# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Helgard G. Raubenheimer' 'Stephanie Cronje' 'Catharine Esterhuysen' 'William Gabrielli' 'Stefan D. Nogai' 'Oliver B. Schuster' 'Christoph Strasser' _publ_contact_author_name 'Helgard G. Raubenheimer' _publ_contact_author_address ; Chemistry and Polymer Science University of Stellenbosch Private Bag X1 Matieland 7602 SOUTH AFRICA ; _publ_contact_author_email HGR@SUN.AC.ZA _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Preparation of tris(azole)phosphine gold(I) complexes: Digold(I) coordination and variation in solid state intermolecular interactions ; data_Compound1d _database_code_depnum_ccdc_archive 'CCDC 659052' _audit_creation_method SHELXL-97 _chemical_name_systematic tris(4,5-dimethylthiazol-2-yl)phosphane _chemical_name_common tris(4,5-dimethylthiazol-2-yl)phosphine _chemical_melting_point 372 _chemical_formula_moiety 'C15 H18 N3 P S3' _chemical_formula_sum 'C15 H18 N3 P S3' _chemical_formula_weight 367.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_int_tables_number 14 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 12.7604(12) _cell_length_b 9.7885(9) _cell_length_c 13.9233(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.800(2) _cell_angle_gamma 90.00 _cell_volume 1702.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6187 _cell_measurement_theta_min 2.427 _cell_measurement_theta_max 28.239 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.528 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.858 _exptl_absorpt_correction_T_max 0.987 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _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_% ? _diffrn_reflns_number 9941 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 26.73 _reflns_number_total 3606 _reflns_number_gt 3327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material X-Seed _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^)+(0.0410P)^2^+0.7989P] 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 3606 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0783 _refine_ls_wR_factor_gt 0.0766 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 P1 P 0.15467(3) 1.15790(4) 0.29097(3) 0.01483(10) Uani 1 1 d . . . S1 S 0.14348(3) 0.90395(4) 0.42896(3) 0.01766(10) Uani 1 1 d . . . N1 N 0.14514(10) 1.15323(13) 0.48552(9) 0.0167(3) Uani 1 1 d . . . C11 C 0.14615(11) 1.07829(15) 0.40773(11) 0.0157(3) Uani 1 1 d . . . C12 C 0.14244(12) 0.93480(16) 0.55052(11) 0.0170(3) Uani 1 1 d . . . C13 C 0.14353(12) 1.07285(16) 0.56704(11) 0.0167(3) Uani 1 1 d . . . C14 C 0.14494(13) 1.14217(17) 0.66342(11) 0.0219(3) Uani 1 1 d . . . H14A H 0.2098 1.1980 0.6812 0.033 Uiso 1 1 calc R . . H14B H 0.1443 1.0731 0.7142 0.033 Uiso 1 1 calc R . . H14C H 0.0817 1.2007 0.6578 0.033 Uiso 1 1 calc R . . C15 C 0.14178(14) 0.81887(17) 0.62075(12) 0.0229(3) Uani 1 1 d . . . H15A H 0.1401 0.8553 0.6860 0.034 Uiso 1 1 calc R . . H15B H 0.2065 0.7636 0.6242 0.034 Uiso 1 1 calc R . . H15C H 0.0784 0.7620 0.5980 0.034 Uiso 1 1 calc R . . S2 S 0.37992(3) 1.02742(4) 0.36983(3) 0.01739(10) Uani 1 1 d . . . N2 N 0.31113(10) 1.08831(13) 0.18932(9) 0.0168(3) Uani 1 1 d . . . C21 C 0.28131(12) 1.08411(14) 0.27359(10) 0.0150(3) Uani 1 1 d . . . C22 C 0.46669(12) 1.00831(15) 0.29086(11) 0.0175(3) Uani 1 1 d . . . C23 C 0.41524(12) 1.04300(15) 0.19820(11) 0.0170(3) Uani 1 1 d . . . C24 C 0.46079(13) 1.02896(17) 0.10777(12) 0.0223(3) Uani 1 1 d . . . H24A H 0.5390 1.0240 0.1263 0.033 Uiso 1 1 calc R . . H24B H 0.4400 1.1082 0.0651 0.033 Uiso 1 1 calc R . . H24C H 0.4332 0.9454 0.0727 0.033 Uiso 1 1 calc R . . C25 C 0.57748(12) 0.95225(16) 0.32437(12) 0.0219(3) Uani 1 1 d . . . H25A H 0.5774 0.8542 0.3100 0.033 Uiso 1 1 calc R . . H25B H 0.6008 0.9667 0.3952 0.033 Uiso 1 1 calc R . . H25C H 0.6267 0.9992 0.2898 0.033 Uiso 1 1 calc R . . S3 S 0.08679(3) 0.89892(4) 0.15489(3) 0.01700(10) Uani 1 1 d . . . N3 N -0.03695(10) 1.09879(13) 0.17288(9) 0.0168(3) Uani 1 1 d . . . C31 C 0.06083(12) 1.05420(15) 0.20429(10) 0.0148(3) Uani 1 1 d . . . C32 C -0.04270(12) 0.89438(15) 0.08791(10) 0.0158(3) Uani 1 1 d . . . C33 C -0.09618(12) 1.00872(16) 0.10730(11) 0.0170(3) Uani 1 1 d . . . C34 C -0.21012(13) 1.04318(18) 0.06334(12) 0.0251(4) Uani 1 1 d . . . H34A H -0.2546 1.0271 0.1119 0.038 Uiso 1 1 calc R . . H34B H -0.2353 0.9855 0.0057 0.038 Uiso 1 1 calc R . . H34C H -0.2151 1.1395 0.0437 0.038 Uiso 1 1 calc R . . C35 C -0.08259(13) 0.78006(16) 0.01859(11) 0.0208(3) Uani 1 1 d . . . H35A H -0.1042 0.7032 0.0552 0.031 Uiso 1 1 calc R . . H35B H -0.0255 0.7506 -0.0143 0.031 Uiso 1 1 calc R . . H35C H -0.1442 0.8115 -0.0305 0.031 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 P1 0.0169(2) 0.01348(19) 0.01398(18) 0.00016(13) 0.00276(14) 0.00033(14) S1 0.0234(2) 0.01451(18) 0.01609(19) -0.00035(13) 0.00634(14) -0.00010(13) N1 0.0159(6) 0.0184(6) 0.0154(6) -0.0012(5) 0.0023(5) -0.0009(5) C11 0.0144(7) 0.0155(7) 0.0171(7) 0.0005(6) 0.0032(5) -0.0001(5) C12 0.0141(7) 0.0223(8) 0.0152(7) 0.0002(6) 0.0043(5) 0.0005(6) C13 0.0134(7) 0.0205(7) 0.0160(7) 0.0000(6) 0.0025(5) -0.0001(6) C14 0.0246(8) 0.0245(8) 0.0169(7) -0.0027(6) 0.0047(6) -0.0011(6) C15 0.0294(9) 0.0217(8) 0.0194(7) 0.0036(6) 0.0092(6) 0.0023(7) S2 0.01704(19) 0.0196(2) 0.01492(18) 0.00255(13) 0.00178(14) 0.00019(13) N2 0.0182(6) 0.0160(6) 0.0163(6) -0.0002(5) 0.0038(5) -0.0018(5) C21 0.0155(7) 0.0134(6) 0.0153(7) 0.0006(5) 0.0013(5) -0.0015(5) C22 0.0169(7) 0.0143(7) 0.0217(8) -0.0010(6) 0.0048(6) -0.0024(5) C23 0.0169(7) 0.0150(7) 0.0195(7) -0.0010(6) 0.0046(6) -0.0021(6) C24 0.0201(8) 0.0271(8) 0.0206(8) -0.0006(6) 0.0064(6) 0.0014(6) C25 0.0174(8) 0.0215(8) 0.0255(8) 0.0001(6) 0.0015(6) 0.0010(6) S3 0.01617(19) 0.01529(19) 0.01802(19) -0.00190(13) -0.00007(14) 0.00267(13) N3 0.0178(6) 0.0191(6) 0.0136(6) 0.0006(5) 0.0037(5) 0.0023(5) C31 0.0176(7) 0.0139(7) 0.0133(7) 0.0011(5) 0.0041(5) 0.0010(5) C32 0.0158(7) 0.0187(7) 0.0121(7) 0.0017(5) 0.0014(5) -0.0011(5) C33 0.0168(7) 0.0207(7) 0.0140(7) 0.0021(6) 0.0040(5) 0.0007(6) C34 0.0183(8) 0.0319(9) 0.0235(8) -0.0036(7) 0.0003(6) 0.0046(7) C35 0.0229(8) 0.0198(8) 0.0179(7) -0.0013(6) 0.0002(6) -0.0015(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 P1 C11 1.8260(15) . ? S1 C11 1.7334(15) . ? S1 C12 1.7220(15) . ? N1 C11 1.3104(19) . ? N1 C13 1.3847(19) . ? C12 C13 1.370(2) . ? C13 C14 1.500(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C12 C15 1.499(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? P1 C21 1.8309(16) . ? S2 C21 1.7312(15) . ? S2 C22 1.7227(16) . ? N2 C21 1.3059(19) . ? N2 C23 1.3820(19) . ? C22 C23 1.365(2) . ? C23 C24 1.497(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C22 C25 1.499(2) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? P1 C31 1.8247(15) . ? S3 C31 1.7281(15) . ? S3 C32 1.7239(15) . ? N3 C31 1.3097(19) . ? N3 C33 1.3785(19) . ? C32 C33 1.366(2) . ? C33 C34 1.496(2) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C32 C35 1.497(2) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 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 C11 P1 C21 99.45(7) . . ? C11 P1 C31 101.59(7) . . ? C21 P1 C31 99.83(7) . . ? P1 C11 S1 125.37(9) . . ? P1 C11 N1 120.62(11) . . ? S1 C11 N1 113.98(11) . . ? N1 C13 C14 118.47(13) . . ? C11 S1 C12 89.96(7) . . ? C11 N1 C13 111.33(13) . . ? C12 C13 N1 115.09(13) . . ? C12 C13 C14 126.43(14) . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C12 S1 109.64(11) . . ? C13 C12 C15 129.65(14) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C15 C12 S1 120.71(12) . . ? P1 C21 S2 123.06(8) . . ? P1 C21 N2 122.24(11) . . ? S2 C21 N2 113.97(11) . . ? N2 C23 C24 119.06(13) . . ? C21 S2 C22 90.06(7) . . ? C21 N2 C23 111.16(13) . . ? C22 C23 N2 115.59(14) . . ? C22 C23 C24 125.28(14) . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C22 S2 109.18(11) . . ? C23 C22 C25 128.73(14) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C25 C22 S2 121.96(12) . . ? P1 C31 S3 126.82(9) . . ? P1 C31 N3 119.14(11) . . ? S3 C31 N3 114.03(11) . . ? N3 C33 C34 118.82(13) . . ? C31 S3 C32 89.85(7) . . ? C31 N3 C33 111.34(13) . . ? C32 C33 N3 115.25(13) . . ? C32 C33 C34 125.93(14) . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C32 S3 109.52(11) . . ? C33 C32 C35 128.46(14) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C35 C32 S3 121.99(11) . . ? 