# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1796 data_global #======================================================================= # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Ulrich Abram Institut f\"ur Analytische Chemie Technische Universit\"at Dresden D-0162 Dresden Bundesrepublik Deutschland ; _publ_contact_author_phone '049 351 463 2508 ' _publ_contact_author_fax '049 351 463 7188' _publ_contact_author_email 'abram@fz-rossendorf.de' _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Gold Complexes with Thiosemicarbazones: Reactions of bi- and tridentate thiosemicarbazones...... ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Abram, Ulrich' ; Institut f\"ur Analytische Chemie Technische Universit\"at Dresden D-01062 Dresden Bundesrepublik Deutschland ; 'Ortner, Kirstin' ; Institut f\"ur Anorganische Chemie Universit\"at T\"ubingen Auf der Morgenstelle 18 D-72076 T\"ubingen Bundesrepublik Deutschland ; 'Gust, Ronald' ; Institut f\"ur Pharmazie Universit\"at Berlin Koenigin-Louise-Strasse 2-4 D-14195 Berlin Bundesrepublik Deutschland ; 'Sommer, Klaus' ; Institut f\"ur Pharmazie Universit\"at Berlin Koenigin-Louise-Strasse 2-4 D-14195 Berlin Bundesrepublik Deutschland ; #=============================================================== ##################### Structure 1 ################################# data_satscneu _audit_creation_method SHELXL-97 _chemical_name_systematic [Au(Hdamp-C1)Cl(Hsaltsc)]PF6 _chemical_name_common [Au(Hdamp-C1)Cl(Hsaltsc)]PF6 _chemical_formula_moiety [Au(Hdamp-C1)Cl(Hsaltsc)]PF6 _chemical_formula_sum 'C17 H21 Au Cl F6 N4 O P S' _chemical_formula_weight 706.82 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.799(3) _cell_length_b 10.504(1) _cell_length_c 16.973(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.38(1) _cell_angle_gamma 90.00 _cell_volume 2277.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.199 _cell_measurement_theta_max 13.594 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.061 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 6.804 _exptl_absorpt_correction_type 'Psi scans ' _exptl_absorpt_correction_T_min 0.7614 _exptl_absorpt_correction_T_max 0.9528 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4 _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5608 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0769 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 26.94 _reflns_number_total 4938 _reflns_number_gt 3338 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement SET4 _computing_data_reduction 'HELENA (Spek, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1995)' _computing_publication_material SHELX _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 w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+1.1101P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4938 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0916 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0862 _refine_ls_wR_factor_gt 0.0743 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.15731(2) 0.04695(3) 0.061751(15) 0.03424(9) Uani 1 d . . . Cl1 Cl 0.26055(16) 0.11754(18) -0.03745(10) 0.0468(5) Uani 1 d . . . C1 C 0.1691(6) 0.2168(6) 0.1195(4) 0.0358(16) Uani 1 d . . . C2 C 0.0811(6) 0.2933(7) 0.1180(4) 0.0441(18) Uani 1 d . . . H2 H 0.0213 0.2681 0.0883 0.053 Uiso 1 calc R . . C3 C 0.0801(7) 0.4051(7) 0.1591(5) 0.052(2) Uani 1 d . . . H3 H 0.0206 0.4561 0.1567 0.063 Uiso 1 calc R . . C4 C 0.1683(8) 0.4416(8) 0.2045(5) 0.062(2) Uani 1 d . . . H4 H 0.1679 0.5163 0.2339 0.074 Uiso 1 calc R . . C5 C 0.2561(7) 0.3678(9) 0.2059(5) 0.056(2) Uani 1 d . . . H5 H 0.3154 0.3934 0.2360 0.067 Uiso 1 calc R . . C6 C 0.2585(6) 0.2554(7) 0.1633(4) 0.0394(17) Uani 1 d . . . C7 C 0.3592(6) 0.1798(8) 0.1636(4) 0.0453(19) Uani 1 d . . . H7A H 0.3982 0.1931 0.2137 0.054 Uiso 1 calc R . . H7B H 0.3421 0.0900 0.1596 0.054 Uiso 1 calc R . . N8 N 0.4284(6) 0.2142(7) 0.0979(4) 0.0463(17) Uani 1 d . . . H8 H 0.392(6) 0.200(7) 0.062(4) 0.03(2) Uiso 1 d . . . C9 C 0.5237(7) 0.1318(10) 0.1006(5) 0.069(3) Uani 1 d . . . H9A H 0.5033 0.0440 0.1026 0.104 Uiso 1 calc R . . H9B H 0.5676 0.1523 0.1467 0.104 Uiso 1 calc R . . H9C H 0.5615 0.1463 0.0542 0.104 Uiso 1 calc R . . C10 C 0.4541(7) 0.3506(9) 0.0946(5) 0.068(3) Uani 1 d . . . H10A H 0.3907 0.3997 0.0931 0.102 Uiso 1 calc R . . H10B H 0.4909 0.3676 0.0481 0.102 Uiso 1 calc R . . H10C H 0.4973 0.3736 0.1406 0.102 Uiso 1 calc R . . S11 S 0.05461(17) -0.01845(19) 0.15671(11) 0.0483(5) Uani 1 d . . . C12 C 0.0340(6) -0.1729(7) 0.1193(4) 0.0448(18) Uani 1 d . . . N13 N -0.0279(7) -0.2475(9) 0.1629(5) 0.066(2) Uani 1 d . . . H13A H -0.047(10) -0.216(12) 0.203(7) 0.13(5) Uiso 1 d . . . H13B H -0.045(8) -0.322(11) 0.150(6) 0.10(4) Uiso 1 d . . . N14 N 0.0701(5) -0.2200(6) 0.0562(3) 0.0454(16) Uani 1 d . . . N15 N 0.1339(4) -0.1387(5) 0.0160(3) 0.0357(13) Uani 1 d . . . C16 C 0.1827(6) -0.1848(7) -0.0419(4) 0.0373(17) Uani 1 d . . . H16 H 0.212(6) -0.119(8) -0.063(5) 0.06(3) Uiso 1 d . . . C17 C 0.1919(5) -0.3152(7) -0.0690(4) 0.0355(16) Uani 1 d . . . C18 C 0.2251(6) -0.3295(7) -0.1452(4) 0.0390(17) Uani 1 d . . . O19 O 0.2341(5) -0.2221(6) -0.1901(4) 0.0630(18) Uani 1 d . . . H19 H 0.251(8) -0.238(10) -0.237(5) 0.09(3) Uiso 1 d . . . C20 C 0.2495(6) -0.4518(8) -0.1722(4) 0.0494(19) Uani 1 d . . . H20 H 0.2724 -0.4623 -0.2228 0.059 Uiso 1 calc R . . C21 C 0.2399(7) -0.5540(8) -0.1250(5) 0.057(2) Uani 1 d . . . H21 H 0.2581 -0.6343 -0.1428 0.069 Uiso 1 calc R . . C22 C 0.2035(7) -0.5404(8) -0.0513(5) 0.058(2) Uani 1 d . . . H22 H 0.1953 -0.6117 -0.0198 0.070 Uiso 1 calc R . . C23 C 0.1791(7) -0.4219(7) -0.0236(5) 0.051(2) Uani 1 d . . . H23 H 0.1535 -0.4137 0.0263 0.061 Uiso 1 calc R . . P30 P 0.41971(18) -0.2465(2) -0.36233(12) 0.0499(5) Uani 1 d . . . F31 F 0.4403(6) -0.3370(6) -0.2897(3) 0.114(2) Uani 1 d . . . F32 F 0.3940(5) -0.1569(6) -0.4337(3) 0.0947(19) Uani 1 d . . . F33 F 0.3858(6) -0.3631(7) -0.4146(4) 0.118(2) Uani 1 d . . . F34 F 0.5328(5) -0.2629(9) -0.3826(5) 0.151(3) Uani 1 d . . . F35 F 0.4453(7) -0.1323(6) -0.3070(4) 0.134(3) Uani 1 d . . . F36 F 0.3011(5) -0.2356(10) -0.3420(4) 0.137(3) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.03464(14) 0.03173(13) 0.03644(13) -0.00521(14) 0.00286(9) -0.00184(16) Cl1 0.0598(12) 0.0409(10) 0.0406(9) -0.0016(8) 0.0109(9) -0.0081(10) C1 0.044(4) 0.031(4) 0.033(3) -0.008(3) 0.007(3) -0.005(3) C2 0.041(4) 0.042(4) 0.050(4) -0.008(4) 0.006(4) 0.007(4) C3 0.060(5) 0.035(4) 0.064(5) -0.004(4) 0.021(4) 0.002(4) C4 0.079(6) 0.039(5) 0.070(5) -0.020(5) 0.024(5) -0.010(5) C5 0.060(5) 0.055(5) 0.053(5) -0.011(4) 0.008(4) -0.016(5) C6 0.046(4) 0.038(4) 0.034(4) 0.001(3) 0.004(3) -0.009(4) C7 0.039(4) 0.053(5) 0.044(4) 0.005(4) 0.000(3) -0.011(4) N8 0.045(4) 0.052(4) 0.042(4) 0.001(3) 0.002(3) -0.003(4) C9 0.046(5) 0.081(7) 0.082(6) 0.009(6) 0.011(5) 0.014(5) C10 0.076(7) 0.063(6) 0.067(6) 0.004(5) 0.024(5) -0.021(5) S11 0.0568(12) 0.0425(12) 0.0475(10) -0.0119(9) 0.0194(9) -0.0112(10) C12 0.046(5) 0.039(4) 0.050(4) -0.004(4) 0.009(4) 0.000(4) N13 0.087(6) 0.048(5) 0.067(5) -0.007(4) 0.037(5) -0.013(5) N14 0.049(4) 0.040(4) 0.048(4) -0.008(3) 0.007(3) -0.013(3) N15 0.038(3) 0.032(3) 0.036(3) -0.004(3) 0.000(3) -0.004(3) C16 0.041(4) 0.032(4) 0.038(4) 0.005(3) -0.003(3) -0.001(4) C17 0.035(4) 0.037(4) 0.034(4) -0.007(3) 0.003(3) -0.006(3) C18 0.036(4) 0.039(4) 