 1.41(2) . ? C22 H22 0.9500 . ? C23 C24 1.32(2) . ? C23 H23 0.9500 . ? C24 C25 1.38(2) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C30 C31 1.3900 . ? C30 C35 1.3900 . ? C31 C32 1.3900 . ? C31 H31 0.9500 . ? C32 C33 1.3900 . ? C32 H32 0.9500 . ? C33 C34 1.3900 . ? C33 H33 0.9500 . ? C34 C35 1.3900 . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C41 C42 1.366(18) . ? C41 C40 1.373(16) . ? C41 H41 0.9500 . ? C40 C45 1.388(16) . ? C42 C43 1.388(19) . ? C42 H42 0.9500 . ? C43 C44 1.377(17) . ? C43 H43 0.9500 . ? C44 C45 1.390(16) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 172.77(15) . . ? P1 Au1 Au2 101.72(10) . . ? Cl1 Au1 Au2 85.08(12) . . ? P2 Au2 Cl2 172.96(18) . . ? P2 Au2 Au1 93.02(11) . . ? Cl2 Au2 Au1 93.90(13) . . ? C10 P1 C20 106.5(8) . . ? C10 P1 C1 107.2(6) . . ? C20 P1 C1 104.5(6) . . ? C10 P1 Au1 116.5(5) . . ? C20 P1 Au1 109.3(6) . . ? C1 P1 Au1 112.1(5) . . ? C40 P2 C2 108.7(6) . . ? C40 P2 C30 107.5(6) . . ? C2 P2 C30 101.9(6) . . ? C40 P2 Au2 111.6(4) . . ? C2 P2 Au2 115.1(4) . . ? C30 P2 Au2 111.4(4) . . ? C9 O2 H2 109.5 . . ? C6 O3 H3 109.5 . . ? C1 N1 C2 117.1(11) . . ? C1 N1 C3 117.2(11) . . ? C2 N1 C3 117.1(10) . . ? N1 C1 P1 109.7(8) . . ? N1 C1 H1A 109.7 . . ? P1 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? P1 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? N1 C2 P2 114.0(9) . . ? N1 C2 H2A 108.7 . . ? P2 C2 H2A 108.7 . . ? N1 C2 H2B 108.7 . . ? P2 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C8 C3 C4 118.7(11) . . ? C8 C3 N1 116.0(10) . . ? C4 C3 N1 125.3(12) . . ? C5 C4 C3 119.9(12) . . ? C5 C4 C9 118.4(11) . . ? C3 C4 C9 121.8(11) . . ? C4 C5 C6 120.1(12) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C7 122.2(12) . . ? C5 C6 O3 117.6(12) . . ? C7 C6 O3 120.0(13) . . ? C8 C7 C6 115.7(12) . . ? C8 C7 H7 122.1 . . ? C6 C7 H7 122.1 . . ? C7 C8 C3 123.2(11) . . ? C7 C8 H8 118.4 . . ? C3 C8 H8 118.4 . . ? O1 C9 O2 124.0(14) . . ? O1 C9 C4 124.1(13) . . ? O2 C9 C4 111.7(12) . . ? C11 C10 C15 117.4(13) . . ? C11 C10 P1 123.9(10) . . ? C15 C10 P1 118.1(10) . . ? C10 C11 C12 122.9(13) . . ? C10 C11 H11 118.5 . . ? C12 C11 H11 118.5 . . ? C11 C12 C13 119.4(14) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C13 C12 119.1(16) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 121.5(14) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C10 C15 C14 119.6(13) . . ? C10 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C25 C20 C21 118.1(17) . . ? C25 C20 P1 121.6(16) . . ? C21 C20 P1 120.3(14) . . ? C20 C21 C22 121.5(18) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C21 C22 C23 115(2) . . ? C21 C22 H22 122.5 . . ? C23 C22 H22 122.5 . . ? C24 C23 C22 124(2) . . ? C24 C23 H23 117.9 . . ? C22 C23 H23 117.9 . . ? C23 C24 C25 117(2) . . ? C23 C24 H24 121.5 . . ? C25 C24 H24 121.5 . . ? C20 C25 C24 123.1(18) . . ? C20 C25 H25 118.4 . . ? C24 C25 H25 118.4 . . ? C31 C30 C35 120.0 . . ? C31 C30 P2 115.6(9) . . ? C35 C30 P2 124.4(9) . . ? C32 C31 C30 120.0 . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C33 C32 C31 120.0 . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 120.0 . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C30 120.0 . . ? C34 C35 H35 120.0 . . ? C30 C35 H35 120.0 . . ? C42 C41 C40 121.6(15) . . ? C42 C41 H41 119.2 . . ? C40 C41 H41 119.2 . . ? C41 C40 C45 118.6(12) . . ? C41 C40 P2 121.3(11) . . ? C45 C40 P2 119.4(9) . . ? C41 C42 C43 119.4(14) . . ? C41 C42 H42 120.3 . . ? C43 C42 H42 120.3 . . ? C44 C43 C42 120.4(14) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C43 C44 C45 119.1(14) . . ? C43 C44 H44 120.5 . . ? C45 C44 H44 120.5 . . ? C40 C45 C44 120.7(12) . . ? C40 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 Cl1 0.84 2.41 3.202(10) 158 3_566 O3 H3 Cl2 0.84 2.52 3.216(11) 141 3_666 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 2.252 _refine_diff_density_min -2.554 _refine_diff_density_rms 0.223 #== END data_6e _database_code_depnum_ccdc_archive 'CCDC 289361' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H29 Au2 Cl2 N O3 P2, 0.6 (C H4 O)' _chemical_formula_sum 'C33.60 H31.40 Au2 Cl2 N O3.60 P2' _chemical_formula_weight 1033.57 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' 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' _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 10.9153(4) _cell_length_b 12.1624(4) _cell_length_c 15.8034(6) _cell_angle_alpha 74.933(2) _cell_angle_beta 82.592(2) _cell_angle_gamma 73.966(2) _cell_volume 1943.37(12) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 13391 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 25.00 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 982 _exptl_absorpt_coefficient_mu 7.792 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.305 _exptl_absorpt_correction_T_max 0.510 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius Kappa CCD Area detector' _diffrn_measurement_method '\f and \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13391 _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_av_sigmaI/netI 0.0780 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6726 _reflns_number_gt 5003 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHEXTL and local programs' _computing_publication_material 'Bruker SHEXTL and local programs' _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. SQUEEZE used to recover 22 electrons per cell, presumed to be MeOH solvent of crystallisation (18 e per molecule). Therefore 0.6 molecules of MeOH added to the UNIT per molecule of complex. ; _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^)+(0.1202P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 6726 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.1889 _refine_ls_wR_factor_gt 0.1791 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 0.04656(4) 0.21121(4) 0.22623(3) 0.03420(19) Uani 1 1 d . . . Au2 Au 0.25688(4) 0.03432(4) 0.14616(3) 0.03577(19) Uani 1 1 d . . . Cl1 Cl 0.1902(3) 0.2253(3) 0.3149(2) 0.0477(8) Uani 1 1 d . . . Cl2 Cl 0.3442(3) 0.1795(3) 0.05359(18) 