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 S3 C32 C33 N3 0.36(17) . . . . ? S3 C32 C33 C34 179.68(13) . . . . ? N1 C13 C12 S1 0.01(17) . . . . ? N1 C13 C12 C15 179.29(15) . . . . ? N2 C23 C22 S2 2.14(17) . . . . ? N2 C23 C22 C25 177.98(14) . . . . ? C11 P1 C21 S2 -24.99(11) . . . . ? C11 P1 C21 N2 165.30(12) . . . . ? C11 P1 C31 S3 -83.39(11) . . . . ? C11 P1 C31 N3 97.76(12) . . . . ? C11 S1 C12 C13 0.35(12) . . . . ? C11 S1 C12 C15 -179.01(13) . . . . ? C11 N1 C13 C12 -0.50(18) . . . . ? C11 N1 C13 C14 178.52(13) . . . . ? C12 S1 C11 P1 177.12(10) . . . . ? C12 S1 C11 N1 -0.66(12) . . . . ? C13 N1 C11 P1 -177.12(10) . . . . ? C13 N1 C11 S1 0.77(16) . . . . ? C14 C13 C12 S1 -178.92(13) . . . . ? C14 C13 C12 C15 0.4(3) . . . . ? C21 P1 C11 S1 -59.17(11) . . . . ? C21 P1 C11 N1 118.47(12) . . . . ? C21 P1 C31 S3 18.48(11) . . . . ? C21 P1 C31 N3 -160.37(12) . . . . ? C21 S2 C22 C23 -1.17(12) . . . . ? C21 S2 C22 C25 -177.34(13) . . . . ? C21 N2 C23 C22 -2.20(18) . . . . ? C21 N2 C23 C24 174.84(13) . . . . ? C22 S2 C21 P1 -170.50(10) . . . . ? C22 S2 C21 N2 -0.01(12) . . . . ? C23 N2 C21 P1 171.77(10) . . . . ? C23 N2 C21 S2 1.19(16) . . . . ? C24 C23 C22 S2 -174.68(12) . . . . ? C24 C23 C22 C25 1.2(3) . . . . ? C31 P1 C11 S1 42.99(11) . . . . ? C31 P1 C11 N1 -139.36(12) . . . . ? C31 P1 C21 S2 -128.61(9) . . . . ? C31 P1 C21 N2 61.68(13) . . . . ? C31 S3 C32 C33 -0.16(12) . . . . ? C31 S3 C32 C35 178.30(13) . . . . ? C31 N3 C33 C32 -0.42(19) . . . . ? C31 N3 C33 C34 -179.80(14) . . . . ? C32 S3 C31 P1 -178.98(10) . . . . ? C32 S3 C31 N3 -0.08(12) . . . . ? C33 N3 C31 S3 0.29(16) . . . . ? C33 N3 C31 P1 179.28(10) . . . . ? C35 C32 C33 N3 -177.97(14) . . . . ? C35 C32 C33 C34 1.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.505 _refine_diff_density_min -0.194 _refine_diff_density_rms 0.063 #Compound 1b ends #===END ######## ## 2a ## ######## data_Compound2a _database_code_depnum_ccdc_archive 'CCDC 659053' _audit_creation_method SHELXL-97 _chemical_name_systematic chloridotris(1-methylimidazol-2-yl)phosphanegold(I) _chemical_name_common 'tris(1-methylimidazol-2-yl)phosphinegold(I) chloride' _chemical_melting_point 428 _chemical_formula_moiety 'C12 H15 Au Cl N6 P' _chemical_formula_sum 'C12 H15 Au Cl N6 P' _chemical_formula_weight 506.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.765(2) _cell_length_b 18.867(5) _cell_length_c 11.069(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.540(4) _cell_angle_gamma 90.00 _cell_volume 1621.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4102 _cell_measurement_theta_min 3.191 _cell_measurement_theta_max 26.384 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.075 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 9.337 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.335 _exptl_absorpt_correction_T_max 0.522 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area detector' _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_% ? _diffrn_reflns_number 8961 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 26.44 _reflns_number_total 3253 _reflns_number_gt 2740 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material X-Seed _refine_special_details ;Analysis of the thermal displacement ellipsoids after initial refinement suggested that imidazole ring 3 was split. Electron density for a ring in a different orientation (3B) was found and the two parts 3A and 3B constrained with a SAME instruction. Only 3A was refined anisotropically. 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^)+(0.0343P)^2^+3.5260P] 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 3253 _refine_ls_number_parameters 215 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0699 _refine_ls_wR_factor_gt 0.0657 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.99445(3) 0.205291(11) 0.135607(19) 0.02159(9) Uani 1 1 d . . . Cl1 Cl 1.1137(2) 0.09845(8) 0.09033(15) 0.0379(4) Uani 1 1 d . . . P1 P 0.87199(17) 0.30836(7) 0.17833(13) 0.0180(3) Uani 1 1 d . A . N11 N 0.5923(6) 0.2298(3) 0.2411(4) 0.0226(10) Uani 1 1 d . . . C11 C 0.6549(7) 0.2952(3) 0.2294(4) 0.0169(11) Uani 1 1 d . . . N12 N 0.5450(5) 0.3453(2) 0.2710(4) 0.0228(10) Uani 1 1 d . . . C12 C 0.4326(7) 0.2399(3) 0.2919(5) 0.0252(13) Uani 1 1 d . . . H12 H 0.3545 0.2030 0.3115 0.030 Uiso 1 1 calc R . . C13 C 0.4030(7) 0.3097(3) 0.3097(5) 0.0296(14) Uani 1 1 d . . . H13 H 0.3021 0.3301 0.3429 0.035 Uiso 1 1 calc R . . C14 C 0.5672(8) 0.4225(3) 0.2739(6) 0.0302(13) Uani 1 1 d . . . H14A H 0.6789 0.4341 0.3108 0.045 Uiso 1 1 calc R . . H14B H 0.4749 0.4439 0.3214 0.045 Uiso 1 1 calc R . . H14C H 0.5626 0.4412 0.1913 0.045 Uiso 1 1 calc R . . N21 N 1.0341(6) 0.4243(2) 0.2858(5) 0.0278(11) Uani 1 1 d . . . C21 C 0.9716(7) 0.3595(3) 0.2979(5) 0.0210(12) Uani 1 1 d . . . N22 N 0.9907(6) 0.3344(2) 0.4117(4) 0.0241(10) Uani 1 1 d . . . C22 C 1.0945(7) 0.4420(3) 0.3991(6) 0.0356(16) Uani 1 1 d . . . H22 H 1.1474 0.4858 0.4199 0.043 Uiso 1 1 calc R . . C23 C 1.0672(7) 0.3874(4) 0.4768(6) 0.0344(15) Uani 1 1 d . . . H23 H 1.0958 0.3864 0.5604 0.041 Uiso 1 1 calc R . . C24 C 0.9334(8) 0.2661(3) 0.4583(5) 0.0296(13) Uani 1 1 d . . . H24A H 0.8076 0.2632 0.4521 0.044 Uiso 1 1 calc R . . H24B H 0.9690 0.2615 0.5431 0.044 Uiso 1 1 calc R . . H24C H 0.9851 0.2279 0.4109 0.044 Uiso 1 1 calc R . . C31 C 0.8536(8) 0.3690(3) 0.0535(5) 0.0270(13) Uani 1 1 d . . . N31A N 0.708(2) 0.3869(7) 0.0052(10) 0.024(3) Uani 0.80(4) 1 d PD A 1 N32A N 0.999(2) 0.3957(6) -0.0052(14) 0.034(3) Uani 0.80(4) 1 d PD A 1 C32A C 0.753(3) 0.4290(6) -0.0926(10) 0.036(4) Uani 0.80(4) 1 d PD A 1 H32A H 0.6749 0.4502 -0.1482 0.044 Uiso 0.80(4) 1 calc PR A 1 C33A C 0.931(3) 0.4351(5) -0.0962(12) 0.040(4) Uani 0.80(4) 1 d PD A 1 H33A H 0.9942 0.4623 -0.1527 0.047 Uiso 0.80(4) 1 calc PR A 1 C34A C 1.182(2) 0.3843(7) 0.022(2) 0.043(4) Uani 0.80(4) 1 d PD A 1 H34A H 1.2469 0.3835 -0.0535 0.064 Uiso 0.80(4) 1 calc PR A 1 H34B H 1.1968 0.3390 0.0641 0.064 Uiso 0.80(4) 1 calc PR A 1 H34C H 1.2249 0.4228 0.0735 0.064 Uiso 0.80(4) 1 calc PR A 1 N31B N 0.673(6) 0.386(4) 0.016(6) 0.05(2) Uiso 0.20(4) 1 d PD A 2 N32B N 0.958(4) 0.396(3) -0.027(4) 0.009(9) Uiso 0.20(4) 1 d PD A 2 C32B C 0.696(5) 0.427(4) -0.087(6) 0.042(16) Uiso 0.20(4) 1 d PD A 2 H32B H 0.6059 0.4484 -0.1328 0.050 Uiso 0.20(4) 1 calc PR A 2 C33B C 0.869(5) 0.431(2) -0.114(3) 0.010(9) Uiso 0.20(4) 1 d PD A 2 H33B H 0.9166 0.4540 -0.1820 0.012 Uiso 0.20(4) 1 calc PR A 2 C34B C 1.146(4) 0.388(2) -0.012(3) 0.010(9) Uiso 0.20(4) 1 d PD A 2 H34D H 1.2042 0.4306 -0.0392 0.016 Uiso 0.20(4) 1 calc PR A 2 H34E H 1.1842 0.3471 -0.0600 0.016 Uiso 0.20(4) 1 calc PR A 2 H34F H 1.1735 0.3791 0.0735 0.016 Uiso 0.20(4) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.02114(12) 0.01475(13) 0.02889(13) -0.00318(9) 0.00001(8) 0.00454(8) Cl1 0.0469(9) 0.0243(8) 0.0424(9) -0.0086(6) -0.0065(7) 0.0181(7) P1 0.0186(7) 0.0111(7) 0.0243(7) 0.0018(5) 0.0036(5) 0.0002(5) N11 0.024(2) 0.022(3) 0.022(2) 0.0047(19) -0.0038(19) -0.0041(19) C11 0.018(3) 0.017(3) 0.016(3) 0.002(2) -0.003(2) 0.001(2) N12 0.018(2) 0.022(3) 0.029(3) 0.000(2) -0.0014(19) 0.0003(19) C12 0.015(3) 0.037(4) 0.023(3) 0.008(3) -0.003(2) -0.007(2) C13 0.022(3) 0.036(4) 0.031(3) 0.001(3) 0.003(2) -0.002(3) C14 0.028(3) 0.023(3) 0.039(4) -0.003(3) 0.001(3) 0.008(2) N21 0.022(2) 0.013(2) 0.049(3) -0.005(2) 0.009(2) -0.0015(19) C21 0.019(3) 0.015(3) 0.029(3) -0.003(2) 0.007(2) 0.000(2) N22 0.020(2) 0.024(3) 0.029(3) -0.008(2) 0.0019(19) -0.003(2) C22 0.024(3) 0.029(4) 0.054(4) -0.023(3) 0.017(3) -0.010(3) C23 0.025(3) 0.042(4) 0.037(4) -0.015(3) 0.008(3) -0.010(3) C24 0.028(3) 0.037(4) 0.024(3) -0.003(3) 0.000(2) -0.008(3) C31 0.048(4) 0.008(3) 0.025(3) 0.000(2) 0.011(3) 0.002(2) N31A 0.047(6) 0.014(4) 0.012(4) 0.003(3) 0.003(4) 0.012(4) N32A 0.057(8) 0.017(4) 0.027(6) -0.001(4) 0.012(5) -0.002(5) C32A 0.072(12) 0.014(5) 0.022(5) 0.008(3) 0.006(6) 0.016(6) C33A 0.070(11) 0.016(5) 0.033(6) -0.001(4) 0.025(7) -0.010(5) C34A 0.041(7) 0.033(6) 0.056(11) -0.003(6) 0.027(7) 0.001(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 P1 2.2177(14) . ? Au1 Cl1 2.2761(15) . ? P1 C31 1.798(6) . ? P1 C11 1.800(5) . ? P1 C21 1.806(6) . ? N11 C11 1.332(7) . ? N11 C12 1.379(7) . ? C11 N12 1.358(7) . ? N12 C13 1.364(7) . ? N12 C14 1.466(7) . ? C12 C13 1.352(9) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? N21 C21 1.323(7) . ? N21 C22 1.376(8) . ? C21 N22 1.353(7) . ? N22 C23 1.366(7) . ? N22 C24 1.458(8) . ? C22 C23 1.359(10) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C31 N31A 1.294(17) . ? C31 N32B 1.31(4) . ? C31 N32A 1.399(13) . ? C31 N31B 1.49(5) . ? N31A C32A 1.391(11) . ? N32A C33A 1.355(13) . ? N32A C34A 1.469(13) . ? C32A C33A 1.384(16) . ? C32A H32A 0.9500 . ? C33A H33A 0.9500 . ? C34A H34A 0.9800 . ? C34A