Electronic Supplementary Material for CrystEngComm This Journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Edward R.T. Tiekink' _publ_contact_author_address ; Department of Chemistry The University of Texas at San Antonio 6900 Nth Loop 1604 West San Antonio Texas 78249-0698 UNITED STATES OF AMERICA ; _publ_contact_author_email EDWARD.TIEKINK@UTSA.EDU _publ_section_title ; Supramolecular aggregation patterns in the crystal structures of the dinuclear phosphinegold(I) thiolates, [(Ph2P(CH2)4PPh2){AuSC(OR)=NC6H4Y-4}2] for R = Me, Et & iPr, and Y = H, NO2 & Me: the influence on intermolecular interactions exerted by R and Y ; loop_ _publ_author_name 'Edward R.T. Tiekink' 'Soo Yei Ho.' data_dppb[Au(SC(OMe)=NC6H5)]2.2CH2Cl2(1) _database_code_depnum_ccdc_archive 'CCDC 632737' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C46 H48 Au2 Cl4 N2 O2 P2 S2' _chemical_formula_weight 1322.66 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.9628(6) _cell_length_b 10.6131(7) _cell_length_c 12.7053(8) _cell_angle_alpha 114.135(1) _cell_angle_beta 98.032(1) _cell_angle_gamma 92.760(1) _cell_volume 1205.68(13) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4879 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 29.6 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.822 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 642 _exptl_absorpt_coefficient_mu 6.491 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.649 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details '(SADABS, Bruker, 2000 & Blessing, 1995)' _diffrn_ambient_temperature 223(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 'Bruker AXS SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10047 _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_av_sigmaI/netI 0.045 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.8 _diffrn_reflns_theta_max 30.0 _reflns_number_total 6865 _reflns_number_gt 6183 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'Bruker SHEXLTL (Bruker, 2000)' _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^)+(0.0234P)^2^] 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 6865 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.031 _refine_ls_R_factor_gt 0.027 _refine_ls_wR_factor_ref 0.059 _refine_ls_wR_factor_gt 0.057 _refine_ls_goodness_of_fit_ref 1.00 _refine_ls_restrained_S_all 1.00 _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 Au Au 0.091194(11) 0.404745(12) 0.076744(10) 0.02137(4) Uani 1 1 d . . . Cl1 Cl 0.7888(2) 0.1187(2) 0.66240(15) 0.1094(6) Uani 1 1 d . . . Cl2 Cl 0.71550(16) 0.1935(2) 0.8928(2) 0.1101(6) Uani 1 1 d . . . S1 S -0.07033(9) 0.53598(10) 0.17095(7) 0.03190(18) Uani 1 1 d . . . P1 P 0.25024(7) 0.26465(8) 0.00259(7) 0.01872(14) Uani 1 1 d . . . O1 O 0.1273(2) 0.5490(3) 0.3341(2) 0.0373(6) Uani 1 1 d . . . N1 N -0.0624(3) 0.6332(3) 0.4053(2) 0.0339(7) Uani 1 1 d . . . C1 C -0.0032(3) 0.5778(4) 0.3184(3) 0.0283(7) Uani 1 1 d . . . C2 C -0.2008(3) 0.6570(4) 0.3883(3) 0.0309(7) Uani 1 1 d . . . C3 C -0.3054(4) 0.5473(5) 0.3456(3) 0.0404(9) Uani 1 1 d . . . H3 H -0.2836 0.4557 0.3226 0.048 Uiso 1 1 calc R . . C4 C -0.4398(4) 0.5713(5) 0.3365(3) 0.0495(11) Uani 1 1 d . . . H4 H -0.5093 0.4964 0.3075 0.059 Uiso 1 1 calc R . . C5 C -0.4726(4) 0.7042(6) 0.3698(4) 0.0565(13) Uani 1 1 d . . . H5 H -0.5646 0.7206 0.3636 0.068 Uiso 1 1 calc R . . C6 C -0.3709(4) 0.8139(5) 0.4124(4) 0.0527(11) Uani 1 1 d . . . H6 H -0.3935 0.9050 0.4338 0.063 Uiso 1 1 calc R . . C7 C -0.2343(4) 0.7902(4) 0.4240(3) 0.0405(9) Uani 1 1 d . . . H7 H -0.1652 0.8657 0.4564 0.049 Uiso 1 1 calc R . . C8 C 0.1883(4) 0.5791(5) 0.4524(3) 0.0481(11) Uani 1 1 d . . . H8A H 0.1931 0.6781 0.5005 0.072 Uiso 1 1 calc R . . H8B H 0.2796 0.5512 0.4536 0.072 Uiso 1 1 calc R . . H8C H 0.1334 0.5284 0.4829 0.072 Uiso 1 1 calc R . . C9 C 0.3729(3) 0.3311(3) -0.0608(3) 0.0214(6) Uani 1 1 d . . . H9A H 0.4346 0.2610 -0.0925 0.026 Uiso 1 1 calc R . . H9B H 0.3243 0.3474 -0.1259 0.026 Uiso 1 1 calc R . . C10 C 0.4572(3) 0.4664(3) 0.0284(3) 0.0244(6) Uani 1 1 d . . . H10A H 0.5172 0.4470 0.0866 0.029 Uiso 1 1 calc R . . H10B H 0.3956 0.5314 0.0694 0.029 Uiso 1 1 calc R . . C11 C 0.3470(3) 0.2303(3) 0.1180(3) 0.0216(6) Uani 1 1 d . . . C12 C 0.2959(3) 0.2576(4) 0.2210(3) 0.0308(7) Uani 1 1 d . . . H12 H 0.2125 0.2952 0.2305 0.037 Uiso 1 1 calc R . . C13 C 0.3669(4) 0.2297(5) 0.3095(3) 0.0439(9) Uani 1 1 d . . . H13 H 0.3312 0.2473 0.3783 0.053 Uiso 1 1 calc R . . C14 C 0.4894(4) 0.1762(4) 0.2966(3) 0.0416(9) Uani 1 1 d . . . H14 H 0.5380 0.1588 0.3572 0.050 Uiso 1 1 calc R . . C15 C 0.5416(3) 0.1478(4) 0.1950(3) 0.0397(9) Uani 1 1 d . . . H15 H 0.6250 0.1101 0.1863 0.048 Uiso 1 1 calc R . . C16 C 0.4704(3) 0.1751(4) 0.1053(3) 0.0305(7) Uani 1 1 d . . . H16 H 0.5061 0.1561 0.0364 0.037 Uiso 1 1 calc R . . C17 C 0.1797(3) 0.0941(3) -0.1101(3) 0.0216(6) Uani 1 1 d . . . C18 C 0.1415(4) -0.0124(4) -0.0799(3) 0.0345(8) Uani 1 1 d . . . H18 H 0.1549 0.0033 -0.0006 0.041 Uiso 1 1 calc R . . C19 C 0.0839(4) -0.1416(4) -0.1653(4) 0.0426(9) Uani 1 1 d . . . H19 H 0.0594 -0.2134 -0.1439 0.051 Uiso 1 1 calc R . . C20 C 0.0629(4) -0.1644(4) -0.2811(4) 0.0412(9) Uani 1 1 d . . . H20 H 0.0228 -0.2516 -0.3391 0.049 Uiso 1 1 calc R . . C21 C 0.1000(4) -0.0607(4) -0.3122(3) 0.0410(9) Uani 1 1 d . . . H21 H 0.0865 -0.0773 -0.3918 0.049 Uiso 1 1 calc R . . C22 C 0.1575(4) 0.0695(4) -0.2271(3) 0.0347(8) Uani 1 1 d . . . H22 H 0.1814 0.1409 -0.2491 0.042 Uiso 1 1 calc R . . C23 C 0.8330(6) 0.1613(9) 0.8075(6) 0.118(3) Uani 1 1 d . . . H23A H 0.8798 0.0855 0.8152 0.141 Uiso 1 1 calc R . . H23B H 0.9006 0.2438 0.8403 0.141 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 Au 0.02400(6) 0.02329(6) 0.01900(6) 0.00943(4) 0.00753(4) 0.00682(4) Cl1 0.1240(14) 0.1029(14) 0.0719(10) 0.0098(9) -0.0043(10) 0.0528(11) Cl2 0.0738(10) 0.1344(17) 0.1494(18) 0.0750(15) 0.0499(11) 0.0335(10) S1 0.0369(4) 0.0439(5) 0.0209(4) 0.0157(4) 0.0107(3) 0.0241(4) P1 0.0191(3) 0.0193(4) 0.0184(4) 0.0078(3) 0.0056(3) 0.0019(3) O1 0.0325(12) 0.0564(17) 0.0227(12) 0.0144(12) 0.0059(10) 0.0187(11) N1 0.0299(14) 0.0479(19) 0.0213(14) 0.0105(13) 0.0076(11) 0.0092(13) C1 0.0300(16) 0.0355(18) 0.0223(16) 0.0135(14) 0.0069(13) 0.0103(13) C2 0.0282(16) 0.049(2) 0.0165(14) 0.0137(14) 0.0059(12) 0.0089(15) C3 0.0391(19) 0.054(3) 0.0237(17) 0.0127(17) 0.0041(15) 0.0013(17) C4 0.0347(19) 0.081(3) 0.030(2) 0.024(2) 0.0015(16) -0.004(2) C5 0.032(2) 0.109(4) 0.040(2) 0.042(3) 0.0077(18) 0.016(2) C6 0.057(3) 0.068(3) 0.046(2) 0.031(2) 0.020(2) 0.032(2) C7 0.045(2) 0.044(2) 0.034(2) 0.0152(17) 0.0147(17) 0.0099(17) C8 0.0329(19) 0.081(3) 0.0256(19) 0.018(2) 0.0005(15) 0.0165(19) C9 0.0200(13) 0.0249(15) 0.0215(14) 0.0113(12) 0.0061(11) 0.0022(11) C10 0.0286(15) 0.0231(15) 0.0222(15) 0.0103(12) 0.0061(12) -0.0034(12) C11 0.0219(13) 0.0227(15) 0.0224(15) 0.0113(12) 0.0054(11) 0.0021(11) C12 0.0302(16) 0.043(2) 0.0240(16) 0.0171(15) 0.0082(13) 0.0129(14) C13 0.052(2) 0.060(3) 0.033(2) 0.0268(19) 0.0171(18) 0.0212(19) C14 0.046(2) 0.052(2) 0.0311(19) 0.0228(18) 0.0011(17) 0.0130(18) C15 0.0293(17) 0.050(2) 0.047(2) 0.0253(19) 0.0075(16) 0.0163(16) C16 0.0302(16) 0.0346(19) 0.0313(18) 0.0160(15) 0.0106(14) 0.0117(14) C17 0.0185(13) 0.0201(14) 0.0247(15) 0.0066(12) 0.0070(11) 0.0044(11) C18 0.0417(19) 0.0305(19) 0.0301(18) 0.0111(15) 0.0118(15) -0.0076(15) C19 0.046(2) 0.0270(19) 0.050(2) 0.0105(17) 0.0163(18) -0.0114(16) C20 0.0327(18) 0.030(2) 0.044(2) -0.0006(16) 0.0083(16) -0.0063(15) C21 0.049(2) 0.034(2) 0.0284(18) 0.0048(15) -0.0016(17) 0.0014(17) C22 0.0438(19) 0.0288(18) 0.0278(17) 0.0115(14) -0.0024(15) -0.0019(15) C23 0.065(4) 0.184(8) 0.080(5) 0.035(5) 0.014(3) -0.022(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 Au P1 2.2601(8) . ? Au S1 2.3137(8) . ? Cl1 C23 1.694(7) . ? Cl2 C23 1.659(6) . ? S1 C1 1.759(3) . ? P1 C17 1.816(3) . ? P1 C11 1.813(3) . ? P1 C9 1.816(3) . ? O1 C1 1.357(4) . ? O1 C8 1.436(4) . ? N1 C1 1.264(4) . ? N1 C2 1.416(4) . ? C2 C7 1.372(5) . ? C2 C3 1.394(5) . ? C3 C4 1.374(5) . ? C3 H3 0.9400 . ? C4 C5 1.367(7) . ? C4 H4 0.9400 . ? C5 C6 1.376(7) . ? C5 H5 0.9400 . ? C6 C7 1.394(5) . ? C6 H6 0.9400 . ? C7 H7 0.9400 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 C10 1.529(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C10 1.514(5) 2_665 ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C16 1.389(4) . ? C11 C12 1.395(4) . ? C12 C13 1.387(5) . ? C12 H12 0.9400 . ? C13 C14 1.373(5) . ? C13 H13 0.9400 . ? C14 C15 1.384(5) . ? C14 H14 0.9400 . ? C15 C16 1.396(5) . ? C15 H15 0.9400 . ? C16 H16 0.9400 . ? C17 C22 1.383(4) . ? C17 C18 1.387(4) . ? C18 C19 1.386(5) . ? C18 H18 0.9400 . ? C19 C20 1.373(6) . ? C19 H19 0.9400 . ? C20 C21 1.365(5) . ? C20 H20 0.9400 . ? C21 C22 1.392(5) . ? C21 H21 0.9400 . ? C22 H22 0.9400 . ? C23 H23A 0.9800 . ? C23 H23B 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 Au S1 172.37(3) . . ? C1 S1 Au 101.31(11) . . ? C17 P1 C11 104.73(14) . . ? C17 P1 C9 105.29(14) . . ? C11 P1 C9 106.88(13) . . ? C17 P1 Au 114.04(9) . . ? C11 P1 Au 109.05(10) . . ? C9 P1 Au 116.04(10) . . ? C1 O1 C8 116.0(3) . . ? C1 N1 C2 120.3(3) . . ? N1 C1 O1 120.3(3) . . ? N1 C1 S1 126.7(3) . . ? O1 C1 S1 113.0(2) . . ? C7 C2 N1 120.1(3) . . ? C7 C2 C3 118.8(3) . . ? N1 C2 C3 120.9(3) . . ? C4 C3 C2 120.9(4) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C5 C4 C3 120.0(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.0(4) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C7 120.1(4) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C2 C7 C6 120.1(4) . . ? C2 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? O1 C8 H8A 109.5 . . ? O1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 P1 112.4(2) . . ? C10 C9 H9A 109.1 . . ? P1 C9 H9A 109.1 . . ? C10 C9 H9B 109.1 . . ? P1 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? C9 C10 C10 112.2(3) . 2_665 ? C9 C10 H10A 109.2 . . ? C10 C10 H10A 109.2 2_665 . ? C9 C10 H10B 109.2 . . ? C10 C10 H10B 109.2 2_665 . ? H10A C10 H10B 107.9 . . ? C16 C11 C12 119.1(3) . . ? C16 C11 P1 121.3(2) . . ? C12 C11 P1 119.6(2) . . ? C13 C12 C11 120.6(3) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 119.9(3) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.5(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.9(3) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C11 C16 C15 120.0(3) . . ? C11 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C22 C17 C18 118.7(3) . . ? C22 C17 P1 120.8(2) . . ? C18 C17 P1 120.5(2) . . ? C17 C18 C19 120.8(3) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C20 C19 C18 119.8(3) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 120.2(3) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C22 120.4(4) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C17 C22 C21 120.1(3) . . ? C17 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? Cl2 C23 Cl1 120.6(4) . . ? Cl2 C23 H23A 107.2 . . ? Cl1 C23 H23A 107.2 . . ? Cl2 C23 H23B 107.2 . . ? Cl1 C23 H23B 107.2 . . ? H23A C23 H23B 106.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Au S1 C1 38.4(3) . . . . ? S1 Au P1 C17 90.5(2) . . . . ? S1 Au P1 C11 -26.2(3) . . . . ? S1 Au P1 C9 -146.9(2) . . . . ? C2 N1 C1 O1 -176.9(3) . . . . ? C2 N1 C1 S1 5.6(5) . . . . ? C8 O1 C1 N1 2.8(5) . . . . ? C8 O1 C1 S1 -179.3(3) . . . . ? Au S1 C1 N1 -169.8(3) . . . . ? Au S1 C1 O1 12.5(3) . . . . ? C1 N1 C2 C7 -111.9(4) . . . . ? C1 N1 C2 C3 74.2(5) . . . . ? C7 C2 C3 C4 1.5(5) . . . . ? N1 C2 C3 C4 175.6(3) . . . . ? C2 C3 C4 C5 -0.1(6) . . . . ? C3 C4 C5 C6 0.0(6) . . . . ? C4 C5 C6 C7 -1.3(6) . . . . ? N1 C2 C7 C6 -177.0(3) . . . . ? C3 C2 C7 C6 -2.9(5) . . . . ? C5 C6 C7 C2 2.8(6) . . . . ? C17 P1 C9 C10 -172.1(2) . . . . ? C11 P1 C9 C10 -61.0(2) . . . . ? Au P1 C9 C10 60.8(2) . . . . ? P1 C9 C10 C10 -170.8(3) . . . 