0.043(4) -0.007(3) 0.006(3) 0.002(3) O19 0.095(5) 0.045(3) 0.051(4) 0.004(3) 0.028(3) 0.002(3) C20 0.056(5) 0.052(5) 0.042(4) -0.007(4) 0.018(3) -0.002(5) C21 0.063(5) 0.033(4) 0.076(6) -0.013(5) 0.012(4) 0.007(5) C22 0.080(6) 0.031(4) 0.065(5) 0.004(4) 0.021(5) 0.008(5) C23 0.061(5) 0.046(5) 0.047(4) -0.004(4) 0.007(4) -0.005(4) P30 0.0524(13) 0.0566(13) 0.0406(11) 0.0016(10) 0.0035(10) 0.0014(11) F31 0.162(7) 0.098(5) 0.078(4) 0.036(4) -0.024(4) -0.011(5) F32 0.123(5) 0.088(4) 0.072(3) 0.025(3) 0.000(3) 0.012(4) F33 0.154(6) 0.083(4) 0.110(5) -0.030(4) -0.045(5) 0.006(5) F34 0.061(4) 0.213(9) 0.182(7) 0.040(7) 0.043(5) 0.018(5) F35 0.213(8) 0.080(4) 0.102(5) -0.028(4) -0.059(5) 0.016(6) F36 0.077(4) 0.244(10) 0.092(5) 0.011(6) 0.022(4) 0.023(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C1 2.037(6) . ? Au1 N15 2.114(6) . ? Au1 S11 2.2466(19) . ? Au1 Cl1 2.3223(18) . ? C1 C2 1.383(10) . ? C1 C6 1.387(9) . ? C2 C3 1.367(10) . ? C3 C4 1.383(12) . ? C4 C5 1.364(12) . ? C5 C6 1.386(10) . ? C6 C7 1.514(10) . ? C7 N8 1.508(9) . ? N8 C10 1.472(11) . ? N8 C9 1.494(10) . ? S11 C12 1.756(8) . ? C12 N14 1.291(9) . ? C12 N13 1.364(11) . ? N14 N15 1.388(8) . ? N15 C16 1.289(9) . ? C16 C17 1.452(10) . ? C17 C23 1.375(10) . ? C17 C18 1.393(9) . ? C18 O19 1.370(9) . ? C18 C20 1.406(10) . ? C20 C21 1.349(11) . ? C21 C22 1.369(11) . ? C22 C23 1.372(11) . ? P30 F34 1.518(7) . ? P30 F35 1.546(6) . ? P30 F32 1.554(6) . ? P30 F33 1.559(6) . ? P30 F31 1.566(6) . ? P30 F36 1.581(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 N15 171.8(2) . . ? C1 Au1 S11 87.27(19) . . ? N15 Au1 S11 84.57(16) . . ? C1 Au1 Cl1 92.30(19) . . ? N15 Au1 Cl1 95.88(16) . . ? S11 Au1 Cl1 178.74(8) . . ? C2 C1 C6 119.0(6) . . ? C2 C1 Au1 117.6(5) . . ? C6 C1 Au1 123.3(5) . . ? C3 C2 C1 121.5(7) . . ? C2 C3 C4 119.3(8) . . ? C5 C4 C3 119.8(8) . . ? C4 C5 C6 121.2(8) . . ? C5 C6 C1 119.0(7) . . ? C5 C6 C7 119.4(7) . . ? C1 C6 C7 121.6(6) . . ? N8 C7 C6 114.2(6) . . ? C10 N8 C9 112.4(7) . . ? C10 N8 C7 113.7(7) . . ? C9 N8 C7 110.7(7) . . ? C12 S11 Au1 96.0(3) . . ? N14 C12 N13 118.6(8) . . ? N14 C12 S11 126.9(6) . . ? N13 C12 S11 114.5(6) . . ? C12 N14 N15 115.0(6) . . ? C16 N15 N14 118.0(6) . . ? C16 N15 Au1 124.2(5) . . ? N14 N15 Au1 117.5(4) . . ? N15 C16 C17 130.4(7) . . ? C23 C17 C18 119.0(7) . . ? C23 C17 C16 125.2(6) . . ? C18 C17 C16 115.5(7) . . ? O19 C18 C17 117.9(6) . . ? O19 C18 C20 122.9(6) . . ? C17 C18 C20 119.2(7) . . ? C21 C20 C18 120.2(7) . . ? C20 C21 C22 120.5(8) . . ? C21 C22 C23 120.3(8) . . ? C22 C23 C17 120.7(7) . . ? F34 P30 F35 93.2(5) . . ? F34 P30 F32 93.0(4) . . ? F35 P30 F32 91.8(4) . . ? F34 P30 F33 91.1(5) . . ? F35 P30 F33 175.5(5) . . ? F32 P30 F33 89.6(4) . . ? F34 P30 F31 89.5(4) . . ? F35 P30 F31 88.5(4) . . ? F32 P30 F31 177.4(4) . . ? F33 P30 F31 89.9(4) . . ? F34 P30 F36 177.6(6) . . ? F35 P30 F36 89.0(5) . . ? F32 P30 F36 87.9(4) . . ? F33 P30 F36 86.7(5) . . ? F31 P30 F36 89.5(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N8 H8 Cl1 0.75(7) 2.47(7) 3.216(8) 168(7) . O19 H19 F36 0.86(9) 1.92(9) 2.769(9) 167(10) . _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 26.94 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.731 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.152 ################## Structure 2 ################################ data_komepy _audit_creation_method SHELXL-97 _chemical_name_systematic ; (2-(N,N-dimethylammoniummethyl)phenyl-C)(N-methylpyrrol-2-carboxaldehydetsc) (Cl)Au(III))Cl ; _chemical_name_common [Au(Hdamp-C1)Cl(mepyrtsc)]Cl _chemical_formula_moiety [Au(Hdamp-C1)Cl(mepyrtsc)]Cl _chemical_formula_sum 'C16 H22 Au Cl2 N5 S' _chemical_formula_weight 584.31 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' '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 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 12.8583(14) _cell_length_b 12.559(3) _cell_length_c 12.904(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.206(17) _cell_angle_gamma 90.00 _cell_volume 2067.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.6 _cell_measurement_theta_max 14.82 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.877 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 7.485 _exptl_absorpt_correction_type 'psi scans' _exptl_absorpt_correction_T_min 0.74283 _exptl_absorpt_correction_T_max 0.97173 _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD4 ENRAF NONIUS' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 2 _diffrn_reflns_number 5083 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.1210 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 26.97 _reflns_number_total 4487 _reflns_number_gt 2735 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement 'SET4, CELDIM' _computing_data_reduction HELENA/PLATON _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL, ZORTEP' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'H(8) and H(16) fully refined, others calculated' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4487 _refine_ls_number_parameters 234 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1295 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.013 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.22946(3) 0.04229(3) 0.83506(3) 0.02955(11) Uani 1 d . . . Cl2 Cl 0.6411(2) 0.0695(2) 0.63755(18) 0.0516(8) Uani 1 d . . . Cl1 Cl 0.06289(19) 0.0860(2) 0.87254(19) 0.0438(6) Uani 1 d . . . S11 S 0.39071(19) 0.0028(2) 0.79638(19) 0.0380(6) Uani 1 d . . . C12 C 0.3488(7) -0.0407(8) 0.6680(7) 0.035(2) Uani 1 d . . . N13 N 0.4274(6) -0.0659(6) 0.6115(6) 0.045(2) Uani 1 d . . . H13A H 0.4129 -0.0918 0.5488 0.054 Uiso 1 calc R . . H13B H 0.4923 -0.0562 0.6379 0.054 Uiso 1 calc R . . N14 N 0.2540(6) -0.0559(7) 0.6268(6) 0.0364(19) Uani 1 d . . . N15 N 0.1790(6) -0.0326(6) 0.6914(5) 0.0294(17) Uani 1 d . . . C16 C 0.0833(8) -0.0599(7) 0.6593(7) 0.033(2) Uani 1 d . . . H16 H 0.034(6) -0.026(6) 0.700(6) 0.03(2) Uiso 1 d . . . C17 C 0.0435(8) -0.1084(7) 0.5642(7) 0.033(2) Uani 1 d . . . N18 N -0.0619(6) -0.1355(6) 0.5470(6) 0.037(2) Uani 1 d . . . C19 C -0.1395(8) -0.1182(9) 0.6181(8) 0.051(3) Uani 1 d . . . H19A H -0.1069 -0.0822 0.6804 0.077 Uiso 1 calc R . . H19B H -0.1671 -0.1863 0.6373 0.077 Uiso 1 calc R . . H19C H -0.1961 -0.0748 0.5841 0.077 Uiso 1 calc R . . C20 C -0.0829(9) -0.1835(8) 0.4530(8) 0.047(3) Uani 1 d . . . H20 H -0.1488 -0.2090 0.4235 0.057 Uiso 1 calc R . . C21 C 0.0067(10) -0.1889(8) 0.4083(8) 0.051(3) Uani 1 d . . . H21 H 0.0146 -0.2188 0.3430 0.061 Uiso 1 calc R . . C22 C 0.0845(8) -0.1421(7) 0.4770(7) 0.037(2) Uani 1 d . . . H22 H 0.1548 -0.1346 0.4655 0.045 Uiso 1 calc R . . C1 C 0.2967(7) 0.1142(7) 0.9676(7) 0.029(2) Uani 1 d . . . C2 C 0.3574(7) 0.2046(8) 0.9565(8) 0.039(2) Uani 1 d . . . H2 H 0.3669 0.2285 0.8892 0.046 Uiso 1 calc R . . C3 C 0.4038(7) 0.2595(8) 1.0431(8) 0.044(3) Uani 1 d . . . H3 H 0.4436 0.3211 1.0351 0.052 Uiso 1 calc R . . C4 C 0.3909(8) 0.2232(8) 1.1400(8) 0.043(3) Uani 1 d . . . H4 H 0.4250 0.2586 1.1989 0.051 Uiso 1 calc R . . C5 C 0.3299(8) 0.1368(8) 1.1540(8) 0.040(2) Uani 1 d . . . H5 H 0.3199 0.1151 1.2218 0.048 Uiso 1 calc R . . C6 C 0.2822(7) 0.0805(7) 1.0671(7) 0.030(2) Uani 1 d . . . C7 C 0.2148(8) -0.0139(7) 1.0878(8) 0.038(2) Uani 1 d . . . H7A H 0.1633 0.0084 1.1333 0.045 Uiso 1 calc R . . H7B H 0.1764 -0.0382 1.0216 0.045 Uiso 1 calc R . . N8 N 0.2774(7) -0.1043(6) 1.1379(6) 0.036(2) Uani 1 d . . . H8 