Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Prof. Paul Raithby' _publ_contact_author_email P.R.RAITHBY@BATH.AC.UK loop_ _publ_author_name P.Raithby B.Ahrens A.Bond J.E.Davies O.F.Koentjoro P.Li ; S.J.Teat ; data_cam114a _database_code_depnum_ccdc_archive 'CCDC 665741' _audit_creation_method SHELXL _chemical_name_systematic ; 'Complex 1' ; _chemical_name_common "'Complex 1'" _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C44 H32 Au2 N2 P2' _chemical_formula_weight 1044.59 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.881(2) _cell_length_b 13.638(3) _cell_length_c 16.551(3) _cell_angle_alpha 74.65(3) _cell_angle_beta 83.64(3) _cell_angle_gamma 71.06(3) _cell_volume 1827.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 3749 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 20 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.898 _exptl_crystal_density_method ? _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 8.139 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.225 _exptl_absorpt_correction_T_max 0.347 _exptl_special_details ; 'Disorder in phenyl groups, poor refinement, no H atoms included.' 'Structure includes a quarter of a dichloromethane molecule per trimer,' 'disordered over a symmetry operation.' ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.68870 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS Station 9.8' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device 'Bruker AXS Smart 1K CCD diffractometer' _diffrn_measurement_method 'omega rotation with narrow frames' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9084 _diffrn_reflns_av_R_equivalents 0.0949 _diffrn_reflns_av_sigmaI/netI 0.1587 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 20.00 _reflns_number_total 3749 _reflns_number_observed 2053 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'LSCELL (Clegg, 1997)' _computing_data_reduction 'Bruker SAINT version 5.00 (Bruker, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL PLUS (Sheldrick, 1991)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 17 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1061P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3732 _refine_ls_number_parameters 195 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1387 _refine_ls_R_factor_obs 0.0817 _refine_ls_wR_factor_all 0.2231 _refine_ls_wR_factor_obs 0.2067 _refine_ls_goodness_of_fit_all 1.045 _refine_ls_goodness_of_fit_obs 1.326 _refine_ls_restrained_S_all 1.045 _refine_ls_restrained_S_obs 1.325 _refine_ls_shift/esd_max 0.067 _refine_ls_shift/esd_mean 0.008 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Au1 Au 0.0455(3) 0.6654(2) 0.18671(14) 0.0639(7) Uani 1 d . . C1 C -0.1537(57) 0.7967(43) 0.1390(33) 0.067(14) Uiso 1 d . . C2 C -0.2487(43) 0.8540(33) 0.0975(26) 0.039(10) Uiso 1 d . . C3 C -0.3833(51) 0.9233(39) 0.0538(30) 0.058(12) Uiso 1 d . . N1 N -0.5250(47) 0.9053(34) 0.0510(27) 0.070(11) Uiso 1 d . . C5 C -0.3485(52) 1.0225(40) -0.0052(31) 0.061(12) Uiso 1 d . . Au2 Au -0.04806(15) 0.83319(12) 0.31327(9) 0.0113(4) Uani 1 d . . C6 C 0.1352(28) 0.7119(22) 0.3638(17) 0.002(6) Uiso 1 d . . C7 C 0.2457(40) 0.6453(31) 0.4042(24) 0.033(9) Uiso 1 d . . C8 C 0.3777(30) 0.5677(23) 0.4558(18) 0.007(6) Uiso 1 d . . N2 N 0.3575(32) 0.4805(24) 0.5039(19) 0.032(7) Uiso 1 d . . C10 C 0.4878(34) 0.4089(25) 0.5535(20) 0.018(7) Uiso 1 d . . P1 P 0.2453(16) 0.5065(10) 0.2203(8) 0.067(4) Uani 1 d . . C11 C 0.2662(33) 0.4434(25) 0.1382(20) 0.020(7) Uiso 1 d D . C12 C 0.4020(45) 0.3788(28) 0.1082(23) 0.052(11) Uiso 1 d D . C13 C 0.4268(51) 0.3309(33) 0.0399(27) 0.063(12) Uiso 1 d D . C14 C 0.3048(43) 0.3503(31) 0.0010(24) 0.043(10) Uiso 1 d D . C15 C 0.1391(73) 0.4260(50) 0.0132(41) 0.108(20) Uiso 1 d D . C16 C 0.1235(44) 0.4633(31) 0.0801(25) 0.047(10) Uiso 1 d D . C21 C 0.1478(53) 0.4038(48) 0.2967(39) 0.017(3) Uiso 0.46(2) d PD 1 C22 C 0.1049(29) 0.4357(23) 0.3707(18) 0.017(3) Uiso 0.46(2) d PD 1 C23 C 0.0599(30) 0.3734(24) 0.4376(18) 0.017(3) Uiso 0.46(2) d PD 1 C24 C 0.0486(65) 0.2573(49) 0.4291(38) 0.017(3) Uiso 0.46(2) d PD 1 C25 C 0.0770(65) 0.2353(49) 0.3543(39) 0.017(3) Uiso 0.46(2) d PD 1 C26 C 0.1363(64) 0.3106(50) 0.2875(39) 0.017(3) Uiso 0.46(2) d PD 1 C21A C 0.2432(58) 0.4335(43) 0.3263(33) 0.017(3) Uiso 0.54(2) d P 2 C22A C 0.3702(58) 0.3356(43) 0.3591(33) 0.017(3) Uiso 0.54(2) d P 2 C23A C 0.3299(58) 0.2665(43) 0.4339(33) 0.017(3) Uiso 0.54(2) d P 2 C24A C 0.1887(58) 0.2905(43) 0.4766(33) 0.017(3) Uiso 0.54(2) d P 2 C25A C 0.1049(29) 0.4357(23) 0.3707(18) 0.017(3) Uiso 0.54(2) d P 2 C26A C 0.0599(30) 0.3734(24) 0.4376(18) 0.017(3) Uiso 0.54(2) d P 2 C31 C 0.4691(28) 0.5204(30) 0.2154(23) 0.070(13) Uiso 1.00(2) d G . C32 C 0.5012(42) 0.6066(28) 0.2315(31) 0.155(30) Uiso 1 d G . C33 C 0.6578(51) 0.6056(28) 0.2331(32) 0.151(29) Uiso 1 d G . C34 C 0.7824(35) 0.5184(32) 0.2186(25) 0.078(14) Uiso 1 d G . C35 C 0.7503(30) 0.4323(25) 0.2025(23) 0.082(15) Uiso 1 d G . C36 C 0.5937(36) 0.4333(24) 0.2009(22) 0.064(12) Uiso 1 d G . P2 P -0.2447(8) 0.9910(6) 0.2802(5) 0.007(2) Uiso 1 d . . C41 C -0.4453(31) 0.9911(23) 0.2612(18) 0.018(7) Uiso 1 d D . C42 C -0.4927(32) 0.9047(24) 0.2837(17) 0.022(7) Uiso 1 d D . C43 C -0.6313(31) 0.9001(23) 0.2704(17) 0.018(7) Uiso 1 d D . C44 C -0.7366(59) 0.9901(42) 0.2266(32) 0.078(14) Uiso 1 d D . C45 C -0.6921(52) 1.0785(37) 0.1869(28) 0.063(12) Uiso 1 d D . C46 C -0.5379(40) 1.0748(29) 0.2025(22) 0.038(9) Uiso 1 d D . C51 C -0.1992(37) 1.0912(24) 0.1935(18) 0.074(6) Uiso 1 d G . C52 C -0.1444(38) 1.0675(21) 0.1168(22) 0.074(6) Uiso 1 d G . C53 C -0.1009(36) 1.1429(28) 0.0523(17) 0.074(6) Uiso 1 d G . C54 C -0.1121(37) 1.2420(24) 0.0645(18) 0.074(6) Uiso 1 d G . C55 C -0.1669(38) 1.2658(20) 0.1412(22) 0.074(6) Uiso 1 d G . C56 C -0.2104(36) 1.1904(27) 0.2057(16) 0.074(6) Uiso 1 d G . C61 C -0.2517(43) 1.0564(37) 0.3640(30) 0.055(11) Uiso 1 d D . C62 C -0.1930(42) 1.1562(34) 0.3362(28) 0.062(12) Uiso 1 d D . C63 C -0.1709(56) 1.2040(46) 0.3952(39) 0.097(17) Uiso 1 d D . C64 C -0.2078(60) 1.1626(44) 0.4771(36) 0.084(15) Uiso 1 d D . C65 C -0.2412(44) 1.0730(33) 0.4980(25) 0.048(10) Uiso 1 d D . C66 C -0.2565(37) 1.0092(27) 0.4402(22) 0.032(8) Uiso 1 d D . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.0881(13) 0.0417(12) 0.0376(12) -0.0021(9) -0.0093(8) 0.0088(9) Au2 0.0079(6) 0.0129(7) 0.0112(7) 0.0058(5) -0.0076(4) -0.0055(5) P1 0.085(9) 0.030(7) 0.047(8) 0.011(5) 0.006(6) 0.017(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 C1 2.11(5) . ? Au1 P1 2.289(11) . ? Au1 Au2 3.351(2) . ? C1 C2 1.10(5) . ? C2 C3 1.39(6) . ? C3 N1 1.37(6) . ? C3 C5 1.54(7) . ? N1 C5 1.37(6) 2_475 ? C5 N1 1.37(6) 2_475 ? Au2 C6 1.98(2) . ? Au2 P2 2.265(7) . ? C6 C7 1.22(4) . ? C7 C8 1.47(5) . ? C8 N2 1.30(4) . ? C8 C10 1.32(4) 2_666 ? N2 C10 1.42(4) . ? C10 C8 1.32(4) 2_666 ? P1 C11 1.76(3) . ? P1 C21A 1.77(6) . ? P1 C21 1.98(7) . ? P1 C31 2.05(3) . ? C11 C12 1.37(5) . ? C11 C16 1.59(5) . ? C12 C13 1.41(6) . ? C13 C14 1.24(5) . ? C14 C15 1.53(7) . ? C15 C16 1.31(7) . ? C21 C26 1.36(9) . ? C21 C22 1.38(7) . ? C22 C23 1.32(4) . ? C23 C24 1.66(7) . ? C24 C25 1.33(9) . ? C25 C26 1.47(9) . ? C21A C25A 1.36(6) . ? C21A C22A 1.46(7) . ? C22A C23A 1.43(8) . ? C23A C24A 1.36(8) . ? C24A C26A 1.39(6) . ? C25A C26A 1.32(4) . ? C31 C32 1.39 . ? C31 C36 1.39 . ? C32 C33 1.39 . ? C33 C34 1.39 . ? C34 C35 1.39 . ? C35 C36 1.39 . ? P2 C51 1.81(3) . ? P2 C61 1.82(5) . ? P2 C41 1.84(3) . ? C41 C42 1.33(4) . ? C41 C46 1.38(5) . ? C42 C43 1.30(4) . ? C43 C44 1.36(6) . ? C44 C45 1.37(7) . ? C45 C46 1.40(5) . ? C51 C52 1.39 . ? C51 C56 1.39 . ? C52 C53 1.39 . ? C53 C54 1.39 . ? C54 C55 1.39 . ? C55 C56 1.39 . ? C61 C66 1.26(5) . ? C61 C62 1.55(7) . ? C62 C63 1.37(7) . ? C63 C64 1.37(8) . ? C64 C65 1.30(7) . ? C65 C66 1.50(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 P1 168.0(14) . . ? C1 Au1 Au2 71.1(14) . . ? P1 Au1 Au2 120.3(4) . . ? C2 C1 Au1 162.3(47) . . ? C1 C2 C3 172.3(56) . . ? N1 C3 C2 127.4(46) . . ? N1 C3 C5 120.6(36) . . ? C2 C3 C5 111.5(38) . . ? C5 N1 C3 123.8(43) 2_475 . ? N1 C5 C3 115.1(39) 2_475 . ? C6 Au2 P2 165.3(7) . . ? C6 Au2 Au1 73.9(7) . . ? P2 Au2 Au1 120.6(2) . . ? C7 C6 Au2 170.2(25) . . ? C6 C7 C8 177.5(35) . . ? N2 C8 C10 124.7(25) . 2_666 ? N2 C8 C7 119.2(26) . . ? C10 C8 C7 116.0(29) 2_666 . ? C8 N2 C10 117.0(26) . . ? C8 C10 N2 118.2(29) 2_666 . ? C11 P1 C21A 120.6(21) . . ? C11 P1 C21 92.3(22) . . ? C11 P1 C31 99.3(15) . . ? C21A P1 C31 98.2(20) . . ? C21 P1 C31 131.2(17) . . ? C11 P1 Au1 107.5(11) . . ? C21A P1 Au1 115.2(18) . . ? C21 P1 Au1 106.2(15) . . ? C31 P1 Au1 114.8(12) . . ? C12 C11 C16 108.5(30) . . ? C12 C11 P1 128.6(24) . . ? C16 C11 P1 122.7(24) . . ? C11 C12 C13 130.8(34) . . ? C14 C13 C12 114.2(40) . . ? C13 C14 C15 128.1(44) . . ? C16 C15 C14 113.8(44) . . ? C15 C16 C11 124.0(39) . . ? C26 C21 C22 122.1(57) . . ? C26 C21 P1 129.6(48) . . ? C22 C21 P1 107.9(38) . . ? C23 C22 C21 121.1(37) . . ? C22 C23 C24 117.9(31) . . ? C25 C24 C23 118.2(53) . . ? C24 C25 C26 116.5(57) . . ? C21 C26 C25 123.6(56) . . ? C25A C21A C22A 111.4(46) . . ? C25A C21A P1 121.6(33) . . ? C22A C21A P1 121.7(39) . . ? C23A C22A C21A 115.4(45) . . ? C24A C23A C22A 124.2(47) . . ? C23A C24A C26A 119.3(48) . . ? C26A C25A C21A 135.6(31) . . ? C25A C26A C24A 111.9(31) . . ? C32 C31 C36 120.0 . . ? C32 C31 P1 123.9(21) . . ? C36 C31 P1 115.9(21) . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C35 C36 C31 120.0 . . ? C51 P2 C61 98.2(19) . . ? C51 P2 C41 105.7(14) . . ? C61 P2 C41 110.7(15) . . ? C51 P2 Au2 115.5(11) . . ? C61 P2 Au2 105.7(13) . . ? C41 P2 Au2 119.1(10) . . ? C42 C41 C46 115.1(27) . . ? C42 C41 P2 123.6(22) . . ? C46 C41 P2 119.1(26) . . ? C43 C42 C41 126.0(28) . . ? C42 C43 C44 117.9(35) . . ? C43 C44 C45 121.5(44) . . ? C44 C45 C46 116.0(41) . . ? C41 C46 C45 120.8(37) . . ? C52 C51 C56 120.0 . . ? C52 C51 P2 120.5(21) . . ? C56 C51 P2 119.4(21) . . ? C53 C52 C51 120.0 . . ? C52 C53 C54 120.0 . . ? C55 C54 C53 120.0 . . ? C54 C55 C56 120.0 . . ? C55 C56 C51 120.0 . . ? C66 C61 C62 120.8(38) . . ? C66 C61 P2 122.2(36) . . ? C62 C61 P2 113.8(33) . . ? C63 C62 C61 119.8(46) . . ? C64 C63 C62 117.5(56) . . ? C65 C64 C63 120.1(53) . . ? C64 C65 C66 126.8(43) . . ? C61 C66 C65 113.2(36) . . ? _refine_diff_density_max 1.865 _refine_diff_density_min -2.735 _refine_diff_density_rms 0.286 ####END data_pr0105 _database_code_depnum_ccdc_archive 'CCDC 665742' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Complex 2 ; _chemical_name_common 'Complex 2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H71 Au2 Cl2 N P2' _chemical_formula_weight 1164.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 9.1956(3) _cell_length_b 10.3609(3) _cell_length_c 12.8658(4) _cell_angle_alpha 103.998(2) _cell_angle_beta 100.256(2) _cell_angle_gamma 96.941(2) _cell_volume 1153.00(6) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9236 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description colourless _exptl_crystal_colour plate _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 6.571 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.493 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 12208 _diffrn_reflns_av_R_equivalents 0.1206 _diffrn_reflns_av_sigmaI/netI 0.0868 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5234 _reflns_number_gt 4596 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1011P)^2^+1.8974P] 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 5234 _refine_ls_number_parameters 246 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1603 _refine_ls_wR_factor_gt 0.1525 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.14189(3) 0.26423(3) 0.039015(19) 0.03295(14) Uani 1 1 d . . . P1 P 0.0048(2) 0.2108(2) -0.13653(15) 0.0316(4) Uani 1 1 d . . . C1 C 0.2616(10) 0.3254(9) 0.1931(6) 0.0368(17) Uani 1 1 d . . . C2 C 0.3352(9) 0.3761(9) 0.2854(7) 0.0405(18) Uani 1 1 d . . . C3 C 0.4188(9) 0.4378(10) 0.3945(6) 0.0393(18) Uani 1 1 d . . . C4 C 0.4427(13) 0.5754(11) 0.4380(7) 0.059(3) Uani 0.75 1 d P . 1 H4 H 0.4032 0.6299 0.3940 0.071 Uiso 0.75 1 calc PR . 1 C5 C 0.4794(11) 0.3643(10) 0.4584(7) 0.052(2) Uani 0.75 1 d P . 1 H5 H 0.4673 0.2691 0.4305 0.062 Uiso 0.75 1 calc PR . 1 N1A N 0.4427(13) 0.5754(11) 0.4380(7) 0.059(3) Uani 0.25 1 d P . 2 N1B N 0.4794(11) 0.3643(10) 0.4584(7) 0.052(2) Uani 0.25 1 d P . 2 C6 C 0.0196(11) 0.0409(10) -0.2206(7) 0.059(3) Uani 1 1 d D . . H6A H -0.0379 -0.0198 -0.1867 0.070 Uiso 1 1 calc R . . C7 C 0.1666(15) 0.0012(11) -0.2031(9) 0.088(5) Uani 1 1 d D . . H7A H 0.2020 0.0116 -0.1237 0.106 Uiso 1 1 calc R . . H7B H 0.2379 0.0634 -0.2252 0.106 Uiso 1 1 calc R . . C8 C 0.1699(12) -0.1416(8) -0.2648(7) 0.052(2) Uani 1 1 d D . . H8A H 0.2756 -0.1529 -0.2632 0.063 Uiso 1 1 calc R . . H8B H 0.1264 -0.2042 -0.2268 0.063 Uiso 1 1 calc R . . C9 C 0.0857(17) -0.1796(12) -0.3817(9) 0.101(6) Uani 1 1 d D . . H9A H 0.1479 -0.1383 -0.4245 0.121 Uiso 1 1 calc R . . H9B H 0.0731 -0.2788 -0.4108 0.121 Uiso 1 1 calc R . . C10 C -0.0603(13) -0.1404(13) -0.4004(9) 0.081(4) Uani 1 1 d D . . H10A H -0.1324 -0.2059 -0.3820 0.098 Uiso 1 1 calc R . . H10B H -0.0922 -0.1484 -0.4797 0.098 Uiso 1 1 calc R . . C11 C -0.0722(10) 0.0011(8) -0.3370(6) 0.0419(19) Uani 1 1 d D . . H11A H -0.0375 0.0666 -0.3758 0.050 Uiso 1 1 calc R . . H11B H -0.1787 0.0056 -0.3352 0.050 Uiso 1 1 calc R . . C12 C -0.1966(8) 0.2046(7) -0.1414(6) 0.0345(15) Uani 1 1 d D . . H12A H -0.2485 0.1909 -0.2194 0.041 Uiso 1 1 calc R . . C13 C -0.2246(8) 0.3396(8) -0.0738(7) 0.0428(19) Uani 1 1 d D . . H13A H -0.1897 0.4134 -0.1048 0.051 Uiso 1 1 calc R . . H13B H -0.1679 0.3595 0.0029 0.051 Uiso 1 1 calc R . . C14 C -0.3934(10) 