0.0460(8) Uani 1 1 d . . . P1 P -0.1067(3) 0.2128(3) 0.14521(18) 0.0338(7) Uani 1 1 d . . . P2 P 0.1831(3) -0.1220(3) 0.21451(19) 0.0364(8) Uani 1 1 d . . . O1 O -0.3471(8) -0.0365(9) 0.4523(5) 0.050(3) Uani 1 1 d . . . O2 O -0.5321(9) -0.0535(10) 0.4169(5) 0.056(3) Uani 1 1 d . . . H2 H -0.5544 -0.0429 0.4676 0.084 Uiso 1 1 calc R . . O3 O -0.1896(9) -0.1060(9) 0.0681(5) 0.049(2) Uani 1 1 d . . . H3 H -0.2353 -0.1290 0.0410 0.073 Uiso 1 1 calc R . . N1 N -0.0649(8) -0.0268(8) 0.1734(6) 0.030(2) Uani 1 1 d . . . C1 C -0.0755(11) 0.0763(10) 0.1037(7) 0.032(3) Uani 1 1 d . . . H1A H -0.1459 0.0833 0.0674 0.039 Uiso 1 1 calc R . . H1B H 0.0046 0.0687 0.0659 0.039 Uiso 1 1 calc R . . C2 C 0.0435(11) -0.1294(12) 0.1629(7) 0.039(3) Uani 1 1 d . . . H2A H 0.0650 -0.1273 0.0998 0.047 Uiso 1 1 calc R . . H2B H 0.0193 -0.2038 0.1913 0.047 Uiso 1 1 calc R . . C3 C -0.1836(11) -0.0589(12) 0.2042(7) 0.037(3) Uani 1 1 d . . . C4 C -0.2467(12) -0.0985(11) 0.1497(7) 0.037(3) Uani 1 1 d . . . C5 C -0.3674(12) -0.1195(14) 0.1772(8) 0.050(4) Uani 1 1 d . . . H5 H -0.4128 -0.1406 0.1391 0.060 Uiso 1 1 calc R . . C6 C -0.4197(13) -0.1096(14) 0.2598(8) 0.049(4) Uani 1 1 d . . . H6 H -0.4995 -0.1276 0.2794 0.059 Uiso 1 1 calc R . . C7 C -0.3562(12) -0.0730(11) 0.3154(7) 0.035(3) Uani 1 1 d . . . C8 C -0.2379(10) -0.0508(10) 0.2868(7) 0.030(3) Uani 1 1 d . . . H8 H -0.1932 -0.0294 0.3251 0.036 Uiso 1 1 calc R . . C9 C -0.4157(12) -0.0561(12) 0.4004(8) 0.041(3) Uani 1 1 d . . . C10 C -0.1219(13) 0.3282(10) 0.0462(7) 0.039(3) Uani 1 1 d . . . C11 C -0.0117(18) 0.3419(18) -0.0058(10) 0.080(6) Uani 1 1 d . . . H11 H 0.0688 0.2917 0.0122 0.096 Uiso 1 1 calc R . . C12 C -0.018(2) 0.4274(18) -0.0829(11) 0.090(7) Uani 1 1 d . . . H12 H 0.0584 0.4382 -0.1169 0.108 Uiso 1 1 calc R . . C13 C -0.133(3) 0.4963(15) -0.1100(10) 0.082(6) Uani 1 1 d . . . H13 H -0.1375 0.5494 -0.1662 0.098 Uiso 1 1 calc R . . C14 C -0.243(2) 0.4917(15) -0.0599(12) 0.075(5) Uani 1 1 d . . . H14 H -0.3221 0.5452 -0.0778 0.090 Uiso 1 1 calc R . . C15 C -0.2369(17) 0.4065(15) 0.0186(11) 0.069(5) Uani 1 1 d . . . H15 H -0.3131 0.4016 0.0543 0.083 Uiso 1 1 calc R . . C20 C -0.2630(10) 0.2258(11) 0.2053(7) 0.034(3) Uani 1 1 d . . . C21 C -0.2696(12) 0.2426(12) 0.2915(7) 0.041(3) Uani 1 1 d . . . H21 H -0.1970 0.2498 0.3148 0.049 Uiso 1 1 calc R . . C22 C -0.3859(11) 0.2484(13) 0.3413(8) 0.046(3) Uani 1 1 d . . . H22 H -0.3947 0.2640 0.3979 0.055 Uiso 1 1 calc R . . C23 C -0.4872(13) 0.2313(13) 0.3077(9) 0.054(4) Uani 1 1 d . . . H23 H -0.5638 0.2296 0.3435 0.065 Uiso 1 1 calc R . . C24 C -0.4812(12) 0.2168(12) 0.2243(9) 0.045(3) Uani 1 1 d . . . H24 H -0.5544 0.2099 0.2016 0.054 Uiso 1 1 calc R . . C25 C -0.3679(12) 0.2121(12) 0.1731(8) 0.044(3) Uani 1 1 d . . . H25 H -0.3624 0.1993 0.1158 0.053 Uiso 1 1 calc R . . C30 C 0.2985(12) -0.2586(13) 0.2037(9) 0.046(3) Uani 1 1 d . . . C31 C 0.3887(13) -0.2595(13) 0.1327(9) 0.051(4) Uani 1 1 d . . . H31 H 0.3867 -0.1881 0.0897 0.061 Uiso 1 1 calc R . . C32 C 0.4784(15) -0.3572(16) 