H 0.311(9) -0.074(9) 1.206(9) 0.09(4) Uiso 1 d . . . C9 C 0.2034(9) -0.1863(8) 1.1712(8) 0.056(3) Uani 1 d . . . H9A H 0.1558 -0.1528 1.2139 0.084 Uiso 1 calc R . . H9B H 0.2430 -0.2415 1.2112 0.084 Uiso 1 calc R . . H9C H 0.1636 -0.2176 1.1098 0.084 Uiso 1 calc R . . C10 C 0.3518(9) -0.1491(9) 1.0709(9) 0.059(3) Uani 1 d . . . H10A H 0.3897 -0.2079 1.1067 0.088 Uiso 1 calc R . . H10B H 0.4010 -0.0943 1.0560 0.088 Uiso 1 calc R . . H10C H 0.3135 -0.1742 1.0060 0.088 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.02676(17) 0.03615(18) 0.02522(16) -0.0010(2) 0.00126(12) 0.0013(2) Cl2 0.0388(14) 0.083(2) 0.0316(13) 0.0034(13) -0.0015(11) -0.0038(14) Cl1 0.0286(13) 0.0646(17) 0.0383(13) -0.0071(12) 0.0043(11) 0.0077(12) S11 0.0274(13) 0.0552(15) 0.0305(13) -0.0082(11) 0.0005(11) 0.0014(11) C12 0.032(5) 0.038(5) 0.034(5) -0.002(5) 0.002(4) -0.009(6) N13 0.034(5) 0.071(7) 0.033(4) -0.012(4) 0.010(4) 0.007(4) N14 0.027(4) 0.051(5) 0.032(4) -0.011(4) 0.007(3) -0.004(4) N15 0.027(4) 0.031(4) 0.030(4) 0.002(4) 0.005(3) 0.000(4) C16 0.036(6) 0.027(6) 0.034(5) 0.005(4) 0.000(4) 0.006(5) C17 0.033(6) 0.029(5) 0.036(6) -0.005(4) -0.002(5) 0.000(5) N18 0.033(5) 0.035(5) 0.041(5) 0.001(4) -0.005(4) -0.005(4) C19 0.034(6) 0.058(7) 0.061(7) -0.001(6) 0.002(6) -0.003(6) C20 0.044(7) 0.051(7) 0.042(7) 0.009(6) -0.012(6) -0.013(6) C21 0.073(9) 0.043(6) 0.032(6) 0.001(5) -0.009(6) -0.005(6) C22 0.039(6) 0.033(6) 0.036(6) 0.003(4) -0.006(5) 0.004(5) C1 0.023(5) 0.031(5) 0.032(5) -0.008(4) 0.007(4) 0.007(4) C2 0.034(6) 0.046(6) 0.038(6) 0.003(5) 0.014(5) -0.001(5) C3 0.031(6) 0.043(6) 0.056(7) -0.006(5) 0.002(5) -0.014(5) C4 0.042(7) 0.050(7) 0.034(6) -0.011(5) -0.003(5) -0.004(5) C5 0.039(6) 0.039(6) 0.041(6) 0.002(5) 0.006(5) 0.005(5) C6 0.023(5) 0.039(5) 0.029(5) -0.009(4) 0.000(4) 0.002(4) C7 0.045(6) 0.033(6) 0.035(5) 0.008(4) 0.003(5) 0.001(5) N8 0.044(5) 0.029(4) 0.034(5) 0.000(4) 0.002(4) -0.006(4) C9 0.067(8) 0.036(6) 0.062(8) 0.009(6) -0.002(6) -0.022(6) C10 0.062(8) 0.060(8) 0.057(8) -0.012(6) 0.016(7) 0.014(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C1 2.029(8) . ? Au1 N15 2.106(7) . ? Au1 S11 2.248(3) . ? Au1 Cl1 2.320(2) . ? S11 C12 1.763(9) . ? C12 N14 1.281(11) . ? C12 N13 1.356(11) . ? N13 H13A 0.8700 . ? N13 H13B 0.8700 . ? N14 N15 1.383(9) . ? N15 C16 1.295(11) . ? C16 C17 1.408(12) . ? C16 H16 0.97(8) . ? C17 C22 1.368(12) . ? C17 N18 1.387(11) . ? N18 C20 1.352(12) . ? N18 C19 1.454(12) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 C21 1.354(15) . ? C20 H20 0.9400 . ? C21 C22 1.381(13) . ? C21 H21 0.9400 . ? C22 H22 0.9400 . ? C1 C6 1.387(12) . ? C1 C2 1.395(12) . ? C2 C3 1.383(13) . ? C2 H2 0.9400 . ? C3 C4 1.362(13) . ? C3 H3 0.9400 . ? C4 C5 1.364(13) . ? C4 H4 0.9400 . ? C5 C6 1.401(12) . ? C5 H5 0.9400 . ? C6 C7 1.512(12) . ? C7 N8 1.492(11) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? N8 C10 1.478(12) . ? N8 C9 1.501(12) . ? N8 H8 1.01(12) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 N15 172.6(3) . . ? C1 Au1 S11 88.7(2) . . ? N15 Au1 S11 84.1(2) . . ? C1 Au1 Cl1 91.5(2) . . ? N15 Au1 Cl1 95.7(2) . . ? S11 Au1 Cl1 178.81(10) . . ? C12 S11 Au1 95.4(3) . . ? N14 C12 N13 118.4(8) . . ? N14 C12 S11 126.8(7) . . ? N13 C12 S11 114.6(7) . . ? C12 N13 H13A 120.0 . . ? C12 N13 H13B 120.0 . . ? H13A N13 H13B 120.0 . . ? C12 N14 N15 114.6(7) . . ? C16 N15 N14 117.2(7) . . ? C16 N15 Au1 125.1(6) . . ? N14 N15 Au1 117.7(5) . . ? N15 C16 C17 128.4(9) . . ? N15 C16 H16 112(5) . . ? C17 C16 H16 117(5) . . ? C22 C17 N18 105.2(8) . . ? C22 C17 C16 135.7(10) . . ? N18 C17 C16 119.1(9) . . ? C20 N18 C17 109.5(9) . . ? C20 N18 C19 123.8(9) . . ? C17 N18 C19 126.6(8) . . ? N18 C19 H19A 109.5 . . ? N18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N18 C20 C21 108.6(10) . . ? N18 C20 H20 125.7 . . ? C21 C20 H20 125.7 . . ? C20 C21 C22 107.0(10) . . ? C20 C21 H21 126.5 . . ? C22 C21 H21 126.5 . . ? C17 C22 C21 109.7(10) . . ? C17 C22 H22 125.1 . . ? C21 C22 H22 125.1 . . ? C6 C1 C2 119.1(8) . . ? C6 C1 Au1 123.5(7) . . ? C2 C1 Au1 117.4(7) . . ? C3 C2 C1 120.8(9) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C4 C3 C2 119.0(9) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 121.8(10) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C4 C5 C6 119.8(9) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C1 C6 C5 119.4(9) . . ? C1 C6 C7 123.3(8) . . ? C5 C6 C7 117.2(9) . . ? N8 C7 C6 112.6(8) . . ? N8 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? N8 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? C10 N8 C7 112.9(8) . . ? C10 N8 C9 112.7(8) . . ? C7 N8 C9 108.6(8) . . ? C10 N8 H8 114(7) . . ? C7 N8 H8 104(7) . . ? C9 N8 H8 103(7) . . ? N8 C9 H9A 109.5 . . ? N8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N8 C10 H10A 109.5 . . ? N8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N13 H13A Cl2 0.87 2.43 3.224(8) 151.3 3_656 N8 H8 Cl2 1.01(12) 2.03(12) 2.987(8) 157(10) 3_657 N13 H13B Cl2 0.87 2.48 3.213(9) 142.3 . _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 26.97 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 1.418 _refine_diff_density_min -0.954 _refine_diff_density_rms 0.210 ##################### Structure 3 ################################## data_orgmepy _audit_creation_method SHELXL-97 _chemical_name_systematic 'Pyridoxalmethylthiosemicarbazone hydrochloride' _chemical_name_common 'H2pydoxmetsc x HCl' _chemical_formula_moiety 'H2pydoxmetsc x HCl' _chemical_formula_sum 'C10 H15 Cl N4 O2 S' _chemical_formula_weight 290.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P(-)1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7002(7) _cell_length_b 8.0500(9) _cell_length_c 12.461(1) _cell_angle_alpha 74.076(9) _cell_angle_beta 75.846(8) _cell_angle_gamma 64.490(8) _cell_volume 663.2(1) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.97 _cell_measurement_theta_max 25.16 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 304 _exptl_absorpt_coefficient_mu 4.046 _exptl_absorpt_correction_type 'Psi-scans' _exptl_absorpt_correction_T_min 0.6320 _exptl_absorpt_correction_T_max 0.9775 _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4 _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 2.5 _diffrn_reflns_number 3164 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 6.21 _diffrn_reflns_theta_max 64.95 _reflns_number_total 2253 _reflns_number_gt 1930 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement SET4 _computing_data_reduction HELENA _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP, SCHAKAL' _computing_publication_material SHELXL97 _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 w=1/[\s^2^(Fo^2^)+(0.0910P)^2^+1.1712P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'difmap, geom' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.009(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2253 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0661 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.2058 _refine_ls_wR_factor_gt 0.1927 _refine_ls_goodness_of_fit_ref 1.240 _refine_ls_restrained_S_all 1.240 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S11 S 0.18935(16) 0.65426(15) 0.13453(9) 0.0356(4) Uani 1 d . . . C12 C 0.0793(6) 0.8521(6) 0.1855(4) 0.0300(9) Uani 1 d . . . N14 N 0.0929(5) 1.0192(5) 0.1264(3) 0.0331(8) Uani 1 d . . . N15 N 0.2154(5) 1.0177(5) 0.0275(3) 0.0289(8) Uani 1 d . . . C16 C 0.2322(6) 