0.3312(10) -0.0763(9) 0.060(3) Uani 1 1 d D . . H14A H -0.4110 0.4173 -0.0309 0.072 Uiso 1 1 calc R . . H14B H -0.4482 0.3186 -0.1525 0.072 Uiso 1 1 calc R . . C15 C -0.4544(11) 0.2171(11) -0.0343(9) 0.065(3) Uani 1 1 d D . . H15A H -0.5632 0.2149 -0.0379 0.078 Uiso 1 1 calc R . . H15B H -0.4040 0.2315 0.0433 0.078 Uiso 1 1 calc R . . C16 C -0.4287(11) 0.0835(9) -0.1027(9) 0.059(3) Uani 1 1 d D . . H16A H -0.4857 0.0658 -0.1791 0.070 Uiso 1 1 calc R . . H16B H -0.4659 0.0095 -0.0728 0.070 Uiso 1 1 calc R . . C17 C -0.2621(9) 0.0864(8) -0.1019(7) 0.0452(19) Uani 1 1 d D . . H17A H -0.2484 0.0005 -0.1501 0.054 Uiso 1 1 calc R . . H17B H -0.2069 0.0944 -0.0266 0.054 Uiso 1 1 calc R . . C18 C 0.0591(8) 0.3470(8) -0.1996(6) 0.0356(16) Uani 1 1 d D . . H18A H 0.0513 0.4326 -0.1464 0.043 Uiso 1 1 calc R . . C19 C 0.2245(9) 0.3591(13) -0.2058(9) 0.062(3) Uani 1 1 d D . . H19A H 0.2860 0.3637 -0.1331 0.074 Uiso 1 1 calc R . . H19B H 0.2394 0.2778 -0.2591 0.074 Uiso 1 1 calc R . . C20 C 0.2768(10) 0.4838(12) -0.2404(8) 0.056(3) Uani 1 1 d D . . H20A H 0.3822 0.4855 -0.2479 0.068 Uiso 1 1 calc R . . H20B H 0.2728 0.5656 -0.1829 0.068 Uiso 1 1 calc R . . C21 C 0.1795(10) 0.4860(9) -0.3492(6) 0.046(2) Uani 1 1 d D . . H21A H 0.2112 0.5717 -0.3666 0.055 Uiso 1 1 calc R . . H21B H 0.1929 0.4106 -0.4087 0.055 Uiso 1 1 calc R . . C22 C 0.0162(10) 0.4730(8) -0.3423(7) 0.045(2) Uani 1 1 d D . . H22A H -0.0456 0.4694 -0.4147 0.054 Uiso 1 1 calc R . . H22B H 0.0016 0.5539 -0.2885 0.054 Uiso 1 1 calc R . . C23 C -0.0369(9) 0.3481(8) -0.3088(7) 0.0408(18) Uani 1 1 d D . . H23A H -0.0316 0.2666 -0.3660 0.049 Uiso 1 1 calc R . . H23B H -0.1428 0.3458 -0.3023 0.049 Uiso 1 1 calc R . . Cl1 Cl 0.4459(7) 0.0803(5) 0.5875(3) 0.1174(16) Uani 1 1 d D . . C24 C 0.469(4) -0.079(3) 0.523(3) 0.117(13) Uani 0.50 1 d PD . -1 H24A H 0.3692 -0.1386 0.4960 0.140 Uiso 0.50 1 calc PR . -1 H24B H 0.5302 -0.1164 0.5758 0.140 Uiso 0.50 1 calc PR . -1 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 0.03387(19) 0.0386(2) 0.02013(18) 0.00119(12) -0.00130(12) 0.00667(12) P1 0.0303(9) 0.0371(10) 0.0213(9) -0.0005(7) 0.0001(7) 0.0074(8) C1 0.042(4) 0.043(4) 0.017(3) 0.000(3) 0.000(3) 0.004(3) C2 0.035(4) 0.055(5) 0.026(4) 0.009(3) -0.001(3) 0.001(4) C3 0.030(4) 0.061(5) 0.023(3) 0.007(3) 0.005(3) 0.002(3) C4 0.072(7) 0.062(6) 0.032(4) 0.012(4) -0.012(4) 0.007(5) C5 0.059(5) 0.053(5) 0.032(4) 0.001(4) -0.006(4) 0.006(4) N1A 0.072(7) 0.062(6) 0.032(4) 0.012(4) -0.012(4) 0.007(5) N1B 0.059(5) 0.053(5) 0.032(4) 0.001(4) -0.006(4) 0.006(4) C6 0.047(5) 0.060(6) 0.044(5) -0.021(4) -0.016(4) 0.025(4) C7 0.118(11) 0.056(6) 0.058(7) -0.026(5) -0.039(7) 0.055(7) C8 0.063(6) 0.033(4) 0.054(5) 0.004(4) 0.002(5) 0.016(4) C9 0.169(16) 0.051(6) 0.056(7) -0.018(5) -0.022(8) 0.058(9) C10 0.067(7) 0.096(9) 0.046(6) -0.041(6) -0.005(5) 0.029(7) C11 0.053(5) 0.036(4) 0.027(4) -0.004(3) -0.001(3) 0.010(4) C12 0.032(4) 0.041(4) 0.026(3) 0.003(3) 0.004(3) 0.006(3) C13 0.030(4) 0.044(4) 0.053(5) 0.002(4) 0.012(3) 0.017(3) C14 0.043(5) 0.073(7) 0.068(7) 0.011(5) 0.025(5) 0.028(5) C15 0.046(5) 0.093(8) 0.065(7) 0.023(6) 0.032(5) 0.011(5) C16 0.067(7) 0.060(6) 0.048(5) 0.012(5) 0.023(5) -0.004(5) C17 0.050(5) 0.049(5) 0.036(4) 0.011(4) 0.012(4) 0.003(4) C18 0.031(4) 0.047(4) 0.027(3) 0.007(3) 0.005(3) 0.008(3) C19 0.032(4) 0.111(9) 0.062(6) 0.053(6) 0.010(4) 0.025(5) C20 0.036(5) 0.081(7) 0.053(6) 0.026(5) 0.005(4) 0.001(5) C21 0.064(6) 0.047(5) 0.032(4) 0.013(3) 0.017(4) 0.019(4) C22 0.054(5) 0.037(4) 0.039(4) 0.006(3) -0.002(4) 0.013(4) C23 0.042(4) 0.040(4) 0.037(4) 0.012(3) 0.001(3) 0.005(3) Cl1 0.167(5) 0.111(3) 0.077(2) 0.030(2) 0.032(3) 0.017(3) C24 0.12(3) 0.061(16) 0.17(4) 0.04(2) 0.03(3) 0.003(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C1 1.998(7) . ? Au1 P1 2.2823(19) . ? P1 C12 1.835(8) . ? P1 C18 1.851(8) . ? P1 C6 1.865(8) . ? C1 C2 1.212(11) . ? C2 C3 1.425(11) . ? C3 C5 1.345(13) . ? C3 C4 1.375(14) . ? C4 C5 1.353(12) 2_666 ? C4 H4 0.9500 . ? C5 C4 1.353(12) 2_666 ? C5 H5 0.9500 . ? C6 C7 1.455(12) . ? C6 C11 1.514(10) . ? C6 H6A 1.0000 . ? C7 C8 1.507(10) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.497(12) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.445(13) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.523(11) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C17 1.533(10) . ? C12 C13 1.535(9) . ? C12 H12A 1.0000 . ? C13 C14 1.538(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.503(12) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.520(12) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.527(12) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C23 1.524(9) . ? C18 C19 1.529(10) . ? C18 H18A 1.0000 . ? C19 C20 1.518(12) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.527(11) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.511(11) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.514(10) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? Cl1 C24 1.72(2) . ? Cl1 C24 1.74(2) 2_656 ? C24 Cl1 1.74(2) 2_656 ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 P1 175.7(2) . . ? C12 P1 C18 105.3(3) . . ? C12 P1 C6 104.6(4) . . ? C18 P1 C6 112.4(5) . . ? C12 P1 Au1 112.1(2) . . ? C18 P1 Au1 108.7(2) . . ? C6 P1 Au1 113.4(3) . . ? C2 C1 Au1 173.2(8) . . ? C1 C2 C3 178.6(10) . . ? C5 C3 C4 117.2(8) . . ? C5 C3 C2 121.6(9) . . ? C4 C3 C2 121.2(8) . . ? C5 C4 C3 122.1(9) 2_666 . ? C5 C4 H4 119.0 2_666 . ? C3 C4 H4 119.0 . . ? C3 C5 C4 120.7(9) . 2_666 ? C3 C5 H5 119.7 . . ? C4 C5 H5 119.7 2_666 . ? C7 C6 C11 117.5(8) . . ? C7 C6 P1 116.3(6) . . ? C11 C6 P1 114.8(6) . . ? C7 C6 H6A 101.4 . . ? C11 C6 H6A 101.4 . . ? P1 C6 H6A 101.4 . . ? C6 C7 C8 114.4(8) . . ? C6 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? C6 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C7 113.6(7) . . ? C9 C8 H8A 108.9 . . ? C7 C8 H8A 108.9 . . ? C9 C8 H8B 108.9 . . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C10 C9 C8 116.0(9) . . ? C10 C9 H9A 108.3 . . ? C8 C9 H9A 108.3 . . ? C10 C9 H9B 108.3 . . ? C8 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? C9 C10 C11 116.5(8) . . ? C9 C10 H10A 108.2 . . ? C11 C10 H10A 108.2 . . ? C9 C10 H10B 108.2 . . ? C11 C10 H10B 108.2 . . ? H10A C10 H10B 107.3 . . ? C6 C11 C10 112.5(7) . . ? C6 C11 H11A 109.1 . . ? C10 C11 H11A 109.1 . . ? C6 C11 H11B 109.1 . . ? C10 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? C17 C12 C13 111.2(6) . . ? C17 C12 P1 111.6(5) . . ? C13 C12 P1 110.0(5) . . ? C17 C12 H12A 108.0 . . ? C13 C12 H12A 108.0 . . ? P1 C12 H12A 108.0 . . ? C12 C13 C14 109.2(6) . . ? C12 C13 H13A 109.8 . . ? C14 C13 H13A 109.8 . . ? C12 C13 H13B 109.8 . . ? C14 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? C15 C14 C13 112.3(8) . . ? C15 C14 H14A 109.1 . . ? C13 C14 H14A 109.1 . . ? C15 C14 H14B 109.1 . . ? C13 C14 H14B 109.1 . . ? H14A C14 H14B 107.9 . . ? C14 C15 C16 110.2(7) . . ? C14 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? C14 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? C15 C16 C17 110.6(7) . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C16 C17 C12 111.6(7) . . ? C16 C17 H17A 109.3 . . ? C12 C17 H17A 109.3 . . ? C16 C17 H17B 109.3 . . ? C12 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C23 C18 C19 110.3(6) . . ? C23 C18 P1 118.5(5) . . ? C19 C18 P1 111.0(6) . . ? C23 C18 H18A 105.3 . . ? C19 C18 H18A 105.3 . . ? P1 C18 H18A 105.3 . . ? C20 C19 C18 111.5(7) . . ? C20 C19 H19A 109.3 . . ? C18 C19 H19A 109.3 . . ? C20 C19 H19B 109.3 . . ? C18 C19 H19B 109.3 . . ? H19A C19 H19B 108.0 . . ? C19 C20 C21 111.5(7) . . ? C19 C20 H20A 109.3 . . ? C21 C20 H20A 109.3 . . ? C19 C20 H20B 109.3 . . ? C21 C20 H20B 109.3 . . ? H20A C20 H20B 108.0 . . ? C22 C21 C20 110.3(7) . . ? C22 C21 H21A 109.6 . . ? C20 C21 H21A 109.6 . . ? C22 C21 H21B 109.6 . . ? C20 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C21 C22 C23 112.3(7) . . ? C21 C22 H22A 109.1 . . ? C23 C22 H22A 109.1 . . ? C21 C22 H22B 109.1 . . ? C23 C22 H22B 109.1 . . ? H22A C22 H22B 107.9 . . ? C22 C23 C18 110.9(6) . . ? C22 C23 H23A 109.5 . . ? C18 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 108.0 . . ? C24 Cl1 C24 68.0(17) . 2_656 ? Cl1 C24 Cl1 112.0(17) . 2_656 ? Cl1 C24 H24A 109.2 . . ? Cl1 C24 H24A 109.2 2_656 . ? Cl1 C24 H24B 109.2 . . ? Cl1 C24 H24B 109.2 2_656 . ? H24A C24 H24B 107.9 . . ? 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 C1 Au1 P1 C12 -84(3) . . . . ? C1 Au1 P1 C18 32(3) . . . . ? C1 Au1 P1 C6 158(3) . . . . ? P1 Au1 C1 C2 -8(10) . . . . ? Au1 C1 C2 C3 55(44) . . . . ? C1 C2 C3 C5 136(41) . . . . ? C1 C2 C3 C4 -45(41) . . . . ? C5 C3 C4 C5 -1.5(17) . . . 2_666 ? C2 C3 C4 C5 179.4(10) . . . 2_666 ? C4 C3 C5 C4 1.5(17) . . . 2_666 ? C2 C3 C5 C4 -179.4(9) . . . 2_666 ? C12 P1 C6 C7 -160.8(11) . . . . ? C18 P1 C6 C7 85.4(11) . . . . ? Au1 P1 C6 C7 -38.3(12) . . . . ? C12 P1 C6 C11 56.5(9) . . . . ? C18 P1 C6 C11 -57.3(9) . . . . ? Au1 P1 C6 C11 179.0(7) . . . . ? C11 C6 C7 C8 -43.7(18) . . . . ? P1 C6 C7 C8 174.5(9) . . . . ? C6 C7 C8 C9 44.7(18) . . . . ? C7 C8 C9 C10 -45.0(19) . . . . ? C8 C9 C10 C11 43(2) . . . . ? C7 C6 C11 C10 39.9(16) . . . . ? P1 C6 C11 C10 -177.9(9) . . . . ? C9 C10 C11 C6 -39.0(17) . . . . ? C18 P1 C12 C17 174.4(5) . . . . ? C6 P1 C12 C17 55.7(6) . . . . ? Au1 P1 C12 C17 -67.6(5) . . . . ? C18 P1 C12 C13 -61.7(6) . . . . ? C6 P1 C12 C13 179.6(6) . . . . ? Au1 P1 C12 C13 56.3(6) . . . . ? C17 C12 C13 C14 -54.4(9) . . . . ? P1 C12 C13 C14 -178.5(6) . . . . ? C12 C13 C14 C15 57.2(11) . . . . ? C13 C14 C15 C16 -58.8(12) . . . . ? C14 C15 C16 C17 57.1(12) . . . . ? C15 C16 C17 C12 -55.9(10) . . . . ? C13 C12 C17 C16 55.1(9) . . . . ? P1 C12 C17 C16 178.3(6) . . . . ? C12 P1 C18 C23 -48.3(7) . . . . ? C6 P1 C18 C23 65.0(7) . . . . ? Au1 P1 C18 C23 -168.6(5) . . . . ? C12 P1 C18 C19 -177.4(6) . . . . ? C6 P1 C18 C19 -64.1(7) . . . . ? Au1 P1 C18 C19 62.3(7) . . . . ? C23 C18 C19 C20 55.7(11) . . . . ? P1 C18 C19 C20 -171.0(7) . . . . ? C18 C19 C20 C21 -55.6(12) . . . . ? C19 C20 C21 C22 54.8(11) . . . . ? C20 C21 C22 C23 -55.6(10) . . . . ? C21 C22 C23 C18 56.7(9) . . . . ? C19 C18 C23 C22 -55.7(10) . . . . ? P1 C18 C23 C22 174.9(6) . . . . ? C24 Cl1 C24 Cl1 0.000(1) 2_656 . . 2_656 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 3.325 _refine_diff_density_min -2.842 _refine_diff_density_rms 0.258 ####END data_pr9926 _database_code_depnum_ccdc_archive 'CCDC 665743' _audit_creation_method SHELXL _chemical_name_systematic ; 'Complex 3' ; _chemical_name_common "'Complex 3'" _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C45 H33 Au2 N P2' _chemical_formula_weight 1043.60 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.524(4) _cell_length_b 8.705(2) _cell_length_c 18.646(3) _cell_angle_alpha 90.00 _cell_angle_beta 120.30(3) _cell_angle_gamma 90.00 _cell_volume 3717.1(16) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5889 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 25.08 _exptl_crystal_description 'Pale yellow' _exptl_crystal_colour Block _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.865 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 8.004 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8524 _exptl_absorpt_correction_T_max 0.9713 _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_standards_number 'not applicable' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5889 _diffrn_reflns_av_R_equivalents 0.0904 _diffrn_reflns_av_sigmaI/netI 0.1493 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.08 _reflns_number_total 3264 _reflns_number_observed 1856 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius HKL Scalepack' _computing_data_reduction 'Nonius HKL Denzo & Scalepack' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 8 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_hydrogen_treatment geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3256 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1316 _refine_ls_R_factor_obs 0.0529 _refine_ls_wR_factor_all 0.2116 _refine_ls_wR_factor_obs 0.1025 _refine_ls_goodness_of_fit_all 1.032 _refine_ls_goodness_of_fit_obs 0.981 _refine_ls_restrained_S_all 1.491 _refine_ls_restrained_S_obs 0.981 _refine_ls_shift/esd_max 0.086 _refine_ls_shift/esd_mean 0.009 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Au1 Au 0.07931(3) 0.03221(6) 0.06004(4) 0.0381(3) Uani 1 d . . C1 C 0.0406(7) 0.1591(17) 0.1068(9) 0.038(4) Uani 1 d . . C2 C 0.0278(7) 0.2401(16) 0.1480(9) 0.037(4) Uani 1 d . . C3 C 0.0141(6) 0.3301(16) 0.2012(9) 0.032(4) Uani 1 d . . C4 C 0.0169(7) 0.4877(17) 0.2011(9) 0.042(4) Uani 1 d . . H4A H 0.0301 0.5386 0.1685 0.050 Uiso 1 calc R . C5 C 0.0000 0.5736(25) 0.2500 0.049(6) Uani 1 d S . H5 H 0.0000 0.6827 0.2500 0.059 Uiso 1 calc SR . N1 N 0.0000 0.2481(17) 0.2500 0.036(4) Uani 1 d S . P1 P 0.1405(2) -0.0945(4) 0.0279(2) 0.0340(10) Uani 1 d . . C11 C 0.1474(8) -0.0079(13) -0.0551(10) 0.035(4) Uani 1 d . . C12 C 0.2013(7) 0.0498(15) -0.0410(10) 0.037(4) Uani 1 d . . H12A H 0.2356 0.0443 0.0123 0.044 Uiso 1 calc R . C13 C 0.2022(8) 0.1144(17) -0.1078(13) 0.055(5) Uani 1 d . . H13A H 0.2381 0.1544 -0.0997 0.066 Uiso 1 calc R . C14 C 0.1525(9) 0.1236(17) -0.1874(11) 0.053(5) Uani 1 d . . H14A H 0.1543 0.1662 -0.2329 0.063 Uiso 1 calc R . C15 C 0.1000(7) 0.0672(16) -0.1968(10) 0.046(4) Uani 1 d . . H15A H 0.0653 0.0742 -0.2495 0.056 Uiso 1 calc R . C16 C 0.0978(8) 0.0031(15) -0.1323(11) 0.047(5) Uani 1 d . . H16A H 0.0618 -0.0348 -0.1403 0.057 Uiso 1 calc R . C21 C 0.1250(7) -0.2937(14) 0.0011(9) 0.033(4) Uani 1 d . . C22 C 0.0931(7) -0.3782(17) 0.0316(9) 0.040(4) Uani 1 d . . H22A H 0.0790 -0.3249 0.0624 0.049 Uiso 1 calc R . C23 C 0.0822(8) -0.5321(20) 0.0180(11) 0.059(5) Uani 1 d . . H23A H 0.0614 -0.5850 0.0396 0.070 Uiso 1 calc R . C24 C 0.1022(8) -0.6102(19) -0.0282(11) 0.062(5) Uani 1 d . . H24A H 0.0954 -0.7174 -0.0379 0.074 Uiso 1 calc R . C25 C 0.1327(8) -0.5295(20) -0.0605(11) 0.066(6) Uani 1 d . . H25A H 0.1468 -0.5840 -0.0909 0.080 Uiso 1 calc R . C26 C 0.1426(7) -0.3690(17) -0.0485(10) 0.044(4) Uani 1 d . . H26A H 0.1607 -0.3145 -0.0736 0.053 Uiso 1 calc R . C31 C 0.2130(6) -0.0954(15) 0.1170(9) 0.031(4) Uani 1 d . . C32 C 0.2307(8) 0.0150(17) 0.1769(11) 0.049(4) Uani 1 d . . H32A H 0.2031 0.0913 0.1705 0.058 Uiso 1 calc R . C33 C 0.2868(8) 0.0240(20) 0.2472(11) 0.065(5) Uani 1 d . . H33A H 0.2974 0.1066 0.2855 0.078 Uiso 1 calc R . C34 C 0.3244(7) -0.0870(18) 0.2585(10) 0.047(4) Uani 1 d . . H34A H 0.3618 -0.0867 0.3074 0.057 Uiso 1 calc R . C35 C 0.3113(8) -0.1971(17) 0.2039(13) 0.054(5) Uani 1 d . . H35A H 0.3396 -0.2721 0.2116 0.064 Uiso 1 calc R . C36 C 0.2548(7) -0.2029(16) 0.1336(10) 0.039(4) Uani 1 d . . H36A H 0.2454 -0.2859 0.0959 0.047 Uiso 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 0.0463(4) 0.0338(4) 0.0457(4) 0.0020(3) 0.0317(4) 0.0056(3) C1 0.032(11) 0.054(10) 0.026(9) 0.003(7) 0.013(9) 0.007(8) C2 0.034(11) 0.041(9) 0.038(11) 0.010(8) 0.019(9) 0.000(7) C3 0.025(9) 0.021(9) 0.045(11) 0.006(7) 0.013(8) 0.012(6) C4 0.039(10) 0.060(13) 0.036(10) 0.005(8) 0.026(9) 0.005(8) C5 0.025(14) 0.055(15) 0.070(18) 0.000 0.025(14) 0.000 N1 0.027(11) 0.033(10) 0.059(14) 0.000 0.031(11) 0.000 P1 0.038(3) 0.028(2) 0.042(3) -0.001(2) 0.024(2) 0.002(2) C11 0.053(11) 0.018(8) 0.042(11) -0.001(6) 0.030(10) 0.003(7) C12 0.043(11) 0.035(9) 0.045(10) 0.009(8) 0.031(9) 0.010(8) C13 0.067(15) 0.036(10) 0.097(17) 0.005(10) 0.068(14) 0.006(9) C14 0.087(17) 0.045(11) 0.044(12) -0.005(9) 0.047(13) 0.001(10) C15 0.039(11) 0.042(10) 0.039(11) -0.014(8) 0.005(9) -0.001(8) C16 0.070(14) 0.034(10) 0.052(13) 0.004(8) 0.042(12) 0.007(8) C21 0.039(11) 0.027(8) 0.035(10) -0.001(7) 0.020(9) 0.007(7) C22 0.051(11) 0.035(11) 0.031(10) 0.008(7) 0.018(9) 0.004(8) C23 0.084(15) 0.036(10) 0.046(11) 0.003(9) 0.025(11) -0.007(10) C24 0.070(15) 0.027(10) 0.066(14) 0.011(9) 0.017(12) -0.009(9) C25 0.056(13) 0.049(11) 0.063(13) -0.028(10) 0.007(11) 0.022(10) C26 0.037(11) 0.047(11) 0.044(11) -0.011(8) 0.016(9) -0.004(8) C31 0.044(11) 0.025(8) 0.034(9) -0.005(7) 0.027(9) 0.002(7) C32 0.045(12) 0.055(11) 0.057(12) 0.000(9) 0.034(10) 0.008(8) C33 0.035(12) 0.076(13) 0.058(13) -0.038(10) 0.005(10) -0.001(10) C34 0.037(11) 0.046(10) 0.048(12) -0.005(9) 0.013(9) 0.010(8) C35 0.050(13) 0.044(11) 0.089(16) 0.023(10) 0.051(13) 0.025(9) C36 0.042(12) 0.042(10) 0.030(10) -0.004(7) 0.014(10) 0.008(8) _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 C1 1.984(15) . ? Au1 P1 2.279(4) . ? C1 C2 1.21(2) . ? C2 C3 1.45(2) . ? C3 N1 1.35(2) . ? C3 C4 1.37(2) . ? C4 C5 1.42(2) . ? C5 C4 1.42(2) 2 ? N1 C3 1.35(2) 2 ? P1 C21 1.794(13) . ? P1 C31 1.80(2) . ? P1 C11 1.812(14) . ? C11 C16 1.38(2) . ? C11 C12 1.41(2) . ? C12 C13 1.38(2) . ? C13 C14 1.41(2) . ? C14 C15 1.40(2) . ? C15 C16 1.35(2) . ? C21 C26 1.39(2) . ? C21 C22 1.44(2) . ? C22 C23 1.37(2) . ? C23 C24 1.40(2) . ? C24 C25 1.41(2) . ? C25 C26 1.42(2) . ? C31 C32 1.36(2) . ? C31 C36 1.36(2) . ? C32 C33 1.40(2) . ? C33 C34 1.33(2) . ? C34 C35 1.31(2) . ? C35 C36 1.41(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 P1 168.6(5) . . ? C2 C1 Au1 167.4(14) . . ? C1 C2 C3 176.6(15) . . ? N1 C3 C4 124.2(13) . . ? N1 C3 C2 115.2(12) . . ? C4 C3 C2 120.5(13) . . ? C3 C4 C5 119.4(14) . . ? C4 C5 C4 116.3(20) 2 . ? C3 N1 C3 116.2(16) 2 . ? C21 P1 C31 103.9(7) . . ? C21 P1 C11 105.8(6) . . ? C31 P1 C11 105.6(7) . . ? C21 P1 Au1 116.6(5) . . ? C31 P1 Au1 109.3(4) . . ? C11 P1 Au1 114.6(5) . . ? C16 C11 C12 120.9(14) . . ? C16 C11 P1 117.8(12) . . ? C12 C11 P1 121.2(12) . . ? C13 C12 C11 117.0(16) . . ? C12 C13 C14 122.9(16) . . ? C13 C14 C15 117.2(15) . . ? C16 C15 C14 121.2(16) . . ? C15 C16 C11 120.7(17) . . ? C26 C21 C22 118.9(12) . . ? C26 C21 P1 122.3(11) . . ? C22 C21 P1 118.8(10) . . ? C23 C22 C21 122.6(14) . . ? C22 C23 C24 118.8(16) . . ? C23 C24 C25 119.8(15) . . ? C26 C25 C24 121.5(16) . . ? C25 C26 C21 118.1(15) . . ? C32 C31 C36 113.1(15) . . ? C32 C31 P1 121.3(12) . . ? C36 C31 P1 125.5(11) . . ? C31 C32 C33 124.7(15) . . ? C34 C33 C32 117.7(16) . . ? C35 C34 C33 121.7(17) . . ? C34 C35 C36 119.3(15) . . ? C31 C36 C35 123.3(14) . . ? _refine_diff_density_max 1.199 _refine_diff_density_min -1.051 _refine_diff_density_rms 0.250 ####END data_pr0054 _database_code_depnum_ccdc_archive 'CCDC 665744' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Complex 4' ; _chemical_name_common "'Complex 4'" _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H36 Au2 N2 P2' _chemical_formula_weight 1120.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.0693(1) _cell_length_b 13.7695(4) _cell_length_c 21.3934(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.947(2) _cell_angle_gamma 90.00 _cell_volume 2067.16(9) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 18945 _cell_measurement_theta_min 3.53 _cell_measurement_theta_max 27.49 _exptl_crystal_description Needle _exptl_crystal_colour Orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.800 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1076 _exptl_absorpt_coefficient_mu 7.204 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2211 _exptl_absorpt_correction_T_max 0.7146 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18945 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4705 _reflns_number_gt 3943 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; "Collect" data collection software, Nonius B.V., 1998. ; _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; "Collect" data collection software, Nonius B.V., 1998. ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1991)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+2.2934P] 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 4705 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0719 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 1.17898(2) 0.837595(12) 0.741443(7) 0.03037(7) Uani 1 1 d . . . P1 P 1.35648(15) 0.83491(8) 0.65946(5) 0.0276(2) Uani 1 1 d . . . C1 C 1.0064(6) 0.8483(3) 0.8092(2) 0.0314(9) Uani 1 1 d . . . C2 C 0.8955(6) 0.8691(3) 0.84515(19) 0.0319(9) Uani 1 1 d . . . C3 C 0.7713(5) 0.9026(3) 0.88874(18) 0.0286(9) Uani 1 1 d . . . C4 C 0.5794(6) 0.8774(4) 0.8861(2) 0.0440(11) Uani 1 1 d . . . H4A H 0.5236 0.8340 0.8545 0.053 Uiso 1 1 calc R . . C5 C 0.4716(6) 0.9158(4) 0.9294(2) 0.0416(12) Uani 1 1 d . . . H5A H 0.3403 0.8997 0.9274 0.050 Uiso 1 1 calc R . . C6 C 0.5537(5) 0.9780(3) 0.97604(18) 0.0285(9) Uani 1 1 d . . . N1 N 0.7375(5) 1.0043(3) 0.97879(17) 0.0394(9) Uani 1 1 d . . . C7 C 0.8394(6) 0.9673(4) 0.9361(2) 0.0407(11) Uani 1 1 d . . . H7A H 0.9690 0.9866 0.9381 0.049 Uiso 1 1 calc R . . C101 C 1.1982(6) 0.8267(3) 0.5862(2) 0.0297(9) Uani 1 1 d . . . C102 C 1.0436(6) 0.8911(3) 0.5784(2) 0.0362(10) Uani 1 1 d . . . H10A H 1.0253 0.9366 0.6105 0.043 Uiso 1 1 calc R . . C103 C 0.9180(6) 0.8877(4) 0.5237(2) 0.0438(12) Uani 1 1 d . . . H10B H 0.8157 0.9328 0.5179 0.053 Uiso 1 1 calc R . . C104 C 0.9380(7) 0.8210(4) 0.4782(2) 0.0477(13) Uani 1 1 d . . . H10C H 0.8489 0.8189 0.4412 0.057 Uiso 1 1 calc R . . C105 C 1.0866(7) 0.7570(4) 0.4857(2) 0.0473(12) Uani 1 1 d . . . H10D H 1.1005 0.7105 0.4538 0.057 Uiso 1 1 calc R . . C106 C 1.2182(6) 0.7592(4) 0.5398(2) 0.0393(10) Uani 1 1 d . . . H10E H 1.3211 0.7143 0.5447 0.047 Uiso 1 1 calc R . . C111 C 1.5287(6) 0.7370(3) 0.65976(19) 0.0318(9) Uani 1 1 d . . . C112 C 1.5323(10) 0.6653(4) 0.7044(3) 0.0672(19) Uani 1 1 d . . . H11A H 1.4413 0.6653 0.7336 0.081 Uiso 1 1 calc R . . C113 C 1.6697(10) 0.5925(5) 0.7067(3) 0.082(2) Uani 1 1 d . . . H11B H 1.6717 0.5427 0.7375 0.099 Uiso 1 1 calc R . . C114 C 1.8016(8) 0.5922(4) 0.6649(3) 0.0587(15) Uani 1 1 d . . . H11C H 1.8961 0.5428 0.6670 0.070 Uiso 1 1 calc R . . C115 C 1.7968(7) 0.6632(3) 0.6203(3) 0.0504(14) Uani 1 1 d . . . H11D H 1.8866 0.6624 0.5907 0.060 Uiso 1 1 calc R . . C116 C 1.6631(6) 0.7357(4) 0.6180(2) 0.0441(12) Uani 1 1 d . . . H11E H 1.6629 0.7855 0.5873 0.053 Uiso 1 1 calc R . . C121 C 1.5008(6) 0.9432(3) 0.65095(19) 0.0297(9) Uani 1 1 d . . . C122 C 1.6504(6) 0.9618(4) 0.6979(2) 0.0417(11) Uani 1 1 d . . . H12A H 1.6726 0.9195 0.7331 0.050 Uiso 1 1 calc R . . C123 C 1.7659(6) 1.0410(4) 0.6936(2) 0.0475(13) Uani 1 1 d . . . H12B H 1.8692 1.0523 0.7255 0.057 Uiso 1 1 calc R . . C124 C 1.7343(7) 1.1043(4) 0.6438(3) 0.0495(13) Uani 1 1 d . . . H12C H 1.8126 1.1600 0.6421 0.059 Uiso 1 1 calc R . . C125 C 1.5880(8) 1.0865(4) 0.5962(3) 0.0600(15) Uani 1 1 d . . . H12D H 1.5669 1.1291 0.5611 0.072 Uiso 1 1 calc R . . C126 C 1.4719(7) 1.0053(4) 0.6002(2) 0.0472(12) Uani 1 1 d . . . H12E H 1.3715 0.9927 0.5675 0.057 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 0.03140(10) 0.03793(12) 0.02364(10) 0.00092(7) 0.01088(6) 0.00366(6) P1 0.0294(5) 0.0325(6) 0.0226(5) 0.0021(4) 0.0099(4) 0.0029(4) C1 0.032(2) 0.041(3) 0.023(2) 0.0015(17) 0.0101(16) 0.0049(17) C2 0.029(2) 0.039(2) 0.028(2) 0.0018(19) 0.0043(16) 0.0038(18) C3 0.0271(19) 0.037(2) 0.0229(19) 0.0056(17) 0.0097(15) 0.0050(16) C4 0.036(2) 0.065(3) 0.033(2) -0.014(2) 0.0094(19) -0.005(2) C5 0.025(2) 0.065(3) 0.037(2) -0.010(2) 0.0142(18) -0.006(2) C6 0.0225(17) 0.039(2) 0.0252(19) 0.0054(18) 0.0068(14) 0.0025(16) N1 0.0277(17) 0.056(3) 0.0370(19) -0.0105(18) 0.0142(14) -0.0047(16) C7 0.027(2) 0.057(3) 0.040(3) -0.008(2) 0.0143(18) -0.007(2) C101 0.030(2) 0.033(2) 0.027(2) 0.0049(17) 0.0061(16) -0.0056(16) C102 0.039(2) 0.036(3) 0.034(2) 0.0018(19) 0.0062(18) 0.0001(19) C103 0.034(2) 0.053(3) 0.044(3) 0.014(2) 0.0035(19) 0.000(2) C104 0.044(3) 0.064(4) 0.034(3) 0.002(2) -0.002(2) -0.010(2) C105 0.051(3) 0.055(3) 0.036(3) -0.015(2) 0.004(2) -0.008(2) C106 0.039(2) 0.043(3) 0.036(2) -0.005(2) 0.0081(19) -0.001(2) C111 0.033(2) 0.033(2) 0.031(2) 0.0068(18) 0.0103(16) 0.0014(17) C112 0.090(5) 0.054(4) 0.068(4) 0.030(3) 0.053(4) 0.031(3) C113 0.114(5) 0.057(4) 0.086(5) 0.047(4) 0.054(4) 0.042(4) C114 0.063(3) 0.050(3) 0.066(4) 0.006(3) 0.021(3) 0.022(3) C115 0.043(3) 0.044(3) 0.070(4) -0.001(3) 0.030(3) 0.002(2) C116 0.044(3) 0.040(3) 0.053(3) 0.015(2) 0.026(2) 0.008(2) C121 0.032(2) 0.031(2) 0.028(2) -0.0028(17) 0.0084(16) 0.0018(17) C122 0.041(2) 0.054(3) 0.029(2) 0.002(2) 0.0001(18) -0.005(2) C123 0.037(2) 0.062(4) 0.044(3) -0.012(2) 0.006(2) -0.009(2) C124 0.050(3) 0.042(3) 0.060(3) -0.009(3) 0.020(2) -0.013(2) C125 0.064(3) 0.052(4) 0.061(4) 0.021(3) -0.003(3) -0.014(3) C126 0.048(3) 0.048(3) 0.043(3) 0.015(2) -0.007(2) -0.012(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 C1 2.011(4) . ? Au1 P1 2.2769(11) . ? P1 C111 1.816(4) . ? P1 C101 1.816(4) . ? P1 C121 1.828(4) . ? C1 C2 1.197(6) . ? C2 C3 1.432(5) . ? C3 C7 1.389(6) . ? C3 C4 1.396(6) . ? C4 C5 1.376(6) . ? C5 C6 1.388(6) . ? C6 N1 1.344(5) . ? C6 C6 1.477(8) 3_677 ? N1 C7 1.332(5) . ? C101 C106 1.380(6) . ? C101 C102 1.401(6) . ? C102 C103 1.381(6) . ? C103 C104 1.359(7) . ? C104 C105 1.366(7) . ? C105 C106 1.394(6) . ? C111 C112 1.372(6) . ? C111 C116 1.381(6) . ? C112 C113 1.392(8) . ? C113 C114 1.368(8) . ? C114 C115 1.364(7) . ? C115 C116 1.372(6) . ? C121 C126 1.378(6) . ? C121 C122 1.391(6) . ? C122 C123 1.372(7) . ? C123 C124 1.373(7) . ? C124 C125 1.383(7) . ? C125 C126 1.396(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 P1 174.84(12) . . ? C111 P1 C101 107.4(2) . . ? C111 P1 C121 102.9(2) . . ? C101 P1 C121 104.93(18) . . ? C111 P1 Au1 116.17(14) . . ? C101 P1 Au1 109.07(14) . . ? C121 P1 Au1 115.45(13) . . ? C2 C1 Au1 169.2(4) . . ? C1 C2 C3 174.7(5) . . ? C7 C3 C4 116.1(4) . . ? C7 C3 C2 119.7(4) . . ? C4 C3 C2 124.2(4) . . ? C5 C4 C3 119.4(4) . . ? C4 C5 C6 120.3(4) . . ? N1 C6 C5 121.1(4) . . ? N1 C6 C6 115.7(4) . 3_677 ? C5 C6 C6 123.1(4) . 3_677 ? C7 N1 C6 117.8(4) . . ? N1 C7 C3 125.2(4) . . ? C106 C101 C102 119.2(4) . . ? C106 C101 P1 123.8(3) . . ? C102 C101 P1 116.9(3) . . ? C103 C102 C101 119.4(4) . . ? C104 C103 C102 121.2(5) . . ? C103 C104 C105 119.8(5) . . ? C104 C105 C106 120.7(5) . . ? C101 C106 C105 119.7(4) . . ? C112 C111 C116 118.9(4) . . ? C112 C111 P1 119.6(3) . . ? C116 C111 P1 121.4(3) . . ? C111 C112 C113 119.9(5) . . ? C114 C113 C112 120.4(5) . . ? C115 C114 C113 119.6(5) . . ? C114 C115 C116 120.4(5) . . ? C115 C116 C111 120.7(4) . . ? C126 C121 C122 118.8(4) . . ? C126 C121 P1 123.6(3) . . ? C122 C121 P1 117.6(3) . . ? C123 C122 C121 120.3(4) . . ? C122 C123 C124 120.9(4) . . ? C123 C124 C125 119.8(5) . . ? C124 C125 C126 119.3(5) . . ? C121 C126 C125 120.9(4) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.848 _refine_diff_density_min -1.630 _refine_diff_density_rms 0.129 ####END data_pr9935 _database_code_depnum_ccdc_archive 'CCDC 665745' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Complex 5' ; _chemical_name_common "'Complex 5'" _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H40 Au2 Cl4 N2 P2' _chemical_formula_weight 1290.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 9.4980(12) _cell_length_b 10.9270(8) _cell_length_c 12.4680(16) _cell_angle_alpha 72.057(6) _cell_angle_beta 81.173(5) _cell_angle_gamma 79.945(6) _cell_volume 1205.