H34B 0.9800 . ? C34A H34C 0.9800 . ? N31B C32B 1.39(2) . ? N32B C33B 1.35(2) . ? N32B C34B 1.47(2) . ? C32B C33B 1.38(2) . ? C32B H32B 0.9500 . ? C33B H33B 0.9500 . ? C34B H34D 0.9800 . ? C34B H34E 0.9800 . ? C34B H34F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 178.59(5) . . ? C31 P1 C11 105.2(3) . . ? C31 P1 C21 104.7(3) . . ? C11 P1 C21 103.9(2) . . ? C31 P1 Au1 115.13(18) . . ? C11 P1 Au1 110.50(17) . . ? C21 P1 Au1 116.31(18) . . ? C11 N11 C12 104.1(5) . . ? N11 C11 N12 112.4(5) . . ? N11 C11 P1 120.2(4) . . ? N12 C11 P1 127.1(4) . . ? C11 N12 C13 106.0(5) . . ? C11 N12 C14 128.7(5) . . ? C13 N12 C14 125.3(5) . . ? C13 C12 N11 110.4(5) . . ? C13 C12 H12 124.8 . . ? N11 C12 H12 124.8 . . ? C12 C13 N12 107.2(5) . . ? C12 C13 H13 126.4 . . ? N12 C13 H13 126.4 . . ? N12 C14 H14A 109.5 . . ? N12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C21 N21 C22 104.7(5) . . ? N21 C21 N22 112.4(5) . . ? N21 C21 P1 125.1(4) . . ? N22 C21 P1 122.5(4) . . ? C21 N22 C23 106.1(5) . . ? C21 N22 C24 127.4(5) . . ? C23 N22 C24 126.4(5) . . ? C23 C22 N21 109.9(5) . . ? C23 C22 H22 125.1 . . ? N21 C22 H22 125.1 . . ? C22 C23 N22 106.9(6) . . ? C22 C23 H23 126.6 . . ? N22 C23 H23 126.6 . . ? N22 C24 H24A 109.5 . . ? N22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N31A C31 N32B 99.5(12) . . ? N31A C31 N32A 114.8(8) . . ? N32B C31 N31B 108(2) . . ? N32A C31 N31B 123.4(18) . . ? N31A C31 P1 123.1(7) . . ? N32B C31 P1 136.2(13) . . ? N32A C31 P1 121.8(9) . . ? N31B C31 P1 114.7(19) . . ? C31 N31A C32A 104.0(11) . . ? C33A N32A C31 103.5(10) . . ? C33A N32A C34A 127.0(9) . . ? C31 N32A C34A 129.5(9) . . ? C33A C32A N31A 109.3(9) . . ? C33A C32A H32A 125.3 . . ? N31A C32A H32A 125.3 . . ? N32A C33A C32A 108.2(7) . . ? N32A C33A H33A 125.9 . . ? C32A C33A H33A 125.9 . . ? C32B N31B C31 103(2) . . ? C31 N32B C33B 111(2) . . ? C31 N32B C34B 120(2) . . ? C33B N32B C34B 129(3) . . ? C33B C32B N31B 110(2) . . ? C33B C32B H32B 125.1 . . ? N31B C32B H32B 125.1 . . ? N32B C33B C32B 108(2) . . ? N32B C33B H33B 125.8 . . ? C32B C33B H33B 125.8 . . ? N32B C34B H34D 109.5 . . ? N32B C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? N32B C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? 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 C12 N11 C11 N12 0.7(6) . . . . ? C12 N11 C11 P1 174.5(4) . . . . ? C31 P1 C11 N11 127.2(4) . . . . ? C21 P1 C11 N11 -123.0(4) . . . . ? Au1 P1 C11 N11 2.4(5) . . . . ? C31 P1 C11 N12 -59.9(5) . . . . ? C21 P1 C11 N12 49.9(5) . . . . ? Au1 P1 C11 N12 175.3(4) . . . . ? N11 C11 N12 C13 -1.0(6) . . . . ? P1 C11 N12 C13 -174.3(4) . . . . ? N11 C11 N12 C14 180.0(5) . . . . ? P1 C11 N12 C14 6.6(8) . . . . ? C11 N11 C12 C13 -0.1(6) . . . . ? N11 C12 C13 N12 -0.4(6) . . . . ? C11 N12 C13 C12 0.8(6) . . . . ? C14 N12 C13 C12 179.9(5) . . . . ? C22 N21 C21 N22 -0.9(6) . . . . ? C22 N21 C21 P1 179.4(4) . . . . ? C31 P1 C21 N21 -7.5(5) . . . . ? C11 P1 C21 N21 -117.6(5) . . . . ? Au1 P1 C21 N21 120.8(4) . . . . ? C31 P1 C21 N22 172.8(4) . . . . ? C11 P1 C21 N22 62.7(5) . . . . ? Au1 P1 C21 N22 -58.9(5) . . . . ? N21 C21 N22 C23 1.4(6) . . . . ? P1 C21 N22 C23 -178.9(4) . . . . ? N21 C21 N22 C24 178.3(5) . . . . ? P1 C21 N22 C24 -1.9(8) . . . . ? C21 N21 C22 C23 0.1(6) . . . . ? N21 C22 C23 N22 0.8(7) . . . . ? C21 N22 C23 C22 -1.2(6) . . . . ? C24 N22 C23 C22 -178.2(5) . . . . ? C11 P1 C31 N31A -9.8(9) . . . . ? C21 P1 C31 N31A -118.9(9) . . . . ? Au1 P1 C31 N31A 112.1(8) . . . . ? C11 P1 C31 N32B -175(3) . . . . ? C21 P1 C31 N32B 76(3) . . . . ? Au1 P1 C31 N32B -53(3) . . . . ? C11 P1 C31 N32A 175.6(8) . . . . ? C21 P1 C31 N32A 66.5(8) . . . . ? Au1 P1 C31 N32A -62.5(8) . . . . ? C11 P1 C31 N31B -6(4) . . . . ? C21 P1 C31 N31B -115(4) . . . . ? Au1 P1 C31 N31B 116(4) . . . . ? N32A C31 N31A C32A -0.3(14) . . . . ? P1 C31 N31A C32A -175.3(7) . . . . ? N31A C31 N32A C33A 1.6(13) . . . . ? P1 C31 N32A C33A 176.6(6) . . . . ? N31A C31 N32A C34A -177.8(13) . . . . ? P1 C31 N32A C34A -2.8(16) . . . . ? C31 N31A C32A C33A -1.1(14) . . . . ? C31 N32A C33A C32A -2.2(12) . . . . ? C34A N32A C33A C32A 177.2(12) . . . . ? N31A C32A C33A N32A 2.1(14) . . . . ? N32B C31 N31B C32B -2(7) . . . . ? P1 C31 N31B C32B -174(4) . . . . ? N31B C31 N32B C33B 1(6) . . . . ? P1 C31 N32B C33B 170(2) . . . . ? N31B C31 N32B C34B 180(5) . . . . ? P1 C31 N32B C34B -11(6) . . . . ? C31 N31B C32B C33B 3(8) . . . . ? C31 N32B C33B C32B 1(6) . . . . ? C34B N32B C33B C32B -178(6) . . . . ? N31B C32B C33B N32B -3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.173 _refine_diff_density_min -0.895 _refine_diff_density_rms 0.164 #Compound 2a ends #===END ########### ## 2b(i) ## ########### data_Compound2b(i) _database_code_depnum_ccdc_archive 'CCDC 659054' _audit_creation_method SHELXL-97 _chemical_name_systematic chlorido[tris(thiazol-2-yl)phosphane]gold(I) _chemical_name_common 'tris(thiazol-2-yl)phosphanegold(I) chloride' _chemical_melting_point 404 _chemical_formula_moiety 'C9 H6 Au Cl N3 P S3' _chemical_formula_sum 'C9 H6 Au Cl N3 P S3' _chemical_formula_weight 515.75 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' Au Au -2.0133 8.8022 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_int_tables_number 14 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 10.3829(1) _cell_length_b 16.2935(1) _cell_length_c 17.2073(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.3216(4) _cell_angle_gamma 90.00 _cell_volume 2908.63(5) _cell_formula_units_Z 8 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 5560 _cell_measurement_theta_min 2.641 _cell_measurement_theta_max 28.272 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 10.823 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.520 _exptl_absorpt_correction_T_max 0.583 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ? _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area detector' _diffrn_measurement_method '\w- and \f-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21538 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5711 _reflns_number_gt 5042 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material X-Seed _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^)+(0.0152P)^2^+5.3055P] 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 5711 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0272 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0439 _refine_ls_wR_factor_gt 0.0422 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.751580(13) 0.063437(9) 0.222702(8) 0.02848(5) Uani 1 1 d . . . Cl1 Cl 0.53966(9) 0.07931(7) 0.18643(6) 0.0400(2) Uani 1 1 d . . . P1 P 0.95113(9) 0.04230(6) 0.26936(6) 0.0273(2) Uani 1 1 d . . . S11 S 1.23007(9) 0.02517(7) 0.20988(6) 0.0409(3) Uani 1 1 d . . . N11 N 1.0344(3) -0.0528(2) 0.1527(2) 0.0425(9) Uani 1 1 d . . . C11 C 1.0688(3) 0.0001(2) 0.2062(2) 0.0288(8) Uani 1 1 d . . . C12 C 1.2515(4) -0.0406(3) 0.1353(2) 0.0417(10) Uani 1 1 d . . . H12 H 1.3309 -0.0506 0.1127 0.050 Uiso 1 1 calc R . . C13 C 1.1406(4) -0.0763(3) 0.1129(3) 0.0470(11) Uani 1 1 d . . . H13 H 1.1353 -0.1151 0.0724 0.056 Uiso 1 1 calc R . . S21 S 0.95702(12) 0.22743(7) 0.30218(8) 0.0546(3) Uani 1 1 d . . . N21 N 1.1411(3) 0.1321(2) 0.3442(2) 0.0388(8) Uani 1 1 d . . . C21 C 1.0276(3) 0.1332(2) 0.3087(2) 0.0282(8) Uani 1 1 d . . . C22 C 1.0883(5) 0.2684(3) 0.3491(3) 0.0517(13) Uani 1 1 d . . . H22 H 1.0988 0.3243 0.3612 0.062 Uiso 1 1 calc R . . C23 C 1.1754(4) 0.2097(3) 0.3667(3) 0.0434(11) Uani 1 1 d . . . H23 H 1.2546 0.2212 0.3928 0.052 Uiso 1 1 calc R . . S31 S 1.06804(14) -0.09762(11) 0.37440(10) 0.0800(5) Uani 1 1 d . . . N31 N 0.8561(4) -0.0279(3) 0.3970(3) 0.0573(11) Uani 1 1 d . . . C31 C 0.9512(3) -0.0277(2) 0.3508(2) 0.0298(8) Uani 1 1 d . . . C32 C 0.9842(4) -0.1275(3) 0.4523(3) 0.0520(12) Uani 1 1 d . . . H32 H 1.0106 -0.1683 0.4881 0.062 Uiso 1 1 calc R . . C33 C 0.8756(4) -0.0845(3) 0.4551(3) 0.0526(13) Uani 1 1 d . . . H33 H 0.8163 -0.0925 0.4942 0.063 Uiso 1 1 calc R . . Au2 Au 0.756758(13) 0.203405(10) 0.071929(9) 0.03150(5) Uani 1 1 d . . . Cl2 Cl 0.96252(9) 0.15555(8) 0.08369(7) 0.0485(3) Uani 1 1 d . . . P2 P 0.55852(9) 0.25329(6) 0.05766(6) 0.0287(2) Uani 1 1 d . . . S41 S 0.27837(9) 0.18287(7) 0.04839(7) 0.0397(2) Uani 1 1 d . . . N41 N 0.4689(3) 0.1217(2) -0.02259(19) 0.0390(8) Uani 1 1 d . . . C41 C 0.4372(3) 0.1809(2) 0.0244(2) 0.0284(8) Uani 1 1 d . . . C42 C 0.2521(4) 0.0991(3) -0.0087(2) 0.0404(10) Uani 1 1 d . . . H42 H 0.1718 0.0732 -0.0167 0.049 Uiso 1 1 calc R . . C43 C 0.3618(4) 0.0745(3) -0.0411(2) 0.0428(10) Uani 1 1 d . . . H43 H 