1.1717(6) -0.0279(4) 0.0291(9) Uani 1 d . . . C17 C 0.3617(6) 1.1652(5) -0.1351(3) 0.0274(9) Uani 1 d . . . C18 C 0.4527(6) 0.9991(6) -0.1799(4) 0.0290(9) Uani 1 d . . . C19 C 0.5698(6) 0.9980(6) -0.2851(4) 0.0323(9) Uani 1 d . . . N20 N 0.5948(5) 1.1549(5) -0.3400(3) 0.0317(8) Uani 1 d . . . C21 C 0.5151(6) 1.3158(6) -0.2994(4) 0.0325(9) Uani 1 d . . . C22 C 0.3986(6) 1.3252(6) -0.1968(4) 0.0290(9) Uani 1 d . . . N13 N -0.0315(6) 0.8679(6) 0.2863(3) 0.0379(9) Uani 1 d . . . C27 C -0.0657(8) 0.7120(8) 0.3655(4) 0.0474(12) Uani 1 d . . . H27A H -0.0773 0.6314 0.3247 0.071 Uiso 1 calc R . . H27B H -0.1850 0.7592 0.4167 0.071 Uiso 1 calc R . . H27C H 0.0422 0.6409 0.4082 0.071 Uiso 1 calc R . . O23 O 0.4338(5) 0.8372(4) -0.1275(3) 0.0377(8) Uani 1 d . . . C24 C 0.6633(8) 0.8299(7) -0.3387(4) 0.0450(12) Uani 1 d . . . H24A H 0.5717 0.8264 -0.3785 0.068 Uiso 1 calc R . . H24B H 0.7020 0.7175 -0.2809 0.068 Uiso 1 calc R . . H24C H 0.7770 0.8363 -0.3914 0.068 Uiso 1 calc R . . C25 C 0.3157(7) 1.5064(6) -0.1545(4) 0.0354(10) Uani 1 d . . . O26 O 0.1154(5) 1.6096(4) -0.1700(3) 0.0402(8) Uani 1 d . . . Cl1 Cl 0.79864(19) 1.21924(18) -0.58116(10) 0.0514(5) Uani 1 d . . . H20 H 0.661(9) 1.146(9) -0.406(6) 0.056(17) Uiso 1 d . . . H21 H 0.549(7) 1.404(7) -0.343(4) 0.029(12) Uiso 1 d . . . H23 H 0.357(9) 0.874(8) -0.064(6) 0.056(17) Uiso 1 d . . . H25A H 0.385(7) 1.589(7) -0.198(4) 0.039(13) Uiso 1 d . . . H25B H 0.319(7) 1.487(7) -0.076(5) 0.041(14) Uiso 1 d . . . H26 H 0.115(9) 1.641(9) -0.244(6) 0.063(19) Uiso 1 d . . . H13 H -0.085(8) 1.000(9) 0.305(5) 0.052(15) Uiso 1 d . . . H16 H 0.173(8) 1.272(8) -0.003(5) 0.042(15) Uiso 1 d . . . H14 H 0.009(13) 1.143(13) 0.150(8) 0.11(3) Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S11 0.0410(7) 0.0286(6) 0.0374(7) -0.0064(4) -0.0067(5) -0.0131(5) C12 0.027(2) 0.034(2) 0.029(2) -0.0050(17) -0.0049(16) -0.0125(17) N14 0.0355(19) 0.0297(19) 0.0298(18) -0.0060(15) 0.0027(15) -0.0124(15) N15 0.0284(18) 0.0301(18) 0.0271(17) -0.0063(14) -0.0032(14) -0.0103(14) C16 0.032(2) 0.024(2) 0.032(2) -0.0072(17) -0.0051(17) -0.0098(17) C17 0.031(2) 0.024(2) 0.028(2) -0.0027(16) -0.0087(16) -0.0111(16) C18 0.031(2) 0.028(2) 0.031(2) -0.0050(16) -0.0069(17) -0.0131(17) C19 0.035(2) 0.031(2) 0.033(2) -0.0084(17) -0.0041(17) -0.0135(18) N20 0.0333(19) 0.032(2) 0.0297(19) -0.0070(15) -0.0014(15) -0.0141(15) C21 0.039(2) 0.027(2) 0.033(2) -0.0027(18) -0.0046(18) -0.0161(19) C22 0.032(2) 0.026(2) 0.030(2) -0.0065(16) -0.0054(17) -0.0113(17) N13 0.041(2) 0.039(2) 0.032(2) -0.0074(16) 0.0007(16) -0.0181(17) C27 0.058(3) 0.053(3) 0.036(3) -0.006(2) 0.003(2) -0.032(3) O23 0.0488(19) 0.0263(16) 0.0371(17) -0.0080(13) 0.0049(14) -0.0185(14) C24 0.056(3) 0.034(3) 0.041(3) -0.012(2) 0.007(2) -0.019(2) C25 0.043(2) 0.030(2) 0.037(3) -0.0063(19) -0.006(2) -0.016(2) O26 0.0387(18) 0.0300(17) 0.046(2) -0.0114(14) -0.0017(14) -0.0078(13) Cl1 0.0624(8) 0.0451(8) 0.0333(7) -0.0028(5) 0.0005(5) -0.0156(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S11 C12 1.669(5) . ? C12 N13 1.339(6) . ? C12 N14 1.379(6) . ? N14 N15 1.357(5) . ? N15 C16 1.287(6) . ? C16 C17 1.457(6) . ? C17 C22 1.412(6) . ? C17 C18 1.415(6) . ? C18 O23 1.340(5) . ? C18 C19 1.398(6) . ? C19 N20 1.331(6) . ? C19 C24 1.488(6) . ? N20 C21 1.354(6) . ? C21 C22 1.370(6) . ? C22 C25 1.506(6) . ? N13 C27 1.448(6) . ? C25 O26 1.435(6) . ? 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 N13 C12 N14 112.5(4) . . ? N13 C12 S11 124.6(3) . . ? N14 C12 S11 122.9(3) . . ? N15 N14 C12 118.1(4) . . ? C16 N15 N14 119.0(4) . . ? N15 C16 C17 117.3(4) . . ? C22 C17 C18 118.6(4) . . ? C22 C17 C16 120.6(4) . . ? C18 C17 C16 120.8(4) . . ? O23 C18 C19 116.1(4) . . ? O23 C18 C17 124.0(4) . . ? C19 C18 C17 120.0(4) . . ? N20 C19 C18 118.3(4) . . ? N20 C19 C24 119.1(4) . . ? C18 C19 C24 122.5(4) . . ? C19 N20 C21 123.9(4) . . ? N20 C21 C22 120.3(4) . . ? C21 C22 C17 118.9(4) . . ? C21 C22 C25 118.3(4) . . ? C17 C22 C25 122.8(4) . . ? C12 N13 C27 123.4(4) . . ? O26 C25 C22 110.9(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N20 H20 Cl1 0.86(7) 2.22(7) 3.050(4) 162(6) . O23 H23 N15 0.90(7) 1.69(7) 2.553(5) 159(6) . O23 H23 S11 0.90(7) 2.99(6) 3.622(3) 129(5) . O26 H26 Cl1 0.89(7) 2.24(7) 3.064(4) 153(6) 2_684 N13 H13 Cl1 1.04(6) 2.30(7) 3.280(4) 157(5) 1_456 N14 H14 O26 1.00(10) 1.86(10) 2.852(5) 169(8) 2_585 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 64.95 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.449 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.114 ################ Structure 4 ######################################### data_pydoxme _audit_creation_method SHELXL-97 _chemical_name_systematic [Au(Hdamp-C1)Cl(H2pydoxmetsc)C]Cl2*MeOH _chemical_name_common [Au(Hdamp-C1)Cl(H2pydoxmetsc)l]Cl2*MeOH _chemical_formula_moiety [Au(Hdamp-C1)Cl(H2pydoxmetsc)]Cl2*MeOH _chemical_formula_sum 'C20 H31 Au Cl3 N5 O3 S' _chemical_formula_weight 724.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.736(2) _cell_length_b 11.1800(10) _cell_length_c 13.085(2) _cell_angle_alpha 77.352(7) _cell_angle_beta 84.752(9) _cell_angle_gamma 82.996(7) _cell_volume 1376.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 5.742 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD4 Enraf Nonius' _diffrn_measurement_method 'image plate DIP' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3345 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 26.32 _reflns_number_total 3345 _reflns_number_gt 3314 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 (Enraf-Nonius)' _computing_cell_refinement 'DENZO' _computing_data_reduction 'DENZO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL, ZORTEP' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+9.7775P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3345 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1238 _refine_ls_wR_factor_gt 0.1234 _refine_ls_goodness_of_fit_ref 1.270 _refine_ls_restrained_S_all 1.270 _refine_ls_shift/su_max 0.009 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.16064(4) 0.47495(4) 0.23997(3) 0.02449(15) Uani 1 d . . . Cl1 Cl 0.1783(3) 0.4225(3) 0.0769(2) 0.0365(7) Uani 1 d . . . Cl2 Cl 0.8536(4) 0.2850(4) 0.3436(3) 0.0520(10) Uani 1 d . . . Cl3 Cl 0.3662(4) 0.7208(3) 0.1051(3) 0.0510(10) Uani 1 d . . . S11 S 0.1461(4) 0.5236(3) 0.4001(2) 0.0340(7) Uani 1 d . . . N15 N 0.0302(10) 0.6430(9) 0.1980(8) 0.028(2) Uani 1 d . . . N14 N -0.0050(11) 0.7135(9) 0.2715(8) 0.031(2) Uani 1 d . . . C1 C 0.2809(13) 0.3182(11) 0.2948(10) 0.031(3) Uani 1 d . . . C2 C 0.2230(13) 0.2075(12) 0.3080(11) 0.036(3) Uani 1 d . . . H2 H 0.1301 0.2088 0.2908 0.043 Uiso 1 calc R . . C3 C 0.2979(15) 0.0958(13) 0.3454(13) 0.043(3) Uani 1 d . . . H3 H 0.2567 0.0211 0.3545 0.052 Uiso 1 calc R . . C4 C 0.4351(15) 0.0939(12) 0.3699(11) 0.039(3) Uani 1 d . . . H4 H 0.4892 0.0176 0.3928 0.046 Uiso 1 calc R . . C5 C 0.4913(14) 0.2031(13) 0.3607(11) 0.037(3) Uani 1 d . . . H5 H 0.5823 0.2012 0.3822 0.045 Uiso 1 calc R . . C6 C 0.4183(12) 0.3166(11) 0.3207(9) 0.029(3) Uani 1 d . . . C7 C 0.4892(15) 0.4320(12) 0.3055(12) 0.040(3) Uani 1 d . . . H7A H 0.4218 0.5045 0.2821 0.047 Uiso 1 calc R . . H7B H 0.5215 0.4387 0.3734 0.047 Uiso 1 calc R . . N8 N 0.6106(12) 0.4330(12) 0.2261(10) 0.040(3) Uani 1 d . . . C9 C 0.6755(15) 0.5478(14) 0.2127(15) 0.051(4) Uani 1 d . . . H9A H 0.6957 0.5601 0.2815 0.077 Uiso 1 calc R . . H9B H 