2_665 ? C17 P1 C11 C16 72.8(3) . . . . ? C9 P1 C11 C16 -38.6(3) . . . . ? Au P1 C11 C16 -164.8(2) . . . . ? C17 P1 C11 C12 -106.1(3) . . . . ? C9 P1 C11 C12 142.5(3) . . . . ? Au P1 C11 C12 16.3(3) . . . . ? C16 C11 C12 C13 -0.2(5) . . . . ? P1 C11 C12 C13 178.8(3) . . . . ? C11 C12 C13 C14 0.8(6) . . . . ? C12 C13 C14 C15 -1.1(6) . . . . ? C13 C14 C15 C16 0.8(6) . . . . ? C12 C11 C16 C15 -0.1(5) . . . . ? P1 C11 C16 C15 -179.0(3) . . . . ? C14 C15 C16 C11 -0.2(6) . . . . ? C11 P1 C17 C22 -148.9(3) . . . . ? C9 P1 C17 C22 -36.3(3) . . . . ? Au P1 C17 C22 92.0(3) . . . . ? C11 P1 C17 C18 34.0(3) . . . . ? C9 P1 C17 C18 146.5(3) . . . . ? Au P1 C17 C18 -85.1(3) . . . . ? C22 C17 C18 C19 0.9(5) . . . . ? P1 C17 C18 C19 178.1(3) . . . . ? C17 C18 C19 C20 -0.7(6) . . . . ? C18 C19 C20 C21 0.8(6) . . . . ? C19 C20 C21 C22 -0.9(6) . . . . ? C18 C17 C22 C21 -1.0(5) . . . . ? P1 C17 C22 C21 -178.2(3) . . . . ? C20 C21 C22 C17 1.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 30.0 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.06 # # 0.80 A from Au # _refine_diff_density_min -1.07 # # 0.29 A from Cl2 # _refine_diff_density_rms 0.122 # Attachment '21.CIF' data_dppb[Au(SC(OEt)=NC6H5)]2(2) _database_code_depnum_ccdc_archive 'CCDC 632738' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C46 H48 Au2 N2 O2 P2 S2' _chemical_formula_weight 1180.86 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' 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' S S 0.1246 0.1234 '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 8.4818(6) _cell_length_b 11.9828(8) _cell_length_c 12.1684(8) _cell_angle_alpha 105.973(1) _cell_angle_beta 99.485(1) _cell_angle_gamma 106.821(1) _cell_volume 1097.24(13) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5728 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 29.9 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.787 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 574 _exptl_absorpt_coefficient_mu 6.885 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.462 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details '(SADABS, Bruker, 2000 & Blessing, 1995)' _diffrn_ambient_temperature 223(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 'Bruker AXS SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9225 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_av_sigmaI/netI 0.043 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.8 _diffrn_reflns_theta_max 30.0 _reflns_number_total 6265 _reflns_number_gt 5960 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'Bruker SHEXLTL (Bruker, 2000)' _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^)+(0.0424P)^2^+0.2837P] 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 6265 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.038 _refine_ls_R_factor_gt 0.035 _refine_ls_wR_factor_ref 0.090 _refine_ls_wR_factor_gt 0.089 _refine_ls_goodness_of_fit_ref 1.16 _refine_ls_restrained_S_all 1.16 _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 Au Au 0.198667(19) 0.057701(13) 0.260308(13) 0.03209(6) Uani 1 1 d . . . S1 S 0.22430(19) 0.24270(11) 0.39730(10) 0.0435(3) Uani 1 1 d . . . P1 P 0.15975(13) -0.11539(10) 0.11005(9) 0.02880(19) Uani 1 1 d . . . O1 O 0.2337(4) 0.0979(3) 0.5199(3) 0.0404(7) Uani 1 1 d . . . N1 N 0.2118(5) 0.2794(3) 0.6255(3) 0.0361(7) Uani 1 1 d . . . C1 C 0.2232(5) 0.2107(4) 0.5293(4) 0.0344(8) Uani 1 1 d . . . C2 C 0.2023(5) 0.3975(4) 0.6375(4) 0.0356(8) Uani 1 1 d . . . C3 C 0.0728(7) 0.4259(5) 0.6827(6) 0.0563(14) Uani 1 1 d . . . H3 H -0.0026 0.3680 0.7061 0.068 Uiso 1 1 calc R . . C4 C 0.0552(9) 0.5387(6) 0.6932(8) 0.073(2) Uani 1 1 d . . . H4 H -0.0367 0.5549 0.7196 0.087 Uiso 1 1 calc R . . C5 C 0.1683(8) 0.6280(5) 0.6662(6) 0.0634(16) Uani 1 1 d . . . H5 H 0.1557 0.7051 0.6752 0.076 Uiso 1 1 calc R . . C6 C 0.3007(7) 0.6028(5) 0.6257(5) 0.0483(11) Uani 1 1 d . . . H6 H 0.3795 0.6634 0.6071 0.058 Uiso 1 1 calc R . . C7 C 0.3190(6) 0.4895(5) 0.6120(4) 0.0418(10) Uani 1 1 d . . . H7 H 0.4111 0.4740 0.5853 0.050 Uiso 1 1 calc R . . C8 C 0.2206(7) 0.0588(5) 0.6205(4) 0.0442(10) Uani 1 1 d . . . H8A H 0.1070 0.0480 0.6337 0.053 Uiso 1 1 calc R . . H8B H 0.3065 0.1206 0.6920 0.053 Uiso 1 1 calc R . . C8A C 0.2507(9) -0.0638(5) 0.5917(6) 0.0595(15) Uani 1 1 d . . . H8A1 H 0.2431 -0.0943 0.6574 0.089 Uiso 1 1 calc R . . H8A2 H 0.3633 -0.0516 0.5787 0.089 Uiso 1 1 calc R . . H8A3 H 0.1649 -0.1237 0.5207 0.089 Uiso 1 1 calc R . . C9 C 0.2654(5) -0.0844(4) -0.0033(4) 0.0348(8) Uani 1 1 d . . . H9A H 0.2462 -0.1634 -0.0646 0.042 Uiso 1 1 calc R . . H9B H 0.2140 -0.0361 -0.0408 0.042 Uiso 1 1 calc R . . C10 C 0.4563(5) -0.0140(4) 0.0468(4) 0.0334(8) Uani 1 1 d . . . H10A H 0.5080 -0.0632 0.0829 0.040 Uiso 1 1 calc R . . H10B H 0.4755 0.0641 0.1093 0.040 Uiso 1 1 calc R . . C11 C 0.2312(5) -0.2271(4) 0.1565(4) 0.0305(8) Uani 1 1 d . . . C12 C 0.3129(6) -0.1975(5) 0.2758(4) 0.0391(9) Uani 1 1 d . . . H12 H 0.3338 -0.1190 0.3311 0.047 Uiso 1 1 calc R . . C13 C 0.3626(7) -0.2853(6) 0.3113(5) 0.0524(13) Uani 1 1 d . . . H13 H 0.4196 -0.2657 0.3910 0.063 Uiso 1 1 calc R . . C14 C 0.3293(7) -0.4008(5) 0.2310(6) 0.0531(13) Uani 1 1 d . . . H14 H 0.3636 -0.4595 0.2564 0.064 Uiso 1 1 calc R . . C15 C 0.2470(6) -0.4313(5) 0.1147(5) 0.0479(12) Uani 1 1 d . . . H15 H 0.2246 -0.5108 0.0610 0.057 Uiso 1 1 calc R . . C16 C 0.1958(6) -0.3454(4) 0.0753(4) 0.0392(9) Uani 1 1 d . . . H16 H 0.1385 -0.3665 -0.0047 0.047 Uiso 1 1 calc R . . C17 C -0.0660(5) -0.1988(4) 0.0379(4) 0.0298(7) Uani 1 1 d . . . C18 C -0.1683(6) -0.2360(5) 0.1098(4) 0.0406(10) Uani 1 1 d . . . H18 H -0.1190 -0.2211 0.1899 0.049 Uiso 1 1 calc R . . C19 C -0.3438(6) -0.2954(5) 0.0615(5) 0.0488(12) Uani 1 1 d . . . H19 H -0.4132 -0.3189 0.1099 0.059 Uiso 1 1 calc R . . C20 C -0.4172(6) -0.3202(5) -0.0565(5) 0.0462(11) Uani 1 1 d . . . H20 H -0.5358 -0.3608 -0.0886 0.055 Uiso 1 1 calc R . . C21 C -0.3151(6) -0.2850(5) -0.1267(4) 0.0412(10) Uani 1 1 d . . . H21 H -0.3649 -0.3010 -0.2070 0.049 Uiso 1 1 calc R . . C22 C -0.1389(6) -0.2258(4) -0.0808(4) 0.0361(8) Uani 1 1 d . . . H22 H -0.0701 -0.2045 -0.1303 0.043 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 Au 0.03826(9) 0.02957(9) 0.02920(9) 0.01030(6) 0.01236(6) 0.01094(6) S1 0.0698(8) 0.0333(5) 0.0318(5) 0.0124(4) 0.0192(5) 0.0200(5) P1 0.0295(4) 0.0289(5) 0.0289(5) 0.0107(4) 0.0106(4) 0.0091(4) O1 0.0538(18) 0.0326(15) 0.0381(16) 0.0141(13) 0.0165(14) 0.0158(14) N1 0.0439(19) 0.0328(18) 0.0284(16) 0.0093(14) 0.0098(14) 0.0100(15) C1 0.038(2) 0.035(2) 0.0299(19) 0.0125(16) 0.0103(16) 0.0105(16) C2 0.037(2) 0.034(2) 0.032(2) 0.0104(16) 0.0076(16) 0.0095(16) C3 0.059(3) 0.043(3) 0.077(4) 0.024(3) 0.039(3) 0.017(2) C4 0.072(4) 0.055(4) 0.114(6) 0.036(4) 0.055(4) 0.033(3) C5 0.070(4) 0.039(3) 0.085(5) 0.024(3) 0.026(3) 0.019(3) C6 0.051(3) 0.036(2) 0.050(3) 0.016(2) 0.009(2) 0.005(2) C7 0.039(2) 0.045(2) 0.037(2) 0.0115(19) 0.0098(18) 0.0097(19) C8 0.051(3) 0.042(2) 0.039(2) 0.021(2) 0.013(2) 0.009(2) C8A 0.080(4) 0.043(3) 0.060(3) 0.030(3) 0.016(3) 0.019(3) C9 0.0344(19) 0.035(2) 0.034(2) 0.0136(16) 0.0146(16) 0.0067(16) C10 0.0320(18) 0.035(2) 0.034(2) 0.0131(16) 0.0130(15) 0.0092(16) C11 0.0234(16) 0.0298(18) 0.037(2) 0.0133(15) 0.0066(14) 0.0062(14) C12 0.034(2) 0.043(2) 0.036(2) 0.0147(18) 0.0041(17) 0.0105(17) C13 0.041(2) 0.066(3) 0.055(3) 0.035(3) 0.005(2) 0.017(2) C14 0.043(2) 0.052(3) 0.078(4) 0.037(3) 0.016(3) 0.022(2) C15 0.041(2) 0.035(2) 0.071(4) 0.019(2) 0.016(2) 0.0187(19) C16 0.035(2) 0.034(2) 0.045(2) 0.0107(18) 0.0086(18) 0.0113(17) C17 0.0305(17) 0.0310(19) 0.0318(19) 0.0118(15) 0.0109(15) 0.0142(15) C18 0.036(2) 0.051(3) 0.032(2) 0.0112(19) 0.0140(17) 0.0107(19) C19 0.036(2) 0.060(3) 0.051(3) 0.016(2) 0.022(2) 0.015(2) C20 0.033(2) 0.050(3) 0.052(3) 0.014(2) 0.0082(19) 0.0133(19) C21 0.040(2) 0.043(2) 0.040(2) 0.0170(19) 0.0024(18) 0.0156(19) C22 0.038(2) 0.039(2) 0.036(2) 0.0183(18) 0.0115(17) 0.0141(17) _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 Au P1 2.2520(10) . ? Au S1 2.3040(11) . ? S1 C1 1.752(4) . ? P1 C17 1.814(4) . ? P1 C11 1.803(4) . ? P1 C9 1.827(4) . ? O1 C1 1.355(5) . ? O1 C8 1.435(6) . ? N1 C1 1.269(5) . ? N1 C2 1.409(6) . ? C2 C3 1.391(7) . ? C2 C7 1.397(6) . ? C3 C4 1.377(8) . ? C3 H3 0.9400 . ? C4 C5 1.369(9) . ? C4 H4 0.9400 . ? C5 C6 1.376(8) . ? C5 H5 0.9400 . ? C6 C7 1.379(7) . ? C6 H6 0.9400 . ? C7 H7 0.9400 . ? C8 C8A 1.520(8) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? C8A H8A3 0.9700 . ? C9 C10 1.518(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C10 1.518(8) 2_655 ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.398(6) . ? C11 C16 1.401(6) . ? C12 C13 1.385(7) . ? C12 H12 0.9400 . ? C13 C14 1.374(9) . ? C13 H13 0.9400 . ? C14 C15 1.365(8) . ? C14 H14 0.9400 . ? C15 C16 1.393(7) . ? C15 H15 0.9400 . ? C16 H16 0.9400 . ? C17 C22 1.380(6) . ? C17 C18 1.399(6) . ? C18 C19 1.391(7) . ? C18 H18 0.9400 . ? C19 C20 1.378(8) . ? C19 H19 0.9400 . ? C20 C21 1.374(7) . ? C20 H20 0.9400 . ? C21 C22 1.393(6) . ? C21 H21 0.9400 . ? C22 H22 0.9400 . ? 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 Au S1 173.23(4) . . ? C1 S1 Au 104.29(15) . . ? C17 P1 C11 103.92(18) . . ? C17 P1 C9 107.68(19) . . ? C11 P1 C9 107.0(2) . . ? C17 P1 Au 110.58(13) . . ? C11 P1 Au 113.82(14) . . ? C9 P1 Au 113.24(15) . . ? C1 O1 C8 116.6(4) . . ? C1 N1 C2 121.4(4) . . ? N1 C1 O1 120.5(4) . . ? N1 C1 S1 127.2(4) . . ? O1 C1 S1 112.3(3) . . ? C3 C2 C7 118.0(5) . . ? C3 C2 N1 117.8(4) . . ? C7 C2 N1 124.1(4) . . ? C4 C3 C2 120.1(5) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 121.6(6) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C4 C5 C6 118.9(5) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? C7 C6 C5 120.6(5) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C2 120.7(5) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? O1 C8 C8A 106.2(4) . . ? O1 C8 H8A 110.5 . . ? C8A C8 H8A 110.5 . . ? O1 C8 H8B 110.5 . . ? C8A C8 H8B 110.5 . . ? H8A C8 H8B 108.7 . . ? C8 C8A H8A1 109.5 . . ? C8 C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C8 C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? C10 C9 P1 112.6(3) . . ? C10 C9 H9A 109.1 . . ? P1 C9 H9A 109.1 . . ? C10 C9 H9B 109.1 . . ? P1 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? C9 C10 C10 112.7(4) . 2_655 ? C9 C10 H10A 109.1 . . ? C10 C10 H10A 109.1 2_655 . ? C9 C10 H10B 109.1 . . ? C10 C10 H10B 109.1 2_655 . ? H10A C10 H10B 107.8 . . ? C12 C11 C16 120.2(4) . . ? C12 C11 P1 119.5(3) . . ? C16 C11 P1 120.2(3) . . ? C13 C12 C11 119.1(5) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 C13 C12 120.5(5) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C15 C14 C13 120.8(5) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 120.4(5) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C11 118.9(5) . . ? C15 C16 H16 120.5 . . ? C11 C16 H16 120.5 . . ? C22 C17 C18 119.8(4) . . ? C22 C17 P1 123.9(3) . . ? C18 C17 P1 116.3(3) . . ? C17 C18 C19 119.3(4) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C20 C19 C18 120.9(5) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 119.2(4) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C20 C21 C22 121.1(5) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C17 C22 C21 119.5(4) . . ? C17 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? 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 P1 Au S1 C1 153.9(3) . . . . ? S1 Au P1 C17 -63.3(4) . . . . ? S1 Au P1 C11 -179.9(3) . . . . ? S1 Au P1 C9 57.6(4) . . . . ? C2 N1 C1 O1 179.5(4) . . . . ? C2 N1 C1 S1 -1.6(7) . . . . ? C8 O1 C1 N1 3.7(6) . . . . ? C8 O1 C1 S1 -175.4(3) . . . . ? Au S1 C1 N1 -169.9(4) . . . . ? Au S1 C1 O1 9.1(3) . . . . ? C1 N1 C2 C3 130.1(5) . . . . ? C1 N1 C2 C7 -52.9(6) . . . . ? C7 C2 C3 C4 4.6(9) . . . . ? N1 C2 C3 C4 -178.3(6) . . . . ? C2 C3 C4 C5 -3.6(12) . . . . ? C3 C4 C5 C6 1.1(12) . . . . ? C4 C5 C6 C7 0.2(10) . . . . ? C5 C6 C7 C2 0.9(8) . . . . ? C3 C2 C7 C6 -3.3(7) . . . . ? N1 C2 C7 C6 179.8(4) . . . . ? C1 O1 C8 C8A -175.4(4) . . . . ? C17 P1 C9 C10 179.8(3) . . . . ? C11 P1 C9 C10 -69.0(3) . . . . ? Au P1 C9 C10 57.2(3) . . . . ? P1 C9 C10 C10 -178.8(4) . . . 