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8406 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 25.03 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.778 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 622 _exptl_absorpt_coefficient_mu 6.405 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.403 _exptl_absorpt_correction_T_max 0.429 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10292 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0572 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4218 _reflns_number_gt 3668 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; "Collect" data collection software, Nonius B.V., 1998. ; _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; "Collect" data collection software, Nonius B.V., 1998. ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1991)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One phenyl group is disorderd over two sites, the occupancy parameter was refined to 0.32182. The dichloromethane molecule is disorderd over two sites, the occupancy parameter was refined to 0.41863. ; _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^)+(0.0021P)^2^+0.8800P] 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 4218 _refine_ls_number_parameters 363 _refine_ls_number_restraints 419 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0655 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 0.996 _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 0.53100(2) 0.439728(16) 0.328057(17) 0.04545(9) Uani 1 1 d . A . P1 P 0.65331(13) 0.61113(10) 0.23932(11) 0.0392(3) Uani 1 1 d . . . N1 N 0.1416(4) 0.0991(3) 0.4689(3) 0.0351(8) Uani 1 1 d U . . C2 C 0.0680(4) 0.0009(4) 0.5235(4) 0.0342(10) Uani 1 1 d U . . C3 C 0.1126(5) -0.0971(4) 0.6184(4) 0.0450(12) Uani 1 1 d U . . H3 H 0.0551 -0.1637 0.6569 0.054 Uiso 1 1 calc R . . C4 C 0.2413(5) -0.0957(5) 0.6553(5) 0.0518(13) Uani 1 1 d U . . H4 H 0.2758 -0.1632 0.7181 0.062 Uiso 1 1 calc R . . C5 C 0.3189(5) 0.0041(4) 0.6004(4) 0.0465(12) Uani 1 1 d U . . H5 H 0.4076 0.0075 0.6251 0.056 Uiso 1 1 calc R . . C6 C 0.2660(5) 0.1015(4) 0.5072(4) 0.0382(10) Uani 1 1 d U . . C7 C 0.3465(5) 0.2095(4) 0.4474(4) 0.0422(11) Uani 1 1 d U A . C8 C 0.4153(5) 0.2926(4) 0.4045(4) 0.0412(11) Uani 1 1 d U . . C11 C 0.8225(5) 0.6049(4) 0.2925(4) 0.0424(11) Uani 1 1 d DU A . C12 C 0.9041(5) 0.4837(5) 0.3295(4) 0.0514(13) Uani 1 1 d DU . . H12 H 0.8675 0.4075 0.3312 0.062 Uiso 1 1 calc R A . C13 C 1.0384(6) 0.4743(6) 0.3638(5) 0.0675(16) Uani 1 1 d DU A . H13 H 1.0929 0.3914 0.3903 0.081 Uiso 1 1 calc R . . C14 C 1.0925(6) 0.5821(6) 0.3598(5) 0.0746(17) Uani 1 1 d DU . . H14 H 1.1867 0.5749 0.3799 0.090 Uiso 1 1 calc R A . C15 C 1.0121(6) 0.7022(6) 0.3269(6) 0.0751(17) Uani 1 1 d DU A . H15 H 1.0493 0.7772 0.3274 0.090 Uiso 1 1 calc R . . C16 C 0.8771(6) 0.7141(5) 0.2930(5) 0.0561(14) Uani 1 1 d DU . . H16 H 0.8218 0.7973 0.2700 0.067 Uiso 1 1 calc R A . C21 C 0.713(3) 0.637(3) 0.082(2) 0.048(6) Uani 0.32(3) 1 d PDU A 1 C22 C 0.839(3) 0.686(3) 0.029(2) 0.071(6) Uani 0.32(3) 1 d PDU A 1 H22 H 0.9013 0.7056 0.0720 0.085 Uiso 0.32(3) 1 calc PR A 1 C23 C 0.875(2) 0.705(4) -0.0863(19) 0.079(6) Uani 0.32(3) 1 d PDU A 1 H23 H 0.9606 0.7407 -0.1224 0.095 Uiso 0.32(3) 1 calc PR A 1 C24 C 0.787(4) 0.674(3) -0.149(2) 0.070(7) Uani 0.32(3) 1 d PDU A 1 H24 H 0.8160 0.6811 -0.2264 0.084 Uiso 0.32(3) 1 calc PR A 1 C25 C 0.658(4) 0.633(3) -0.099(2) 0.068(7) Uani 0.32(3) 1 d PDU A 1 H25 H 0.5947 0.6177 -0.1441 0.081 Uiso 0.32(3) 1 calc PR A 1 C26 C 0.620(3) 0.614(3) 0.016(3) 0.054(6) Uani 0.32(3) 1 d PDU A 1 H26 H 0.5304 0.5843 0.0504 0.065 Uiso 0.32(3) 1 calc PR A 1 C21' C 0.6929(14) 0.6253(13) 0.0917(11) 0.040(3) Uani 0.68(3) 1 d PDU A 2 C22' C 0.8306(13) 0.6229(15) 0.0370(10) 0.060(3) Uani 0.68(3) 1 d PDU A 2 H22' H 0.9097 0.6138 0.0785 0.072 Uiso 0.68(3) 1 calc PR A 2 C23' C 0.8546(13) 0.6336(18) -0.0773(10) 0.076(4) Uani 0.68(3) 1 d PDU A 2 H23' H 0.9500 0.6296 -0.1138 0.091 Uiso 0.68(3) 1 calc PR A 2 C24' C 0.7403(15) 0.6501(16) -0.1385(11) 0.062(3) Uani 0.68(3) 1 d PDU A 2 H24' H 0.7567 0.6600 -0.2176 0.074 Uiso 0.68(3) 1 calc PR A 2 C25' C 0.6022(15) 0.6524(13) -0.0850(12) 0.054(3) Uani 0.68(3) 1 d PDU A 2 H25' H 0.5236 0.6626 -0.1273 0.065 Uiso 0.68(3) 1 calc PR A 2 C26' C 0.5770(13) 0.6400(14) 0.0294(11) 0.046(3) Uani 0.68(3) 1 d PDU A 2 H26' H 0.4816 0.6415 0.0660 0.055 Uiso 0.68(3) 1 calc PR A 2 C31 C 0.5441(5) 0.7628(4) 0.2448(4) 0.0370(10) Uani 1 1 d DU A . C32 C 0.5569(5) 0.8783(4) 0.1591(4) 0.0496(13) Uani 1 1 d DU . . H32 H 0.6279 0.8807 0.0962 0.059 Uiso 1 1 calc R A . C33 C 0.4653(6) 0.9904(5) 0.1660(5) 0.0590(15) Uani 1 1 d DU A . H33 H 0.4750 1.0697 0.1082 0.071 Uiso 1 1 calc R . . C34 C 0.3605(6) 0.9873(5) 0.2562(5) 0.0587(14) Uani 1 1 d DU . . H34 H 0.2966 1.0637 0.2593 0.070 Uiso 1 1 calc R A . C35 C 0.3488(6) 0.8728(5) 0.3422(5) 0.0542(13) Uani 1 1 d DU A . H35 H 0.2782 0.8710 0.4053 0.065 Uiso 1 1 calc R . . C36 C 0.4392(5) 0.7612(4) 0.3364(4) 0.0444(11) Uani 1 1 d DU . . H36 H 0.4300 0.6826 0.3953 0.053 Uiso 1 1 calc R A . C99 C 0.887(3) 0.162(2) 1.033(3) 0.141(10) Uani 0.419(13) 1 d PDU B 1 H99A H 0.9878 0.1740 1.0021 0.169 Uiso 0.419(13) 1 calc PR B 1 H99B H 0.8880 0.1016 1.1110 0.169 Uiso 0.419(13) 1 calc PR B 1 Cl1 Cl 0.7882(7) 0.3109(5) 1.0376(6) 0.110(3) Uani 0.419(13) 1 d PD B 1 Cl2 Cl 0.8114(11) 0.0959(8) 0.9487(8) 0.138(4) Uani 0.419(13) 1 d PD B 1 C99' C 0.844(4) 0.089(3) 1.017(3) 0.190(11) Uani 0.581(13) 1 d PDU B 2 H99C H 0.8800 0.0669 1.0917 0.229 Uiso 0.581(13) 1 calc PR B 2 H99D H 0.7558 0.0475 1.0304 0.229 Uiso 0.581(13) 1 calc PR B 2 Cl1' Cl 0.968(13) -0.004(17) 0.944(11) 1.06(8) Uani 0.581(13) 1 d PD . 2 Cl2' Cl 0.781(2) 0.256(3) 0.986(3) 0.585(19) Uani 0.581(13) 1 d PD B 2 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 0.04256(13) 0.03689(12) 0.05378(14) -0.00635(8) -0.00822(9) -0.00672(8) P1 0.0399(7) 0.0341(6) 0.0420(7) -0.0103(5) -0.0038(6) -0.0025(5) N1 0.029(2) 0.0327(18) 0.042(2) -0.0123(16) -0.0013(17) -0.0003(14) C2 0.028(2) 0.032(2) 0.041(3) -0.0139(19) 0.0035(19) 0.0007(17) C3 0.041(3) 0.042(3) 0.048(3) -0.007(2) -0.005(2) -0.008(2) C4 0.043(3) 0.048(3) 0.057(3) -0.001(2) -0.015(3) -0.006(2) C5 0.042(3) 0.046(3) 0.052(3) -0.010(2) -0.016(2) -0.005(2) C6 0.031(2) 0.038(2) 0.047(3) -0.018(2) -0.002(2) -0.0004(17) C7 0.035(3) 0.043(3) 0.049(3) -0.014(2) -0.014(2) 0.004(2) C8 0.040(3) 0.039(2) 0.043(3) -0.010(2) -0.011(2) 0.002(2) C11 0.036(3) 0.048(3) 0.042(3) -0.017(2) 0.001(2) -0.0012(19) C12 0.052(3) 0.053(3) 0.046(3) -0.018(2) -0.008(3) 0.009(2) C13 0.052(4) 0.087(4) 0.051(3) -0.016(3) -0.009(3) 0.020(3) C14 0.039(3) 0.117(5) 0.068(4) -0.031(4) -0.009(3) -0.001(3) C15 0.054(4) 0.096(4) 0.089(5) -0.035(4) -0.014(3) -0.025(3) C16 0.050(3) 0.056(3) 0.065(4) -0.021(3) -0.005(3) -0.007(2) C21 0.046(12) 0.054(13) 0.043(10) -0.017(10) -0.004(8) 0.006(10) C22 0.059(9) 0.096(15) 0.055(8) -0.018(11) 0.004(8) -0.016(11) C23 0.065(11) 0.103(16) 0.054(8) -0.011(12) 0.007(8) -0.003(11) C24 0.073(15) 0.079(15) 0.043(9) -0.018(10) 0.007(9) 0.015(11) C25 0.077(15) 0.081(13) 0.050(9) -0.035(10) -0.008(12) 0.005(13) C26 0.065(13) 0.054(12) 0.050(10) -0.026(9) 