0.6122 0.6174 0.1791 0.077 Uiso 1 calc R . . H9C H 0.7620 0.5427 0.1685 0.077 Uiso 1 calc R . . C10 C 0.5764(17) 0.4118(15) 0.1239(11) 0.046(4) Uani 1 d . . . H10A H 0.5319 0.3355 0.1353 0.069 Uiso 1 calc R . . H10B H 0.6616 0.4048 0.0786 0.069 Uiso 1 calc R . . H10C H 0.5129 0.4811 0.0902 0.069 Uiso 1 calc R . . C12 C 0.0447(13) 0.6664(11) 0.3648(9) 0.029(3) Uani 1 d . . . N13 N 0.0179(14) 0.7327(11) 0.4390(9) 0.037(3) Uani 1 d . . . C27 C -0.0520(18) 0.8558(13) 0.4204(12) 0.047(4) Uani 1 d . . . H27A H -0.0602 0.8868 0.4854 0.071 Uiso 1 calc R . . H27B H -0.1447 0.8548 0.3973 0.071 Uiso 1 calc R . . H27C H 0.0014 0.9095 0.3659 0.071 Uiso 1 calc R . . C16 C -0.0099(13) 0.6898(10) 0.1037(9) 0.027(3) Uani 1 d . . . C17 C -0.0890(13) 0.8054(10) 0.0634(9) 0.028(3) Uani 1 d . . . C18 C -0.2035(13) 0.8564(11) 0.1188(10) 0.033(3) Uani 1 d . . . C19 C -0.2809(13) 0.9642(11) 0.0704(10) 0.031(3) Uani 1 d . . . N20 N -0.2434(12) 1.0175(11) -0.0285(9) 0.032(3) Uani 1 d . . . C21 C -0.1342(16) 0.9706(13) -0.0835(11) 0.036(3) Uani 1 d . . . C22 C -0.0557(13) 0.8656(11) -0.0428(10) 0.031(3) Uani 1 d . . . O23 O -0.2442(10) 0.8070(9) 0.2174(7) 0.033(2) Uani 1 d . . . C24 C -0.4059(17) 1.0214(14) 0.1280(14) 0.048(4) Uani 1 d . . . H24A H -0.4462 1.0963 0.0819 0.073 Uiso 1 calc R . . H24B H -0.3769 1.0423 0.1911 0.073 Uiso 1 calc R . . H24C H -0.4753 0.9624 0.1481 0.073 Uiso 1 calc R . . C25 C 0.0661(14) 0.8161(11) -0.1072(10) 0.031(3) Uani 1 d . . . H25A H 0.1488 0.7964 -0.0654 0.038 Uiso 1 calc R . . H25B H 0.0450 0.7393 -0.1256 0.038 Uiso 1 calc R . . O26 O 0.0939(12) 0.9031(9) -0.1989(9) 0.044(2) Uani 1 d . . . C30 C -0.400(3) 1.2406(19) -0.3867(17) 0.075(6) Uani 1 d . . . H30A H -0.4940 1.2175 -0.3639 0.113 Uiso 1 calc R . . H30B H -0.3694 1.2137 -0.4523 0.113 Uiso 1 calc R . . H30C H -0.4013 1.3303 -0.3983 0.113 Uiso 1 calc R . . O30 O -0.3065(19) 1.1821(14) -0.3068(13) 0.082(5) Uani 1 d . . . H30 H -0.3010 1.2299 -0.2663 0.124 Uiso 1 calc R . . H8 H 0.665(18) 0.392(15) 0.251(13) 0.040 Uiso 1 d . . . H13 H 0.039(15) 0.703(13) 0.489(12) 0.03(4) Uiso 1 d . . . H16 H 0.023(17) 0.640(13) 0.055(12) 0.040 Uiso 1 d . . . H20 H -0.27(2) 1.068(19) -0.063(17) 0.07(7) Uiso 1 d . . . H21 H -0.130(18) 0.998(15) -0.140(14) 0.040 Uiso 1 d . . . H23 H -0.176(17) 0.762(14) 0.248(13) 0.040 Uiso 1 d . . . H26 H 0.116(18) 0.875(14) -0.250(14) 0.040 Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.0208(2) 0.0290(2) 0.0243(2) -0.00652(15) -0.00236(17) -0.00300(16) Cl1 0.0389(17) 0.0414(17) 0.0326(16) -0.0143(13) -0.0047(15) -0.0041(14) Cl2 0.0328(17) 0.086(3) 0.0413(19) -0.0288(19) -0.0156(17) 0.0135(17) Cl3 0.055(2) 0.0411(19) 0.053(2) -0.0041(15) -0.013(2) 0.0048(17) S11 0.0375(17) 0.0388(17) 0.0251(15) -0.0072(12) -0.0039(15) -0.0001(14) N15 0.021(5) 0.038(6) 0.027(5) -0.011(4) -0.001(5) -0.003(4) N14 0.036(6) 0.030(5) 0.030(5) -0.011(4) -0.009(5) 0.003(5) C1 0.026(6) 0.036(7) 0.031(6) -0.010(5) -0.002(6) -0.002(5) C2 0.022(6) 0.045(8) 0.040(8) -0.006(6) -0.002(6) -0.005(6) C3 0.035(7) 0.038(8) 0.058(10) -0.015(7) 0.004(8) -0.006(6) C4 0.034(7) 0.030(7) 0.045(8) 0.001(6) -0.004(7) 0.009(6) C5 0.033(7) 0.048(8) 0.027(6) 0.000(5) 0.003(6) -0.005(6) C6 0.023(6) 0.034(6) 0.027(6) -0.001(5) -0.005(6) -0.001(5) C7 0.036(7) 0.037(7) 0.047(8) -0.004(6) -0.015(7) -0.011(6) N8 0.023(5) 0.048(7) 0.049(8) -0.007(5) -0.011(6) -0.001(5) C9 0.025(7) 0.055(9) 0.075(12) -0.011(8) -0.005(8) -0.015(7) C10 0.044(9) 0.060(9) 0.032(7) -0.004(6) -0.001(7) -0.013(7) C12 0.035(7) 0.037(7) 0.017(5) -0.008(5) -0.001(6) -0.005(5) N13 0.050(8) 0.034(6) 0.024(6) -0.004(5) -0.004(6) 0.005(5) C27 0.067(10) 0.035(7) 0.041(8) -0.013(6) 0.001(8) -0.004(7) C16 0.030(6) 0.027(6) 0.027(6) -0.013(5) -0.006(6) -0.001(5) C17 0.031(6) 0.030(6) 0.024(6) -0.010(5) -0.002(5) -0.006(5) C18 0.032(6) 0.031(6) 0.039(7) -0.015(5) -0.017(6) 0.005(5) C19 0.025(6) 0.030(6) 0.035(7) -0.003(5) -0.006(6) 0.000(5) N20 0.031(6) 0.026(6) 0.037(6) -0.003(5) -0.005(5) -0.004(5) C21 0.042(7) 0.036(7) 0.031(7) -0.008(5) -0.016(7) 0.000(6) C22 0.034(6) 0.031(6) 0.031(6) -0.011(5) -0.007(6) -0.007(5) O23 0.027(4) 0.044(5) 0.026(5) -0.004(4) -0.002(4) 0.002(4) C24 0.044(8) 0.040(8) 0.063(10) -0.018(7) -0.012(9) 0.010(7) C25 0.037(7) 0.028(6) 0.030(6) -0.007(5) -0.002(6) -0.004(5) O26 0.051(6) 0.043(6) 0.038(6) -0.011(4) 0.010(6) -0.008(5) C30 0.091(16) 0.079(13) 0.063(13) -0.020(10) -0.004(13) -0.030(12) O30 0.103(13) 0.066(9) 0.079(10) -0.025(8) 0.011(11) -0.007(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C1 2.015(12) . ? Au1 N15 2.130(10) . ? Au1 S11 2.266(3) . ? Au1 Cl1 2.320(3) . ? S11 C12 1.764(13) . ? N15 C16 1.305(15) . ? N15 N14 1.368(14) . ? N14 C12 1.329(15) . ? C1 C2 1.393(18) . ? C1 C6 1.406(15) . ? C2 C3 1.38(2) . ? C3 C4 1.399(19) . ? C4 C5 1.375(19) . ? C5 C6 1.396(18) . ? C6 C7 1.504(17) . ? C7 N8 1.50(2) . ? N8 C9 1.469(18) . ? N8 C10 1.481(17) . ? C12 N13 1.334(16) . ? N13 C27 1.439(18) . ? C16 C17 1.441(17) . ? C17 C18 1.403(18) . ? C17 C22 1.432(18) . ? C18 O23 1.332(17) . ? C18 C19 1.398(17) . ? C19 N20 1.339(19) . ? C19 C24 1.52(2) . ? N20 C21 1.35(2) . ? C21 C22 1.352(18) . ? C22 C25 1.511(19) . ? C25 O26 1.398(17) . ? C30 O30 1.45(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 N15 174.2(4) . . ? C1 Au1 S11 90.1(3) . . ? N15 Au1 S11 84.1(3) . . ? C1 Au1 Cl1 89.0(3) . . ? N15 Au1 Cl1 96.8(3) . . ? S11 Au1 Cl1 179.07(11) . . ? C12 S11 Au1 96.4(4) . . ? C16 N15 N14 116.6(10) . . ? C16 N15 Au1 124.6(8) . . ? N14 N15 Au1 118.5(7) . . ? C12 N14 N15 115.0(10) . . ? C2 C1 C6 119.5(11) . . ? C2 C1 Au1 117.5(8) . . ? C6 C1 Au1 123.0(9) . . ? C3 C2 C1 121.3(11) . . ? C2 C3 C4 119.3(12) . . ? C5 C4 C3 119.7(12) . . ? C4 C5 C6 121.8(11) . . ? C5 C6 C1 118.4(11) . . ? C5 C6 C7 119.1(10) . . ? C1 C6 C7 122.5(11) . . ? N8 C7 C6 112.0(12) . . ? C9 N8 C10 111.3(14) . . ? C9 N8 C7 110.1(12) . . ? C10 N8 C7 113.8(10) . . ? N14 C12 N13 117.9(11) . . ? N14 C12 S11 125.9(9) . . ? N13 C12 S11 116.2(8) . . ? C12 N13 C27 123.3(11) . . ? N15 C16 C17 130.1(10) . . ? C18 C17 C22 118.5(11) . . ? C18 C17 C16 123.9(12) . . ? C22 C17 C16 117.4(12) . . ? O23 C18 C19 116.8(12) . . ? O23 C18 C17 123.2(11) . . ? C19 C18 C17 120.0(13) . . ? N20 C19 C18 118.9(13) . . ? N20 C19 C24 119.8(12) . . ? C18 C19 C24 121.3(13) . . ? C19 N20 C21 122.4(13) . . ? N20 C21 C22 122.1(14) . . ? C21 C22 C17 118.1(13) . . ? C21 C22 C25 120.5(13) . . ? C17 C22 C25 121.4(11) . . ? O26 C25 C22 110.2(11) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O30 H30 Cl3 0.84 2.31 3.050(15) 147.2 2_575 N8 H8 Cl2 0.71(15) 2.34(15) 3.049(11) 170(15) . N13 H13 Cl2 0.71(14) 2.54(12) 3.170(11) 149(14) 2_666 O23 H23 N14 0.86(15) 1.72(16) 2.530(13) 157(17) . O23 H23 N15 0.86(15) 2.39(17) 3.074(14) 137(14) . O26 H26 Cl2 0.81(17) 2.35(15) 3.095(10) 153(17) 2_665 N20 H20 Cl3 0.7(2) 2.4(2) 3.012(13) 152(23) 2_575 _diffrn_measured_fraction_theta_max 0.599 _diffrn_reflns_theta_full 26.32 _diffrn_measured_fraction_theta_full 0.599 _refine_diff_density_max 1.382 _refine_diff_density_min -1.691 _refine_diff_density_rms 0.129 ########################## Structure 5 ############################# data_ptsc _audit_creation_method SHELXL-97 _chemical_name_systematic '[Au(Hdamp-C1)(Ptsc)]Cl2 * 1.5 CH3OH ' _chemical_name_common ? _chemical_formula_moiety '[Au(Hdamp-C1)(Ptsc)]Cl2 * 1.5 CH3OH ' _chemical_formula_sum 'C30.50 H36 Au Cl2 N4 O1.50 P S' _chemical_formula_weight 813.