0.3649 0.0285 -0.0739 0.051 Uiso 1 1 calc R . . S51 S 0.67226(10) 0.39138(8) -0.04110(7) 0.0463(3) Uani 1 1 d . . . N51 N 0.4305(3) 0.3635(2) -0.0390(2) 0.0433(9) Uani 1 1 d . . . C51 C 0.5413(4) 0.3372(3) -0.0106(2) 0.0323(9) Uani 1 1 d . . . C52 C 0.5709(4) 0.4529(3) -0.0945(3) 0.0431(10) Uani 1 1 d . . . H52 H 0.5969 0.4973 -0.1251 0.052 Uiso 1 1 calc R . . C53 C 0.4485(4) 0.4291(3) -0.0868(3) 0.0460(11) Uani 1 1 d . . . H53 H 0.3792 0.4559 -0.1128 0.055 Uiso 1 1 calc R . . S61 S 0.60168(14) 0.30305(11) 0.22764(8) 0.0705(4) Uani 1 1 d . . . N61 N 0.3843(4) 0.3202(3) 0.1561(2) 0.0543(11) Uani 1 1 d . . . C61 C 0.5016(4) 0.2948(2) 0.1475(2) 0.0330(9) Uani 1 1 d . . . C62 C 0.4758(6) 0.3421(4) 0.2764(3) 0.0676(16) Uani 1 1 d . . . H62 H 0.4804 0.3585 0.3288 0.081 Uiso 1 1 calc R . . C63 C 0.3707(6) 0.3462(3) 0.2304(3) 0.0592(14) Uani 1 1 d . . . H63 H 0.2918 0.3657 0.2480 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01976(7) 0.03249(9) 0.03293(8) -0.00106(6) -0.00198(6) -0.00107(5) Cl1 0.0211(4) 0.0533(6) 0.0449(6) 0.0083(5) -0.0059(4) -0.0008(4) P1 0.0195(4) 0.0278(5) 0.0344(5) -0.0037(4) -0.0013(4) -0.0006(4) S11 0.0230(5) 0.0564(7) 0.0435(6) -0.0034(5) 0.0033(4) -0.0030(4) N11 0.039(2) 0.039(2) 0.050(2) -0.0134(17) 0.0101(17) -0.0090(16) C11 0.0279(19) 0.0226(19) 0.036(2) 0.0010(16) 0.0040(16) -0.0020(15) C12 0.037(2) 0.050(3) 0.039(2) 0.006(2) 0.0126(19) 0.010(2) C13 0.053(3) 0.040(3) 0.049(3) -0.012(2) 0.018(2) 0.003(2) S21 0.0468(7) 0.0307(6) 0.0836(9) -0.0113(6) -0.0297(6) 0.0122(5) N21 0.0318(18) 0.0294(19) 0.054(2) -0.0058(16) -0.0130(16) 0.0014(14) C21 0.0258(19) 0.0227(19) 0.036(2) -0.0052(16) -0.0028(16) 0.0018(14) C22 0.051(3) 0.030(2) 0.072(3) -0.011(2) -0.023(2) 0.003(2) C23 0.039(2) 0.032(2) 0.058(3) -0.009(2) -0.018(2) -0.0022(18) S31 0.0612(9) 0.0984(12) 0.0833(10) 0.0518(9) 0.0384(8) 0.0527(8) N31 0.042(2) 0.066(3) 0.066(3) 0.025(2) 0.022(2) 0.021(2) C31 0.0237(19) 0.032(2) 0.033(2) -0.0047(17) 0.0020(16) 0.0008(15) C32 0.049(3) 0.053(3) 0.055(3) 0.021(2) 0.011(2) 0.014(2) C33 0.042(3) 0.061(3) 0.056(3) 0.022(2) 0.020(2) 0.013(2) Au2 0.02088(8) 0.04152(10) 0.03224(9) -0.00322(7) 0.00262(6) -0.00125(6) Cl2 0.0252(5) 0.0660(8) 0.0545(7) 0.0104(6) 0.0060(5) 0.0097(5) P2 0.0215(5) 0.0384(6) 0.0265(5) -0.0024(4) 0.0030(4) -0.0017(4) S41 0.0238(5) 0.0407(6) 0.0550(7) 0.0059(5) 0.0057(4) -0.0012(4) N41 0.0367(19) 0.051(2) 0.0295(18) -0.0075(16) 0.0054(15) -0.0097(16) C41 0.0239(19) 0.036(2) 0.0257(19) 0.0054(16) -0.0001(15) -0.0013(15) C42 0.033(2) 0.043(3) 0.045(2) 0.012(2) -0.0079(19) -0.0106(18) C43 0.050(3) 0.047(3) 0.031(2) -0.0063(19) 0.0013(19) -0.015(2) S51 0.0264(5) 0.0570(7) 0.0558(7) 0.0122(6) 0.0080(5) -0.0084(5) N51 0.0272(18) 0.057(2) 0.046(2) 0.0158(18) -0.0038(16) -0.0095(16) C51 0.0260(19) 0.043(2) 0.028(2) 0.0000(18) 0.0033(16) -0.0073(17) C52 0.040(2) 0.049(3) 0.041(2) 0.010(2) 0.0040(19) -0.0092(19) C53 0.036(2) 0.056(3) 0.045(3) 0.016(2) -0.007(2) -0.008(2) S61 0.0546(8) 0.1111(13) 0.0450(7) -0.0366(8) -0.0081(6) 0.0015(8) N61 0.045(2) 0.076(3) 0.043(2) 0.001(2) 0.0072(18) 0.019(2) C61 0.038(2) 0.030(2) 0.030(2) 0.0008(17) 0.0019(17) -0.0012(17) C62 0.089(4) 0.074(4) 0.041(3) -0.028(3) 0.019(3) -0.014(3) C63 0.072(4) 0.053(3) 0.054(3) -0.010(3) 0.022(3) 0.015(3) _geom_special_details ;All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 Au2 3.4563(2) . ? Au1 Cl1 2.2774(9) . ? Au1 P1 2.2184(9) . ? Cl1 S11 3.3732(13) 1_455 ? P1 C11 1.804(4) . ? S11 C11 1.722(4) . ? S11 C12 1.694(4) . ? N11 C11 1.300(5) . ? C12 C13 1.332(6) . ? C12 H12 0.9400 . ? C13 H13 0.9400 . ? C13 N11 1.377(5) . ? P1 C21 1.800(4) . ? S21 C21 1.703(4) . ? S21 C22 1.693(4) . ? N21 C21 1.304(5) . ? C22 C23 1.342(6) . ? C22 H22 0.9400 . ? C23 H23 0.9400 . ? C23 N21 1.365(5) . ? P1 C31 1.807(4) . ? S31 C31 1.701(4) . ? S31 C32 1.699(5) . ? N31 C31 1.293(5) . ? C32 C33 1.330(6) . ? C32 H32 0.9400 . ? C33 H33 0.9400 . ? C33 N31 1.369(6) . ? Au2 Cl2 2.2755(10) . ? Au2 P2 2.2174(10) . ? S41 Cl2 3.3887(14) 1_455 ? P2 C41 1.801(4) . ? S41 C41 1.716(4) . ? S41 C42 1.697(5) . ? N41 C41 1.310(5) . ? C42 C43 1.348(6) . ? C42 H42 0.9400 . ? C43 H43 0.9400 . ? C43 N41 1.378(5) . ? P2 C51 1.807(4) . ? S51 C51 1.721(4) . ? S51 C52 1.697(5) . ? N51 C51 1.304(5) . ? C52 C53 1.340(6) . ? C52 H52 0.9400 . ? C53 H53 0.9400 . ? C53 N51 1.366(5) . ? P2 C61 1.808(4) . ? S61 C61 1.699(4) . ? S61 C62 1.704(6) . ? N61 C61 1.300(5) . ? C62 C63 1.323(8) . ? C62 H62 0.9400 . ? C63 H63 0.9400 . ? C63 N61 1.360(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 P1 Au1 Cl1 174.06(4) . . ? P1 Au1 Au2 109.35(3) . . ? Au1 Cl1 S11 148.46(5) . 1_455 ? Cl1 Au1 Au2 76.33(3) . . ? C11 P1 Au1 119.10(13) . . ? C21 P1 Au1 113.57(12) . . ? C31 P1 Au1 110.48(12) . . ? C11 P1 C21 103.94(17) . . ? C11 P1 C31 104.36(17) . . ? C21 P1 C31 103.97(18) . . ? S11 C11 P1 124.7(2) . . ? N11 C11 P1 120.4(3) . . ? N11 C11 S11 115.0(3) . . ? S11 C12 H12 124.6 . . ? N11 C13 H13 122.1 . . ? C11 N11 C13 109.5(4) . . ? C12 S11 C11 88.8(2) . . ? C12 C13 N11 115.8(4) . . ? C12 C13 H13 122.1 . . ? C13 C12 S11 110.9(3) . . ? C13 C12 H12 124.6 . . ? S21 C21 P1 122.3(2) . . ? N21 C21 P1 122.7(3) . . ? N21 C21 S21 114.9(3) . . ? S21 C22 H22 124.8 . . ? N21 C23 H23 122.3 . . ? C21 N21 C23 109.9(3) . . ? C22 S21 C21 89.3(2) . . ? C22 C23 N21 115.4(4) . . ? C22 C23 H23 122.3 . . ? C23 C22 S21 110.4(3) . . ? C23 C22 H22 124.8 . . ? S31 C31 P1 125.8(2) . . ? N31 C31 P1 120.2(3) . . ? N31 C31 S31 114.0(3) . . ? S31 C32 H32 125.1 . . ? N31 C33 H33 122.3 . . ? C31 N31 C33 110.9(4) . . ? C32 S31 C31 89.8(2) . . ? C32 C33 N31 115.4(4) . . ? C32 C33 H33 122.3 . . ? C33 C32 S31 109.8(4) . . ? C33 C32 H32 125.1 . . ? P2 Au2 Cl2 178.03(4) . . ? Cl2 Au2 Au1 75.54(3) . . ? P2 Au2 Au1 106.40(3) . . ? C41 S41 Cl2 170.71(15) . 1_455 ? C42 S41 Cl2 82.20(15) . 1_455 ? C41 P2 Au2 115.41(13) . . ? C51 P2 Au2 114.60(13) . . ? C61 P2 Au2 112.13(13) . . ? C41 P2 C51 103.83(17) . . ? C41 P2 C61 105.50(18) . . ? C51 P2 C61 104.25(18) . . ? S41 C41 P2 125.3(2) . . ? N41 C41 P2 119.2(3) . . ? N41 C41 S41 115.4(3) . . ? S41 C42 H42 124.5 . . ? N41 C43 H43 122.4 . . ? C41 N41 C43 109.4(3) . . ? C42 S41 C41 88.8(2) . . ? C42 C43 N41 115.2(4) . . ? C42 C43 H43 122.4 . . ? C43 C42 S41 111.1(3) . . ? C43 C42 H42 124.5 . . ? S51 C51 P2 121.9(2) . . ? N51 C51 P2 123.7(3) . . ? N51 C51 S51 114.4(3) . . ? S51 C52 H52 124.9 . . ? N51 C53 H53 122.0 . . ? C51 N51 C53 110.1(3) . . ? C52 S51 C51 89.3(2) . . ? C52 C53 N51 116.1(4) . . ? C52 C53 H53 122.0 . . ? C53 C52 S51 110.2(3) . . ? C53 C52 H52 124.9 . . ? S61 C61 P2 120.9(2) . . ? N61 C61 P2 123.8(3) . . ? N61 C61 S61 115.3(3) . . ? S61 C62 H62 124.6 . . ? N61 C63 H63 122.2 . . ? C61 S61 C62 88.5(3) . . ? C61 N61 C63 109.9(4) . . ? C62 C63 N61 115.6(5) . . ? C62 C63 H63 122.2 . . ? C63 C62 S61 110.8(4) . . ? C63 C62 H62 124.6 . . ? 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 Cl1 Au1 Au2 Cl2 -162.52(4) . . . . ? Cl1 Au1 Au2 P2 17.81(4) . . . . ? P1 Au1 Au2 Cl2 19.28(4) . . . . ? P1 Au1 Au2 P2 -160.39(4) . . . . ? Au1 P1 C11 S11 145.53(19) . . . . ? Au1 P1 C21 S21 -5.5(3) . . . . ? Au1 P1 C31 S31 146.3(2) . . . . ? Au2 P2 C41 S41 148.54(19) . . . . ? Au2 P2 C51 S51 -16.8(3) . . . . ? Au2 P2 C61 S61 7.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.817 _refine_diff_density_min -0.802 _refine_diff_density_rms 0.102 #Compound 2b(i) ends #===END ############ ## 2b(ii) ## ############ data_Compound2b(ii) _database_code_depnum_ccdc_archive 'CCDC 659055' _audit_creation_method SHELXL-97 _chemical_name_systematic chlorido[tris(thiazol-2-yl)phosphane]gold(I) _chemical_name_common 'tris(thiazol-2-yl)phosphanegold(I) chloride' _chemical_melting_point ? _chemical_formula_moiety 'C9 H6 Au Cl N3 P S3' _chemical_formula_sum 'C9 H6 Au Cl N3 P S3' _chemical_formula_weight 515.