2_655 ? C17 P1 C11 C12 -124.6(3) . . . . ? C9 P1 C11 C12 121.7(3) . . . . ? Au P1 C11 C12 -4.2(4) . . . . ? C17 P1 C11 C16 51.6(4) . . . . ? C9 P1 C11 C16 -62.2(4) . . . . ? Au P1 C11 C16 171.9(3) . . . . ? C16 C11 C12 C13 1.9(6) . . . . ? P1 C11 C12 C13 178.0(4) . . . . ? C11 C12 C13 C14 -1.2(7) . . . . ? C12 C13 C14 C15 0.1(8) . . . . ? C13 C14 C15 C16 0.3(8) . . . . ? C14 C15 C16 C11 0.4(7) . . . . ? C12 C11 C16 C15 -1.5(6) . . . . ? P1 C11 C16 C15 -177.6(3) . . . . ? C11 P1 C17 C22 -116.2(4) . . . . ? C9 P1 C17 C22 -2.9(4) . . . . ? Au P1 C17 C22 121.3(3) . . . . ? C11 P1 C17 C18 64.0(4) . . . . ? C9 P1 C17 C18 177.3(3) . . . . ? Au P1 C17 C18 -58.5(4) . . . . ? C22 C17 C18 C19 -2.7(7) . . . . ? P1 C17 C18 C19 177.1(4) . . . . ? C17 C18 C19 C20 1.4(8) . . . . ? C18 C19 C20 C21 -0.4(8) . . . . ? C19 C20 C21 C22 0.6(8) . . . . ? C18 C17 C22 C21 3.0(7) . . . . ? P1 C17 C22 C21 -176.8(3) . . . . ? C20 C21 C22 C17 -1.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 30.0 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.77 # # 0.79 A from Au # _refine_diff_density_min -0.96 _refine_diff_density_rms 0.148 # Attachment '31.CIF' data_dppb[Au(SC(OiPr)=NC6H5)]2(3) _database_code_depnum_ccdc_archive 'CCDC 632739' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C48 H52 Au2 N2 O2 P2 S2' _chemical_formula_weight 1208.91 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9734(12) _cell_length_b 10.5472(14) _cell_length_c 25.098(3) _cell_angle_alpha 90 _cell_angle_beta 92.957(3) _cell_angle_gamma 90 _cell_volume 2372.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 884 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 26.8 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 6.372 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.438 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details '(SADABS, Bruker, 2000 & Blessing, 1995)' _diffrn_ambient_temperature 223(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 'Bruker AXS SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 19326 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_av_sigmaI/netI 0.044 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.6 _diffrn_reflns_theta_max 30.0 _reflns_number_total 6891 _reflns_number_gt 5353 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'Bruker SHEXLTL (Bruker, 2000)' _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^)+(0.0331P)^2^] 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 6891 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.048 _refine_ls_R_factor_gt 0.033 _refine_ls_wR_factor_ref 0.077 _refine_ls_wR_factor_gt 0.071 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.02 _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 Au Au 0.065549(15) 0.117655(13) 0.062897(5) 0.03965(5) Uani 1 1 d . . . S1 S -0.14363(12) 0.00753(11) 0.08607(4) 0.0508(2) Uani 1 1 d . . . P1 P 0.26412(11) 0.23641(10) 0.04202(4) 0.0410(2) Uani 1 1 d . . . O1 O -0.0216(3) 0.0732(3) 0.17888(11) 0.0589(7) Uani 1 1 d . . . N1 N -0.2475(4) -0.0230(3) 0.18440(13) 0.0526(8) Uani 1 1 d . . . C1 C -0.1457(4) 0.0163(4) 0.15584(15) 0.0463(9) Uani 1 1 d . . . C2 C -0.3745(5) -0.0890(5) 0.16265(15) 0.0514(10) Uani 1 1 d . . . C3 C -0.5140(5) -0.0345(5) 0.16280(18) 0.0636(12) Uani 1 1 d . . . H3 H -0.5239 0.0495 0.1746 0.076 Uiso 1 1 calc R . . C4 C -0.6400(6) -0.1023(7) 0.1457(2) 0.0817(19) Uani 1 1 d . . . H4 H -0.7344 -0.0635 0.1454 0.098 Uiso 1 1 calc R . . C5 C -0.6276(7) -0.2255(8) 0.1293(2) 0.097(2) Uani 1 1 d . . . H5 H -0.7131 -0.2717 0.1180 0.116 Uiso 1 1 calc R . . C6 C -0.4895(8) -0.2809(6) 0.1294(2) 0.0888(18) Uani 1 1 d . . . H6 H -0.4804 -0.3653 0.1179 0.107 Uiso 1 1 calc R . . C7 C -0.3629(6) -0.2137(5) 0.14615(18) 0.0642(12) Uani 1 1 d . . . H7 H -0.2688 -0.2529 0.1463 0.077 Uiso 1 1 calc R . . C8 C -0.0096(6) 0.0802(5) 0.23732(18) 0.0637(12) Uani 1 1 d . . . H8 H -0.0610 0.0067 0.2527 0.076 Uiso 1 1 calc R . . C8A C -0.0802(8) 0.1981(7) 0.2537(3) 0.114(3) Uani 1 1 d . . . H8A1 H -0.1857 0.1959 0.2432 0.171 Uiso 1 1 calc R . . H8A2 H -0.0339 0.2694 0.2367 0.171 Uiso 1 1 calc R . . H8A3 H -0.0679 0.2071 0.2921 0.171 Uiso 1 1 calc R . . C8B C 0.1545(6) 0.0745(7) 0.2526(2) 0.0876(17) Uani 1 1 d . . . H8B1 H 0.1945 -0.0061 0.2415 0.131 Uiso 1 1 calc R . . H8B2 H 0.1694 0.0829 0.2910 0.131 Uiso 1 1 calc R . . H8B3 H 0.2054 0.1430 0.2353 0.131 Uiso 1 1 calc R . . C9 C 0.3988(4) 0.1612(4) 0.00084(14) 0.0429(8) Uani 1 1 d . . . H9A H 0.3557 0.1554 -0.0358 0.052 Uiso 1 1 calc R . . H9B H 0.4874 0.2154 0.0002 0.052 Uiso 1 1 calc R . . C10 C 0.4472(4) 0.0291(4) 0.01928(14) 0.0454(9) Uani 1 1 d . . . H10A H 0.3591 -0.0252 0.0216 0.054 Uiso 1 1 calc R . . H10B H 0.4970 0.0344 0.0549 0.054 Uiso 1 1 calc R . . C11 C 0.2152(5) 0.3779(4) 0.00326(17) 0.0487(9) Uani 1 1 d . . . C12 C 0.1272(5) 0.3621(4) -0.0429(2) 0.0595(11) Uani 1 1 d . . . H12 H 0.0918 0.2809 -0.0524 0.071 Uiso 1 1 calc R . . C13 C 0.0903(6) 0.4650(5) -0.0756(2) 0.0724(14) Uani 1 1 d . . . H13 H 0.0311 0.4530 -0.1072 0.087 Uiso 1 1 calc R . . C14 C 0.1400(6) 0.5839(5) -0.0617(3) 0.0771(16) Uani 1 1 d . . . H14 H 0.1168 0.6534 -0.0841 0.093 Uiso 1 1 calc R . . C15 C 0.2240(7) 0.6009(5) -0.0150(3) 0.086(2) Uani 1 1 d . . . H15 H 0.2547 0.6830 -0.0050 0.103 Uiso 1 1 calc R . . C16 C 0.2646(6) 0.4985(4) 0.0177(2) 0.0670(13) Uani 1 1 d . . . H16 H 0.3244 0.5109 0.0491 0.080 Uiso 1 1 calc R . . C17 C 0.3621(4) 0.2912(4) 0.10246(15) 0.0493(9) Uani 1 1 d . . . C18 C 0.5164(5) 0.2901(6) 0.10908(18) 0.0738(15) Uani 1 1 d . . . H18 H 0.5739 0.2604 0.0814 0.089 Uiso 1 1 calc R . . C19 C 0.5863(6) 0.3322(7) 0.1562(2) 0.0886(19) Uani 1 1 d . . . H19 H 0.6910 0.3323 0.1602 0.106 Uiso 1 1 calc R . . C20 C 0.5030(7) 0.3740(5) 0.1971(2) 0.0815(18) Uani 1 1 d . . . H20 H 0.5507 0.4031 0.2290 0.098 Uiso 1 1 calc R . . C21 C 0.3519(7) 0.3732(5) 0.1914(2) 0.0777(16) Uani 1 1 d . . . H21 H 0.2950 0.4014 0.2195 0.093 Uiso 1 1 calc R . . C22 C 0.2818(5) 0.3314(5) 0.14478(18) 0.0659(13) Uani 1 1 d . . . H22 H 0.1770 0.3301 0.1416 0.079 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 Au 0.03813(8) 0.04750(9) 0.03345(8) -0.00047(6) 0.00325(5) -0.00363(6) S1 0.0511(5) 0.0700(7) 0.0312(5) -0.0019(4) 0.0015(4) -0.0217(5) P1 0.0385(5) 0.0528(5) 0.0319(5) -0.0045(4) 0.0049(4) -0.0057(4) O1 0.0546(17) 0.088(2) 0.0339(15) -0.0026(14) -0.0021(12) -0.0179(16) N1 0.0471(18) 0.075(2) 0.0356(17) 0.0034(16) 0.0026(14) -0.0093(17) C1 0.048(2) 0.057(2) 0.0339(19) -0.0001(16) -0.0016(16) 0.0011(18) C2 0.049(2) 0.076(3) 0.0289(18) 0.0128(18) 0.0015(16) -0.011(2) C3 0.054(3) 0.090(4) 0.046(3) 0.017(2) 0.003(2) -0.001(2) C4 0.050(3) 0.141(6) 0.053(3) 0.029(3) -0.004(2) -0.012(3) C5 0.082(4) 0.150(7) 0.059(4) 0.017(4) -0.001(3) -0.061(5) C6 0.119(5) 0.088(4) 0.059(3) 0.005(3) 0.006(3) -0.046(4) C7 0.073(3) 0.074(3) 0.047(3) 0.009(2) 0.004(2) -0.014(3) C8 0.064(3) 0.090(3) 0.037(2) -0.008(2) -0.003(2) -0.008(3) C8A 0.120(5) 0.145(6) 0.074(4) -0.038(4) -0.016(4) 0.048(5) C8B 0.078(4) 0.121(5) 0.061(3) -0.005(3) -0.021(3) -0.011(4) C9 0.0408(19) 0.059(2) 0.0290(17) -0.0040(16) 0.0027(14) -0.0043(17) C10 0.0390(19) 0.069(3) 0.0287(17) 0.0008(16) 0.0068(14) 0.0032(18) C11 0.048(2) 0.052(2) 0.048(2) 0.0007(17) 0.0170(18) -0.0033(18) C12 0.060(3) 0.057(3) 0.062(3) 0.001(2) 0.005(2) 0.004(2) C13 0.067(3) 0.081(4) 0.070(3) 0.021(3) 0.008(3) 0.015(3) C14 0.067(3) 0.071(3) 0.097(5) 0.026(3) 0.033(3) 0.017(3) C15 0.093(4) 0.048(3) 0.122(6) 0.004(3) 0.047(4) -0.009(3) C16 0.073(3) 0.060(3) 0.069(3) -0.003(2) 0.018(3) -0.020(2) C17 0.049(2) 0.064(3) 0.035(2) -0.0093(17) 0.0050(17) -0.0107(19) C18 0.054(3) 0.128(5) 0.040(2) -0.024(3) 0.010(2) -0.025(3) C19 0.059(3) 0.156(6) 0.051(3) -0.026(3) 0.004(2) -0.036(3) C20 0.082(4) 0.118(5) 0.045(3) -0.029(3) 0.003(2) -0.034(3) C21 0.079(4) 0.110(5) 0.045(3) -0.030(3) 0.012(2) -0.009(3) C22 0.053(2) 0.098(4) 0.047(3) -0.025(2) 0.006(2) 0.000(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 Au P1 2.2616(10) . ? Au S1 2.3072(10) . ? S1 C1 1.755(4) . ? P1 C17 1.808(4) . ? P1 C9 1.813(4) . ? P1 C11 1.822(4) . ? O1 C1 1.367(5) . ? O1 C8 1.467(5) . ? N1 C1 1.260(5) . ? N1 C2 1.421(5) . ? C2 C3 1.378(6) . ? C2 C7 1.384(7) . ? C3 C4 1.387(7) . ? C4 C5 1.369(9) . ? C5 C6 1.370(9) . ? C6 C7 1.386(7) . ? C8 C8A 1.464(8) . ? C8 C8B 1.504(7) . ? C9 C10 1.525(6) . ? C10 C10 1.518(7) 3_655 ? C11 C12 1.377(7) . ? C11 C16 1.389(6) . ? C12 C13 1.390(6) . ? C13 C14 1.370(8) . ? C14 C15 1.372(9) . ? C15 C16 1.394(8) . ? C17 C18 1.386(6) . ? C17 C22 1.381(6) . ? C18 C19 1.382(6) . ? C19 C20 1.373(7) . ? C20 C21 1.356(8) . ? C21 C22 1.372(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 P1 Au S1 176.53(4) . . ? C1 S1 Au 106.00(14) . . ? C17 P1 C9 107.96(18) . . ? C17 P1 C11 106.2(2) . . ? C9 P1 C11 101.71(18) . . ? C17 P1 Au 109.72(13) . . ? C9 P1 Au 116.50(13) . . ? C11 P1 Au 113.97(14) . . ? C1 O1 C8 117.5(3) . . ? C1 N1 C2 122.2(3) . . ? N1 C1 O1 120.1(4) . . ? N1 C1 S1 126.6(3) . . ? O1 C1 S1 113.3(3) . . ? C3 C2 C7 118.7(4) . . ? C3 C2 N1 120.4(4) . . ? C7 C2 N1 120.6(4) . . ? C2 C3 C4 120.7(5) . . ? C5 C4 C3 120.3(6) . . ? C6 C5 C4 119.5(6) . . ? C5 C6 C7 120.6(6) . . ? C2 C7 C6 120.3(5) . . ? O1 C8 C8A 108.2(4) . . ? O1 C8 C8B 105.9(4) . . ? C8A C8 C8B 113.2(5) . . ? C10 C9 P1 114.5(2) . . ? C9 C10 C10 110.7(4) . 3_655 ? C12 C11 C16 119.4(4) . . ? C12 C11 P1 117.5(3) . . ? C16 C11 P1 123.1(4) . . ? C11 C12 C13 120.7(5) . . ? C14 C13 C12 120.0(6) . . ? C15 C14 C13 119.6(5) . . ? C14 C15 C16 121.2(5) . . ? C15 C16 C11 119.0(5) . . ? C18 C17 C22 117.9(4) . . ? C18 C17 P1 122.5(3) . . ? C22 C17 P1 119.5(3) . . ? C17 C18 C19 120.4(4) . . ? C20 C19 C18 120.1(5) . . ? C21 C20 C19 120.0(5) . . ? C22 C21 C20 120.2(5) . . ? C21 C22 C17 121.3(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Au S1 C1 -65.6(6) . . . . ? S1 Au P1 C17 68.7(6) . . . . ? S1 Au P1 C9 -168.3(6) . . . . ? S1 Au P1 C11 -50.2(6) . . . . ? C2 N1 C1 O1 -176.4(4) . . . . ? C2 N1 C1 S1 4.1(6) . . . . ? C8 O1 C1 N1 3.0(6) . . . . ? C8 O1 C1 S1 -177.4(3) . . . . ? Au S1 C1 N1 174.0(4) . . . . ? Au S1 C1 O1 -5.5(3) . . . . ? C1 N1 C2 C3 -112.6(5) . . . . ? C1 N1 C2 C7 74.2(6) . . . . ? C7 C2 C3 C4 -1.3(6) . . . . ? N1 C2 C3 C4 -174.7(4) . . . . ? C2 C3 C4 C5 1.2(7) . . . . ? C3 C4 C5 C6 -0.7(8) . . . . ? C4 C5 C6 C7 0.4(8) . . . . ? C3 C2 C7 C6 1.0(6) . . . . ? N1 C2 C7 C6 174.3(4) . . . . ? C5 C6 C7 C2 -0.6(8) . . . . ? C1 O1 C8 C8A -89.5(6) . . . . ? C1 O1 C8 C8B 148.8(4) . . . . ? C17 P1 C9 C10 76.0(3) . . . . ? C11 P1 C9 C10 -172.4(3) . . . . ? Au P1 C9 C10 -47.9(3) . . . . ? P1 C9 C10 C10 176.8(3) . . . 3_655 ? C17 P1 C11 C12 -174.3(3) . . . . ? C9 P1 C11 C12 72.9(4) . . . . ? Au P1 C11 C12 -53.3(4) . . . . ? C17 P1 C11 C16 6.9(4) . . . . ? C9 P1 C11 C16 -106.0(4) . . . . ? Au P1 C11 C16 127.8(3) . . . . ? C16 C11 C12 C13 1.4(7) . . . . ? P1 C11 C12 C13 -177.5(4) . . . . ? C11 C12 C13 C14 -0.7(7) . . . . ? C12 C13 C14 C15 -1.2(8) . . . . ? C13 C14 C15 C16 2.5(8) . . . . ? C14 C15 C16 C11 -1.8(8) . . . . ? C12 C11 C16 C15 -0.2(7) . . . . ? P1 C11 C16 C15 178.6(4) . . . . ? C9 P1 C17 C18 9.1(5) . . . . ? C11 P1 C17 C18 -99.4(4) . . . . ? Au P1 C17 C18 137.0(4) . . . . ? C9 P1 C17 C22 -168.4(4) . . . . ? C11 P1 C17 C22 83.2(4) . . . . ? Au P1 C17 C22 -40.5(4) . . . . ? C22 C17 C18 C19 -2.1(8) . . . . ? P1 C17 C18 C19 -179.6(5) . . . . ? C17 C18 C19 C20 0.9(10) . . . . ? C18 C19 C20 C21 0.4(10) . . . . ? C19 C20 C21 C22 -0.3(10) . . . . ? C20 C21 C22 C17 -1.0(9) . . . . ? C18 C17 C22 C21 2.2(8) . . . . ? P1 C17 C22 C21 179.