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.596(3) _cell_length_b 11.2571(6) _cell_length_c 18.363(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.803(14) _cell_angle_gamma 90.00 _cell_volume 3418.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.38 _cell_measurement_theta_max 13.67 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1612 _exptl_absorpt_coefficient_mu 4.598 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.89965 _exptl_absorpt_correction_T_max 0.98454 _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD 4 Enraf Nonius' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 2.8 _diffrn_reflns_number 8241 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7455 _reflns_number_gt 5558 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement SET4 _computing_data_reduction 'HELENA, PLATON' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL, ZORTEP' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+5.9998P] 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 'riding model, FMAP for H(8)' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7455 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0804 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.925273(13) 0.828706(18) 0.777073(11) 0.02045(7) Uani 1 d . . . P1 P 1.01460(9) 0.98241(13) 0.76283(8) 0.0222(3) Uani 1 d . . . S11 S 0.83952(9) 0.67814(14) 0.80671(9) 0.0308(3) Uani 1 d . . . Cl1 Cl 0.67398(11) 0.43774(14) 0.86653(9) 0.0404(4) Uani 1 d . . . Cl2 Cl 0.41623(13) 0.12531(16) 0.03186(11) 0.0555(5) Uani 1 d . . . C12 C 0.7724(4) 0.7720(5) 0.8501(3) 0.0261(13) Uani 1 d . . . N13 N 0.7140(3) 0.7178(5) 0.8819(3) 0.0338(12) Uani 1 d . . . H13A H 0.6792 0.7593 0.9041 0.041 Uiso 1 calc R . . H13B H 0.7103 0.6408 0.8806 0.041 Uiso 1 calc R . . N14 N 0.7770(3) 0.8872(4) 0.8526(3) 0.0265(11) Uani 1 d . . . N15 N 0.8391(3) 0.9390(4) 0.8193(3) 0.0228(10) Uani 1 d . . . C16 C 0.8370(4) 1.0534(5) 0.8197(3) 0.0245(12) Uani 1 d . . . H16 H 0.7940 1.0857 0.8434 0.029 Uiso 1 calc R . . C1 C 1.0102(4) 0.7073(5) 0.7494(3) 0.0261(13) Uani 1 d . . . C2 C 1.0541(4) 0.6549(6) 0.8085(4) 0.0364(15) Uani 1 d . . . H2 H 1.0420 0.6736 0.8563 0.044 Uiso 1 calc R . . C3 C 1.1158(4) 0.5748(6) 0.7977(4) 0.0472(18) Uani 1 d . . . H3 H 1.1454 0.5392 0.8378 0.057 Uiso 1 calc R . . C4 C 1.1331(4) 0.5482(6) 0.7266(4) 0.0449(18) Uani 1 d . . . H4 H 1.1756 0.4958 0.7187 0.054 Uiso 1 calc R . . C5 C 1.0891(4) 0.5973(5) 0.6687(4) 0.0331(14) Uani 1 d . . . H5 H 1.1010 0.5774 0.6211 0.040 Uiso 1 calc R . . C6 C 1.0267(3) 0.6765(5) 0.6787(3) 0.0256(11) Uani 1 d . . . C7 C 0.9825(3) 0.7289(5) 0.6121(3) 0.0260(12) Uani 1 d . . . H7A H 1.0217 0.7541 0.5782 0.031 Uiso 1 calc R . . H7B H 0.9529 0.7995 0.6262 0.031 Uiso 1 calc R . . N8 N 0.9238(4) 0.6425(5) 0.5739(3) 0.0317(13) Uani 1 d . . . H8 H 0.946(5) 0.595(8) 0.570(5) 0.06(3) Uiso 1 d . . . C9 C 0.8592(4) 0.6086(6) 0.6216(4) 0.0356(15) Uani 1 d . . . H9A H 0.8230 0.5517 0.5962 0.053 Uiso 1 calc R . . H9B H 0.8289 0.6787 0.6334 0.053 Uiso 1 calc R . . H9C H 0.8835 0.5731 0.6663 0.053 Uiso 1 calc R . . C10 C 0.8876(5) 0.6939(7) 0.5028(4) 0.0476(18) Uani 1 d . . . H10A H 0.8509 0.6365 0.4785 0.071 Uiso 1 calc R . . H10B H 0.9304 0.7122 0.4717 0.071 Uiso 1 calc R . . H10C H 0.8582 0.7659 0.5124 0.071 Uiso 1 calc R . . C20 C 0.9631(4) 1.1234(5) 0.7579(3) 0.0264(13) Uani 1 d . . . C21 C 0.8895(4) 1.1417(5) 0.7900(3) 0.0250(12) Uani 1 d . . . C22 C 0.8603(4) 1.2579(5) 0.7952(4) 0.0340(15) Uani 1 d . . . H22 H 0.8127 1.2714 0.8183 0.041 Uiso 1 calc R . . C23 C 0.9001(4) 1.3525(5) 0.7669(4) 0.0423(17) Uani 1 d . . . H23 H 0.8792 1.4298 0.7702 0.051 Uiso 1 calc R . . C24 C 0.9706(4) 1.3338(6) 0.7337(4) 0.0441(17) Uani 1 d . . . H24 H 0.9971 1.3982 0.7136 0.053 Uiso 1 calc R . . C25 C 1.0022(4) 1.2210(6) 0.7301(4) 0.0367(15) Uani 1 d . . . H25 H 1.0510 1.2096 0.7085 0.044 Uiso 1 calc R . . C30 C 1.0752(4) 0.9715(5) 0.6861(3) 0.0288(13) Uani 1 d . . . C31 C 1.0480(4) 1.0152(6) 0.6179(3) 0.0390(16) Uani 1 d . . . H31 H 0.9986 1.0562 0.6111 0.047 Uiso 1 calc R . . C32 C 1.0952(5) 0.9971(8) 0.5596(4) 0.054(2) Uani 1 d . . . H32 H 1.0782 1.0289 0.5135 0.065 Uiso 1 calc R . . C33 C 1.1657(5) 0.9341(8) 0.5680(4) 0.061(3) Uani 1 d . . . H33 H 1.1960 0.9210 0.5277 0.073 Uiso 1 calc R . . C34 C 1.1921(5) 0.8902(7) 0.6349(4) 0.051(2) Uani 1 d . . . H34 H 1.2410 0.8476 0.6407 0.061 Uiso 1 calc R . . C35 C 1.1477(4) 0.9077(6) 0.6945(4) 0.0365(15) Uani 1 d . . . H35 H 1.1661 0.8768 0.7404 0.044 Uiso 1 calc R . . C40 C 1.0829(3) 0.9936(5) 0.8449(3) 0.0268(12) Uani 1 d . . . C41 C 1.0625(4) 0.9438(6) 0.9094(3) 0.0380(15) Uani 1 d . . . H41 H 1.0157 0.8969 0.9097 0.046 Uiso 1 calc R . . C42 C 1.1108(5) 0.9623(7) 0.9737(4) 0.0477(19) Uani 1 d . . . H42 H 1.0966 0.9288 1.0178 0.057 Uiso 1 calc R . . C43 C 1.1800(5) 1.0305(8) 0.9726(4) 0.052(2) Uani 1 d . . . H43 H 1.2124 1.0441 1.0163 0.062 Uiso 1 calc R . . C44 C 1.2018(4) 1.0778(7) 0.9094(4) 0.0469(18) Uani 1 d . . . H44 H 1.2501 1.1213 0.9090 0.056 Uiso 1 calc R . . C45 C 1.1532(4) 1.0621(6) 0.8455(4) 0.0411(16) Uani 1 d . . . H45 H 1.1674 1.0977 0.8020 0.049 Uiso 1 calc R . . O50 O 0.7156(12) 0.2605(18) 0.187(2) 0.26(2) Uani 0.50 d P . . H50 H 0.7437 0.2496 0.2265 0.387 Uiso 0.50 calc PR . . C51 C 0.7483(19) 0.209(2) 0.1355(11) 0.130(13) Uani 0.50 d P . . H51A H 0.7984 0.2493 0.1269 0.196 Uiso 0.50 calc PR . . H51B H 0.7118 0.2118 0.0914 0.196 Uiso 0.50 calc PR . . H51C H 0.7598 0.1269 0.1486 0.196 Uiso 0.50 calc PR . . O60 O 0.1628(5) 0.6392(9) 0.0015(5) 0.126(7) Uani 0.50 d P . . H60 H 0.2109 0.6594 0.0019 0.190 Uiso 0.50 calc PR . . C61 C 0.1577(5) 0.5346(9) 0.0372(5) 0.076(6) Uani 0.50 d PR . . H61A H 0.2091 0.4934 0.0381 0.114 Uiso 0.50 calc PR . . H61B H 0.1157 0.4860 0.0123 0.114 Uiso 0.50 calc PR . . H61C H 0.1446 0.5495 0.0869 0.114 Uiso 0.50 calc PR . . O70 O 0.0583(5) 0.3174(9) -0.0492(5) 0.141(8) Uani 0.50 d PR . . H70 H 0.0149 0.3411 -0.0699 0.211 Uiso 0.50 calc PR . . C71 C 0.0547(5) 0.3221(9) 0.0219(5) 0.095(8) Uani 0.50 d PR . . H71A H 0.0808 0.3941 0.0408 0.142 Uiso 0.50 calc PR . . H71B H 0.0821 0.2536 0.0445 0.142 Uiso 0.50 calc PR . . H71C H -0.0014 0.3221 0.0330 0.142 Uiso 0.50 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.02276(10) 0.01571(10) 0.02373(10) 0.00009(10) 0.00708(7) 0.00086(11) P1 0.0218(7) 0.0213(7) 0.0239(7) 0.0002(6) 0.0039(6) -0.0020(6) S11 0.0369(8) 0.0160(7) 0.0428(8) -0.0020(7) 0.0217(7) -0.0011(7) Cl1 0.0537(10) 0.0263(8) 0.0415(9) 0.0010(7) 0.0051(8) -0.0119(7) Cl2 0.0755(14) 0.0340(9) 0.0637(12) 0.0155(8) 0.0464(11) 0.0134(9) C12 0.029(3) 0.022(3) 0.028(3) -0.001(2) 0.009(3) -0.002(3) N13 0.038(3) 0.020(2) 0.047(3) -0.004(2) 0.023(3) -0.004(2) N14 0.033(3) 0.017(2) 0.032(3) -0.003(2) 0.014(2) -0.001(2) N15 0.025(2) 0.018(2) 0.026(2) 0.0002(19) 0.008(2) -0.001(2) C16 0.027(3) 0.017(3) 0.030(3) -0.002(2) 0.009(2) 0.003(2) C1 0.026(3) 0.018(3) 0.035(3) 0.003(2) 0.007(3) 0.002(2) C2 0.033(3) 0.036(4) 0.041(3) 0.004(3) 0.004(3) 0.010(3) C3 0.042(4) 0.037(4) 0.061(5) 0.004(4) -0.002(4) 0.011(3) C4 0.031(4) 0.031(4) 0.073(5) -0.003(4) 0.008(3) 0.009(3) C5 0.028(3) 0.023(3) 0.049(4) -0.006(3) 0.012(3) 0.000(3) C6 0.022(3) 0.019(3) 0.037(3) -0.003(3) 0.010(2) 0.002(3) C7 0.030(3) 0.020(3) 0.030(3) -0.006(2) 0.013(2) -0.004(2) N8 0.039(3) 0.023(3) 0.035(3) -0.004(2) 0.013(2) 0.002(2) C9 0.032(3) 0.036(4) 0.040(4) -0.006(3) 0.010(3) -0.009(3) C10 0.056(5) 