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0705(4) _cell_length_b 8.6077(4) _cell_length_c 10.5184(5) _cell_angle_alpha 72.425(1) _cell_angle_beta 84.882(1) _cell_angle_gamma 75.129(1) _cell_volume 673.20(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4954 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 11.690 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.167 _exptl_absorpt_correction_T_max 0.310 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _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_% ? _diffrn_reflns_number 7454 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 26.73 _reflns_number_total 2842 _reflns_number_gt 2744 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material X-Seed _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^)+(0.0223P)^2^+0.2556P] 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 2842 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0202 _refine_ls_R_factor_gt 0.0192 _refine_ls_wR_factor_ref 0.0453 _refine_ls_wR_factor_gt 0.0449 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.116482(15) 0.090358(16) 0.066485(12) 0.01268(5) Uani 1 1 d . . . Cl1 Cl -0.03412(11) 0.30700(11) -0.09921(9) 0.01750(18) Uani 1 1 d . . . P1 P 0.28515(11) -0.10899(11) 0.22117(9) 0.01137(18) Uani 1 1 d . . . S11 S 0.64529(11) -0.11257(11) 0.31503(9) 0.01550(18) Uani 1 1 d . . . N11 N 0.3750(4) 0.1257(4) 0.3085(3) 0.0133(6) Uani 1 1 d . . . C11 C 0.4293(4) -0.0220(4) 0.2876(3) 0.0115(7) Uani 1 1 d . . . C12 C 0.6630(5) 0.0590(5) 0.3579(4) 0.0171(8) Uani 1 1 d . . . H12 H 0.7661 0.0743 0.3838 0.021 Uiso 1 1 calc R . . C13 C 0.5092(5) 0.1693(5) 0.3493(4) 0.0165(7) Uani 1 1 d . . . H13 H 0.4943 0.2718 0.3704 0.020 Uiso 1 1 calc R . . S21 S 0.27458(12) -0.43093(12) 0.46025(9) 0.0190(2) Uani 1 1 d . . . N21 N 0.0518(4) -0.1490(4) 0.4209(3) 0.0163(6) Uani 1 1 d . . . C21 C 0.1892(4) -0.2264(4) 0.3692(3) 0.0120(7) Uani 1 1 d . . . C22 C 0.1113(4) -0.4111(5) 0.5742(3) 0.0175(8) Uani 1 1 d . . . H22 H 0.0957 -0.4978 0.6519 0.021 Uiso 1 1 calc R . . C23 C 0.0079(5) -0.2552(5) 0.5381(4) 0.0165(7) Uani 1 1 d . . . H23 H -0.0890 -0.2209 0.5903 0.020 Uiso 1 1 calc R . . S31 S 0.46891(12) -0.21811(11) -0.01333(9) 0.01568(18) Uani 1 1 d . . . N31 N 0.5378(4) -0.3965(4) 0.2273(3) 0.0163(6) Uani 1 1 d . . . C31 C 0.4342(4) -0.2614(4) 0.1556(3) 0.0119(7) Uani 1 1 d . . . C32 C 0.6339(4) -0.3921(4) 0.0127(4) 0.0157(7) Uani 1 1 d . . . H32 H 0.7038 -0.4284 -0.0555 0.019 Uiso 1 1 calc R . . C33 C 0.6510(5) -0.4714(5) 0.1448(4) 0.0167(8) Uani 1 1 d . . . H33 H 0.7358 -0.5724 0.1786 0.020 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01167(8) 0.01194(8) 0.01302(8) -0.00239(6) -0.00195(5) -0.00125(5) Cl1 0.0154(4) 0.0145(4) 0.0194(5) -0.0007(4) -0.0053(3) -0.0016(3) P1 0.0112(4) 0.0114(4) 0.0103(4) -0.0026(4) -0.0006(3) -0.0011(3) S11 0.0127(4) 0.0147(4) 0.0179(5) -0.0047(4) -0.0024(3) -0.0006(3) N11 0.0165(15) 0.0120(15) 0.0102(14) -0.0016(12) -0.0021(11) -0.0026(12) C11 0.0089(16) 0.0136(17) 0.0105(16) -0.0034(14) 0.0016(12) -0.0008(13) C12 0.0203(19) 0.0192(19) 0.0146(18) -0.0061(15) 0.0010(14) -0.0085(15) C13 0.0204(19) 0.0176(19) 0.0142(18) -0.0062(15) 0.0004(14) -0.0077(15) S21 0.0154(4) 0.0152(5) 0.0190(5) 0.0010(4) 0.0041(3) 0.0005(4) N21 0.0148(15) 0.0166(16) 0.0168(16) -0.0064(13) 0.0042(12) -0.0025(12) C21 0.0126(17) 0.0125(17) 0.0104(17) -0.0027(14) -0.0043(13) -0.0017(13) C22 0.0135(18) 0.024(2) 0.0151(19) -0.0054(16) 0.0024(14) -0.0064(16) C23 0.0140(17) 0.0203(19) 0.0151(18) -0.0052(15) 0.0003(14) -0.0042(15) S31 0.0191(4) 0.0154(4) 0.0110(4) -0.0034(3) 0.0018(3) -0.0027(4) N31 0.0163(15) 0.0148(16) 0.0171(16) -0.0064(13) -0.0007(12) -0.0003(12) C31 0.0135(17) 0.0141(17) 0.0084(16) -0.0027(14) 0.0002(13) -0.0046(14) C32 0.0163(18) 0.0142(18) 0.0184(19) -0.0085(15) 0.0051(14) -0.0043(14) C33 0.0137(17) 0.0157(18) 0.022(2) -0.0085(16) -0.0003(14) -0.0024(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 Au1 P1 2.2260(9) . ? Au1 Cl1 2.2900(9) . ? Au1 Au1 3.3459(3) 2 ? P1 C31 1.798(4) . ? P1 C21 1.812(4) . ? P1 C11 1.819(4) . ? S11 C12 1.711(4) . ? S11 C11 1.728(3) . ? N11 C11 1.313(4) . ? N11 C13 1.373(5) . ? C12 C13 1.346(5) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? S21 C22 1.711(3) . ? S21 C21 1.723(3) . ? N21 C21 1.304(4) . ? N21 C23 1.374(5) . ? C22 C23 1.347(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? S31 C32 1.699(4) . ? S31 C31 1.714(3) . ? N31 C31 1.306(5) . ? N31 C33 1.378(5) . ? C32 C33 1.352(5) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 174.30(3) . . ? Cl1 Au1 Au1 75.78(2) . 2 ? P1 Au1 Au1 108.50(2) . 2 ? C11 P1 Au1 110.89(11) . . ? C21 P1 Au1 119.33(11) . . ? C31 P1 Au1 113.27(11) . . ? C11 P1 C21 103.48(16) . . ? C11 P1 C31 101.55(15) . . ? C21 P1 C31 106.46(16) . . ? S11 C11 P1 124.7(2) . . ? N11 C11 P1 120.3(2) . . ? N11 C11 S11 114.9(3) . . ? S11 C12 H12 125.0 . . ? N11 C13 H13 121.7 . . ? C11 S11 C12 89.14(17) . . ? C11 N11 C13 109.5(3) . . ? C12 C13 N11 116.5(3) . . ? C12 C13 H13 121.7 . . ? C13 C12 S11 110.0(3) . . ? C13 C12 H12 125.0 . . ? S21 C21 P1 125.6(2) . . ? N21 C21 P1 118.9(3) . . ? N21 C21 S21 115.2(3) . . ? S21 C22 H22 124.8 . . ? N21 C23 H23 122.2 . . ? C21 S21 C22 88.78(17) . . ? C21 N21 C23 110.0(3) . . ? C22 C23 N21 115.6(3) . . ? C22 C23 H23 122.2 . . ? C23 C22 S21 110.4(3) . . ? C23 C22 H22 124.8 . . ? S31 C31 P1 119.4(2) . . ? N31 C31 P1 124.9(3) . . ? N31 C31 S31 115.1(3) . . ? S31 C32 H32 125.0 . . ? N31 C33 H33 122.1 . . ? C31 S31 C32 89.58(18) . . ? C31 N31 C33 109.5(3) . . ? C32 C33 N31 115.9(3) . . ? C32 C33 H33 122.1 . . ? C33 C32 S31 109.9(3) . . ? C33 C32 H32 125.0 . . ? 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 Au1 Au1 P1 C11 174.98(11) 2 . . . ? Au1 Au1 P1 C21 -64.99(13) 2 . . . ? Au1 Au1 P1 C31 61.56(13) 2 . . . ? Au1 P1 C11 S11 -135.71(19) . . . . ? Au1 P1 C11 N11 38.9(3) . . . . ? Au1 P1 C21 S21 150.24(17) . . . . ? Au1 P1 C21 N21 -36.3(3) . . . . ? Au1 P1 C31 S31 14.7(2) . . . . ? Au1 P1 C31 N31 -174.9(3) . . . . ? S11 C12 C13 N11 -0.7(4) . . . . ? S21 C22 C23 N21 0.8(4) . . . . ? S31 C32 C33 N31 -0.9(4) . . . . ? C11 S11 C12 C13 0.3(3) . . . . ? C11 P1 C21 S21 -86.0(2) . . . . ? C11 P1 C21 N21 87.4(3) . . . . ? C11 P1 C31 S31 -104.2(2) . . . . ? C11 P1 C31 N31 66.2(3) . . . . ? C11 N11 C13 C12 0.8(5) . . . . ? C12 S11 C11 P1 175.1(2) . . . . ? C12 S11 C11 N11 0.2(3) . . . . ? C13 N11 C11 S11 -0.6(4) . . . . ? C13 N11 C11 P1 -175.7(2) . . . . ? C21 S21 C22 C23 -1.0(3) . . . . ? C21 P1 C11 S11 95.2(2) . . . . ? C21 P1 C11 N11 -90.2(3) . . . . ? C21 P1 C31 S31 147.8(2) . . . . ? C21 P1 C31 N31 -41.8(3) . . . . ? C21 N21 C23 C22 -0.1(5) . . . . ? C22 S21 C21 P1 174.7(2) . . . . ? C22 S21 C21 N21 1.0(3) . . . . ? C23 N21 C21 S21 -0.7(4) . . . . ? C23 N21 C21 P1 -174.8(2) . . . . ? C31 S31 C32 C33 0.6(3) . . . . ? C31 P1 C11 S11 -15.1(3) . . . . ? C31 P1 C11 N11 159.5(3) . . . . ? C31 P1 C21 S21 20.6(3) . . . . ? C31 P1 C21 N21 -166.0(3) . . . . ? C31 N31 C33 C32 0.9(5) . . . . ? C32 S31 C31 P1 171.2(2) . . . . ? C32 S31 C31 N31 -0.1(3) . . . . ? C33 N31 C31 S31 -0.4(4) . . . . ? C33 N31 C31 P1 -171.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.384 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.134 #Compund 2b(ii) ends #===END ############# ## 2b(iii) ## ############# data_Compound2b(iii) _database_code_depnum_ccdc_archive 'CCDC 659056' _audit_creation_method SHELXL-97 _chemical_name_systematic chlorido[tris(thiazol-2-yl)phosphane]gold(I) _chemical_name_common 'tris(thiazol-2-yl)phosphanegold(I) chloride' _chemical_melting_point ? _chemical_formula_moiety 'C9 H6 Au Cl N3 P S3' _chemical_formula_sum 'C9 H6 Au Cl N3 P S3' _chemical_formula_weight 515.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6111(15) _cell_length_b 8.7006(15) _cell_length_c 9.5117(17) _cell_angle_alpha 90.821(3) _cell_angle_beta 97.446(3) _cell_angle_gamma 106.515(3) _cell_volume 676.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5845 _cell_measurement_theta_min 2.163 _cell_measurement_theta_max 28.277 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 11.634 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.091 _exptl_absorpt_correction_T_max 0.196 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area detector' _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_% ? _diffrn_reflns_number 7937 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3162 _reflns_number_gt 3073 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material X-Seed _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^)+(0.0145P)^2^+0.5242P] 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 3162 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0195 _refine_ls_R_factor_gt 0.0187 _refine_ls_wR_factor_ref 0.0442 _refine_ls_wR_factor_gt 0.0439 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.441517(13) 1.019446(13) 0.193160(11) 0.01345(5) Uani 1 1 d . . . P1 P 0.26880(10) 0.82241(10) 0.28682(9) 0.01298(16) Uani 1 1 d . . . Cl1 Cl 0.60757(10) 1.22345(10) 0.08459(9) 0.02200(17) Uani 1 1 d . . . S21 S -0.06256(10) 0.56491(10) 0.16481(9) 0.02102(17) Uani 1 1 d . . . S11 S 0.51483(10) 0.62893(10) 0.27161(9) 0.02017(17) Uani 1 1 d . . . S31 S 0.11503(12) 0.72257(10) 0.56219(9) 0.02567(19) Uani 1 1 d . . . C31 C 0.2152(4) 0.8669(4) 0.4575(3) 0.0138(6) Uani 1 1 d . . . N11 