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.0 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.59 # # 0.79 A from Au # _refine_diff_density_min -0.43 _refine_diff_density_rms 0.126 # Attachment '51.CIF' data_dppb[Au(SC(OEt)=NC6H4NO2-p)]2(5) _database_code_depnum_ccdc_archive 'CCDC 632740' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C46 H46 Au2 N4 O6 P2 S2' _chemical_formula_weight 1270.86 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' 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' S S 0.1246 0.1234 '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 9.2907(5) _cell_length_b 11.4082(6) _cell_length_c 12.0751(6) _cell_angle_alpha 115.352(1) _cell_angle_beta 91.155(1) _cell_angle_gamma 90.652(1) _cell_volume 1156.07(10) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6174 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 30.0 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.825 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 618 _exptl_absorpt_coefficient_mu 6.549 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.356 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details '(SADABS, Bruker, 2000 & Blessing, 1995)' _diffrn_ambient_temperature 223(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 'Bruker AXS SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9746 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_av_sigmaI/netI 0.045 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.9 _diffrn_reflns_theta_max 30.0 _reflns_number_total 6631 _reflns_number_gt 6045 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'Bruker SHEXLTL (Bruker, 2000)' _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^)+(0.0305P)^2^] 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 6631 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.030 _refine_ls_R_factor_gt 0.027 _refine_ls_wR_factor_ref 0.064 _refine_ls_wR_factor_gt 0.063 _refine_ls_goodness_of_fit_ref 1.00 _refine_ls_restrained_S_all 1.00 _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 Au Au 0.187591(11) 0.205978(9) 0.459149(9) 0.02002(4) Uani 1 1 d . . . S1 S 0.01971(9) 0.11224(7) 0.30106(7) 0.02616(16) Uani 1 1 d . . . P1 P 0.34310(8) 0.30506(7) 0.61886(7) 0.01796(14) Uani 1 1 d . . . O1 O 0.0441(3) 0.3540(2) 0.3383(2) 0.0298(5) Uani 1 1 d . . . O2 O -0.5412(4) -0.2548(3) 0.0000(3) 0.0647(10) Uani 1 1 d . . . O3 O -0.4056(5) -0.2979(3) -0.1542(3) 0.0764(11) Uani 1 1 d . . . N1 N -0.1403(3) 0.2445(3) 0.2048(3) 0.0320(6) Uani 1 1 d . . . N2 N -0.4430(4) -0.2267(3) -0.0508(3) 0.0460(9) Uani 1 1 d . . . C1 C -0.0365(3) 0.2457(3) 0.2757(3) 0.0237(6) Uani 1 1 d . . . C2 C -0.2178(3) 0.1278(3) 0.1398(3) 0.0276(6) Uani 1 1 d . . . C3 C -0.3319(4) 0.0941(3) 0.1938(3) 0.0335(7) Uani 1 1 d . . . H3 H -0.3581 0.1506 0.2735 0.040 Uiso 1 1 calc R . . C4 C -0.4075(4) -0.0220(3) 0.1312(3) 0.0351(8) Uani 1 1 d . . . H4 H -0.4845 -0.0450 0.1678 0.042 Uiso 1 1 calc R . . C5 C -0.3677(4) -0.1029(3) 0.0145(3) 0.0322(7) Uani 1 1 d . . . C6 C -0.2582(4) -0.0691(4) -0.0431(3) 0.0380(8) Uani 1 1 d . . . H6 H -0.2345 -0.1243 -0.1240 0.046 Uiso 1 1 calc R . . C7 C -0.1846(4) 0.0469(4) 0.0201(3) 0.0356(8) Uani 1 1 d . . . H7 H -0.1109 0.0716 -0.0184 0.043 Uiso 1 1 calc R . . C8 C 0.0045(4) 0.4705(3) 0.3268(3) 0.0311(7) Uani 1 1 d . . . H8A H -0.0771 0.5109 0.3788 0.037 Uiso 1 1 calc R . . H8B H -0.0230 0.4500 0.2416 0.037 Uiso 1 1 calc R . . C8A C 0.1333(4) 0.5599(4) 0.3667(4) 0.0488(10) Uani 1 1 d . . . H8A1 H 0.1113 0.6393 0.3595 0.073 Uiso 1 1 calc R . . H8A2 H 0.2134 0.5184 0.3152 0.073 Uiso 1 1 calc R . . H8A3 H 0.1587 0.5801 0.4513 0.073 Uiso 1 1 calc R . . C9 C 0.4125(3) 0.4574(3) 0.6231(3) 0.0242(6) Uani 1 1 d . . . H9A H 0.3350 0.5203 0.6444 0.029 Uiso 1 1 calc R . . H9B H 0.4889 0.4930 0.6865 0.029 Uiso 1 1 calc R . . C10 C 0.4721(3) 0.4367(3) 0.4994(3) 0.0242(6) Uani 1 1 d . . . H10A H 0.3960 0.3994 0.4358 0.029 Uiso 1 1 calc R . . H10B H 0.5505 0.3748 0.4789 0.029 Uiso 1 1 calc R . . C11 C 0.5053(3) 0.2183(3) 0.6166(3) 0.0217(6) Uani 1 1 d . . . C12 C 0.5660(4) 0.1438(3) 0.5038(3) 0.0303(7) Uani 1 1 d . . . H12 H 0.5150 0.1286 0.4306 0.036 Uiso 1 1 calc R . . C13 C 0.7014(4) 0.0922(3) 0.4994(4) 0.0405(9) Uani 1 1 d . . . H13 H 0.7437 0.0451 0.4233 0.049 Uiso 1 1 calc R . . C14 C 0.7736(4) 0.1096(3) 0.6056(4) 0.0441(10) Uani 1 1 d . . . H14 H 0.8657 0.0751 0.6022 0.053 Uiso 1 1 calc R . . C15 C 0.7111(4) 0.1781(4) 0.7179(4) 0.0454(10) Uani 1 1 d . . . H15 H 0.7589 0.1863 0.7904 0.054 Uiso 1 1 calc R . . C16 C 0.5784(4) 0.2344(4) 0.7237(4) 0.0346(8) Uani 1 1 d . . . H16 H 0.5379 0.2835 0.8002 0.042 Uiso 1 1 calc R . . C17 C 0.2628(3) 0.3401(3) 0.7645(3) 0.0225(6) Uani 1 1 d . . . C18 C 0.2919(5) 0.4530(4) 0.8684(3) 0.0424(9) Uani 1 1 d . . . H18 H 0.3524 0.5181 0.8653 0.051 Uiso 1 1 calc R . . C19 C 0.2308(6) 0.4691(5) 0.9775(4) 0.0646(15) Uani 1 1 d . . . H19 H 0.2514 0.5455 1.0488 0.077 Uiso 1 1 calc R . . C20 C 0.1412(5) 0.3766(5) 0.9839(4) 0.0588(13) Uani 1 1 d . . . H20 H 0.0999 0.3899 1.0587 0.071 Uiso 1 1 calc R . . C21 C 0.1118(5) 0.2641(4) 0.8807(4) 0.0477(10) Uani 1 1 d . . . H21 H 0.0515 0.1994 0.8848 0.057 Uiso 1 1 calc R . . C22 C 0.1707(4) 0.2464(3) 0.7710(3) 0.0325(7) Uani 1 1 d . . . H22 H 0.1486 0.1703 0.7000 0.039 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 Au 0.02235(6) 0.01830(6) 0.01843(6) 0.00733(4) -0.00539(4) -0.00560(4) S1 0.0318(4) 0.0186(3) 0.0257(4) 0.0080(3) -0.0127(3) -0.0072(3) P1 0.0197(3) 0.0165(3) 0.0175(3) 0.0074(3) -0.0040(3) -0.0051(3) O1 0.0313(12) 0.0196(10) 0.0378(13) 0.0124(10) -0.0125(10) -0.0078(9) O2 0.077(2) 0.0571(19) 0.062(2) 0.0290(17) -0.0265(18) -0.0405(18) O3 0.098(3) 0.0466(18) 0.050(2) -0.0112(16) -0.0155(19) -0.0211(19) N1 0.0318(14) 0.0284(13) 0.0347(15) 0.0135(12) -0.0145(12) -0.0085(11) N2 0.055(2) 0.0356(16) 0.0420(19) 0.0128(15) -0.0243(16) -0.0145(15) C1 0.0257(14) 0.0228(13) 0.0228(14) 0.0105(12) -0.0052(11) -0.0050(11) C2 0.0272(15) 0.0264(15) 0.0277(16) 0.0109(13) -0.0116(12) -0.0045(12) C3 0.0408(19) 0.0365(17) 0.0207(15) 0.0103(13) -0.0064(13) -0.0057(15) C4 0.0352(18) 0.0409(18) 0.0305(17) 0.0171(15) -0.0064(14) -0.0107(15) C5 0.0340(17) 0.0280(15) 0.0284(17) 0.0071(13) -0.0156(14) -0.0070(13) C6 0.040(2) 0.0365(19) 0.0277(17) 0.0047(15) -0.0034(15) -0.0003(15) C7 0.0306(17) 0.0416(19) 0.0321(18) 0.0138(16) -0.0022(14) -0.0060(15) C8 0.0334(17) 0.0224(14) 0.0398(19) 0.0158(14) -0.0038(14) -0.0023(13) C8A 0.045(2) 0.0315(18) 0.073(3) 0.026(2) 0.000(2) -0.0098(16) C9 0.0270(15) 0.0177(12) 0.0269(15) 0.0088(11) -0.0031(12) -0.0057(11) C10 0.0281(15) 0.0196(13) 0.0263(15) 0.0114(12) -0.0016(12) -0.0078(11) C11 0.0197(13) 0.0198(12) 0.0288(15) 0.0137(12) -0.0013(11) -0.0027(10) C12 0.0335(17) 0.0251(15) 0.0345(18) 0.0148(14) 0.0049(14) 0.0010(13) C13 0.0375(19) 0.0258(16) 0.061(3) 0.0203(17) 0.0161(18) 0.0065(14) C14 0.0265(17) 0.0300(17) 0.085(3) 0.034(2) 0.0023(19) 0.0048(14) C15 0.036(2) 0.043(2) 0.065(3) 0.031(2) -0.0195(19) -0.0036(16) C16 0.0316(17) 0.0371(18) 0.0374(19) 0.0186(16) -0.0097(15) -0.0003(14) C17 0.0224(14) 0.0240(13) 0.0196(13) 0.0079(11) -0.0013(11) -0.0011(11) C18 0.050(2) 0.0359(19) 0.0274(18) 0.0009(15) -0.0003(16) -0.0113(17) C19 0.076(3) 0.069(3) 0.0219(19) -0.006(2) 0.009(2) -0.008(3) C20 0.058(3) 0.089(4) 0.028(2) 0.024(2) 0.0161(19) 0.006(3) C21 0.043(2) 0.062(3) 0.045(2) 0.030(2) 0.0135(18) -0.002(2) C22 0.0334(17) 0.0342(17) 0.0291(17) 0.0127(14) 0.0044(14) -0.0041(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au P1 2.2513(7) . ? Au S1 2.3052(7) . ? S1 C1 1.760(3) . ? P1 C11 1.807(3) . ? P1 C17 1.808(3) . ? P1 C9 1.826(3) . ? O1 C1 1.347(3) . ? O1 C8 1.445(4) . ? O2 N2 1.223(5) . ? O3 N2 1.223(5) . ? N1 C1 1.272(4) . ? N1 C2 1.402(4) . ? N2 C5 1.452(4) . ? C2 C7 1.385(5) . ? C2 C3 1.389(5) . ? C3 C4 1.385(5) . ? C3 H3 0.9400 . ? C4 C5 1.374(5) . ? C4 H4 0.9400 . ? C5 C6 1.385(5) . ? C6 C7 1.376(5) . ? C6 H6 0.9400 . ? C7 H7 0.9400 . ? C8 C8A 1.494(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? C8A H8A3 0.9700 . ? C9 C10 1.526(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C10 1.523(5) 2_666 ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.395(4) . ? C11 C16 1.388(4) . ? C12 C13 1.388(5) . ? C12 H12 0.9400 . ? C13 C14 1.370(6) . ? C13 H13 0.9400 . ? C14 C15 1.387(6) . ? C14 H14 0.9400 . ? C15 C16 1.386(5) . ? C15 H15 0.9400 . ? C16 H16 0.9400 . ? C17 C18 1.378(4) . ? C17 C22 1.391(4) . ? C18 C19 1.384(6) . ? C18 H18 0.9400 . ? C19 C20 1.366(7) . ? C19 H19 0.9400 . ? C20 C21 1.372(6) . ? C20 H20 0.9400 . ? C21 C22 1.377(5) . ? C21 H21 0.9400 . ? C22 H22 0.9400 . ? 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 Au S1 177.06(3) . . ? C1 S1 Au 102.33(10) . . ? C11 P1 C17 105.77(14) . . ? C11 P1 C9 102.82(14) . . ? C17 P1 C9 108.06(14) . . ? C11 P1 Au 115.87(10) . . ? C17 P1 Au 112.64(10) . . ? C9 P1 Au 110.97(10) . . ? C1 O1 C8 117.7(2) . . ? C1 N1 C2 118.4(3) . . ? O3 N2 O2 123.0(4) . . ? O3 N2 C5 118.5(4) . . ? O2 N2 C5 118.5(3) . . ? N1 C1 O1 121.2(3) . . ? N1 C1 S1 125.6(2) . . ? O1 C1 S1 113.2(2) . . ? C7 C2 C3 119.2(3) . . ? C7 C2 N1 120.5(3) . . ? C3 C2 N1 120.2(3) . . ? C4 C3 C2 120.6(3) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 118.7(3) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C4 C5 C6 121.8(3) . . ? C4 C5 N2 119.3(3) . . ? C6 C5 N2 118.9(3) . . ? C7 C6 C5 118.8(3) . . ? C7 C6 H6 120.6 . . ? C5 C6 H6 120.6 . . ? C2 C7 C6 120.8(3) . . ? C2 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? O1 C8 C8A 106.9(3) . . ? O1 C8 H8A 110.3 . . ? C8A C8 H8A 110.3 . . ? O1 C8 H8B 110.3 . . ? C8A C8 H8B 110.3 . . ? H8A C8 H8B 108.6 . . ? C8 C8A H8A1 109.5 . . ? C8 C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C8 C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? C10 C9 P1 110.96(19) . . ? C10 C9 H9A 109.4 . . ? P1 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? P1 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C9 C10 C10 111.7(3) . 2_666 ? C9 C10 H10A 109.3 . . ? C10 C10 H10A 109.3 2_666 . ? C9 C10 H10B 109.3 . . ? C10 C10 H10B 109.3 2_666 . ? H10A C10 H10B 108.0 . . ? C12 C11 C16 119.4(3) . . ? C12 C11 P1 118.5(2) . . ? C16 C11 P1 121.8(3) . . ? C13 C12 C11 120.1(3) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 120.2(4) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.1(3) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 120.2(4) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C11 120.0(4) . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? C18 C17 C22 119.4(3) . . ? C18 C17 P1 122.9(3) . . ? C22 C17 P1 117.6(2) . . ? C17 C18 C19 119.0(4) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? C20 C19 C18 121.5(4) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C21 C20 C19 119.7(4) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 119.8(4) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C17 120.6(3) . . ? C21 C22 H22 119.7 . . ? C17 C22 H22 119.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Au S1 C1 51.8(5) . . . . ? S1 Au P1 C11 168.2(5) . . . . ? S1 Au P1 C17 46.3(5) . . . . ? S1 Au P1 C9 -75.0(5) . . . . ? C2 N1 C1 O1 178.4(3) . . . . ? C2 N1 C1 S1 -0.2(5) . . . . ? C8 O1 C1 N1 3.0(5) . . . . ? C8 O1 C1 S1 -178.2(2) . . . . ? Au S1 C1 N1 -172.3(3) . . . . ? Au S1 C1 O1 9.0(2) . . . . ? C1 N1 C2 C7 -96.4(4) . . . . ? C1 N1 C2 C3 85.7(4) . . . . ? C7 C2 C3 C4 3.2(5) . . . . ? N1 C2 C3 C4 -178.9(3) . . . . ? C2 C3 C4 C5 -0.2(5) . . . . ? C3 C4 C5 C6 -2.5(5) . . . . ? C3 C4 C5 N2 178.1(3) . . . . ? O3 N2 C5 C4 -179.5(4) . . . . ? O2 N2 C5 C4 0.7(5) . . . . ? O3 N2 C5 C6 1.0(5) . . . . ? O2 N2 C5 C6 -178.8(4) . . . . ? C4 C5 C6 C7 2.1(6) . . . . ? N2 C5 C6 C7 -178.4(3) . . . . ? C3 C2 C7 C6 -3.5(5) . . . . ? N1 C2 C7 C6 178.5(3) . . . . ? C5 C6 C7 C2 0.9(6) . . . . ? C1 O1 C8 C8A -161.0(3) . . . . ? C11 P1 C9 C10 72.7(2) . . . . ? C17 P1 C9 C10 -175.8(2) . . . . ? Au P1 C9 C10 -51.8(2) . . . . ? P1 C9 C10 C10 179.0(3) . . . 2_666 ? C17 P1 C11 C12 160.2(2) . . . . ? C9 P1 C11 C12 -86.5(2) . . . . ? Au P1 C11 C12 34.7(3) . . . . ? C17 P1 C11 C16 -26.5(3) . . . . ? C9 P1 C11 C16 86.7(3) . . . . ? Au P1 C11 C16 -152.1(2) . . . . ? C16 C11 C12 C13 -3.3(5) . . . . ? P1 C11 C12 C13 170.1(2) . . . . ? C11 C12 C13 C14 2.6(5) . . . . ? C12 C13 C14 C15 0.6(5) . . . . ? C13 C14 C15 C16 -3.1(5) . . . . ? C14 C15 C16 C11 2.4(5) . . . . ? C12 C11 C16 C15 0.8(5) . . . . ? P1 C11 C16 C15 -172.4(3) . . . . ? C11 P1 C17 C18 91.2(3) . . . . ? C9 P1 C17 C18 -18.3(3) . . . . ? Au P1 C17 C18 -141.2(3) . . . . ? C11 P1 C17 C22 -87.0(3) . . . . ? C9 P1 C17 C22 163.4(3) . . . . ? Au P1 C17 C22 40.5(3) . . . . ? C22 C17 C18 C19 1.3(6) . . . . ? P1 C17 C18 C19 -177.0(4) . . . . ? C17 C18 C19 C20 -0.8(8) . . . . ? C18 C19 C20 C21 0.7(9) . . . . ? C19 C20 C21 C22 -1.1(8) . . . . ? C20 C21 C22 C17 1.6(6) . . . . ? C18 C17 C22 C21 -1.7(6) . . . . ? P1 C17 C22 C21 176.