0.1223(11) 0.065(4) Uani 1 1 d . . . H32 H 0.5404 -0.3535 0.0743 0.078 Uiso 1 1 calc R . . C33 C 0.4793(18) -0.4603(17) 0.1808(12) 0.087(6) Uani 1 1 d . . . H33 H 0.5414 -0.5298 0.1736 0.104 Uiso 1 1 calc R . . C34 C 0.386(2) -0.4651(17) 0.2544(13) 0.106(8) Uani 1 1 d . . . H34 H 0.3841 -0.5377 0.2950 0.128 Uiso 1 1 calc R . . C35 C 0.299(2) -0.3601(16) 0.2645(11) 0.098(8) Uani 1 1 d . . . H35 H 0.2392 -0.3601 0.3141 0.117 Uiso 1 1 calc R . . C40 C 0.1360(10) -0.1382(11) 0.3308(7) 0.031(3) Uani 1 1 d . . . C41 C 0.1911(11) -0.0844(13) 0.3786(7) 0.042(3) Uani 1 1 d . . . H41 H 0.2495 -0.0391 0.3503 0.051 Uiso 1 1 calc R . . C42 C 0.1599(13) -0.0977(14) 0.4666(8) 0.050(4) Uani 1 1 d . . . H42 H 0.2020 -0.0668 0.5005 0.060 Uiso 1 1 calc R . . C43 C 0.0676(12) -0.1556(13) 0.5070(8) 0.045(3) Uani 1 1 d . . . H43 H 0.0433 -0.1598 0.5674 0.054 Uiso 1 1 calc R . . C44 C 0.0106(12) -0.2071(13) 0.4605(7) 0.046(3) Uani 1 1 d . . . H44 H -0.0491 -0.2509 0.4888 0.055 Uiso 1 1 calc R . . C45 C 0.0428(12) -0.1933(13) 0.3713(8) 0.042(3) Uani 1 1 d . . . H45 H -0.0008 -0.2227 0.3373 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.0284(3) 0.0522(4) 0.0214(3) -0.0098(2) 0.00540(19) -0.0115(2) Au2 0.0309(3) 0.0553(4) 0.0191(3) -0.0087(2) 0.0069(2) -0.0114(2) Cl1 0.0358(17) 0.075(2) 0.0345(16) -0.0074(16) 0.0002(14) -0.0241(17) Cl2 0.0516(19) 0.072(2) 0.0221(14) -0.0150(14) 0.0094(13) -0.0299(18) P1 0.0378(17) 0.0404(19) 0.0215(14) -0.0090(13) 0.0036(13) -0.0078(14) P2 0.0276(16) 0.057(2) 0.0173(14) -0.0048(14) 0.0073(12) -0.0072(15) O1 0.050(5) 0.101(8) 0.016(4) -0.022(4) 0.011(4) -0.044(6) O2 0.051(6) 0.101(8) 0.030(5) -0.029(5) 0.017(4) -0.038(6) O3 0.055(6) 0.086(7) 0.022(4) -0.030(5) 0.012(4) -0.034(5) N1 0.026(5) 0.041(6) 0.021(4) -0.011(4) 0.003(4) -0.001(4) C1 0.027(6) 0.043(7) 0.023(6) -0.009(5) 0.005(5) -0.003(5) C2 0.036(7) 0.063(9) 0.020(6) -0.016(6) 0.007(5) -0.013(6) C3 0.027(6) 0.059(9) 0.021(6) -0.004(6) 0.004(5) -0.012(6) C4 0.049(8) 0.045(8) 0.018(5) -0.010(5) 0.011(5) -0.017(6) C5 0.047(8) 0.102(12) 0.024(6) -0.036(7) 0.003(6) -0.037(8) C6 0.046(8) 0.076(10) 0.036(7) -0.019(7) 0.011(6) -0.033(8) C7 0.047(7) 0.039(7) 0.023(6) -0.010(5) 0.008(5) -0.018(6) C8 0.023(6) 0.042(7) 0.024(6) -0.014(5) 0.004(5) -0.003(5) C9 0.036(7) 0.062(9) 0.029(6) -0.010(6) 0.016(6) -0.027(7) C10 0.067(9) 0.025(7) 0.018(5) 0.005(5) -0.008(6) -0.006(6) C11 0.075(12) 0.110(16) 0.043(9) 0.006(9) -0.003(9) -0.026(11) C12 0.15(2) 0.075(14) 0.052(10) 0.003(10) -0.008(12) -0.053(14) C13 0.17(2) 0.039(10) 0.037(8) 0.019(7) -0.037(12) -0.031(12) C14 0.101(14) 0.055(11) 0.066(11) 0.008(9) -0.047(11) -0.019(10) C15 0.070(11) 0.067(11) 0.062(10) -0.007(9) -0.016(9) -0.005(9) C20 0.022(6) 0.038(7) 0.033(6) -0.017(5) 0.002(5) 0.012(5) C21 0.041(7) 0.061(9) 0.026(6) -0.016(6) 0.000(5) -0.016(6) C22 0.022(6) 0.075(10) 0.043(7) -0.033(7) 0.014(6) -0.003(6) C23 0.035(7) 0.071(11) 0.060(9) -0.036(8) 0.017(7) -0.011(7) C24 0.027(6) 0.064(10) 0.053(8) -0.027(7) -0.005(6) -0.014(6) C25 