0.050(5) 0.035(4) 0.006(3) -0.001(3) -0.001(4) C20 0.028(3) 0.020(3) 0.030(3) -0.001(2) 0.000(3) -0.002(2) C21 0.025(3) 0.013(3) 0.036(3) 0.000(2) 0.001(2) 0.000(2) C22 0.035(4) 0.024(3) 0.044(4) 0.000(3) 0.007(3) 0.002(3) C23 0.046(4) 0.015(3) 0.065(5) 0.004(3) 0.003(4) 0.002(3) C24 0.043(4) 0.022(3) 0.067(5) 0.008(3) 0.007(3) -0.011(3) C25 0.035(4) 0.029(3) 0.046(4) 0.003(3) 0.005(3) -0.004(3) C30 0.028(3) 0.032(3) 0.027(3) -0.001(3) 0.008(2) -0.013(3) C31 0.040(4) 0.048(4) 0.029(3) -0.001(3) 0.007(3) -0.020(3) C32 0.071(5) 0.058(5) 0.034(4) -0.003(4) 0.015(4) -0.035(5) C33 0.070(6) 0.069(6) 0.050(5) -0.031(4) 0.042(4) -0.037(5) C34 0.042(4) 0.051(5) 0.063(5) -0.025(4) 0.029(4) -0.016(4) C35 0.036(4) 0.029(3) 0.047(4) -0.009(3) 0.018(3) -0.015(3) C40 0.025(3) 0.030(3) 0.025(3) -0.004(3) 0.001(2) 0.005(3) C41 0.033(3) 0.048(4) 0.033(3) 0.000(3) 0.002(3) -0.002(3) C42 0.055(5) 0.062(5) 0.026(3) 0.004(3) -0.002(3) 0.004(4) C43 0.045(4) 0.069(5) 0.039(4) -0.013(4) -0.011(3) 0.019(4) C44 0.038(4) 0.044(4) 0.056(5) -0.013(4) -0.011(3) -0.004(3) C45 0.036(4) 0.047(4) 0.040(4) -0.001(3) 0.005(3) -0.005(3) O50 0.086(13) 0.085(14) 0.63(6) -0.03(3) 0.18(2) 0.018(11) C51 0.21(3) 0.10(2) 0.062(13) 0.038(13) -0.089(18) -0.07(2) O60 0.196(19) 0.123(14) 0.053(8) 0.000(9) -0.038(10) 0.095(13) C61 0.033(9) 0.120(18) 0.075(13) -0.023(13) -0.003(8) -0.009(10) O70 0.19(2) 0.114(15) 0.127(15) 0.028(12) 0.056(14) 0.084(14) C71 0.080(14) 0.13(2) 0.070(13) -0.025(14) -0.030(11) 0.023(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C1 2.057(6) . ? Au1 N15 2.091(5) . ? Au1 S11 2.3074(15) . ? Au1 P1 2.3075(15) . ? P1 C20 1.801(6) . ? P1 C30 1.803(6) . ? P1 C40 1.812(6) . ? S11 C12 1.772(6) . ? C12 N14 1.300(7) . ? C12 N13 1.321(7) . ? N14 N15 1.372(6) . ? N15 C16 1.289(7) . ? C16 C21 1.458(8) . ? C1 C2 1.387(9) . ? C1 C6 1.393(8) . ? C2 C3 1.392(9) . ? C3 C4 1.392(10) . ? C4 C5 1.356(10) . ? C5 C6 1.390(8) . ? C6 C7 1.493(8) . ? C7 N8 1.507(8) . ? N8 C9 1.491(8) . ? N8 C10 1.506(9) . ? C20 C25 1.395(8) . ? C20 C21 1.415(8) . ? C21 C22 1.400(8) . ? C22 C23 1.378(9) . ? C23 C24 1.380(10) . ? C24 C25 1.377(9) . ? C30 C31 1.384(9) . ? C30 C35 1.399(9) . ? C31 C32 1.394(9) . ? C32 C33 1.366(12) . ? C33 C34 1.363(12) . ? C34 C35 1.383(9) . ? C40 C41 1.377(8) . ? C40 C45 1.398(9) . ? C41 C42 1.387(9) . ? C42 C43 1.384(11) . ? C43 C44 1.354(11) . ? C44 C45 1.379(9) . ? O50 C51 1.28(3) . ? O60 C61 1.3538 . ? O70 C71 1.3130 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 N15 171.8(2) . . ? C1 Au1 S11 91.09(16) . . ? N15 Au1 S11 83.93(13) . . ? C1 Au1 P1 90.59(17) . . ? N15 Au1 P1 93.58(13) . . ? S11 Au1 P1 172.89(5) . . ? C20 P1 C30 108.3(3) . . ? C20 P1 C40 104.0(3) . . ? C30 P1 C40 107.7(3) . . ? C20 P1 Au1 111.1(2) . . ? C30 P1 Au1 116.3(2) . . ? C40 P1 Au1 108.7(2) . . ? C12 S11 Au1 95.3(2) . . ? N14 C12 N13 119.2(6) . . ? N14 C12 S11 125.0(5) . . ? N13 C12 S11 115.8(4) . . ? C12 N14 N15 116.9(5) . . ? C16 N15 N14 113.6(5) . . ? C16 N15 Au1 128.0(4) . . ? N14 N15 Au1 118.4(3) . . ? N15 C16 C21 131.5(5) . . ? C2 C1 C6 119.4(5) . . ? C2 C1 Au1 114.5(4) . . ? C6 C1 Au1 126.0(4) . . ? C1 C2 C3 120.6(6) . . ? C2 C3 C4 119.0(7) . . ? C5 C4 C3 120.5(6) . . ? C4 C5 C6 121.1(6) . . ? C5 C6 C1 119.3(6) . . ? C5 C6 C7 117.8(5) . . ? C1 C6 C7 122.9(5) . . ? C6 C7 N8 112.3(5) . . ? C9 N8 C10 110.7(6) . . ? C9 N8 C7 111.1(5) . . ? C10 N8 C7 110.6(5) . . ? C25 C20 C21 118.8(6) . . ? C25 C20 P1 118.7(5) . . ? C21 C20 P1 122.0(4) . . ? C22 C21 C20 118.8(5) . . ? C22 C21 C16 112.9(5) . . ? C20 C21 C16 128.3(5) . . ? C23 C22 C21 121.1(6) . . ? C22 C23 C24 119.9(6) . . ? C25 C24 C23 120.2(6) . . ? C24 C25 C20 121.2(6) . . ? C31 C30 C35 119.6(6) . . ? C31 C30 P1 121.5(5) . . ? C35 C30 P1 118.6(5) . . ? C30 C31 C32 118.8(7) . . ? C33 C32 C31 121.3(7) . . ? C34 C33 C32 119.9(7) . . ? C33 C34 C35 120.6(8) . . ? C34 C35 C30 119.8(7) . . ? C41 C40 C45 118.9(6) . . ? C41 C40 P1 120.3(5) . . ? C45 C40 P1 120.5(5) . . ? C40 C41 C42 120.4(6) . . ? C43 C42 C41 119.4(7) . . ? C44 C43 C42 120.8(7) . . ? C43 C44 C45 120.1(7) . . ? C44 C45 C40 120.3(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N13 H13A Cl2 0.87 2.43 3.297(5) 178.9 3_666 N8 H8 Cl2 0.66(8) 2.61(9) 3.112(6) 135(9) 4_666 N13 H13B Cl1 0.87 2.37 3.230(5) 168.6 . _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 1.359 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.145 #################### Structure 6 ####################### data_acpyph _audit_creation_method SHELXL-97 _chemical_name_systematic [Au(Hdamp-C1)(2-AcetylpyridinPhenyltsc)]Cl2*2MeOH _chemical_name_common '[Au(Hdamp-C1)(apphtsc)]Cl2 x 2MeOH' _chemical_formula_moiety [Au(Hdamp-C1)(2- AcetylpyridinPhenyltsc)]Cl2 _chemical_formula_sum 'C25 H34 Au Cl2 N5 O2 S' _chemical_formula_weight 736.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1, -y-1/2, z-1/2' _cell_length_a 13.943(3) _cell_length_b 13.410(4) _cell_length_c 15.292(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.05(2) _cell_angle_gamma 90.00 _cell_volume 2815.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.6 _cell_measurement_theta_max 12.77 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 5.521 _exptl_absorpt_correction_type 'Psi scans' _exptl_absorpt_correction_T_min 0.6768 _exptl_absorpt_correction_T_max 0.9816 _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD4 Enraf Nonius' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 3.5 _diffrn_reflns_number 6845 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 29.65 _reflns_number_total 6099 _reflns_number_gt 4561 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 (Enraf-Nonius)' _computing_cell_refinement 'SET4, CELDIM' _computing_data_reduction HELENA/PLATON _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL, ZORTEP' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+24.4659P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6099 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1078 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.381048(18) 0.01824(2) 0.87647(2) 0.02328(9) Uani 1 d . . . Cl1 Cl 0.37899(15) -0.11727(17) 0.65810(16) 0.0395(5) Uani 1 d . . . Cl2 Cl -0.00886(14) 0.33837(17) 1.05587(16) 0.0392(5) Uani 1 d . . . S11 S 0.46365(13) 0.15415(15) 0.86000(15) 0.0284(4) Uani 1 d . . . N15 N 0.4965(4) -0.0591(5) 0.8822(4) 0.0242(14) Uani 1 d . . . N19 N 0.3373(4) -0.1236(5) 0.8956(5) 0.0284(15) Uani 1 d . . . C1 C 0.2665(5) 0.0980(6) 0.8731(6) 0.0282(18) Uani 1 d . . . C2 C 0.2407(6) 0.1158(7) 0.9626(6) 0.037(2) Uani 1 d . . . H2 H 0.2763 0.0866 1.0141 0.045 Uiso 1 calc R . . C3 C 0.1662(6) 0.1738(7) 0.9659(7) 0.044(2) Uani 1 d . . . H3 H 0.1445 0.1871 1.0196 0.052 Uiso 1 calc R . . C4 C 0.1196(6) 0.2160(7) 0.8841(7) 0.046(3) Uani 1 d . . . H4 H 0.0685 0.2610 0.8868 0.055 Uiso 1 calc R . . C5 C 0.1433(6) 0.1961(7) 0.7950(7) 0.042(2) Uani 1 d . . . H5 H 0.1067 0.2264 0.7445 0.050 Uiso 1 calc R . . C6 C 0.2166(5) 0.1354(6) 0.7867(6) 0.0287(18) Uani 1 d . . . C7 C 0.2369(5) 0.1128(6) 0.6875(6) 0.0320(19) Uani 1 d . . . H7A H 0.2460 0.1771 0.6596 0.038 Uiso 1 calc R . . H7B H 0.2991 0.0771 0.6935 0.038 Uiso 1 calc R . . N8 N 0.1650(4) 0.0559(6) 0.6255(5) 0.0315(16) Uani 1 d . . . H8 H 0.120(7) 0.093(7) 0.609(6) 0.040 Uiso 1 d . . . C9 C 0.1894(6) 0.0346(7) 0.5282(6) 0.037(2) Uani 1 d . . . H9A H 0.1363 -0.0025 0.4934 0.056 Uiso 1 calc R . . H9B H 0.2490 -0.0039 0.5335 0.056 Uiso 1 calc R . . H9C