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.98 _diffrn_reflns_theta_full 30.0 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.72 _refine_diff_density_min -2.46 # # 0.82 A from Au # _refine_diff_density_rms 0.165 # Attachment '61.CIF' data_dppb[Au(SC(OiPr)=NC6H4NO2-p)]2.MeOH _database_code_depnum_ccdc_archive 'CCDC 632741' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C49 H54 Au2 N4 O7 P2 S2' _chemical_formula_weight 1330.95 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' 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' S S 0.1246 0.1234 '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 8.872(2) _cell_length_b 12.310(3) _cell_length_c 12.717(3) _cell_angle_alpha 104.028(5) _cell_angle_beta 90.272(5) _cell_angle_gamma 107.186(5) _cell_volume 1282.9(6) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1003 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 26.6 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 5.907 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.567 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details '(SADABS, Bruker, 2000 & Blessing, 1995)' _diffrn_ambient_temperature 223(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 'Bruker AXS SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9873 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_sigmaI/netI 0.087 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.7 _diffrn_reflns_theta_max 30.0 _reflns_number_total 7227 _reflns_number_gt 4887 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'Bruker SHEXLTL (Bruker, 2000)' _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^)+(0.0662P)^2^+0.6328P] 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 7227 _refine_ls_number_parameters 297 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.096 _refine_ls_R_factor_gt 0.048 _refine_ls_wR_factor_ref 0.136 _refine_ls_wR_factor_gt 0.113 _refine_ls_goodness_of_fit_ref 1.01 _refine_ls_restrained_S_all 1.01 _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 Au Au 0.18861(4) 0.03429(3) 0.25845(2) 0.03527(10) Uani 1 1 d . . . S1 S 0.2441(3) 0.19674(19) 0.40472(16) 0.0528(6) Uani 1 1 d . . . P1 P 0.1455(2) -0.11115(16) 0.10389(13) 0.0283(4) Uani 1 1 d . . . O1 O 0.2463(7) 0.0294(5) 0.4972(4) 0.0466(14) Uani 1 1 d . . . O2 O 0.1594(10) 0.7007(7) 0.7705(6) 0.077(2) Uani 1 1 d . . . O3 O 0.4080(11) 0.7529(7) 0.7440(7) 0.091(3) Uani 1 1 d . . . O4 O 0.067(2) 0.4740(17) 0.4609(15) 0.103(6) Uiso 0.50 1 d PD . . N1 N 0.2549(9) 0.2024(6) 0.6167(5) 0.0441(16) Uani 1 1 d . . . N2 N 0.2808(11) 0.6770(7) 0.7436(6) 0.056(2) Uani 1 1 d . . . C1 C 0.2509(10) 0.1434(7) 0.5205(6) 0.0430(18) Uani 1 1 d . . . C2 C 0.2635(10) 0.3216(7) 0.6447(6) 0.0409(18) Uani 1 1 d . . . C3 C 0.1422(11) 0.3544(9) 0.6976(7) 0.053(2) Uani 1 1 d . . . H3 H 0.0545 0.2964 0.7118 0.064 Uiso 1 1 calc R . . C4 C 0.1474(12) 0.4702(9) 0.7298(7) 0.057(2) Uani 1 1 d . . . H4 H 0.0639 0.4919 0.7652 0.068 Uiso 1 1 calc R . . C5 C 0.2771(11) 0.5538(8) 0.7093(6) 0.048(2) Uani 1 1 d . . . C6 C 0.4012(10) 0.5255(8) 0.6577(6) 0.048(2) Uani 1 1 d . . . H6 H 0.4894 0.5841 0.6450 0.058 Uiso 1 1 calc R . . C7 C 0.3921(10) 0.4080(8) 0.6251(6) 0.0437(19) Uani 1 1 d . . . H7 H 0.4751 0.3865 0.5890 0.052 Uiso 1 1 calc R . . C8 C 0.2333(11) -0.0274(8) 0.5868(6) 0.048(2) Uani 1 1 d . . . H8 H 0.1502 -0.0092 0.6333 0.058 Uiso 1 1 calc R . . C9 C 0.3884(13) 0.0130(9) 0.6527(9) 0.071(3) Uani 1 1 d . . . H9A H 0.4128 0.0958 0.6893 0.106 Uiso 1 1 calc R . . H9B H 0.4707 0.0016 0.6052 0.106 Uiso 1 1 calc R . . H9C H 0.3825 -0.0320 0.7063 0.106 Uiso 1 1 calc R . . C10 C 0.1853(15) -0.1565(9) 0.5313(8) 0.075(3) Uani 1 1 d . . . H10A H 0.0839 -0.1792 0.4899 0.112 Uiso 1 1 calc R . . H10B H 0.1767 -0.2011 0.5855 0.112 Uiso 1 1 calc R . . H10C H 0.2645 -0.1726 0.4827 0.112 Uiso 1 1 calc R . . C11 C 0.2716(8) -0.0636(6) -0.0002(5) 0.0296(14) Uani 1 1 d . . . H11A H 0.2560 -0.1299 -0.0644 0.036 Uiso 1 1 calc R . . H11B H 0.2415 -0.0014 -0.0223 0.036 Uiso 1 1 calc R . . C12 C 0.4459(8) -0.0177(6) 0.0429(5) 0.0313(15) Uani 1 1 d . . . H12A H 0.4616 0.0504 0.1054 0.038 Uiso 1 1 calc R . . H12B H 0.4741 -0.0790 0.0680 0.038 Uiso 1 1 calc R . . C13 C 0.1951(8) -0.2382(6) 0.1226(6) 0.0340(15) Uani 1 1 d . . . C14 C 0.1724(10) -0.3371(7) 0.0363(7) 0.0432(18) Uani 1 1 d . . . H14 H 0.1285 -0.3395 -0.0320 0.052 Uiso 1 1 calc R . . C15 C 0.2153(11) -0.4326(8) 0.0516(9) 0.056(2) Uani 1 1 d . . . H15 H 0.2022 -0.4991 -0.0068 0.067 Uiso 1 1 calc R . . C16 C 0.2782(11) -0.4296(9) 0.1543(9) 0.058(2) Uani 1 1 d . . . H16 H 0.3045 -0.4947 0.1657 0.070 Uiso 1 1 calc R . . C17 C 0.3009(12) -0.3293(9) 0.2385(8) 0.059(2) Uani 1 1 d . . . H17 H 0.3469 -0.3248 0.3068 0.071 Uiso 1 1 calc R . . C18 C 0.2566(10) -0.2366(8) 0.2225(7) 0.0464(19) Uani 1 1 d . . . H18 H 0.2684 -0.1705 0.2811 0.056 Uiso 1 1 calc R . . C19 C -0.0585(8) -0.1698(6) 0.0440(5) 0.0308(14) Uani 1 1 d . . . C20 C -0.1769(9) -0.1900(7) 0.1126(6) 0.0385(17) Uani 1 1 d . . . H20 H -0.1512 -0.1681 0.1882 0.046 Uiso 1 1 calc R . . C21 C -0.3322(9) -0.2416(8) 0.0725(7) 0.047(2) Uani 1 1 d . . . H21 H -0.4123 -0.2557 0.1201 0.056 Uiso 1 1 calc R . . C22 C -0.3708(10) -0.2736(8) -0.0412(7) 0.047(2) Uani 1 1 d . . . H22 H -0.4767 -0.3100 -0.0695 0.057 Uiso 1 1 calc R . . C23 C -0.2532(10) -0.2513(7) -0.1100(6) 0.0439(19) Uani 1 1 d . . . H23 H -0.2794 -0.2708 -0.1853 0.053 Uiso 1 1 calc R . . C24 C -0.0977(9) -0.2009(7) -0.0697(5) 0.0361(16) Uani 1 1 d . . . H24 H -0.0177 -0.1870 -0.1174 0.043 Uiso 1 1 calc R . . C25 C 0.194(2) 0.5393(17) 0.4269(16) 0.058(5) Uiso 0.50 1 d PD . . 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 Au 0.04843(18) 0.03129(16) 0.02543(13) 0.00445(10) 0.00220(10) 0.01348(12) S1 0.0968(18) 0.0334(11) 0.0275(9) 0.0051(8) 0.0034(10) 0.0212(12) P1 0.0308(9) 0.0302(9) 0.0237(7) 0.0059(7) 0.0041(6) 0.0096(7) O1 0.070(4) 0.035(3) 0.033(3) 0.005(2) 0.002(2) 0.016(3) O2 0.107(6) 0.063(5) 0.065(4) -0.001(4) 0.027(4) 0.045(5) O3 0.107(7) 0.039(4) 0.112(7) 0.005(4) -0.004(5) 0.013(5) N1 0.068(5) 0.035(4) 0.029(3) 0.006(3) 0.001(3) 0.018(3) N2 0.082(6) 0.039(4) 0.045(4) 0.003(3) 0.005(4) 0.020(4) C1 0.050(5) 0.034(4) 0.045(4) 0.008(3) 0.001(3) 0.016(4) C2 0.058(5) 0.034(4) 0.029(3) 0.002(3) 0.000(3) 0.017(4) C3 0.049(5) 0.054(6) 0.056(5) 0.014(4) 0.011(4) 0.014(4) C4 0.065(6) 0.051(6) 0.054(5) 0.004(4) 0.021(4) 0.026(5) C5 0.069(6) 0.037(5) 0.035(4) 0.003(3) 0.005(4) 0.018(4) C6 0.050(5) 0.045(5) 0.039(4) -0.001(4) 0.000(3) 0.009(4) C7 0.042(4) 0.051(5) 0.034(4) 0.004(3) 0.000(3) 0.015(4) C8 0.068(6) 0.044(5) 0.029(4) 0.012(3) -0.003(3) 0.010(4) C9 0.077(7) 0.053(6) 0.072(6) 0.004(5) -0.031(5) 0.015(5) C10 0.105(9) 0.045(6) 0.059(6) 0.016(5) -0.013(6) 0.000(6) C11 0.038(4) 0.026(3) 0.025(3) 0.006(3) 0.004(3) 0.010(3) C12 0.037(4) 0.032(4) 0.026(3) 0.012(3) 0.007(3) 0.009(3) C13 0.029(3) 0.029(4) 0.041(4) 0.010(3) 0.005(3) 0.003(3) C14 0.050(5) 0.029(4) 0.051(4) 0.009(3) 0.002(4) 0.013(4) C15 0.055(5) 0.034(5) 0.080(7) 0.012(4) 0.010(5) 0.016(4) C16 0.059(6) 0.044(5) 0.084(7) 0.030(5) 0.001(5) 0.024(5) C17 0.070(6) 0.060(6) 0.062(6) 0.032(5) 0.003(5) 0.029(5) C18 0.042(4) 0.044(5) 0.054(5) 0.016(4) 0.001(4) 0.011(4) C19 0.034(4) 0.030(4) 0.032(3) 0.009(3) 0.001(3) 0.014(3) C20 0.042(4) 0.046(5) 0.028(3) 0.009(3) 0.009(3) 0.014(4) C21 0.029(4) 0.056(6) 0.057(5) 0.025(4) 0.009(3) 0.008(4) C22 0.038(4) 0.045(5) 0.058(5) 0.019(4) 0.003(4) 0.008(4) C23 0.052(5) 0.040(5) 0.037(4) 0.008(3) -0.005(3) 0.011(4) C24 0.046(4) 0.038(4) 0.027(3) 0.013(3) 0.009(3) 0.011(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 Au P1 2.2576(17) . ? Au S1 2.304(2) . ? S1 C1 1.759(8) . ? P1 C13 1.812(8) . ? P1 C19 1.823(7) . ? P1 C11 1.830(7) . ? O1 C1 1.350(9) . ? O1 C8 1.464(10) . ? O2 N2 1.226(10) . ? O3 N2 1.233(11) . ? O4 C25 1.315(10) . ? O4 O4 1.73(4) 2_566 ? N1 C1 1.256(10) . ? N1 C2 1.402(10) . ? N2 C5 1.463(11) . ? C2 C7 1.382(12) . ? C2 C3 1.381(12) . ? C3 C4 1.371(13) . ? C4 C5 1.373(14) . ? C5 C6 1.374(12) . ? C6 C7 1.382(12) . ? C8 C9 1.491(12) . ? C8 C10 1.503(13) . ? C11 C12 1.528(10) . ? C12 C12 1.516(13) 2_655 ? C13 C18 1.373(11) . ? C13 C14 1.390(10) . ? C14 C15 1.393(12) . ? C15 C16 1.406(14) . ? C16 C17 1.387(14) . ? C17 C18 1.369(12) . ? C19 C20 1.374(10) . ? C19 C24 1.417(9) . ? C20 C21 1.372(11) . ? C21 C22 1.414(12) . ? C22 C23 1.373(12) . ? C23 C24 1.372(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au S1 173.73(7) . . ? C1 S1 Au 105.7(3) . . ? C13 P1 C19 104.6(3) . . ? C13 P1 C11 104.5(3) . . ? C19 P1 C11 107.8(3) . . ? C13 P1 Au 112.8(2) . . ? C19 P1 Au 115.2(2) . . ? C11 P1 Au 111.2(2) . . ? C1 O1 C8 118.1(6) . . ? C25 O4 O4 125(2) . 2_566 ? C1 N1 C2 123.6(7) . . ? O3 N2 O2 122.8(9) . . ? O3 N2 C5 117.7(9) . . ? O2 N2 C5 119.4(9) . . ? N1 C1 O1 121.7(8) . . ? N1 C1 S1 124.6(7) . . ? O1 C1 S1 113.7(5) . . ? C7 C2 N1 122.3(8) . . ? C7 C2 C3 118.8(8) . . ? N1 C2 C3 118.9(8) . . ? C4 C3 C2 121.2(9) . . ? C3 C4 C5 118.6(8) . . ? C6 C5 C4 122.4(8) . . ? C6 C5 N2 119.6(9) . . ? C4 C5 N2 118.1(8) . . ? C5 C6 C7 117.9(9) . . ? C2 C7 C6 121.3(8) . . ? O1 C8 C9 110.0(8) . . ? O1 C8 C10 104.1(7) . . ? C9 C8 C10 112.2(9) . . ? C12 C11 P1 110.7(4) . . ? C12 C12 C11 112.1(7) 2_655 . ? C18 C13 C14 119.7(7) . . ? C18 C13 P1 119.8(6) . . ? C14 C13 P1 120.4(6) . . ? C13 C14 C15 119.5(8) . . ? C16 C15 C14 120.1(9) . . ? C17 C16 C15 119.0(8) . . ? C16 C17 C18 120.2(9) . . ? C13 C18 C17 121.4(9) . . ? C20 C19 C24 119.5(7) . . ? C20 C19 P1 117.8(5) . . ? C24 C19 P1 122.6(5) . . ? C19 C20 C21 120.9(7) . . ? C20 C21 C22 119.4(7) . . ? C23 C22 C21 119.9(8) . . ? C22 C23 C24 120.6(7) . . ? C23 C24 C19 119.7(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Au S1 C1 -158.8(7) . . . . ? S1 Au P1 C13 137.6(8) . . . . ? S1 Au P1 C19 -102.5(8) . . . . ? S1 Au P1 C11 20.5(8) . . . . ? C2 N1 C1 O1 178.4(7) . . . . ? C2 N1 C1 S1 -3.8(13) . . . . ? C8 O1 C1 N1 4.8(12) . . . . ? C8 O1 C1 S1 -173.2(6) . . . . ? Au S1 C1 N1 -168.9(7) . . . . ? Au S1 C1 O1 9.0(7) . . . . ? C1 N1 C2 C7 -63.9(12) . . . . ? C1 N1 C2 C3 118.8(10) . . . . ? C7 C2 C3 C4 0.5(13) . . . . ? N1 C2 C3 C4 177.9(8) . . . . ? C2 C3 C4 C5 -0.6(15) . . . . ? C3 C4 C5 C6 0.1(14) . . . . ? C3 C4 C5 N2 179.7(8) . . . . ? O3 N2 C5 C6 -13.8(12) . . . . ? O2 N2 C5 C6 166.3(8) . . . . ? O3 N2 C5 C4 166.6(9) . . . . ? O2 N2 C5 C4 -13.3(12) . . . . ? C4 C5 C6 C7 0.6(13) . . . . ? N2 C5 C6 C7 -179.0(7) . . . . ? N1 C2 C7 C6 -177.1(7) . . . . ? C3 C2 C7 C6 0.2(12) . . . . ? C5 C6 C7 C2 -0.7(12) . . . . ? C1 O1 C8 C9 -75.2(10) . . . . ? C1 O1 C8 C10 164.5(8) . . . . ? C13 P1 C11 C12 -66.8(5) . . . . ? C19 P1 C11 C12 -177.7(5) . . . . ? Au P1 C11 C12 55.1(5) . . . . ? P1 C11 C12 C12 177.7(7) . . . 2_655 ? C19 P1 C13 C18 -127.8(6) . . . . ? C11 P1 C13 C18 119.0(6) . . . . ? Au P1 C13 C18 -1.9(7) . . . . ? C19 P1 C13 C14 52.7(7) . . . . ? C11 P1 C13 C14 -60.5(7) . . . . ? Au P1 C13 C14 178.5(5) . . . . ? C18 C13 C14 C15 -1.3(12) . . . . ? P1 C13 C14 C15 178.3(7) . . . . ? C13 C14 C15 C16 1.2(13) . . . . ? C14 C15 C16 C17 -1.9(15) . . . . ? C15 C16 C17 C18 2.6(15) . . . . ? C14 C13 C18 C17 2.0(13) . . . . ? P1 C13 C18 C17 -177.5(7) . . . . ? C16 C17 C18 C13 -2.7(15) . . . . ? C13 P1 C19 C20 81.4(6) . . . . ? C11 P1 C19 C20 -167.8(6) . . . . ? Au P1 C19 C20 -42.9(7) . . . . ? C13 P1 C19 C24 -95.1(7) . . . . ? C11 P1 C19 C24 15.8(7) . . . . ? Au P1 C19 C24 140.6(6) . . . . ? C24 C19 C20 C21 1.2(12) . . . . ? P1 C19 C20 C21 -175.4(7) . . . . ? C19 C20 C21 C22 -0.5(13) . . . . ? C20 C21 C22 C23 -0.9(14) . . . . ? C21 C22 C23 C24 1.6(13) . . . . ? C22 C23 C24 C19 -1.0(12) . . . . ? C20 C19 C24 C23 -0.4(11) . . . . ? P1 C19 C24 C23 176.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 30.0 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 2.24 # # 0.90 A from Au # _refine_diff_density_min -1.91 # # 0.84 A from Au # _refine_diff_density_rms 0.192 # Attachment '71.CIF' data_dppb[Au(SC(OMe)=NC6H4Me-p)]2.2H2O _database_code_depnum_ccdc_archive 'CCDC 632742' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C46 H52 Au2 N2 O4 P2 S2' _chemical_formula_weight 1216.89 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' 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' S S 0.1246 0.1234 '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 13.8791(10) _cell_length_b 13.3279(10) _cell_length_c 26.1381(19) _cell_angle_alpha 90 _cell_angle_beta 104.601(2) _cell_angle_gamma 90 _cell_volume 4678.