0.004(9) -0.012(11) C21' 0.045(5) 0.033(5) 0.041(5) -0.014(5) 0.003(4) -0.005(4) C22' 0.047(5) 0.086(8) 0.048(5) -0.028(6) -0.002(4) -0.001(5) C23' 0.058(6) 0.121(11) 0.050(5) -0.039(7) 0.005(4) 0.001(6) C24' 0.071(9) 0.075(7) 0.040(6) -0.026(6) 0.004(5) 0.000(7) C25' 0.062(6) 0.053(5) 0.052(6) -0.024(4) -0.016(6) 0.004(5) C26' 0.043(5) 0.054(6) 0.041(5) -0.019(4) -0.001(4) -0.003(5) C31 0.037(3) 0.041(2) 0.033(3) -0.0114(19) -0.007(2) -0.0035(19) C32 0.055(3) 0.045(3) 0.039(3) -0.009(2) 0.002(2) 0.003(2) C33 0.082(4) 0.039(3) 0.050(3) -0.011(2) -0.015(3) 0.011(2) C34 0.061(4) 0.052(3) 0.067(4) -0.029(3) -0.021(3) 0.018(2) C35 0.045(3) 0.066(3) 0.062(3) -0.039(3) 0.002(3) -0.005(2) C36 0.045(3) 0.049(3) 0.043(3) -0.019(2) -0.003(2) -0.009(2) C99 0.18(3) 0.13(2) 0.137(18) -0.082(17) -0.062(17) 0.032(18) Cl1 0.119(5) 0.069(4) 0.130(6) -0.014(3) -0.025(3) 0.005(3) Cl2 0.188(8) 0.148(6) 0.103(6) -0.051(5) 0.010(5) -0.083(5) C99' 0.28(3) 0.15(2) 0.18(2) -0.09(2) -0.07(2) 0.004(19) Cl1' 1.17(15) 1.09(8) 0.9(2) -0.34(15) -0.04(13) -0.09(11) Cl2' 0.34(3) 0.62(4) 0.74(5) -0.10(4) -0.10(3) -0.08(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 C8 2.013(5) . ? Au1 P1 2.2738(12) . ? P1 C21' 1.785(13) . ? P1 C31 1.809(4) . ? P1 C11 1.813(5) . ? P1 C21 1.91(3) . ? N1 C2 1.330(5) . ? N1 C6 1.348(6) . ? C2 C3 1.392(6) . ? C2 C2 1.504(9) 2_556 ? C3 C4 1.375(7) . ? C4 C5 1.367(7) . ? C5 C6 1.402(6) . ? C6 C7 1.460(7) . ? C7 C8 1.157(6) . ? C11 C16 1.383(6) . ? C11 C12 1.394(6) . ? C12 C13 1.384(7) . ? C13 C14 1.350(8) . ? C14 C15 1.374(8) . ? C15 C16 1.384(7) . ? C21 C22 1.386(14) . ? C21 C26 1.394(14) . ? C22 C23 1.381(15) . ? C23 C24 1.369(15) . ? C24 C25 1.368(15) . ? C25 C26 1.387(15) . ? C21' C22' 1.379(10) . ? C21' C26' 1.401(10) . ? C22' C23' 1.380(10) . ? C23' C24' 1.376(11) . ? C24' C25' 1.378(11) . ? C25' C26' 1.378(10) . ? C31 C32 1.390(6) . ? C31 C36 1.393(6) . ? C32 C33 1.391(6) . ? C33 C34 1.379(7) . ? C34 C35 1.383(7) . ? C35 C36 1.378(6) . ? C99 Cl2 1.741(17) . ? C99 Cl1 1.744(18) . ? C99' Cl1' 1.75(2) . ? C99' Cl2' 1.759(19) . ? Cl1' Cl1' 1.63(19) 2_757 ? Cl1' C99' 1.91(9) 2_757 ? 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 C8 Au1 P1 177.68(12) . . ? C21' P1 C31 104.7(5) . . ? C21' P1 C11 106.8(5) . . ? C31 P1 C11 107.9(2) . . ? C21' P1 C21 6.6(12) . . ? C31 P1 C21 103.6(9) . . ? C11 P1 C21 101.2(9) . . ? C21' P1 Au1 110.3(4) . . ? C31 P1 Au1 111.14(15) . . ? C11 P1 Au1 115.40(15) . . ? C21 P1 Au1 116.4(9) . . ? C2 N1 C6 117.7(4) . . ? N1 C2 C3 123.1(4) . . ? N1 C2 C2 116.3(4) . 2_556 ? C3 C2 C2 120.6(5) . 2_556 ? C4 C3 C2 118.9(4) . . ? C5 C4 C3 119.0(4) . . ? C4 C5 C6 119.2(5) . . ? N1 C6 C5 122.1(4) . . ? N1 C6 C7 117.7(4) . . ? C5 C6 C7 120.2(4) . . ? C8 C7 C6 176.3(5) . . ? C7 C8 Au1 178.6(4) . . ? C16 C11 C12 118.9(5) . . ? C16 C11 P1 123.4(4) . . ? C12 C11 P1 117.6(4) . . ? C13 C12 C11 120.0(5) . . ? C14 C13 C12 120.5(5) . . ? C13 C14 C15 120.4(6) . . ? C14 C15 C16 120.2(6) . . ? C11 C16 C15 120.0(5) . . ? C22 C21 C26 119.0(17) . . ? C22 C21 P1 122.9(18) . . ? C26 C21 P1 117.9(17) . . ? C23 C22 C21 120.4(16) . . ? C24 C23 C22 120.0(16) . . ? C25 C24 C23 120.3(18) . . ? C24 C25 C26 120.4(17) . . ? C25 C26 C21 119.6(16) . . ? C22' C21' C26' 119.2(9) . . ? C22' C21' P1 123.2(9) . . ? C26' C21' P1 117.6(8) . . ? C21' C22' C23' 120.6(9) . . ? C24' C23' C22' 120.0(9) . . ? C23' C24' C25' 120.0(9) . . ? C26' C25' C24' 120.5(9) . . ? C25' C26' C21' 119.7(8) . . ? C32 C31 C36 119.3(4) . . ? C32 C31 P1 122.5(3) . . ? C36 C31 P1 118.1(3) . . ? C31 C32 C33 119.7(5) . . ? C34 C33 C32 120.5(5) . . ? C33 C34 C35 119.8(5) . . ? C36 C35 C34 120.1(5) . . ? C35 C36 C31 120.5(4) . . ? Cl2 C99 Cl1 109.9(14) . . ? Cl1' C99' Cl2' 133(7) . . ? Cl1' Cl1' C99' 69(3) 2_757 . ? Cl1' Cl1' C99' 58(5) 2_757 2_757 ? C99' Cl1' C99' 128(5) . 2_757 ? 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 C8 Au1 P1 C21' -83(4) . . . . ? C8 Au1 P1 C31 33(4) . . . . ? C8 Au1 P1 C11 156(3) . . . . ? C8 Au1 P1 C21 -85(4) . . . . ? C6 N1 C2 C3 1.0(6) . . . . ? C6 N1 C2 C2 -178.2(4) . . . 2_556 ? N1 C2 C3 C4 -2.6(7) . . . . ? C2 C2 C3 C4 176.7(5) 2_556 . . . ? C2 C3 C4 C5 2.3(8) . . . . ? C3 C4 C5 C6 -0.8(8) . . . . ? C2 N1 C6 C5 0.7(6) . . . . ? C2 N1 C6 C7 -179.8(4) . . . . ? C4 C5 C6 N1 -0.8(7) . . . . ? C4 C5 C6 C7 179.7(5) . . . . ? N1 C6 C7 C8 173(8) . . . . ? C5 C6 C7 C8 -7(8) . . . . ? C6 C7 C8 Au1 -159(15) . . . . ? P1 Au1 C8 C7 12(23) . . . . ? C21' P1 C11 C16 89.1(6) . . . . ? C31 P1 C11 C16 -23.0(5) . . . . ? C21 P1 C11 C16 85.5(10) . . . . ? Au1 P1 C11 C16 -147.9(4) . . . . ? C21' P1 C11 C12 -87.7(6) . . . . ? C31 P1 C11 C12 160.3(4) . . . . ? C21 P1 C11 C12 -91.3(10) . . . . ? Au1 P1 C11 C12 35.4(4) . . . . ? C16 C11 C12 C13 -1.2(7) . . . . ? P1 C11 C12 C13 175.7(4) . . . . ? C11 C12 C13 C14 -1.2(8) . . . . ? C12 C13 C14 C15 3.1(9) . . . . ? C13 C14 C15 C16 -2.6(10) . . . . ? C12 C11 C16 C15 1.7(8) . . . . ? P1 C11 C16 C15 -175.0(5) . . . . ? C14 C15 C16 C11 0.2(10) . . . . ? C21' P1 C21 C22 -169(13) . . . . ? C31 P1 C21 C22 91(2) . . . . ? C11 P1 C21 C22 -20(2) . . . . ? Au1 P1 C21 C22 -146.4(17) . . . . ? C21' P1 C21 C26 15(10) . . . . ? C31 P1 C21 C26 -85(2) . . . . ? C11 P1 C21 C26 164(2) . . . . ? Au1 P1 C21 C26 38(3) . . . . ? C26 C21 C22 C23 -3(2) . . . . ? P1 C21 C22 C23 -179(2) . . . . ? C21 C22 C23 C24 -2(2) . . . . ? C22 C23 C24 C25 5(4) . . . . ? C23 C24 C25 C26 -5(5) . . . . ? C24 C25 C26 C21 1(4) . . . . ? C22 C21 C26 C25 3(3) . . . . ? P1 C21 C26 C25 179(2) . . . . ? C31 P1 C21' C22' 117.8(11) . . . . ? C11 P1 C21' C22' 3.6(12) . . . . ? C21 P1 C21' C22' 36(11) . . . . ? Au1 P1 C21' C22' -122.5(10) . . . . ? C31 P1 C21' C26' -61.9(10) . . . . ? C11 P1 C21' C26' -176.1(9) . . . . ? C21 P1 C21' C26' -144(12) . . . . ? Au1 P1 C21' C26' 57.8(11) . . . . ? C26' C21' C22' C23' -0.6(13) . . . . ? P1 C21' C22' C23' 179.7(9) . . . . ? C21' C22' C23' C24' 1.7(13) . . . . ? C22' C23' C24' C25' -1.8(18) . . . . ? C23' C24' C25' C26' 1(2) . . . . ? C24' C25' C26' C21' 0.1(17) . . . . ? C22' C21' C26' C25' -0.3(16) . . . . ? P1 C21' C26' C25' 179.5(9) . . . . ? C21' P1 C31 C32 -29.1(6) . . . . ? C11 P1 C31 C32 84.3(4) . . . . ? C21 P1 C31 C32 -22.4(10) . . . . ? Au1 P1 C31 C32 -148.2(3) . . . . ? C21' P1 C31 C36 147.9(5) . . . . ? C11 P1 C31 C36 -98.6(4) . . . . ? C21 P1 C31 C36 154.6(10) . . . . ? Au1 P1 C31 C36 28.9(4) . . . . ? C36 C31 C32 C33 0.1(7) . . . . ? P1 C31 C32 C33 177.1(4) . . . . ? C31 C32 C33 C34 -1.0(7) . . . . ? C32 C33 C34 C35 1.8(8) . . . . ? C33 C34 C35 C36 -1.6(8) . . . . ? C34 C35 C36 C31 0.6(7) . . . . ? C32 C31 C36 C35 0.1(7) . . . . ? P1 C31 C36 C35 -177.1(4) . . . . ? Cl2' C99' Cl1' Cl1' 109(13) . . . 2_757 ? Cl2' C99' Cl1' C99' 109(13) . . . 2_757 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.802 _refine_diff_density_min -0.889 _refine_diff_density_rms 0.096