N 0.2373(3) 0.5102(3) 0.3554(3) 0.0203(6) Uani 1 1 d . . . C11 C 0.3299(4) 0.6413(4) 0.3102(3) 0.0146(6) Uani 1 1 d . . . C13 C 0.3164(4) 0.3933(4) 0.3612(4) 0.0218(7) Uani 1 1 d . . . H13 H 0.2682 0.2890 0.3914 0.026 Uiso 1 1 calc R . . N31 N 0.2355(3) 1.0156(3) 0.5024(3) 0.0204(6) Uani 1 1 d . . . C22 C -0.1944(4) 0.6299(4) 0.0470(3) 0.0190(7) Uani 1 1 d . . . H22 H -0.2986 0.5651 0.0039 0.023 Uiso 1 1 calc R . . C21 C 0.0734(4) 0.7544(4) 0.1743(3) 0.0149(6) Uani 1 1 d . . . N21 N 0.0222(3) 0.8578(3) 0.0966(3) 0.0213(6) Uani 1 1 d . . . C23 C -0.1297(4) 0.7863(4) 0.0240(4) 0.0217(7) Uani 1 1 d . . . H23 H -0.1860 0.8430 -0.0386 0.026 Uiso 1 1 calc R . . C32 C 0.0997(4) 0.8717(5) 0.6729(4) 0.0241(7) Uani 1 1 d . . . H32 H 0.0497 0.8548 0.7569 0.029 Uiso 1 1 calc R . . C12 C 0.4662(4) 0.4358(4) 0.3214(4) 0.0217(7) Uani 1 1 d . . . H12 H 0.5352 0.3679 0.3212 0.026 Uiso 1 1 calc R . . C33 C 0.1681(4) 1.0163(4) 0.6251(4) 0.0207(7) Uani 1 1 d . . . H33 H 0.1697 1.1132 0.6733 0.025 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01406(7) 0.01030(7) 0.01453(7) 0.00299(5) 0.00304(4) 0.00061(5) P1 0.0137(4) 0.0100(4) 0.0147(4) 0.0039(3) 0.0024(3) 0.0023(3) Cl1 0.0266(4) 0.0151(4) 0.0196(4) 0.0026(3) 0.0084(3) -0.0039(3) S21 0.0197(4) 0.0136(4) 0.0243(4) 0.0065(3) -0.0026(3) -0.0016(3) S11 0.0173(4) 0.0207(4) 0.0240(4) 0.0008(3) 0.0041(3) 0.0073(3) S31 0.0392(5) 0.0165(4) 0.0211(4) 0.0060(3) 0.0143(4) 0.0031(4) C31 0.0112(14) 0.0145(15) 0.0148(14) 0.0032(12) 0.0019(11) 0.0022(12) N11 0.0200(14) 0.0141(14) 0.0268(15) 0.0064(11) 0.0037(12) 0.0046(11) C11 0.0139(14) 0.0136(15) 0.0159(15) 0.0021(12) 0.0008(12) 0.0039(12) C13 0.0293(18) 0.0096(15) 0.0239(17) 0.0014(13) -0.0032(14) 0.0048(14) N31 0.0198(14) 0.0157(14) 0.0261(15) 0.0020(12) 0.0067(12) 0.0043(12) C22 0.0145(15) 0.0220(17) 0.0165(15) 0.0015(13) -0.0002(12) -0.0003(13) C21 0.0134(14) 0.0132(15) 0.0162(15) 0.0016(12) 0.0028(12) 0.0005(12) N21 0.0188(14) 0.0172(14) 0.0268(15) 0.0078(12) 0.0004(12) 0.0045(12) C23 0.0175(16) 0.0214(18) 0.0249(17) 0.0067(14) -0.0019(13) 0.0057(14) C32 0.0262(18) 0.030(2) 0.0158(16) -0.0006(14) 0.0066(14) 0.0056(16) C12 0.0283(18) 0.0183(17) 0.0204(16) -0.0042(13) -0.0040(14) 0.0131(15) C33 0.0183(16) 0.0198(17) 0.0231(17) -0.0018(14) 0.0038(13) 0.0038(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 Au1 P1 2.2096(8) . ? Au1 Cl1 2.2921(8) . ? Au1 Cl1 3.2660(9) 2_675 ? P1 C11 1.805(3) . ? P1 C21 1.810(3) . ? P1 C31 1.810(3) . ? Cl1 S21 3.4717(12) 1_665 ? S21 C22 1.708(3) . ? S21 C21 1.723(3) . ? S11 C12 1.702(4) . ? S11 C11 1.712(3) . ? S31 C32 1.704(4) . ? S31 C31 1.719(3) . ? C31 N31 1.312(4) . ? N11 C11 1.307(4) . ? N11 C13 1.374(4) . ? C13 C12 1.343(5) . ? C13 H13 0.9500 . ? N31 C33 1.369(4) . ? C22 C23 1.349(5) . ? C22 H22 0.9500 . ? C21 N21 1.308(4) . ? N21 C23 1.366(4) . ? C23 H23 0.9500 . ? C32 C33 1.342(5) . ? C32 H32 0.9500 . ? C12 H12 0.9500 . ? C33 H33 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 176.36(3) . . ? P1 Au1 Cl1 87.61(3) . 2_675 ? Cl1 Au1 Cl1 90.66(3) . 2_675 ? C11 P1 C21 103.38(15) . . ? C11 P1 C31 104.52(14) . . ? C21 P1 C31 103.64(14) . . ? C11 P1 Au1 115.46(11) . . ? C21 P1 Au1 111.45(11) . . ? C31 P1 Au1 116.89(11) . . ? Au1 Cl1 S21 140.83(4) . 1_665 ? C22 S21 C21 88.94(16) . . ? C12 S11 C11 89.27(16) . . ? C32 S31 C31 88.81(17) . . ? N31 C31 S31 115.1(2) . . ? N31 C31 P1 120.9(2) . . ? S31 C31 P1 123.62(18) . . ? C11 N11 C13 109.8(3) . . ? N11 C11 S11 114.9(2) . . ? N11 C11 P1 123.3(2) . . ? S11 C11 P1 121.75(18) . . ? C12 C13 N11 115.7(3) . . ? C12 C13 H13 122.1 . . ? N11 C13 H13 122.1 . . ? C31 N31 C33 109.6(3) . . ? C23 C22 S21 110.4(2) . . ? C23 C22 H22 124.8 . . ? S21 C22 H22 124.8 . . ? N21 C21 S21 114.7(2) . . ? N21 C21 P1 118.8(2) . . ? S21 C21 P1 126.36(19) . . ? C21 N21 C23 110.4(3) . . ? C22 C23 N21 115.6(3) . . ? C22 C23 H23 122.2 . . ? N21 C23 H23 122.2 . . ? C33 C32 S31 110.7(3) . . ? C33 C32 H32 124.7 . . ? S31 C32 H32 124.7 . . ? C13 C12 S11 110.3(3) . . ? C13 C12 H12 124.9 . . ? S11 C12 H12 124.9 . . ? C32 C33 N31 115.9(3) . . ? C32 C33 H33 122.0 . . ? N31 C33 H33 122.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Au1 Cl1 S21 -149.67(7) 2_675 . . 1_665 ? C32 S31 C31 N31 0.0(3) . . . . ? C32 S31 C31 P1 -172.9(2) . . . . ? C11 P1 C31 N31 149.2(3) . . . . ? C21 P1 C31 N31 -102.9(3) . . . . ? Au1 P1 C31 N31 20.2(3) . . . . ? C11 P1 C31 S31 -38.3(2) . . . . ? C21 P1 C31 S31 69.7(2) . . . . ? Au1 P1 C31 S31 -167.32(14) . . . . ? C13 N11 C11 S11 0.4(4) . . . . ? C13 N11 C11 P1 179.6(2) . . . . ? C12 S11 C11 N11 -0.7(3) . . . . ? C12 S11 C11 P1 -179.9(2) . . . . ? C21 P1 C11 N11 -53.5(3) . . . . ? C31 P1 C11 N11 54.7(3) . . . . ? Au1 P1 C11 N11 -175.4(2) . . . . ? C21 P1 C11 S11 125.6(2) . . . . ? C31 P1 C11 S11 -126.2(2) . . . . ? Au1 P1 C11 S11 3.7(2) . . . . ? C11 N11 C13 C12 0.2(4) . . . . ? S31 C31 N31 C33 -0.4(3) . . . . ? P1 C31 N31 C33 172.8(2) . . . . ? C21 S21 C22 C23 -0.5(3) . . . . ? C22 S21 C21 N21 0.8(3) . . . . ? C22 S21 C21 P1 177.0(2) . . . . ? C11 P1 C21 N21 -156.1(3) . . . . ? C31 P1 C21 N21 95.1(3) . . . . ? Au1 P1 C21 N21 -31.4(3) . . . . ? C11 P1 C21 S21 27.9(3) . . . . ? C31 P1 C21 S21 -80.9(2) . . . . ? Au1 P1 C21 S21 152.52(17) . . . . ? S21 C21 N21 C23 -0.9(4) . . . . ? P1 C21 N21 C23 -177.4(2) . . . . ? S21 C22 C23 N21 0.1(4) . . . . ? C21 N21 C23 C22 0.6(4) . . . . ? C31 S31 C32 C33 0.3(3) . . . . ? N11 C13 C12 S11 -0.8(4) . . . . ? C11 S11 C12 C13 0.8(3) . . . . ? S31 C32 C33 N31 -0.6(4) . . . . ? C31 N31 C33 C32 0.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.293 _refine_diff_density_min -1.119 _refine_diff_density_rms 0.133 #Compound 2b(iii) ends #===END ############## ## 2b . DCM ## ############## data_Compound2bDCM _database_code_depnum_ccdc_archive 'CCDC 659057' _audit_creation_method SHELXL-97 _chemical_name_systematic 'chlorido[tris(thiazol-2-yl)phosphane]gold(I) dichloromethane hemisolvate' _chemical_name_common 'tris(thiazol-2-yl)phosphinegold(I) chloride dichloromethane hemisolvate' _chemical_melting_point ? _chemical_formula_moiety 'C9 H6 Au Cl N3 P S3, 0.5(C H2 Cl2)' _chemical_formula_sum 'C9.5 H7 Au Cl2 N3 P S3' _chemical_formula_weight 558.22 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' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.9518(9) _cell_length_b 20.261(2) _cell_length_c 19.413(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.018(2) _cell_angle_gamma 90.00 _cell_volume 3110.6(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1857 _cell_measurement_theta_min 2.271 _cell_measurement_theta_max 25.909 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 10.296 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.117 _exptl_absorpt_correction_T_max 0.596 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area detector' _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_% ? _diffrn_reflns_number 17633 _diffrn_reflns_av_R_equivalents 0.0675 _diffrn_reflns_av_sigmaI/netI 0.0880 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 26.44 _reflns_number_total 6344 _reflns_number_gt 4748 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material X-Seed _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^)+(0.0288P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6344 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.0909 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.57237(4) 0.160161(19) 0.768351(17) 0.01391(10) Uani 1 1 d . . . Au2 Au 0.34624(4) 0.24949(2) 0.858981(17) 0.01349(10) Uani 1 1 d . . . Cl1 Cl 0.3984(3) 0.18516(13) 0.67062(12) 0.0254(6) Uani 1 1 d . . . Cl2 Cl 0.4665(3) 0.19366(12) 0.95326(11) 0.0182(5) Uani 1 1 d . . . Cl3 Cl -0.0369(4) 0.07639(15) 0.54725(13) 0.0376(7) Uani 1 1 d . . . Cl4 Cl 0.2472(4) 0.08250(16) 0.46457(17) 0.0502(9) Uani 1 1 d . . . S11 S 0.8804(3) 0.26079(12) 0.90239(12) 0.0213(6) Uani 1 1 d . . . S21 S 1.1465(3) 0.08536(13) 0.84480(12) 0.0199(6) Uani 1 1 d . . . S31 S 0.7836(3) 0.01714(13) 0.96995(11) 0.0166(5) Uani 1 1 d . . . S41 S 0.5971(3) 0.34913(13) 0.75309(12) 0.0212(6) Uani 1 1 d . . . S51 S 0.2013(3) 0.41838(14) 0.88540(12) 0.0263(6) Uani 1 1 d . . . S61 S 0.0452(3) 0.29823(12) 0.62514(11) 0.0168(5) Uani 1 1 d . . . P1 P 0.7651(3) 0.12313(12) 0.84979(12) 0.0124(5) Uani 1 1 d . . . P2 P 0.2297(3) 0.31300(13) 0.77436(12) 0.0137(5) Uani 1 1 d . . . N11 N 0.9412(9) 0.1558(4) 0.9743(4) 0.0212(19) Uani 1 1 d . . . N21 N 0.9062(8) 0.0568(4) 0.7496(4) 0.0138(17) Uani 1 1 d . . . N31 N 0.5525(8) 0.0235(4) 0.8683(4) 0.0167(18) Uani 1 1 d . . . N41 N 0.3442(8) 0.3843(4) 0.6682(4) 0.0146(17) Uani 1 1 