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4668 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 26.4 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 6.464 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.566 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details '(SADABS, Bruker, 2000 & Blessing, 1995)' _diffrn_ambient_temperature 223(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 'Bruker AXS SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 19265 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_av_sigmaI/netI 0.048 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.6 _diffrn_reflns_theta_max 30.1 _reflns_number_total 6849 _reflns_number_gt 5254 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'Bruker SHEXLTL (Bruker, 2000)' _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^)+(0.0675P)^2^+10.9487P] 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 6849 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.062 _refine_ls_R_factor_gt 0.042 _refine_ls_wR_factor_ref 0.125 _refine_ls_wR_factor_gt 0.118 _refine_ls_goodness_of_fit_ref 1.07 _refine_ls_restrained_S_all 1.07 _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 Au Au 0.241846(17) 0.163786(15) 0.443524(8) 0.03006(8) Uani 1 1 d . . . S1 S 0.28116(14) 0.32105(10) 0.41753(5) 0.0354(3) Uani 1 1 d . . . P1 P 0.22295(11) 0.00061(10) 0.46172(5) 0.0257(3) Uani 1 1 d . . . O1 O 0.2047(4) 0.2259(3) 0.33037(17) 0.0541(14) Uani 1 1 d . . . N1 N 0.2697(6) 0.3764(5) 0.3163(2) 0.0548(18) Uani 1 1 d . . . C1 C 0.2506(6) 0.3129(5) 0.3485(2) 0.0401(15) Uani 1 1 d . . . C2 C 0.3201(6) 0.4675(5) 0.3334(2) 0.0423(16) Uani 1 1 d . . . C3 C 0.4124(6) 0.4844(5) 0.3248(2) 0.0439(16) Uani 1 1 d . . . H3 H 0.4437 0.4334 0.3101 0.053 Uiso 1 1 calc R . . C4 C 0.4604(6) 0.5769(5) 0.3378(3) 0.0458(16) Uani 1 1 d . . . H4 H 0.5241 0.5866 0.3323 0.055 Uiso 1 1 calc R . . C5 C 0.4158(5) 0.6539(4) 0.3585(3) 0.0392(14) Uani 1 1 d . . . C6 C 0.3222(6) 0.6362(5) 0.3664(3) 0.0410(15) Uani 1 1 d . . . H6 H 0.2905 0.6875 0.3807 0.049 Uiso 1 1 calc R . . C7 C 0.2737(6) 0.5450(5) 0.3538(3) 0.0470(17) Uani 1 1 d . . . H7 H 0.2098 0.5355 0.3590 0.056 Uiso 1 1 calc R . . C5' C 0.4670(6) 0.7532(6) 0.3723(3) 0.057(2) Uani 1 1 d . . . H5'1 H 0.5053 0.7523 0.4088 0.086 Uiso 1 1 calc R . . H5'2 H 0.4177 0.8062 0.3673 0.086 Uiso 1 1 calc R . . H5'3 H 0.5113 0.7651 0.3495 0.086 Uiso 1 1 calc R . . C8 C 0.1760(9) 0.2122(7) 0.2738(3) 0.086(4) Uani 1 1 d . . . H8A H 0.1306 0.2653 0.2577 0.129 Uiso 1 1 calc R . . H8B H 0.1433 0.1478 0.2655 0.129 Uiso 1 1 calc R . . H8C H 0.2348 0.2143 0.2601 0.129 Uiso 1 1 calc R . . C9 C 0.1360(4) -0.0332(4) 0.50064(19) 0.0242(10) Uani 1 1 d . . . H9A H 0.1310 -0.1065 0.5013 0.029 Uiso 1 1 calc R . . H9B H 0.1634 -0.0106 0.5371 0.029 Uiso 1 1 calc R . . C10 C 0.0316(4) 0.0101(4) 0.4808(2) 0.0289(11) Uani 1 1 d . . . H10A H 0.0362 0.0826 0.4759 0.035 Uiso 1 1 calc R . . H10B H -0.0004 -0.0197 0.4465 0.035 Uiso 1 1 calc R . . C11 C 0.1898(5) -0.0709(4) 0.4010(2) 0.0303(12) Uani 1 1 d . . . C12 C 0.2276(6) -0.0381(5) 0.3587(2) 0.0435(15) Uani 1 1 d . . . H12 H 0.2692 0.0185 0.3622 0.052 Uiso 1 1 calc R . . C13 C 0.2016(7) -0.0918(6) 0.3113(3) 0.056(2) Uani 1 1 d . . . H13 H 0.2272 -0.0714 0.2829 0.067 Uiso 1 1 calc R . . C14 C 0.1394(7) -0.1739(6) 0.3051(3) 0.055(2) Uani 1 1 d . . . H14 H 0.1197 -0.2070 0.2724 0.066 Uiso 1 1 calc R . . C15 C 0.1066(6) -0.2063(6) 0.3476(3) 0.0509(18) Uani 1 1 d . . . H15 H 0.0675 -0.2646 0.3442 0.061 Uiso 1 1 calc R . . C16 C 0.1294(6) -0.1558(5) 0.3950(3) 0.0408(14) Uani 1 1 d . . . H16 H 0.1045 -0.1786 0.4232 0.049 Uiso 1 1 calc R . . C17 C 0.3393(4) -0.0510(4) 0.5004(2) 0.0277(11) Uani 1 1 d . . . C18 C 0.3918(5) 0.0029(5) 0.5430(3) 0.0434(15) Uani 1 1 d . . . H18 H 0.3692 0.0670 0.5495 0.052 Uiso 1 1 calc R . . C19 C 0.4775(5) -0.0351(6) 0.5764(3) 0.0475(17) Uani 1 1 d . . . H19 H 0.5106 0.0019 0.6063 0.057 Uiso 1 1 calc R . . C20 C 0.5142(5) -0.1254(5) 0.5665(3) 0.0424(15) Uani 1 1 d . . . H20 H 0.5725 -0.1510 0.5892 0.051 Uiso 1 1 calc R . . C21 C 0.4642(5) -0.1797(5) 0.5221(3) 0.0452(16) Uani 1 1 d . . . H21 H 0.4899 -0.2412 0.5138 0.054 Uiso 1 1 calc R . . C22 C 0.3770(5) -0.1422(5) 0.4904(3) 0.0411(15) Uani 1 1 d . . . H22 H 0.3422 -0.1800 0.4612 0.049 Uiso 1 1 calc R . . O2 O 0.0899(12) 0.5835(8) 0.2178(5) 0.048(3) Uani 0.50 1 d P A 1 O3 O 0.0533(18) 0.5339(16) 0.2261(8) 0.136(10) Uani 0.50 1 d P 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 Au 0.03599(14) 0.02939(12) 0.02722(12) 0.00523(8) 0.01243(9) 0.00410(9) S1 0.0568(10) 0.0264(6) 0.0238(6) 0.0019(5) 0.0118(6) 0.0012(6) P1 0.0284(7) 0.0274(6) 0.0236(6) 0.0032(5) 0.0108(5) 0.0025(6) O1 0.096(4) 0.039(2) 0.028(2) -0.0055(18) 0.017(3) -0.021(3) N1 0.098(6) 0.045(3) 0.022(2) 0.001(2) 0.018(3) -0.016(3) C1 0.064(5) 0.031(3) 0.025(3) 0.001(2) 0.011(3) 0.003(3) C2 0.069(5) 0.034(3) 0.023(3) 0.007(2) 0.011(3) -0.001(3) C3 0.061(5) 0.039(3) 0.030(3) 0.006(2) 0.007(3) 0.009(3) C4 0.048(4) 0.050(4) 0.037(3) 0.011(3) 0.007(3) 0.009(3) C5 0.043(4) 0.036(3) 0.033(3) 0.008(2) 0.001(3) 0.002(3) C6 0.054(4) 0.037(3) 0.036(3) -0.003(2) 0.017(3) 0.004(3) C7 0.060(5) 0.048(4) 0.037(3) 0.001(3) 0.021(3) -0.010(3) C5' 0.059(5) 0.053(4) 0.056(4) 0.005(3) 0.008(4) -0.013(4) C8 0.154(11) 0.066(6) 0.033(4) -0.013(4) 0.015(5) -0.037(6) C9 0.028(3) 0.027(2) 0.020(2) 0.0029(18) 0.011(2) 0.001(2) C10 0.032(3) 0.033(3) 0.022(2) 0.006(2) 0.009(2) 0.004(2) C11 0.036(3) 0.034(3) 0.022(2) 0.001(2) 0.008(2) 0.008(2) C12 0.051(4) 0.051(4) 0.034(3) -0.007(3) 0.019(3) 0.004(3) C13 0.077(6) 0.066(5) 0.032(3) 0.001(3) 0.028(4) 0.006(4) C14 0.072(5) 0.059(5) 0.033(3) -0.011(3) 0.010(3) 0.021(4) C15 0.059(5) 0.047(4) 0.045(4) -0.012(3) 0.010(3) 0.002(4) C16 0.048(4) 0.042(3) 0.035(3) -0.002(3) 0.014(3) -0.001(3) C17 0.028(3) 0.032(3) 0.025(2) 0.004(2) 0.011(2) 0.001(2) C18 0.042(4) 0.038(3) 0.048(4) -0.009(3) 0.008(3) 0.009(3) C19 0.040(4) 0.053(4) 0.046(4) -0.006(3) 0.004(3) 0.004(3) C20 0.028(3) 0.048(4) 0.052(4) 0.016(3) 0.012(3) 0.002(3) C21 0.044(4) 0.034(3) 0.059(4) 0.010(3) 0.016(3) 0.013(3) C22 0.044(4) 0.035(3) 0.046(4) 0.003(3) 0.014(3) 0.000(3) O2 0.064(9) 0.037(5) 0.027(5) -0.014(4) -0.020(5) 0.019(5) O3 0.13(2) 0.16(2) 0.085(14) -0.078(15) -0.041(12) 0.078(16) _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 Au P1 2.2556(14) . ? Au S1 2.3107(14) . ? S1 C1 1.749(6) . ? P1 C11 1.807(6) . ? P1 C17 1.811(6) . ? P1 C9 1.820(5) . ? O1 C1 1.351(8) . ? O1 C8 1.443(8) . ? N1 C1 1.268(8) . ? N1 C2 1.417(9) . ? C2 C7 1.392(10) . ? C2 C3 1.373(11) . ? C3 C4 1.402(10) . ? C3 H3 0.9400 . ? C4 C5 1.377(10) . ? C4 H4 0.9400 . ? C5 C6 1.387(10) . ? C5 C5' 1.502(9) . ? C6 C7 1.389(9) . ? C6 H6 0.9400 . ? C7 H7 0.9400 . ? C5' H5'1 0.9700 . ? C5' H5'2 0.9700 . ? C5' H5'3 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 C10 1.523(7) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C10 1.513(10) 5_556 ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.409(8) . ? C11 C16 1.394(9) . ? C12 C13 1.396(9) . ? C12 H12 0.9400 . ? C13 C14 1.378(12) . ? C13 H13 0.9400 . ? C14 C15 1.373(11) . ? C14 H14 0.9400 . ? C15 C16 1.374(9) . ? C15 H15 0.9400 . ? C16 H16 0.9400 . ? C17 C22 1.374(8) . ? C17 C18 1.370(8) . ? C18 C19 1.382(9) . ? C18 H18 0.9400 . ? C19 C20 1.357(10) . ? C19 H19 0.9400 . ? C20 C21 1.395(11) . ? C20 H20 0.9400 . ? C21 C22 1.377(10) . ? C21 H21 0.9400 . ? C22 H22 0.9400 . ? 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 Au S1 170.14(6) . . ? C1 S1 Au 103.5(2) . . ? C11 P1 C17 106.5(3) . . ? C11 P1 C9 107.6(3) . . ? C17 P1 C9 102.6(2) . . ? C11 P1 Au 109.91(19) . . ? C17 P1 Au 110.43(19) . . ? C9 P1 Au 119.02(17) . . ? C1 O1 C8 116.9(5) . . ? C1 N1 C2 122.1(6) . . ? N1 C1 O1 119.9(6) . . ? N1 C1 S1 127.4(5) . . ? O1 C1 S1 112.7(4) . . ? C7 C2 N1 121.2(7) . . ? C7 C2 C3 118.7(6) . . ? N1 C2 C3 119.7(7) . . ? C4 C3 C2 120.7(7) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 121.2(7) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 117.5(6) . . ? C4 C5 C5' 121.2(7) . . ? C6 C5 C5' 121.3(7) . . ? C5 C6 C7 121.9(7) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C2 C7 C6 119.9(7) . . ? C2 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C5 C5' H5'1 109.5 . . ? C5 C5' H5'2 109.5 . . ? H5'1 C5' H5'2 109.5 . . ? C5 C5' H5'3 109.5 . . ? H5'1 C5' H5'3 109.5 . . ? H5'2 C5' H5'3 109.5 . . ? O1 C8 H8A 109.5 . . ? O1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 P1 115.1(3) . . ? C10 C9 H9A 108.5 . . ? P1 C9 H9A 108.5 . . ? C10 C9 H9B 108.5 . . ? P1 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? C10 C10 C9 111.6(5) 5_556 . ? C10 C10 H10A 109.3 5_556 . ? C9 C10 H10A 109.3 . . ? C10 C10 H10B 109.3 5_556 . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C16 119.7(6) . . ? C12 C11 P1 117.6(5) . . ? C16 C11 P1 122.7(5) . . ? C13 C12 C11 118.3(7) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.8 . . ? C12 C13 C14 121.7(7) . . ? C12 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C15 C14 C13 118.7(7) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C16 C15 C14 121.9(7) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C11 119.7(7) . . ? C15 C16 H16 120.2 . . ? C11 C16 H16 120.2 . . ? C22 C17 C18 118.0(6) . . ? C22 C17 P1 123.9(5) . . ? C18 C17 P1 118.1(4) . . ? C17 C18 C19 121.2(6) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C20 C19 C18 120.6(6) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 119.2(6) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C20 C21 C22 119.3(6) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C17 C22 C21 121.7(7) . . ? C17 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Au S1 C1 60.2(4) . . . . ? S1 Au P1 C11 -56.6(4) . . . . ? S1 Au P1 C17 60.6(4) . . . . ? S1 Au P1 C9 178.8(3) . . . . ? C2 N1 C1 O1 -178.2(7) . . . . ? C2 N1 C1 S1 -0.8(13) . . . . ? C8 O1 C1 N1 -2.6(12) . . . . ? C8 O1 C1 S1 179.7(7) . . . . ? Au S1 C1 N1 -170.9(7) . . . . ? Au S1 C1 O1 6.6(6) . . . . ? C1 N1 C2 C7 -71.6(10) . . . . ? C1 N1 C2 C3 115.3(8) . . . . ? C7 C2 C3 C4 1.9(9) . . . . ? N1 C2 C3 C4 175.2(6) . . . . ? C2 C3 C4 C5 -1.3(9) . . . . ? C3 C4 C5 C6 0.5(9) . . . . ? C3 C4 C5 C5' -179.8(6) . . . . ? C4 C5 C6 C7 -0.4(10) . . . . ? C5' C5 C6 C7 179.8(6) . . . . ? N1 C2 C7 C6 -175.0(6) . . . . ? C3 C2 C7 C6 -1.8(9) . . . . ? C5 C6 C7 C2 1.1(10) . . . . ? C11 P1 C9 C10 -74.1(4) . . . . ? C17 P1 C9 C10 173.9(4) . . . . ? Au P1 C9 C10 51.7(4) . . . . ? P1 C9 C10 C10 -172.5(5) . . . 5_556 ? C17 P1 C11 C12 -87.9(5) . . . . ? C9 P1 C11 C12 162.7(5) . . . . ? Au P1 C11 C12 31.7(5) . . . . ? C17 P1 C11 C16 92.0(6) . . . . ? C9 P1 C11 C16 -17.4(6) . . . . ? Au P1 C11 C16 -148.4(5) . . . . ? C16 C11 C12 C13 1.0(10) . . . . ? P1 C11 C12 C13 -179.2(6) . . . . ? C11 C12 C13 C14 1.1(12) . . . . ? C12 C13 C14 C15 -3.4(12) . . . . ? C13 C14 C15 C16 3.8(12) . . . . ? C14 C15 C16 C11 -1.8(11) . . . . ? C12 C11 C16 C15 -0.6(10) . . . . ? P1 C11 C16 C15 179.6(5) . . . . ? C11 P1 C17 C22 -15.6(6) . . . . ? C9 P1 C17 C22 97.3(5) . . . . ? Au P1 C17 C22 -134.8(5) . . . . ? C11 P1 C17 C18 166.1(5) . . . . ? C9 P1 C17 C18 -81.0(5) . . . . ? Au P1 C17 C18 46.9(5) . . . . ? C22 C17 C18 C19 -3.1(10) . . . . ? P1 C17 C18 C19 175.3(6) . . . . ? C17 C18 C19 C20 3.0(11) . . . . ? C18 C19 C20 C21 -0.2(11) . . . . ? C19 C20 C21 C22 -2.3(11) . . . . ? C18 C17 C22 C21 0.5(10) . . . . ? P1 C17 C22 C21 -177.8(5) . . . . ? C20 C21 C22 C17 2.2(11) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.1 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.73 # # 1.21 A from O3 # _refine_diff_density_min -0.56 _refine_diff_density_rms 0.192 # Attachment '81.CIF' data_dppb[Au(SC(OEt)=NC6H4Me-p)]2 _database_code_depnum_ccdc_archive 'CCDC 632743' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C48 H52 Au2 N2 O2 P2 S2' _chemical_formula_weight 1208.91 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.2316(19) _cell_length_b 10.341(2) _cell_length_c 24.703(5) _cell_angle_alpha 90 _cell_angle_beta 99.062(5) _cell_angle_gamma 90 _cell_volume 2328.