0.041(7) 0.059(9) 0.036(7) -0.027(6) -0.006(6) -0.005(7) C30 0.033(7) 0.065(10) 0.038(7) -0.018(7) 0.007(6) -0.005(7) C31 0.044(8) 0.053(9) 0.052(8) -0.011(7) 0.012(7) -0.017(7) C32 0.048(9) 0.074(12) 0.072(11) -0.030(10) 0.026(8) -0.015(8) C33 0.080(13) 0.067(13) 0.082(13) -0.016(10) 0.019(11) 0.020(10) C34 0.126(17) 0.056(12) 0.086(13) 0.013(10) 0.043(13) 0.011(11) C35 0.128(17) 0.058(12) 0.054(10) 0.002(9) 0.040(11) 0.029(11) C40 0.018(5) 0.049(8) 0.017(5) -0.001(5) 0.004(4) -0.006(5) C41 0.028(6) 0.073(10) 0.026(6) -0.019(6) 0.001(5) -0.008(6) C42 0.044(8) 0.081(11) 0.026(6) -0.007(7) -0.008(6) -0.019(7) C43 0.037(7) 0.067(10) 0.021(6) 0.003(6) 0.007(6) -0.013(7) C44 0.041(7) 0.073(10) 0.021(6) 0.007(6) 0.000(6) -0.028(7) C45 0.034(7) 0.065(9) 0.025(6) -0.005(6) -0.008(5) -0.013(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 2.227(3) . ? Au1 Cl1 2.300(3) . ? Au1 Au2 3.0721(7) . ? Au2 P2 2.232(3) . ? Au2 Cl2 2.322(3) . ? P1 C10 1.801(11) . ? P1 C20 1.830(11) . ? P1 C1 1.870(12) . ? P2 C40 1.817(10) . ? P2 C30 1.820(14) . ? P2 C2 1.852(12) . ? O1 C9 1.284(14) . ? O2 C9 1.257(14) . ? O2 H2 0.8400 . ? O3 C4 1.372(13) . ? O3 H3 0.8400 . ? N1 C1 1.426(14) . ? N1 C3 1.443(14) . ? N1 C2 1.492(15) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.378(14) . ? C3 C4 1.415(16) . ? C4 C5 1.404(16) . ? C5 C6 1.376(16) . ? C5 H5 0.9500 . ? C6 C7 1.408(17) . ? C6 H6 0.9500 . ? C7 C8 1.387(15) . ? C7 C9 1.452(15) . ? C8 H8 0.9500 . ? C10 C11 1.39(2) . ? C10 C15 1.39(2) . ? C11 C12 1.38(2) . ? C11 H11 0.9500 . ? C12 C13 1.36(3) . ? C12 H12 0.9500 . ? C13 C14 1.35(3) . ? C13 H13 0.9500 . ? C14 C15 1.39(2) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C20 C25 1.378(17) . ? C20 C21 1.419(15) . ? C21 C22 1.399(16) . ? C21 H21 0.9500 . ? C22 C23 1.372(18) . ? C22 H22 0.9500 . ? C23 C24 1.365(17) . ? C23 H23 0.9500 . ? C24 C25 1.384(17) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C30 C35 1.35(2) . ? C30 C31 1.394(17) . ? C31 C32 1.35(2) . ? C31 H31 0.9500 . ? C32 C33 1.35(2) . ? C32 H32 0.9500 . ? C33 C34 1.44(2) . ? C33 H33 0.9500 . ? C34 C35 1.40(2) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C40 C45 1.371(16) . ? C40 C41 1.398(16) . ? C41 C42 1.368(16) . ? C41 H41 0.9500 . ? C42 C43 1.382(18) . ? C42 H42 0.9500 . ? C43 C44 1.375(18) . ? C43 H43 0.9500 . ? C44 C45 1.387(16) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 174.09(12) . . ? P1 Au1 Au2 95.47(8) . . ? Cl1 Au1 Au2 90.38(9) . . ? P2 Au2 Cl2 169.32(11) . . ? P2 Au2 Au1 95.19(8) . . ? Cl2 Au2 Au1 93.55(9) . . ? C10 P1 C20 108.4(6) . . ? C10 P1 C1 103.2(5) . . ? C20 P1 C1 105.6(6) . . ? C10 P1 Au1 112.8(5) . . ? C20 P1 Au1 112.9(4) . . ? C1 P1 Au1 113.2(4) . . ? C40 P2 C30 106.6(6) . . ? C40 P2 C2 105.6(5) . . ? C30 P2 C2 102.1(6) . . ? C40 P2 Au2 117.3(4) . . ? C30 P2 Au2 111.4(5) . . ? C2 P2 Au2 112.6(4) . . ? C9 O2 H2 109.5 . . ? C4 O3 H3 109.5 . . ? C1 N1 C3 114.9(9) . . ? C1 N1 C2 116.0(8) . . ? C3 N1 C2 113.2(10) . . ? N1 C1 P1 112.2(7) . . ? N1 C1 H1A 109.2 . . ? P1 