H 0.1976 0.0975 0.4989 0.056 Uiso 1 calc R . . C10 C 0.1429(7) -0.0395(6) 0.6730(7) 0.040(2) Uani 1 d . . . H10A H 0.0949 -0.0786 0.6339 0.060 Uiso 1 calc R . . H10B H 0.1175 -0.0224 0.7263 0.060 Uiso 1 calc R . . H10C H 0.2021 -0.0782 0.6891 0.060 Uiso 1 calc R . . C12 C 0.5650(5) 0.0860(6) 0.8631(5) 0.0259(17) Uani 1 d . . . N13 N 0.6333(4) 0.1441(5) 0.8514(5) 0.0327(17) Uani 1 d . . . H13 H 0.6242 0.2078 0.8571 0.039 Uiso 1 calc R . . N14 N 0.5754(4) -0.0109(5) 0.8758(4) 0.0236(13) Uani 1 d . . . C16 C 0.4915(5) -0.1544(6) 0.8863(5) 0.0240(17) Uani 1 d . . . C17 C 0.5672(6) -0.2210(7) 0.8808(7) 0.037(2) Uani 1 d . . . H17A H 0.6257 -0.1840 0.8753 0.056 Uiso 1 calc R . . H17B H 0.5491 -0.2635 0.8292 0.056 Uiso 1 calc R . . H17C H 0.5794 -0.2618 0.9339 0.056 Uiso 1 calc R . . C18 C 0.4027(5) -0.1934(6) 0.8936(6) 0.0293(18) Uani 1 d . . . C20 C 0.2557(6) -0.1527(7) 0.9045(6) 0.035(2) Uani 1 d . . . H20 H 0.2060 -0.1056 0.9059 0.043 Uiso 1 calc R . . C21 C 0.2352(6) -0.2529(7) 0.9126(6) 0.040(2) Uani 1 d . . . H21 H 0.1717 -0.2713 0.9188 0.048 Uiso 1 calc R . . C22 C 0.2997(6) -0.3227(7) 0.9121(6) 0.039(2) Uani 1 d . . . H22 H 0.2847 -0.3905 0.9178 0.046 Uiso 1 calc R . . C23 C 0.3851(6) -0.2937(7) 0.9034(6) 0.035(2) Uani 1 d . . . H23 H 0.4354 -0.3404 0.9037 0.042 Uiso 1 calc R . . C24 C 0.7186(5) 0.1143(6) 0.8310(6) 0.0290(18) Uani 1 d . . . C25 C 0.7356(6) 0.0229(8) 0.7954(7) 0.045(2) Uani 1 d . . . H25 H 0.6876 -0.0269 0.7903 0.054 Uiso 1 calc R . . C26 C 0.8178(7) 0.0048(9) 0.7686(8) 0.058(3) Uani 1 d . . . H26 H 0.8311 -0.0566 0.7437 0.070 Uiso 1 calc R . . C27 C 0.8820(6) 0.0803(10) 0.7792(8) 0.058(3) Uani 1 d . . . H27 H 0.9424 0.0713 0.7610 0.070 Uiso 1 calc R . . C28 C 0.8632(6) 0.1688(9) 0.8152(9) 0.061(3) Uani 1 d . . . H28 H 0.9109 0.2190 0.8193 0.073 Uiso 1 calc R . . C29 C 0.7831(6) 0.1886(8) 0.8444(7) 0.043(2) Uani 1 d . . . H29 H 0.7718 0.2491 0.8720 0.051 Uiso 1 calc R . . C30 C 0.5903(10) -0.0731(10) 0.5770(10) 0.079(4) Uani 1 d . . . H30A H 0.6131 -0.0330 0.5320 0.118 Uiso 1 calc R . . H30B H 0.5406 -0.1191 0.5487 0.118 Uiso 1 calc R . . H30C H 0.6444 -0.1105 0.6100 0.118 Uiso 1 calc R . . O31 O 0.5505(7) -0.0103(8) 0.6357(7) 0.089(3) Uani 1 d . . . H31 H 0.4995 -0.0353 0.6467 0.133 Uiso 1 calc R . . O41 O 0.9600(6) 0.1380(6) 0.1597(6) 0.070(2) Uani 1 d . . . H41 H 0.9534 0.1974 0.1446 0.105 Uiso 1 calc R . . C40 C 0.9645(7) 0.0758(9) 0.0811(9) 0.066(3) Uani 1 d . . . H40A H 0.9322 0.1101 0.0282 0.098 Uiso 1 calc R . . H40B H 0.9321 0.0127 0.0868 0.098 Uiso 1 calc R . . H40C H 1.0320 0.0638 0.0765 0.098 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01162(11) 0.02615(14) 0.03175(17) 0.00206(16) 0.00288(9) - 0.00027(13) Cl1 0.0301(10) 0.0414(13) 0.0461(14) -0.0017(10) 0.0038(9) 0.0042(9) Cl2 0.0191(8) 0.0429(13) 0.0543(15) 0.0008(11) 0.0029(9) -0.0064(8) S11 0.0172(8) 0.0266(10) 0.0413(13) 0.0038(9) 0.0051(8) -0.0004(7) N15 0.012(2) 0.030(4) 0.030(4) 0.005(3) 0.002(2) -0.003(2) N19 0.018(3) 0.031(4) 0.036(4) 0.005(3) 0.005(3) -0.002(3) C1 0.021(3) 0.024(4) 0.041(5) -0.005(4) 0.007(3) -0.003(3) C2 0.023(4) 0.049(6) 0.040(5) -0.003(4) 0.007(4) -0.008(4) C3 0.023(4) 0.048(6) 0.063(7) -0.020(5) 0.017(4) -0.005(4) C4 0.016(3) 0.044(6) 0.074(7) -0.025(5) 0.002(4) 0.002(4) C5 0.023(4) 0.039(5) 0.059(7) -0.012(5) -0.004(4) 0.009(4) C6 0.014(3) 0.027(4) 0.043(5) -0.002(4) -0.001(3) 0.003(3) C7 0.021(3) 0.030(4) 0.044(5) -0.003(4) 0.000(3) 0.001(3) N8 0.014(3) 0.035(4) 0.045(4) 0.001(3) 0.003(3) 0.008(3) C9 0.026(4) 0.048(6) 0.037(5) -0.006(4) 0.003(3) 0.007(4) C10 0.037(4) 0.034(6) 0.049(6) -0.001(4) 0.006(4) -0.006(4) C12 0.011(3) 0.039(5) 0.026(4) 0.006(4) -0.002(3) -0.002(3) N13 0.016(3) 0.032(4) 0.051(5) 0.004(3) 0.009(3) -0.001(3) N14 0.011(2) 0.029(3) 0.031(3) 0.004(3) 0.004(2) -0.005(2) C16 0.016(3) 0.023(4) 0.030(5) -0.002(3) -0.002(3) -0.001(3) C17 0.027(4) 0.034(5) 0.051(6) -0.005(4) 0.009(4) 0.002(3) C18 0.020(4) 0.030(4) 0.037(5) 0.000(4) 0.003(3) -0.004(3) C20 0.022(4) 0.042(5) 0.041(5) 0.001(4) 0.002(4) -0.006(3) C21 0.023(4) 0.048(6) 0.049(6) 0.003(5) 0.006(4) -0.014(4) C22 0.036(4) 0.035(5) 0.044(6) 0.003(4) 0.002(4) -0.016(4) C23 0.024(4) 0.036(5) 0.045(6) 0.006(4) 0.008(4) -0.002(3) C24 0.018(3) 0.037(5) 0.033(5) 0.004(4) 0.009(3) -0.002(3) C25 0.020(3) 0.054(6) 0.062(6) 0.002(5) 0.014(4) -0.007(4) C26 0.036(5) 0.067(8) 0.080(8) 0.013(6) 0.032(5) 0.010(5) C27 0.020(4) 0.090(9) 0.068(8) 0.024(7) 0.016(5) 0.003(5) C28 0.017(4) 0.072(8) 0.096(9) 0.025(7) 0.013(5) -0.005(4) C29 0.017(4) 0.053(6) 0.056(6) 0.009(5) 0.005(4) -0.010(4) C30 0.066(8) 0.074(9) 0.101(11) -0.024(8) 0.025(8) -0.028(7) O31 0.073(6) 0.092(7) 0.104(8) -0.021(6) 0.023(6) -0.040(5) O41 0.045(4) 0.067(6) 0.100(7) 0.031(5) 0.018(4) 0.004(4) C40 0.035(5) 0.058(8) 0.107(11) 0.002(7) 0.021(6) 0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 N15 1.904(6) . ? Au1 C1 1.915(8) . ? Au1 N19 2.035(7) . ? Au1 S11 2.194(2) . ? S11 C12 1.677(8) . ? N15 C16 1.282(10) . ? N15 N14 1.295(8) . ? N19 C20 1.233(10) . ? N19 C18 1.310(10) . ? C1 C6 1.470(12) . ? C1 C2 1.494(12) . ? C2 C3 1.305(12) . ? C3 C4 1.422(14) . ? C4 C5 1.481(14) . ? C5 C6 1.330(11) . ? C6 C7 1.620(12) . ? C7 N8 1.468(10) . ? N8 C10 1.530(11) . ? N8 C9 1.609(11) . ? C12 N13 1.267(9) . ? C12 N14 1.318(11) . ? N13 C24 1.343(9) . ? C16 C18 1.366(10) . ? C16 C17 1.397(11) . ? C18 C23 1.380(12) . ? C20 C21 1.383(13) . ? C21 C22 1.299(13) . ? C22 C23 1.281(11) . ? C24 C29 1.333(12) . ? C24 C25 1.379(13) . ? C25 C26 1.305(12) . ? C26 C27 1.342(16) . ? C27 C28 1.353(17) . ? C28 C29 1.301(13) . ? C30 O31 1.413(15) . ? O41 C40 1.474(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N15 Au1 C1 178.6(3) . . ? N15 Au1 N19 75.9(3) . . ? C1 Au1 N19 104.9(3) . . ? N15 Au1 S11 90.07(19) . . ? C1 Au1 S11 89.1(2) . . ? N19 Au1 S11 165.91(18) . . ? C12 S11 Au1 90.0(3) . . ? C16 N15 N14 123.7(6) . . ? C16 N15 Au1 119.5(5) . . ? N14 N15 Au1 116.6(5) . . ? C20 N19 C18 115.9(8) . . ? C20 N19 Au1 128.1(6) . . ? C18 N19 Au1 115.9(5) . . ? C6 C1 C2 128.1(7) . . ? C6 C1 Au1 118.5(6) . . ? C2 C1 Au1 113.4(6) . . ? C3 C2 C1 116.8(9) . . ? C2 C3 C4 116.6(9) . . ? C3 C4 C5 126.6(8) . . ? C6 C5 C4 119.8(9) . . ? C5 C6 C1 112.0(8) . . ? C5 C6 C7 117.8(8) . . ? C1 C6 C7 130.2(6) . . ? N8 C7 C6 119.4(7) . . ? C7 N8 C10 107.4(7) . . ? C7 N8 C9 117.3(6) . . ? C10 N8 C9 112.6(7) . . ? N13 C12 N14 124.1(7) . . ? N13 C12 S11 108.1(6) . . ? N14 C12 S11 127.8(6) . . ? C12 N13 C24 124.6(8) . . ? N15 N14 C12 115.4(6) . . ? N15 C16 C18 116.3(7) . . ? N15 C16 C17 125.9(7) . . ? C18 C16 C17 117.8(8) . . ? N19 C18 C16 111.9(7) . . ? N19 C18 C23 123.7(7) . . ? C16 C18 C23 124.3(7) . . ? N19 C20 C21 121.7(9) . . ? C22 C21 C20 123.0(8) . . ? C23 C22 C21 116.0(9) . . ? C22 C23 C18 119.6(8) . . ? C29 C24 N13 110.1(8) . . ? C29 C24 C25 124.6(8) . . ? N13 C24 C25 125.2(7) . . ? C26 C25 C24 120.7(9) . . ? C25 C26 C27 115.2(11) . . ? C26 C27 C28 122.6(9) . . ? C29 C28 C27 123.9(10) . . ? C28 C29 C24 113.0(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N8 H8 Cl2 0.81(9) 2.05(10) 2.849(7) 168(9) 4_665 N13 H13 Cl1 0.87 2.36 3.206(8) 165.5 2_556 O31 H31 Cl1 0.83 2.04 2.860(9) 169.3 . O41 H41 Cl2 0.83 2.44 3.189(8) 151.1 1_654 _diffrn_measured_fraction_theta_max 0.737 _diffrn_reflns_theta_full 29.65 _diffrn_measured_fraction_theta_full 0.737 _refine_diff_density_max 1.614 _refine_diff_density_min -0.909 _refine_diff_density_rms 0.188