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4381 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27.0 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.724 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 6.490 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.417 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details '(SADABS, Bruker, 2000 & Blessing, 1995)' _diffrn_ambient_temperature 223(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 'Bruker AXS SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 19064 _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_av_sigmaI/netI 0.058 _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 -34 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.7 _diffrn_reflns_theta_max 30.1 _reflns_number_total 6752 _reflns_number_gt 5331 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'Bruker SHEXLTL (Bruker, 2000)' _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^)+(0.0429P)^2^] 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 6752 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.054 _refine_ls_R_factor_gt 0.037 _refine_ls_wR_factor_ref 0.097 _refine_ls_wR_factor_gt 0.082 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_restrained_S_all 1.04 _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 Au Au 0.081884(18) 0.119083(15) 0.056258(7) 0.03069(7) Uani 1 1 d . . . S1 S -0.11604(14) 0.01776(12) 0.08547(5) 0.0390(3) Uani 1 1 d . . . P1 P 0.26789(12) 0.24152(10) 0.03408(5) 0.0279(2) Uani 1 1 d . . . O1 O 0.0303(4) 0.1188(3) 0.17463(16) 0.0452(9) Uani 1 1 d . . . N1 N -0.1926(4) 0.0403(4) 0.18759(17) 0.0396(9) Uani 1 1 d . . . C1 C -0.1005(5) 0.0584(4) 0.1555(2) 0.0341(10) Uani 1 1 d . . . C2 C -0.3264(5) -0.0268(5) 0.17048(19) 0.0343(10) Uani 1 1 d . . . C3 C -0.4575(6) 0.0373(5) 0.1734(2) 0.0399(11) Uani 1 1 d . . . H3 H -0.4556 0.1249 0.1837 0.048 Uiso 1 1 calc R . . C4 C -0.5909(6) -0.0264(5) 0.1611(2) 0.0417(11) Uani 1 1 d . . . H4 H -0.6783 0.0191 0.1627 0.050 Uiso 1 1 calc R . . C5 C -0.5973(6) -0.1560(6) 0.1467(2) 0.0459(12) Uani 1 1 d . . . C6 C -0.4668(6) -0.2200(5) 0.1441(2) 0.0454(12) Uani 1 1 d . . . H6 H -0.4690 -0.3077 0.1340 0.055 Uiso 1 1 calc R . . C7 C -0.3318(6) -0.1568(5) 0.1562(2) 0.0415(11) Uani 1 1 d . . . H7 H -0.2445 -0.2024 0.1547 0.050 Uiso 1 1 calc R . . C5' C -0.7440(7) -0.2256(7) 0.1333(3) 0.071(2) Uani 1 1 d . . . H5'1 H -0.8217 -0.1696 0.1417 0.106 Uiso 1 1 calc R . . H5'2 H -0.7417 -0.3041 0.1549 0.106 Uiso 1 1 calc R . . H5'3 H -0.7620 -0.2475 0.0946 0.106 Uiso 1 1 calc R . . C8 C 0.0509(6) 0.1624(6) 0.2314(2) 0.0518(14) Uani 1 1 d . . . H8A H 0.1560 0.1721 0.2448 0.062 Uiso 1 1 calc R . . H8B H 0.0120 0.0970 0.2540 0.062 Uiso 1 1 calc R . . C8A C -0.0249(8) 0.2888(7) 0.2370(3) 0.0682(18) Uani 1 1 d . . . H8A1 H -0.0087 0.3152 0.2751 0.102 Uiso 1 1 calc R . . H8A2 H -0.1293 0.2789 0.2245 0.102 Uiso 1 1 calc R . . H8A3 H 0.0143 0.3540 0.2150 0.102 Uiso 1 1 calc R . . C9 C 0.3978(5) 0.1648(4) -0.00416(19) 0.0302(9) Uani 1 1 d . . . H9A H 0.3506 0.1529 -0.0422 0.036 Uiso 1 1 calc R . . H9B H 0.4817 0.2227 -0.0044 0.036 Uiso 1 1 calc R . . C10 C 0.4539(5) 0.0335(4) 0.01922(19) 0.0318(9) Uani 1 1 d . . . H10A H 0.5138 0.0460 0.0553 0.038 Uiso 1 1 calc R . . H10B H 0.3704 -0.0216 0.0239 0.038 Uiso 1 1 calc R . . C11 C 0.2023(5) 0.3793(4) -0.0090(2) 0.0312(9) Uani 1 1 d . . . C12 C 0.1169(6) 0.3543(5) -0.0602(2) 0.0382(11) Uani 1 1 d . . . H12 H 0.0941 0.2686 -0.0710 0.046 Uiso 1 1 calc R . . C13 C 0.0667(5) 0.4553(5) -0.0945(2) 0.0417(12) Uani 1 1 d . . . H13 H 0.0122 0.4382 -0.1292 0.050 Uiso 1 1 calc R . . C14 C 0.0960(6) 0.5809(5) -0.0782(2) 0.0447(12) Uani 1 1 d . . . H14 H 0.0617 0.6495 -0.1018 0.054 Uiso 1 1 calc R . . C15 C 0.1750(6) 0.6062(4) -0.0276(3) 0.0443(13) Uani 1 1 d . . . H15 H 0.1929 0.6924 -0.0164 0.053 Uiso 1 1 calc R . . C16 C 0.2290(5) 0.5066(4) 0.0073(2) 0.0378(11) Uani 1 1 d . . . H16 H 0.2836 0.5252 0.0418 0.045 Uiso 1 1 calc R . . C17 C 0.3714(5) 0.3117(4) 0.09570(18) 0.0297(9) Uani 1 1 d . . . C18 C 0.3038(6) 0.3263(5) 0.1420(2) 0.0446(12) Uani 1 1 d . . . H18 H 0.2074 0.2964 0.1414 0.054 Uiso 1 1 calc R . . C19 C 0.3785(7) 0.3849(5) 0.1889(2) 0.0549(15) Uani 1 1 d . . . H19 H 0.3314 0.3973 0.2195 0.066 Uiso 1 1 calc R . . C20 C 0.5209(7) 0.4244(6) 0.1904(2) 0.0550(15) Uani 1 1 d . . . H20 H 0.5719 0.4626 0.2223 0.066 Uiso 1 1 calc R . . C21 C 0.5887(7) 0.4084(6) 0.1454(2) 0.0527(15) Uani 1 1 d . . . H21 H 0.6862 0.4360 0.1467 0.063 Uiso 1 1 calc R . . C22 C 0.5160(6) 0.3525(5) 0.0985(2) 0.0450(12) Uani 1 1 d . . . H22 H 0.5642 0.3417 0.0680 0.054 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 Au 0.03451(10) 0.02727(9) 0.03111(11) -0.00019(7) 0.00767(7) -0.00012(7) S1 0.0442(7) 0.0419(6) 0.0320(6) -0.0065(5) 0.0096(5) -0.0144(5) P1 0.0310(5) 0.0259(5) 0.0273(6) -0.0006(4) 0.0066(4) 0.0025(4) O1 0.0425(19) 0.053(2) 0.038(2) -0.0105(17) 0.0016(15) -0.0150(15) N1 0.043(2) 0.045(2) 0.029(2) -0.0016(18) 0.0023(17) -0.0078(18) C1 0.038(2) 0.033(2) 0.030(2) -0.0003(19) 0.0014(19) -0.0037(19) C2 0.037(2) 0.043(2) 0.022(2) 0.0051(19) 0.0029(18) -0.004(2) C3 0.048(3) 0.039(2) 0.033(3) 0.003(2) 0.007(2) -0.002(2) C4 0.040(3) 0.052(3) 0.035(3) 0.003(2) 0.009(2) 0.002(2) C5 0.047(3) 0.053(3) 0.039(3) 0.000(2) 0.010(2) -0.015(2) C6 0.059(3) 0.036(2) 0.043(3) -0.006(2) 0.013(2) -0.009(2) C7 0.048(3) 0.044(3) 0.033(3) 0.008(2) 0.008(2) -0.001(2) C5' 0.053(4) 0.074(4) 0.085(5) -0.016(4) 0.010(3) -0.026(3) C8 0.053(3) 0.064(3) 0.036(3) -0.006(3) -0.001(2) -0.015(3) C8A 0.075(4) 0.073(4) 0.056(4) -0.024(4) 0.006(3) -0.011(3) C9 0.028(2) 0.034(2) 0.029(2) -0.0041(19) 0.0070(17) 0.0028(17) C10 0.036(2) 0.035(2) 0.025(2) -0.0040(19) 0.0060(18) 0.0083(18) C11 0.033(2) 0.031(2) 0.032(2) 0.0037(18) 0.0110(18) 0.0041(17) C12 0.047(3) 0.032(2) 0.034(3) 0.001(2) 0.002(2) 0.001(2) C13 0.044(3) 0.045(3) 0.036(3) 0.006(2) 0.003(2) 0.006(2) C14 0.047(3) 0.040(2) 0.049(3) 0.012(2) 0.013(2) 0.012(2) C15 0.051(3) 0.029(2) 0.057(4) 0.006(2) 0.020(3) 0.005(2) C16 0.042(3) 0.033(2) 0.039(3) -0.003(2) 0.007(2) 0.002(2) C17 0.037(2) 0.028(2) 0.025(2) -0.0005(17) 0.0064(17) 0.0005(17) C18 0.046(3) 0.052(3) 0.038(3) -0.007(2) 0.016(2) -0.007(2) C19 0.066(4) 0.068(4) 0.034(3) -0.015(3) 0.016(3) -0.009(3) C20 0.070(4) 0.061(3) 0.033(3) -0.012(3) 0.005(3) -0.015(3) C21 0.046(3) 0.070(4) 0.040(3) -0.010(3) 0.002(2) -0.015(3) C22 0.043(3) 0.055(3) 0.039(3) -0.008(2) 0.015(2) -0.010(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 Au P1 2.2689(12) . ? Au S1 2.3179(13) . ? S1 C1 1.763(5) . ? P1 C17 1.816(4) . ? P1 C11 1.823(4) . ? P1 C9 1.821(4) . ? O1 C1 1.375(5) . ? O1 C8 1.456(7) . ? N1 C1 1.265(6) . ? N1 C2 1.423(6) . ? C2 C3 1.391(7) . ? C2 C7 1.389(7) . ? C3 C4 1.387(7) . ? C3 H3 0.9400 . ? C4 C5 1.386(7) . ? C4 H4 0.9400 . ? C5 C6 1.386(8) . ? C5 C5' 1.523(7) . ? C6 C7 1.397(7) . ? C6 H6 0.9400 . ? C7 H7 0.9400 . ? C5' H5'1 0.9700 . ? C5' H5'2 0.9700 . ? C5' H5'3 0.9700 . ? C8 C8A 1.499(8) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? C8A H8A3 0.9700 . ? C9 C10 1.533(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C10 1.536(8) 3_655 ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C16 1.387(6) . ? C11 C12 1.405(7) . ? C12 C13 1.380(7) . ? C12 H12 0.9400 . ? C13 C14 1.374(7) . ? C13 H13 0.9400 . ? C14 C15 1.370(8) . ? C14 H14 0.9400 . ? C15 C16 1.384(7) . ? C15 H15 0.9400 . ? C16 H16 0.9400 . ? C17 C22 1.391(7) . ? C17 C18 1.394(7) . ? C18 C19 1.390(8) . ? C18 H18 0.9400 . ? C19 C20 1.372(9) . ? C19 H19 0.9400 . ? C20 C21 1.368(9) . ? C20 H20 0.9400 . ? C21 C22 1.372(8) . ? C21 H21 0.9400 . ? C22 H22 0.9400 . ? 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 Au S1 172.35(4) . . ? C1 S1 Au 104.54(16) . . ? C17 P1 C11 105.0(2) . . ? C17 P1 C9 107.8(2) . . ? C11 P1 C9 102.9(2) . . ? C17 P1 Au 109.81(15) . . ? C11 P1 Au 112.48(15) . . ? C9 P1 Au 117.87(15) . . ? C1 O1 C8 116.5(4) . . ? C1 N1 C2 121.6(4) . . ? N1 C1 O1 119.5(4) . . ? N1 C1 S1 128.4(4) . . ? O1 C1 S1 112.2(4) . . ? C3 C2 C7 118.6(4) . . ? C3 C2 N1 118.3(4) . . ? C7 C2 N1 122.9(4) . . ? C2 C3 C4 120.8(5) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 121.0(5) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 118.2(5) . . ? C4 C5 C5' 120.9(5) . . ? C6 C5 C5' 120.9(5) . . ? C7 C6 C5 121.3(5) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C2 120.2(5) . . ? C6 C7 H7 119.9 . . ? C2 C7 H7 119.9 . . ? C5 C5' H5'1 109.5 . . ? C5 C5' H5'2 109.5 . . ? H5'1 C5' H5'2 109.5 . . ? C5 C5' H5'3 109.5 . . ? H5'1 C5' H5'3 109.5 . . ? H5'2 C5' H5'3 109.5 . . ? O1 C8 C8A 111.6(5) . . ? O1 C8 H8A 109.3 . . ? C8A C8 H8A 109.3 . . ? O1 C8 H8B 109.3 . . ? C8A C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C8 C8A H8A1 109.5 . . ? C8 C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C8 C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? C10 C9 P1 113.7(3) . . ? C10 C9 H9A 108.8 . . ? P1 C9 H9A 108.8 . . ? C10 C9 H9B 108.8 . . ? P1 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C10 C10 C9 110.7(5) 3_655 . ? C10 C10 H10A 109.5 3_655 . ? C9 C10 H10A 109.5 . . ? C10 C10 H10B 109.5 3_655 . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? C16 C11 C12 119.0(4) . . ? C16 C11 P1 123.1(4) . . ? C12 C11 P1 118.0(3) . . ? C11 C12 C13 120.0(5) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C14 120.2(5) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 C13 120.0(5) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.9(5) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C11 C16 C15 119.8(5) . . ? C11 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C22 C17 C18 118.4(4) . . ? C22 C17 P1 122.5(4) . . ? C18 C17 P1 119.1(4) . . ? C19 C18 C17 120.2(5) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C20 C19 C18 120.0(6) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.0(5) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 120.7(6) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C17 120.5(5) . . ? C21 C22 H22 119.7 . . ? C17 C22 H22 119.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Au S1 C1 -43.8(4) . . . . ? S1 Au P1 C17 50.5(4) . . . . ? S1 Au P1 C11 -66.1(4) . . . . ? S1 Au P1 C9 174.4(3) . . . . ? C2 N1 C1 O1 -177.1(4) . . . . ? C2 N1 C1 S1 3.9(7) . . . . ? C8 O1 C1 N1 -2.2(7) . . . . ? C8 O1 C1 S1 177.0(4) . . . . ? Au S1 C1 N1 169.9(4) . . . . ? Au S1 C1 O1 -9.1(4) . . . . ? C1 N1 C2 C3 -121.2(5) . . . . ? C1 N1 C2 C7 65.2(7) . . . . ? C7 C2 C3 C4 -1.3(7) . . . . ? N1 C2 C3 C4 -175.1(4) . . . . ? C2 C3 C4 C5 1.1(8) . . . . ? C3 C4 C5 C6 -0.8(8) . . . . ? C3 C4 C5 C5' -179.9(5) . . . . ? C4 C5 C6 C7 0.7(8) . . . . ? C5' C5 C6 C7 179.8(6) . . . . ? C5 C6 C7 C2 -0.9(8) . . . . ? C3 C2 C7 C6 1.2(7) . . . . ? N1 C2 C7 C6 174.7(5) . . . . ? C1 O1 C8 C8A -80.8(6) . . . . ? C17 P1 C9 C10 77.6(4) . . . . ? C11 P1 C9 C10 -171.7(3) . . . . ? Au P1 C9 C10 -47.3(4) . . . . ? P1 C9 C10 C10 172.4(4) . . . 3_655 ? C17 P1 C11 C16 -1.8(5) . . . . ? C9 P1 C11 C16 -114.6(4) . . . . ? Au P1 C11 C16 117.6(4) . . . . ? C17 P1 C11 C12 -179.8(4) . . . . ? C9 P1 C11 C12 67.5(4) . . . . ? Au P1 C11 C12 -60.4(4) . . . . ? C16 C11 C12 C13 2.9(8) . . . . ? P1 C11 C12 C13 -179.0(4) . . . . ? C11 C12 C13 C14 -2.0(8) . . . . ? C12 C13 C14 C15 -0.2(8) . . . . ? C13 C14 C15 C16 1.3(9) . . . . ? C12 C11 C16 C15 -1.8(7) . . . . ? P1 C11 C16 C15 -179.7(4) . . . . ? C14 C15 C16 C11 -0.4(8) . . . . ? C11 P1 C17 C22 -81.6(4) . . . . ? C9 P1 C17 C22 27.6(5) . . . . ? Au P1 C17 C22 157.2(4) . . . . ? C11 P1 C17 C18 98.0(4) . . . . ? C9 P1 C17 C18 -152.8(4) . . . . ? Au P1 C17 C18 -23.2(4) . . . . ? C22 C17 C18 C19 2.4(8) . . . . ? P1 C17 C18 C19 -177.2(4) . . . . ? C17 C18 C19 C20 -2.3(9) . . . . ? C18 C19 C20 C21 1.2(10) . . . . ? C19 C20 C21 C22 -0.2(10) . . . . ? C20 C21 C22 C17 0.4(10) . . . . ? C18 C17 C22 C21 -1.5(8) . . . . ? P1 C17 C22 C21 178.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 30.1 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.59 # # 0.83 A from Au # _refine_diff_density_min -0.89 _refine_diff_density_rms 0.228 # Attachment '91.CIF' data_dppb[Au(SC(OiPr)=NC6H4Me-p)]2 _database_code_depnum_ccdc_archive 'CCDC 632744' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C50 H56 Au2 N2 O2 P2 S2' _chemical_formula_weight 1236.96 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.3315(11) _cell_length_b 10.3035(12) _cell_length_c 24.665(3) _cell_angle_alpha 90 _cell_angle_beta 95.074(3) _cell_angle_gamma 90 _cell_volume 2362.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 827 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 25.