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? P1 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? N1 C2 P2 108.7(8) . . ? N1 C2 H2A 110.0 . . ? P2 C2 H2A 110.0 . . ? N1 C2 H2B 110.0 . . ? P2 C2 H2B 110.0 . . ? H2A C2 H2B 108.3 . . ? C8 C3 C4 118.8(10) . . ? C8 C3 N1 120.8(10) . . ? C4 C3 N1 120.4(9) . . ? O3 C4 C5 122.7(11) . . ? O3 C4 C3 117.2(10) . . ? C5 C4 C3 119.9(10) . . ? C6 C5 C4 119.7(11) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 120.7(11) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C6 118.8(10) . . ? C8 C7 C9 120.9(10) . . ? C6 C7 C9 120.3(11) . . ? C3 C8 C7 121.8(11) . . ? C3 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? O2 C9 O1 123.6(10) . . ? O2 C9 C7 119.0(11) . . ? O1 C9 C7 117.2(10) . . ? C11 C10 C15 117.4(13) . . ? C11 C10 P1 118.2(11) . . ? C15 C10 P1 124.3(11) . . ? C12 C11 C10 120.8(19) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C13 C12 C11 119(2) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C14 C13 C12 122.3(15) . . ? C14 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? C13 C14 C15 118.0(17) . . ? C13 C14 H14 121.0 . . ? C15 C14 H14 121.0 . . ? C14 C15 C10 121.7(17) . . ? C14 C15 H15 119.1 . . ? C10 C15 H15 119.1 . . ? C25 C20 C21 120.4(11) . . ? C25 C20 P1 123.2(8) . . ? C21 C20 P1 116.3(9) . . ? C22 C21 C20 118.3(11) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? C23 C22 C21 119.5(11) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C24 C23 C22 122.0(12) . . ? C24 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C23 C24 C25 119.7(12) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C20 C25 C24 120.0(11) . . ? C20 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C35 C30 C31 119.2(14) . . ? C35 C30 P2 120.6(11) . . ? C31 C30 P2 120.2(11) . . ? C32 C31 C30 122.9(14) . . ? C32 C31 H31 118.5 . . ? C30 C31 H31 118.5 . . ? C31 C32 C33 119.3(15) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C32 C33 C34 120.2(16) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C35 C34 C33 118.3(16) . . ? C35 C34 H34 120.9 . . ? C33 C34 H34 120.9 . . ? C30 C35 C34 120.0(15) . . ? C30 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C45 C40 C41 119.2(10) . . ? C45 C40 P2 122.7(9) . . ? C41 C40 P2 117.9(8) . . ? C42 C41 C40 119.2(12) . . ? C42 C41 H41 120.4 . . ? C40 C41 H41 120.4 . . ? C41 C42 C43 120.7(13) . . ? C41 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? C44 C43 C42 120.7(11) . . ? C44 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C43 C44 C45 118.2(11) . . ? C43 C44 H44 120.9 . . ? C45 C44 H44 120.9 . . ? C40 C45 C44 121.6(12) . . ? C40 C45 H45 119.2 . . ? C44 C45 H45 119.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Au1 Au2 Cl2 -79.03(11) . . . . ? P1 Au1 Au2 P2 -73.73(11) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 Cl2 0.84 2.32 3.148(9) 171 2 O2 H2 O1 0.84 1.84 2.625(12) 154 2_456 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 3.394 _refine_diff_density_min -3.021 _refine_diff_density_rms 0.282 #==END #==END of CIF FILE