d . . . N51 N -0.0069(9) 0.4145(4) 0.7739(4) 0.0185(19) Uani 1 1 d . . . N61 N -0.0159(9) 0.2266(4) 0.7291(4) 0.0209(19) Uani 1 1 d . . . C1 C 0.1212(13) 0.1277(5) 0.5188(5) 0.035(3) Uani 1 1 d . . . H1A H 0.1937 0.1451 0.5593 0.042 Uiso 1 1 calc R . . H1B H 0.0679 0.1657 0.4928 0.042 Uiso 1 1 calc R . . C11 C 0.8688(11) 0.1764(5) 0.9130(4) 0.015(2) Uani 1 1 d . . . C12 C 0.9815(12) 0.2669(5) 0.9840(5) 0.022(2) Uani 1 1 d . . . H12 H 1.0172 0.3072 1.0057 0.026 Uiso 1 1 calc R . . C13 C 1.0043(12) 0.2071(5) 1.0137(5) 0.025(2) Uani 1 1 d . . . H13 H 1.0605 0.2012 1.0589 0.031 Uiso 1 1 calc R . . C21 C 0.9369(11) 0.0866(5) 0.8093(4) 0.014(2) Uani 1 1 d . . . C22 C 1.1956(11) 0.0424(5) 0.7737(5) 0.019(2) Uani 1 1 d . . . H22 H 1.3061 0.0281 0.7665 0.023 Uiso 1 1 calc R . . C23 C 1.0572(11) 0.0315(5) 0.7298(5) 0.017(2) Uani 1 1 d . . . H23 H 1.0615 0.0081 0.6876 0.020 Uiso 1 1 calc R . . C31 C 0.6854(10) 0.0545(5) 0.8967(5) 0.015(2) Uani 1 1 d . . . C32 C 0.6369(10) -0.0444(5) 0.9602(4) 0.015(2) Uani 1 1 d . . . H32 H 0.6350 -0.0819 0.9895 0.019 Uiso 1 1 calc R . . C33 C 0.5231(11) -0.0321(5) 0.9046(5) 0.016(2) Uani 1 1 d . . . H33 H 0.4296 -0.0604 0.8918 0.019 Uiso 1 1 calc R . . C41 C 0.3828(9) 0.3519(4) 0.7257(4) 0.0103(19) Uani 1 1 d . . . C42 C 0.6334(11) 0.3938(5) 0.6831(4) 0.019(2) Uani 1 1 d . . . H42 H 0.7423 0.4070 0.6723 0.023 Uiso 1 1 calc R . . C43 C 0.4863(10) 0.4086(5) 0.6442(5) 0.017(2) Uani 1 1 d . . . H43 H 0.4829 0.4341 0.6031 0.020 Uiso 1 1 calc R . . C51 C 0.1221(11) 0.3838(5) 0.8072(4) 0.017(2) Uani 1 1 d . . . C52 C 0.0528(12) 0.4801(5) 0.8704(5) 0.027(3) Uani 1 1 d . . . H52 H 0.0419 0.5167 0.9001 0.033 Uiso 1 1 calc R . . C53 C -0.0448(11) 0.4693(5) 0.8114(5) 0.022(2) Uani 1 1 d . . . H53 H -0.1357 0.4978 0.7960 0.027 Uiso 1 1 calc R . . C61 C 0.0742(10) 0.2765(5) 0.7108(4) 0.014(2) Uani 1 1 d . . . C62 C -0.1000(10) 0.2372(5) 0.6117(5) 0.021(2) Uani 1 1 d . . . H62 H -0.1625 0.2272 0.5686 0.026 Uiso 1 1 calc R . . C63 C -0.1133(11) 0.2046(5) 0.6722(5) 0.023(2) Uani 1 1 d . . . H63 H -0.1876 0.1682 0.6745 0.028 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01079(17) 0.0184(2) 0.01203(18) 0.00122(17) -0.00100(13) 0.00274(16) Au2 0.01154(17) 0.0182(2) 0.01042(18) 0.00360(16) -0.00040(13) 0.00023(15) Cl1 0.0219(13) 0.0349(16) 0.0177(12) 0.0021(12) -0.0062(10) 0.0062(11) Cl2 0.0200(12) 0.0234(14) 0.0106(11) 0.0030(10) -0.0012(9) 0.0024(10) Cl3 0.0539(18) 0.0333(18) 0.0250(14) -0.0027(13) 0.0017(13) -0.0042(14) Cl4 0.055(2) 0.0329(19) 0.066(2) -0.0092(17) 0.0248(17) -0.0060(15) S11 0.0256(13) 0.0174(15) 0.0199(13) 0.0017(11) -0.0031(10) -0.0009(11) S21 0.0100(11) 0.0276(16) 0.0213(13) 0.0003(12) -0.0019(9) 0.0000(10) S31 0.0109(11) 0.0231(15) 0.0152(12) 0.0042(11) -0.0021(9) -0.0017(10) S41 0.0121(12) 0.0323(17) 0.0190(13) 0.0071(12) 0.0006(10) 0.0012(11) S51 0.0250(14) 0.0360(18) 0.0169(13) -0.0088(12) -0.0030(10) 0.0026(12) S61 0.0195(12) 0.0175(14) 0.0120(12) 0.0040(10) -0.0052(9) -0.0041(10) P1 0.0075(11) 0.0172(14) 0.0119(12) -0.0002(11) -0.0013(9) -0.0012(10) P2 0.0102(12) 0.0194(15) 0.0112(12) 0.0040(11) -0.0006(9) 0.0004(10) N11 0.025(4) 0.013(5) 0.023(4) 0.011(4) -0.006(4) -0.007(4) N21 0.010(4) 0.018(5) 0.015(4) -0.007(4) 0.007(3) -0.003(3) N31 0.007(4) 0.025(5) 0.016(4) -0.013(4) -0.005(3) 0.003(3) N41 0.007(4) 0.021(5) 0.016(4) 0.002(4) 0.001(3) -0.002(3) N51 0.012(4) 0.030(5) 0.013(4) -0.002(4) 0.000(3) 0.001(4) N61 0.018(4) 0.028(5) 0.017(4) 0.003(4) 0.004(3) -0.004(4) C1 0.038(7) 0.026(7) 0.043(7) -0.005(6) 0.010(6) 0.001(5) C11 0.017(5) 0.016(6) 0.012(5) 0.004(4) 0.001(4) 0.000(4) C12 0.024(5) 0.026(7) 0.017(5) 0.000(5) 0.003(4) -0.002(4) C13 0.029(6) 0.028(7) 0.016(5) 0.006(5) -0.011(4) -0.010(5) C21 0.018(5) 0.015(5) 0.010(5) 0.009(4) 0.002(4) 0.005(4) C22 0.011(5) 0.028(6) 0.019(5) 0.001(5) 0.010(4) 0.010(4) C23 0.019(5) 0.022(6) 0.011(5) 0.003(4) 0.007(4) 0.001(4) C31 0.007(4) 0.017(6) 0.021(5) 0.001(4) 0.005(4) 0.001(4) C32 0.016(5) 0.016(5) 0.016(5) -0.006(4) 0.012(4) 0.000(4) C33 0.011(5) 0.013(5) 0.024(5) -0.008(4) 0.004(4) -0.009(4) C41 0.002(4) 0.012(5) 0.016(5) 0.004(4) -0.002(3) -0.002(3) C42 0.008(4) 0.033(7) 0.020(5) 0.000(5) 0.009(4) -0.002(4) C43 0.010(4) 0.020(6) 0.020(5) 0.009(4) 0.002(4) 0.001(4) C51 0.022(5) 0.018(6) 0.013(5) -0.002(4) 0.007(4) -0.002(4) C52 0.030(6) 0.025(7) 0.029(6) -0.006(5) 0.008(5) -0.005(5) C53 0.014(5) 0.026(6) 0.026(6) 0.006(5) 0.002(4) -0.001(4) C61 0.008(4) 0.022(6) 0.011(5) -0.001(4) 0.001(4) -0.001(4) C62 0.007(4) 0.035(7) 0.020(5) -0.005(5) -0.009(4) 0.004(4) C63 0.011(5) 0.038(7) 0.022(6) -0.008(5) 0.006(4) -0.016(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 P1 2.214(2) . ? Au1 Cl1 2.285(2) . ? Au1 Au2 3.2044(5) . ? Au2 P2 2.212(2) . ? Au2 Cl2 2.275(2) . ? Cl2 S61 3.334(3) 4_666 ? Cl3 C1 1.765(10) . ? Cl4 C1 1.781(10) . ? S11 C12 1.704(9) . ? S11 C11 1.726(9) . ? S21 C22 1.711(9) . ? S21 C21 1.736(9) . ? S31 C32 1.704(9) . ? S31 C31 1.723(9) . ? S41 C42 1.682(9) . ? S41 C41 1.732(8) . ? S51 C52 1.724(11) . ? S51 C51 1.729(9) . ? S61 C62 1.693(10) . ? S61 C61 1.712(9) . ? P1 C11 1.772(9) . ? P1 C21 1.805(9) . ? P1 C31 1.813(9) . ? P2 C41 1.799(8) . ? P2 C61 1.811(9) . ? P2 C51 1.819(10) . ? N11 C11 1.333(10) . ? N11 C13 1.354(12) . ? N21 C21 1.307(10) . ? N21 C23 1.396(10) . ? N31 C31 1.301(10) . ? N31 C33 1.363(11) . ? N41 C41 1.304(10) . ? N41 C43 1.359(10) . ? N51 C51 1.312(11) . ? N51 C53 1.377(12) . ? N61 C61 1.311(11) . ? N61 C63 1.356(11) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C12 C13 1.346(13) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C22 C23 1.338(11) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C32 C33 1.357(12) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C42 C43 1.358(11) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C52 C53 1.332(12) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C62 C63 1.361(12) . ? C62 H62 0.9500 . ? C63 H63 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 168.97(9) . . ? P1 Au1 Au2 100.70(6) . . ? Cl1 Au1 Au2 90.29(6) . . ? P2 Au2 Cl2 174.00(9) . . ? P2 Au2 Au1 97.84(6) . . ? Cl2 Au2 Au1 87.03(6) . . ? Au2 Cl2 S61 143.08(10) . 4_666 ? C12 S11 C11 89.2(5) . . ? C22 S21 C21 88.7(4) . . ? C32 S31 C31 89.1(4) . . ? C42 S41 C41 88.9(4) . . ? C52 S51 C51 88.0(5) . . ? C62 S61 C61 89.0(4) . . ? C11 P1 C21 103.5(4) . . ? C11 P1 C31 106.3(4) . . ? C21 P1 C31 103.0(4) . . ? C11 P1 Au1 121.7(3) . . ? C21 P1 Au1 109.1(3) . . ? C31 P1 Au1 111.5(3) . . ? C41 P2 C61 105.8(4) . . ? C41 P2 C51 102.0(4) . . ? C61 P2 C51 104.4(4) . . ? C41 P2 Au2 113.0(3) . . ? C61 P2 Au2 118.1(3) . . ? C51 P2 Au2 112.0(3) . . ? C11 N11 C13 111.3(8) . . ? C21 N21 C23 109.1(7) . . ? C31 N31 C33 110.9(8) . . ? C41 N41 C43 110.3(7) . . ? C51 N51 C53 108.9(8) . . ? C61 N61 C63 108.3(8) . . ? Cl3 C1 Cl4 110.2(6) . . ? Cl3 C1 H1A 109.6 . . ? Cl4 C1 H1A 109.6 . . ? Cl3 C1 H1B 109.6 . . ? Cl4 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? N11 C11 S11 113.2(7) . . ? N11 C11 P1 123.6(7) . . ? S11 C11 P1 123.2(5) . . ? C13 C12 S11 111.3(8) . . ? C13 C12 H12 124.4 . . ? S11 C12 H12 124.4 . . ? C12 C13 N11 115.0(9) . . ? C12 C13 H13 122.5 . . ? N11 C13 H13 122.5 . . ? N21 C21 S21 115.3(6) . . ? N21 C21 P1 119.8(6) . . ? S21 C21 P1 124.9(5) . . ? C23 C22 S21 110.9(7) . . ? C23 C22 H22 124.6 . . ? S21 C22 H22 124.6 . . ? C22 C23 N21 116.0(8) . . ? C22 C23 H23 122.0 . . ? N21 C23 H23 122.0 . . ? N31 C31 S31 114.5(7) . . ? N31 C31 P1 117.9(7) . . ? S31 C31 P1 126.8(5) . . ? C33 C32 S31 110.3(7) . . ? C33 C32 H32 124.9 . . ? S31 C32 H32 124.9 . . ? C32 C33 N31 115.2(8) . . ? C32 C33 H33 122.4 . . ? N31 C33 H33 122.4 . . ? N41 C41 S41 114.5(6) . . ? N41 C41 P2 124.0(6) . . ? S41 C41 P2 121.6(5) . . ? C43 C42 S41 110.9(7) . . ? C43 C42 H42 124.5 . . ? S41 C42 H42 124.5 . . ? C42 C43 N41 115.4(8) . . ? C42 C43 H43 122.3 . . ? N41 C43 H43 122.3 . . ? N51 C51 S51 115.7(7) . . ? N51 C51 P2 125.0(7) . . ? S51 C51 P2 119.1(5) . . ? C53 C52 S51 110.6(8) . . ? C53 C52 H52 124.7 . . ? S51 C52 H52 124.7 . . ? C52 C53 N51 116.6(9) . . ? C52 C53 H53 121.7 . . ? N51 C53 H53 121.7 . . ? N61 C61 S61 116.1(7) . . ? N61 C61 P2 118.9(7) . . ? S61 C61 P2 124.7(5) . . ? C63 C62 S61 109.6(7) . . ? C63 C62 H62 125.2 . . ? S61 C62 H62 125.2 . . ? N61 C63 C62 117.0(9) . . ? N61 C63 H63 121.5 . . ? C62 C63 H63 121.5 . . ? 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 Au1 Au2 P2 158.66(9) . . . . ? Cl1 Au1 Au2 P2 -22.32(9) . . . . ? P1 Au1 Au2 Cl2 -17.81(9) . . . . ? Cl1 Au1 Au2 Cl2 161.21(9) . . . . ? Au1 Au2 Cl2 S61 159.46(16) . . . 