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1212 _exptl_absorpt_coefficient_mu 6.401 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.567 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details '(SADABS, Bruker, 2000 & Blessing, 1995)' _diffrn_ambient_temperature 223(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 'Bruker AXS SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 19232 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.048 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.7 _diffrn_reflns_theta_max 30.0 _reflns_number_total 6866 _reflns_number_gt 5455 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'Bruker SHEXLTL (Bruker, 2000)' _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^)+(0.0434P)^2^+0.1579P] 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 6866 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.054 _refine_ls_R_factor_gt 0.039 _refine_ls_wR_factor_ref 0.092 _refine_ls_wR_factor_gt 0.087 _refine_ls_goodness_of_fit_ref 1.03 _refine_ls_restrained_S_all 1.03 _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 Au Au 0.074293(17) 0.120438(15) 0.058574(7) 0.03338(6) Uani 1 1 d . . . S1 S -0.12900(13) 0.02015(13) 0.08579(5) 0.0423(3) Uani 1 1 d . . . P1 P 0.26205(12) 0.24034(11) 0.03532(4) 0.0307(2) Uani 1 1 d . . . O1 O 0.0007(4) 0.1032(4) 0.17780(14) 0.0538(10) Uani 1 1 d . . . N1 N -0.2272(5) 0.0325(5) 0.18668(17) 0.0526(11) Uani 1 1 d . . . C1 C -0.1262(5) 0.0517(5) 0.1563(2) 0.0449(11) Uani 1 1 d . . . C2 C -0.3568(5) -0.0302(5) 0.16760(18) 0.0445(11) Uani 1 1 d . . . C3 C -0.4872(5) 0.0346(6) 0.1707(2) 0.0478(12) Uani 1 1 d . . . H3 H -0.4877 0.1208 0.1832 0.057 Uiso 1 1 calc R . . C4 C -0.6139(6) -0.0270(6) 0.1557(2) 0.0513(13) Uani 1 1 d . . . H4 H -0.7001 0.0198 0.1567 0.062 Uiso 1 1 calc R . . C5 C -0.6213(6) -0.1547(6) 0.1392(2) 0.0543(14) Uani 1 1 d . . . C6 C -0.4912(6) -0.2201(6) 0.1384(2) 0.0569(14) Uani 1 1 d . . . H6 H -0.4918 -0.3084 0.1288 0.068 Uiso 1 1 calc R . . C7 C -0.3623(6) -0.1594(6) 0.1512(2) 0.0528(13) Uani 1 1 d . . . H7 H -0.2762 -0.2056 0.1488 0.063 Uiso 1 1 calc R . . C5' C -0.7617(6) -0.2194(7) 0.1219(3) 0.0700(18) Uani 1 1 d . . . H5'1 H -0.7646 -0.2422 0.0836 0.105 Uiso 1 1 calc R . . H5'2 H -0.8402 -0.1605 0.1275 0.105 Uiso 1 1 calc R . . H5'3 H -0.7712 -0.2973 0.1433 0.105 Uiso 1 1 calc R . . C8 C 0.0118(7) 0.1360(6) 0.2360(2) 0.0610(16) Uani 1 1 d . . . H8 H -0.0507 0.0770 0.2551 0.073 Uiso 1 1 calc R . . C8A C -0.0363(8) 0.2699(7) 0.2422(3) 0.084(2) Uani 1 1 d . . . H8A1 H -0.1370 0.2770 0.2289 0.126 Uiso 1 1 calc R . . H8A2 H 0.0204 0.3273 0.2214 0.126 Uiso 1 1 calc R . . H8A3 H -0.0241 0.2941 0.2803 0.126 Uiso 1 1 calc R . . C8B C 0.1660(8) 0.1138(7) 0.2569(3) 0.082(2) Uani 1 1 d . . . H8B1 H 0.1904 0.0232 0.2521 0.124 Uiso 1 1 calc R . . H8B2 H 0.1792 0.1360 0.2952 0.124 Uiso 1 1 calc R . . H8B3 H 0.2280 0.1678 0.2367 0.124 Uiso 1 1 calc R . . C9 C 0.3948(5) 0.1619(4) -0.00348(17) 0.0330(9) Uani 1 1 d . . . H9A H 0.3519 0.1483 -0.0408 0.040 Uiso 1 1 calc R . . H9B H 0.4765 0.2210 -0.0053 0.040 Uiso 1 1 calc R . . C10 C 0.4507(5) 0.0334(4) 0.01893(16) 0.0348(9) Uani 1 1 d . . . H10A H 0.3691 -0.0237 0.0243 0.042 Uiso 1 1 calc R . . H10B H 0.5039 0.0475 0.0545 0.042 Uiso 1 1 calc R . . C11 C 0.2028(5) 0.3779(4) -0.00782(18) 0.0346(9) Uani 1 1 d . . . C12 C 0.1219(5) 0.3523(5) -0.05634(19) 0.0429(11) Uani 1 1 d . . . H12 H 0.0972 0.2662 -0.0657 0.052 Uiso 1 1 calc R . . C13 C 0.0766(5) 0.4526(5) -0.0915(2) 0.0455(12) Uani 1 1 d . . . H13 H 0.0242 0.4342 -0.1249 0.055 Uiso 1 1 calc R . . C14 C 0.1084(6) 0.5775(5) -0.0773(2) 0.0491(12) Uani 1 1 d . . . H14 H 0.0780 0.6456 -0.1009 0.059 Uiso 1 1 calc R . . C15 C 0.1851(6) 0.6042(5) -0.0284(2) 0.0491(13) Uani 1 1 d . . . H15 H 0.2049 0.6908 -0.0184 0.059 Uiso 1 1 calc R . . C16 C 0.2333(5) 0.5055(5) 0.00591(19) 0.0420(11) Uani 1 1 d . . . H16 H 0.2872 0.5248 0.0389 0.050 Uiso 1 1 calc R . . C17 C 0.3563(5) 0.3124(5) 0.09565(17) 0.0353(9) Uani 1 1 d . . . C18 C 0.5002(6) 0.3447(6) 0.0984(2) 0.0575(15) Uani 1 1 d . . . H18 H 0.5534 0.3266 0.0686 0.069 Uiso 1 1 calc R . . C19 C 0.5668(7) 0.4030(7) 0.1440(3) 0.0692(19) Uani 1 1 d . . . H19 H 0.6646 0.4254 0.1451 0.083 Uiso 1 1 calc R . . C20 C 0.4906(6) 0.4286(6) 0.1880(2) 0.0598(15) Uani 1 1 d . . . H20 H 0.5370 0.4663 0.2196 0.072 Uiso 1 1 calc R . . C21 C 0.3462(6) 0.3989(5) 0.1859(2) 0.0536(14) Uani 1 1 d . . . H21 H 0.2929 0.4194 0.2154 0.064 Uiso 1 1 calc R . . C22 C 0.2804(6) 0.3388(5) 0.14030(19) 0.0460(12) Uani 1 1 d . . . H22 H 0.1828 0.3155 0.1394 0.055 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 Au 0.03198(9) 0.03436(10) 0.03445(10) -0.00062(7) 0.00656(6) -0.00073(7) S1 0.0419(6) 0.0509(7) 0.0349(6) -0.0042(5) 0.0082(5) -0.0155(5) P1 0.0293(5) 0.0332(5) 0.0304(5) -0.0023(4) 0.0070(4) 0.0002(4) O1 0.047(2) 0.075(3) 0.0387(19) -0.0032(17) 0.0025(16) -0.0106(18) N1 0.045(2) 0.071(3) 0.042(2) -0.002(2) 0.0099(18) -0.010(2) C1 0.036(3) 0.053(3) 0.046(3) 0.004(2) 0.005(2) -0.003(2) C2 0.043(3) 0.060(3) 0.031(2) 0.003(2) 0.0097(19) -0.007(2) C3 0.045(3) 0.057(3) 0.042(3) 0.001(2) 0.009(2) -0.001(2) C4 0.047(3) 0.064(4) 0.043(3) 0.002(3) 0.005(2) 0.007(3) C5 0.049(3) 0.067(4) 0.048(3) 0.003(3) 0.012(2) -0.010(3) C6 0.062(4) 0.046(3) 0.066(4) 0.004(3) 0.020(3) -0.001(3) C7 0.052(3) 0.059(3) 0.048(3) 0.008(3) 0.010(2) 0.003(3) C5' 0.057(4) 0.077(4) 0.077(4) -0.010(4) 0.007(3) -0.028(3) C8 0.060(4) 0.084(5) 0.039(3) -0.006(3) 0.002(2) -0.015(3) C8A 0.091(5) 0.088(5) 0.075(5) -0.023(4) 0.017(4) -0.008(4) C8B 0.068(4) 0.123(7) 0.054(4) 0.000(4) -0.005(3) -0.032(4) C9 0.035(2) 0.035(2) 0.030(2) -0.0023(17) 0.0073(17) 0.0011(18) C10 0.033(2) 0.044(2) 0.027(2) -0.0034(18) 0.0078(16) 0.0082(19) C11 0.031(2) 0.036(2) 0.038(2) 0.0031(19) 0.0088(17) 0.0013(18) C12 0.042(3) 0.046(3) 0.041(3) -0.001(2) 0.003(2) -0.001(2) C13 0.046(3) 0.051(3) 0.040(3) 0.003(2) 0.005(2) 0.012(2) C14 0.049(3) 0.046(3) 0.055(3) 0.012(2) 0.015(2) 0.012(2) C15 0.052(3) 0.036(3) 0.061(3) 0.002(2) 0.015(3) 0.003(2) C16 0.044(3) 0.042(3) 0.041(3) -0.005(2) 0.008(2) -0.003(2) C17 0.035(2) 0.042(2) 0.030(2) -0.0045(18) 0.0097(17) -0.0022(19) C18 0.046(3) 0.081(4) 0.048(3) -0.023(3) 0.014(2) -0.016(3) C19 0.046(3) 0.104(5) 0.058(4) -0.031(3) 0.008(3) -0.021(3) C20 0.060(4) 0.077(4) 0.042(3) -0.019(3) 0.003(3) -0.013(3) C21 0.054(3) 0.065(4) 0.043(3) -0.020(2) 0.014(2) -0.006(3) C22 0.040(3) 0.062(3) 0.037(2) -0.008(2) 0.010(2) -0.002(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 Au P1 2.2589(11) . ? Au S1 2.3113(12) . ? S1 C1 1.768(5) . ? P1 C17 1.819(4) . ? P1 C11 1.828(4) . ? P1 C9 1.820(4) . ? O1 C1 1.362(6) . ? O1 C8 1.469(6) . ? N1 C1 1.269(6) . ? N1 C2 1.415(6) . ? C2 C3 1.396(7) . ? C2 C7 1.391(8) . ? C3 C4 1.365(7) . ? C3 H3 0.9400 . ? C4 C5 1.377(8) . ? C4 H4 0.9400 . ? C5 C6 1.391(8) . ? C5 C5' 1.498(7) . ? C6 C7 1.368(8) . ? C6 H6 0.9400 . ? C7 H7 0.9400 . ? C5' H5'1 0.9700 . ? C5' H5'2 0.9700 . ? C5' H5'3 0.9700 . ? C8 C8A 1.463(8) . ? C8 C8B 1.502(9) . ? C8 H8 0.9900 . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? C8A H8A3 0.9700 . ? C8B H8B1 0.9700 . ? C8B H8B2 0.9700 . ? C8B H8B3 0.9700 . ? C9 C10 1.510(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C10 1.531(8) 3_655 ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.383(6) . ? C11 C16 1.381(6) . ? C12 C13 1.390(7) . ? C12 H12 0.9400 . ? C13 C14 1.359(7) . ? C13 H13 0.9400 . ? C14 C15 1.374(8) . ? C14 H14 0.9400 . ? C15 C16 1.373(7) . ? C15 H15 0.9400 . ? C16 H16 0.9400 . ? C17 C18 1.379(7) . ? C17 C22 1.388(6) . ? C18 C19 1.375(8) . ? C18 H18 0.9400 . ? C19 C20 1.374(8) . ? C19 H19 0.9400 . ? C20 C21 1.379(8) . ? C20 H20 0.9400 . ? C21 C22 1.380(7) . ? C21 H21 0.9400 . ? C22 H22 0.9400 . ? 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 Au S1 173.31(4) . . ? C1 S1 Au 105.24(17) . . ? C17 P1 C11 105.0(2) . . ? C17 P1 C9 108.0(2) . . ? C11 P1 C9 102.9(2) . . ? C17 P1 Au 110.20(14) . . ? C11 P1 Au 111.73(15) . . ? C9 P1 Au 118.03(15) . . ? C1 O1 C8 117.0(4) . . ? C1 N1 C2 122.2(4) . . ? N1 C1 O1 119.8(5) . . ? N1 C1 S1 127.2(4) . . ? O1 C1 S1 113.0(3) . . ? C3 C2 C7 117.7(5) . . ? C3 C2 N1 119.2(5) . . ? C7 C2 N1 122.8(5) . . ? C2 C3 C4 120.1(5) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 123.0(5) . . ? C3 C4 H4 118.5 . . ? C5 C4 H4 118.5 . . ? C6 C5 C4 116.5(5) . . ? C6 C5 C5' 121.5(6) . . ? C4 C5 C5' 121.9(6) . . ? C5 C6 C7 121.7(6) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C2 C7 C6 120.9(5) . . ? C2 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C5 C5' H5'1 109.5 . . ? C5 C5' H5'2 109.5 . . ? H5'1 C5' H5'2 109.5 . . ? C5 C5' H5'3 109.5 . . ? H5'1 C5' H5'3 109.5 . . ? H5'2 C5' H5'3 109.5 . . ? O1 C8 C8A 108.8(5) . . ? O1 C8 C8B 106.4(5) . . ? C8A C8 C8B 113.7(6) . . ? O1 C8 H8 109.3 . . ? C8A C8 H8 109.3 . . ? C8B C8 H8 109.3 . . ? C8 C8A H8A1 109.5 . . ? C8 C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C8 C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? C8 C8B H8B1 109.5 . . ? C8 C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? C8 C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C10 C9 P1 115.2(3) . . ? C10 C9 H9A 108.5 . . ? P1 C9 H9A 108.5 . . ? C10 C9 H9B 108.5 . . ? P1 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? C9 C10 C10 112.2(4) . 3_655 ? C9 C10 H10A 109.2 . . ? C10 C10 H10A 109.2 3_655 . ? C9 C10 H10B 109.2 . . ? C10 C10 H10B 109.2 3_655 . ? H10A C10 H10B 107.9 . . ? C12 C11 C16 118.6(4) . . ? C12 C11 P1 118.0(4) . . ? C16 C11 P1 123.4(4) . . ? C11 C12 C13 120.7(5) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C14 119.7(5) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 120.0(5) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.6(5) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C11 C16 C15 120.3(5) . . ? C11 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C22 118.5(4) . . ? C18 C17 P1 122.4(3) . . ? C22 C17 P1 119.0(4) . . ? C17 C18 C19 120.8(5) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C20 C19 C18 120.2(6) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 120.0(5) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C22 119.6(5) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C21 C22 C17 120.9(5) . . ? C21 C22 H22 119.6 . . ? C17 C22 H22 119.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Au S1 C1 -60.3(4) . . . . ? S1 Au P1 C17 63.9(4) . . . . ? S1 Au P1 C11 -52.5(4) . . . . ? S1 Au P1 C9 -171.4(3) . . . . ? C2 N1 C1 O1 -174.8(5) . . . . ? C2 N1 C1 S1 5.8(8) . . . . ? C8 O1 C1 N1 -1.0(7) . . . . ? C8 O1 C1 S1 178.4(4) . . . . ? Au S1 C1 N1 168.5(5) . . . . ? Au S1 C1 O1 -10.9(4) . . . . ? C1 N1 C2 C3 -122.2(6) . . . . ? C1 N1 C2 C7 64.9(7) . . . . ? C7 C2 C3 C4 -2.7(7) . . . . ? N1 C2 C3 C4 -175.9(4) . . . . ? C2 C3 C4 C5 2.7(8) . . . . ? C3 C4 C5 C6 0.0(8) . . . . ? C3 C4 C5 C5' -178.8(5) . . . . ? C4 C5 C6 C7 -2.6(8) . . . . ? C5' C5 C6 C7 176.3(5) . . . . ? C3 C2 C7 C6 0.2(7) . . . . ? N1 C2 C7 C6 173.2(5) . . . . ? C5 C6 C7 C2 2.5(8) . . . . ? C1 O1 C8 C8A -89.8(6) . . . . ? C1 O1 C8 C8B 147.3(5) . . . . ? C17 P1 C9 C10 76.6(4) . . . . ? C11 P1 C9 C10 -172.7(3) . . . . ? Au P1 C9 C10 -49.2(4) . . . . ? P1 C9 C10 C10 173.9(4) . . . 3_655 ? C17 P1 C11 C12 -177.4(4) . . . . ? C9 P1 C11 C12 69.6(4) . . . . ? Au P1 C11 C12 -58.0(4) . . . . ? C17 P1 C11 C16 1.8(4) . . . . ? C9 P1 C11 C16 -111.2(4) . . . . ? Au P1 C11 C16 121.2(4) . . . . ? C16 C11 C12 C13 2.3(7) . . . . ? P1 C11 C12 C13 -178.5(4) . . . . ? C11 C12 C13 C14 -2.0(7) . . . . ? C12 C13 C14 C15 0.0(8) . . . . ? C13 C14 C15 C16 1.5(8) . . . . ? C12 C11 C16 C15 -0.7(7) . . . . ? P1 C11 C16 C15 -179.9(4) . . . . ? C14 C15 C16 C11 -1.2(8) . . . . ? C11 P1 C17 C18 -86.2(5) . . . . ? C9 P1 C17 C18 23.1(5) . . . . ? Au P1 C17 C18 153.4(4) . . . . ? C11 P1 C17 C22 92.4(4) . . . . ? C9 P1 C17 C22 -158.4(4) . . . . ? Au P1 C17 C22 -28.1(4) . . . . ? C22 C17 C18 C19 -0.7(9) . . . . ? P1 C17 C18 C19 177.8(5) . . . . ? C17 C18 C19 C20 0.8(11) . . . . ? C18 C19 C20 C21 -1.7(11) . . . . ? C19 C20 C21 C22 2.6(10) . . . . ? C20 C21 C22 C17 -2.5(9) . . . . ? C18 C17 C22 C21 1.5(8) . . . . ? P1 C17 C22 C21 -177.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.0 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.83 # # 0.77 A from Au # _refine_diff_density_min -0.49 _refine_diff_density_rms 0.134