4_666 ? Cl1 Au1 P1 C11 138.6(5) . . . . ? Au2 Au1 P1 C11 -46.6(3) . . . . ? Cl1 Au1 P1 C21 18.4(6) . . . . ? Au2 Au1 P1 C21 -166.8(3) . . . . ? Cl1 Au1 P1 C31 -94.7(6) . . . . ? Au2 Au1 P1 C31 80.1(3) . . . . ? Au1 Au2 P2 C41 -53.4(3) . . . . ? Au1 Au2 P2 C61 70.8(3) . . . . ? Au1 Au2 P2 C51 -167.9(3) . . . . ? C13 N11 C11 S11 0.9(10) . . . . ? C13 N11 C11 P1 -177.2(7) . . . . ? C12 S11 C11 N11 -1.3(7) . . . . ? C12 S11 C11 P1 176.8(6) . . . . ? C21 P1 C11 N11 -79.7(8) . . . . ? C31 P1 C11 N11 28.4(9) . . . . ? Au1 P1 C11 N11 157.4(6) . . . . ? C21 P1 C11 S11 102.3(6) . . . . ? C31 P1 C11 S11 -149.5(5) . . . . ? Au1 P1 C11 S11 -20.5(7) . . . . ? C11 S11 C12 C13 1.4(8) . . . . ? S11 C12 C13 N11 -1.2(11) . . . . ? C11 N11 C13 C12 0.2(12) . . . . ? C23 N21 C21 S21 -0.5(10) . . . . ? C23 N21 C21 P1 -178.7(6) . . . . ? C22 S21 C21 N21 0.6(7) . . . . ? C22 S21 C21 P1 178.6(6) . . . . ? C11 P1 C21 N21 -163.7(7) . . . . ? C31 P1 C21 N21 85.7(8) . . . . ? Au1 P1 C21 N21 -32.9(8) . . . . ? C11 P1 C21 S21 18.3(7) . . . . ? C31 P1 C21 S21 -92.3(6) . . . . ? Au1 P1 C21 S21 149.2(5) . . . . ? C21 S21 C22 C23 -0.5(8) . . . . ? S21 C22 C23 N21 0.3(11) . . . . ? C21 N21 C23 C22 0.1(11) . . . . ? C33 N31 C31 S31 0.1(10) . . . . ? C33 N31 C31 P1 171.1(6) . . . . ? C32 S31 C31 N31 0.9(7) . . . . ? C32 S31 C31 P1 -169.1(6) . . . . ? C11 P1 C31 N31 152.8(7) . . . . ? C21 P1 C31 N31 -98.7(7) . . . . ? Au1 P1 C31 N31 18.1(8) . . . . ? C11 P1 C31 S31 -37.5(7) . . . . ? C21 P1 C31 S31 71.0(7) . . . . ? Au1 P1 C31 S31 -172.2(5) . . . . ? C31 S31 C32 C33 -1.6(7) . . . . ? S31 C32 C33 N31 2.0(10) . . . . ? C31 N31 C33 C32 -1.4(11) . . . . ? C43 N41 C41 S41 -0.5(10) . . . . ? C43 N41 C41 P2 179.3(7) . . . . ? C42 S41 C41 N41 0.0(7) . . . . ? C42 S41 C41 P2 -179.8(6) . . . . ? C61 P2 C41 N41 39.8(9) . . . . ? C51 P2 C41 N41 -69.1(8) . . . . ? Au2 P2 C41 N41 170.5(7) . . . . ? C61 P2 C41 S41 -140.5(6) . . . . ? C51 P2 C41 S41 110.6(6) . . . . ? Au2 P2 C41 S41 -9.7(6) . . . . ? C41 S41 C42 C43 0.5(8) . . . . ? S41 C42 C43 N41 -0.9(11) . . . . ? C41 N41 C43 C42 0.9(12) . . . . ? C53 N51 C51 S51 1.0(10) . . . . ? C53 N51 C51 P2 -174.2(7) . . . . ? C52 S51 C51 N51 -1.8(8) . . . . ? C52 S51 C51 P2 173.8(6) . . . . ? C41 P2 C51 N51 86.6(9) . . . . ? C61 P2 C51 N51 -23.4(9) . . . . ? Au2 P2 C51 N51 -152.4(7) . . . . ? C41 P2 C51 S51 -88.5(6) . . . . ? C61 P2 C51 S51 161.5(5) . . . . ? Au2 P2 C51 S51 32.6(6) . . . . ? C51 S51 C52 C53 2.0(8) . . . . ? S51 C52 C53 N51 -2.0(11) . . . . ? C51 N51 C53 C52 0.7(12) . . . . ? C63 N61 C61 S61 -0.2(10) . . . . ? C63 N61 C61 P2 -175.5(7) . . . . ? C62 S61 C61 N61 0.7(8) . . . . ? C62 S61 C61 P2 175.7(6) . . . . ? C41 P2 C61 N61 155.9(7) . . . . ? C51 P2 C61 N61 -96.9(8) . . . . ? Au2 P2 C61 N61 28.2(9) . . . . ? C41 P2 C61 S61 -18.9(7) . . . . ? C51 P2 C61 S61 88.2(6) . . . . ? Au2 P2 C61 S61 -146.7(5) . . . . ? C61 S61 C62 C63 -1.0(7) . . . . ? C61 N61 C63 C62 -0.6(12) . . . . ? S61 C62 C63 N61 1.2(11) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.663 _refine_diff_density_min -2.172 _refine_diff_density_rms 0.258 #Compound 2bDCM ends #===END ########### ## 2c(i) ## ########### data_Compound2c(i) _database_code_depnum_ccdc_archive 'CCDC 659058' _audit_creation_method SHELXL-97 _chemical_name_systematic chlorido[tris(4-methylthiazol-2-yl)phosphane]gold(I) _chemical_name_common 'tris(4-methylthiazol-2-yl)phosphanegold(I) chloride' _chemical_melting_point 394 _chemical_formula_moiety 'C12 H12 Au Cl N3 P S3' _chemical_formula_sum 'C12 H12 Au Cl N3 P S3' _chemical_formula_weight 557.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_int_tables_number 15 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 23.574(2) _cell_length_b 10.7660(9) _cell_length_c 17.2010(15) _cell_angle_alpha 90.00 _cell_angle_beta 128.280(1) _cell_angle_gamma 90.00 _cell_volume 3426.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5916 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.20 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 9.195 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.179 _exptl_absorpt_correction_T_max 0.399 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _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_% ? _diffrn_reflns_number 9974 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 26.73 _reflns_number_total 3639 _reflns_number_gt 3390 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material X-Seed _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^)+(0.0245P)^2^+1.1125P] 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 3639 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0225 _refine_ls_R_factor_gt 0.0204 _refine_ls_wR_factor_ref 0.0482 _refine_ls_wR_factor_gt 0.0473 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.072085(6) 0.175748(11) 0.268879(8) 0.01444(5) Uani 1 1 d . . . Cl1 Cl 0.03549(4) 0.34490(7) 0.16733(6) 0.02139(17) Uani 1 1 d . . . P1 P 0.12931(4) 0.01727(8) 0.37207(6) 0.01401(16) Uani 1 1 d . . . S11 S 0.28564(4) 0.07997(8) 0.55860(6) 0.01922(17) Uani 1 1 d . . . N11 N 0.25172(13) 0.0289(3) 0.38858(19) 0.0177(6) Uani 1 1 d . . . C11 C 0.22520(16) 0.0353(3) 0.4362(2) 0.0149(6) Uani 1 1 d . . . C12 C 0.35090(16) 0.0900(3) 0.5442(2) 0.0202(7) Uani 1 1 d . . . H12 H 0.3995 0.1137 0.5950 0.024 Uiso 1 1 calc R . . C13 C 0.32410(17) 0.0596(3) 0.4503(2) 0.0193(7) Uani 1 1 d . . . C14 C 0.36535(18) 0.0615(4) 0.4101(3) 0.0267(8) Uani 1 1 d . . . H14A H 0.4157 0.0846 0.4630 0.040 Uiso 1 1 calc R . . H14B H 0.3435 0.1223 0.3562 0.040 Uiso 1 1 calc R . . H14C H 0.3637 -0.0211 0.3848 0.040 Uiso 1 1 calc R . . S21 S 0.08391(5) 0.08568(9) 0.50324(7) 0.0286(2) Uani 1 1 d . . . N21 N 0.16269(13) -0.1006(3) 0.53394(18) 0.0177(6) Uani 1 1 d . . . C21 C 0.12718(16) -0.0074(3) 0.4739(2) 0.0170(6) Uani 1 1 d . . . C22 C 0.1158(2) -0.0074(3) 0.6025(3) 0.0285(8) Uani 1 1 d . . . H22 H 0.1064 0.0052 0.6483 0.034 Uiso 1 1 calc R . . C23 C 0.15654(17) -0.1027(3) 0.6082(2) 0.0202(7) Uani 1 1 d . . . C24 C 0.1906(2) -0.2061(3) 0.6818(3) 0.0256(8) Uani 1 1 d . . . H24A H 0.2044 -0.1763 0.7453 0.038 Uiso 1 1 calc R . . H24B H 0.2337 -0.2353 0.6908 0.038 Uiso 1 1 calc R . . H24C H 0.1561 -0.2747 0.6578 0.038 Uiso 1 1 calc R . . S31 S 0.15238(4) -0.26640(8) 0.36938(6) 0.02248(18) Uani 1 1 d . . . N31 N 0.05298(14) -0.1410(3) 0.21562(19) 0.0161(5) Uani 1 1 d . . . C31 C 0.10709(16) -0.1306(3) 0.3111(2) 0.0161(6) Uani 1 1 d . . . C32 C 0.09560(18) -0.3419(3) 0.2594(2) 0.0204(7) Uani 1 1 d . . . H32 H 0.0981 -0.4281 0.2502 0.025 Uiso 1 1 calc R . . C33 C 0.04587(16) -0.2624(3) 0.1860(2) 0.0159(6) Uani 1 1 d . . . C34 C -0.01261(18) -0.2981(3) 0.0809(2) 0.0213(7) Uani 1 1 d . . . H34A H -0.0097 -0.3873 0.0725 0.032 Uiso 1 1 calc R . . H34B H -0.0068 -0.2515 0.0373 0.032 Uiso 1 1 calc R . . H34C H -0.0598 -0.2789 0.0638 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01189(7) 0.01374(8) 0.01659(7) -0.00007(4) 0.00828(6) 0.00036(4) Cl1 0.0176(4) 0.0173(4) 0.0256(4) 0.0054(3) 0.0116(3) 0.0026(3) P1 0.0130(4) 0.0150(4) 0.0152(4) -0.0009(3) 0.0093(3) -0.0006(3) S11 0.0146(4) 0.0245(5) 0.0162(4) -0.0033(3) 0.0083(3) -0.0025(3) N11 0.0144(13) 0.0216(15) 0.0182(13) 0.0014(11) 0.0106(11) 0.0001(11) C11 0.0143(14) 0.0129(16) 0.0164(14) 0.0003(12) 0.0090(12) 0.0015(12) C12 0.0122(15) 0.0207(18) 0.0239(16) -0.0005(13) 0.0094(14) -0.0012(13) C13 0.0160(16) 0.0162(17) 0.0248(16) 0.0023(13) 0.0122(14) -0.0001(13) C14 0.0211(17) 0.031(2) 0.0332(19) 0.0027(16) 0.0193(16) -0.0006(15) S21 0.0388(5) 0.0272(5) 0.0335(5) 0.0042(4) 0.0293(4) 0.0114(4) N21 0.0175(13) 0.0213(15) 0.0172(13) -0.0020(11) 0.0121(11) -0.0013(11) C21 0.0147(15) 0.0188(17) 0.0204(15) -0.0026(13) 0.0123(13) -0.0024(13) C22 0.044(2) 0.029(2) 0.0304(19) -0.0010(15) 0.0320(18) 0.0015(17) C23 0.0216(17) 0.0208(18) 0.0210(16) -0.0034(13) 0.0147(14) -0.0054(14) C24 0.031(2) 0.026(2) 0.0231(17) 0.0014(15) 0.0183(16) -0.0026(15) S31 0.0233(4) 0.0174(4) 0.0165(4) -0.0001(3) 0.0072(3) 0.0044(3) N31 0.0155(13) 0.0157(14) 0.0175(13) -0.0014(11) 0.0104(11) -0.0017(11) C31 0.0141(15) 0.0174(17) 0.0202(15) 0.0016(13) 0.0123(13) 0.0004(13) C32 0.0231(17) 0.0174(18) 0.0181(16) -0.0043(13) 0.0114(14) 0.0002(13) C33 0.0171(16) 0.0163(17) 0.0201(15) -0.0006(12) 0.0145(13) -0.0007(13) C34 0.0203(17) 0.0208(18) 0.0189(16) -0.0025(13) 0.0101(14) 0.0015(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 Au1 Au1 3.0394(4) 2 ? Au1 Cl1 2.2901(8) . ? Au1 P1 2.2169(8) . ? P1 C11 1.810(3) . ? P1 C21 1.803(3) . ? P1 C31 1.797(3) . ? S11 C11 1.726(3) . ? S11 C12 1.707(3) . ? N11 C11 1.304(4) . ? N11 C13 1.380(4) . ? C12 C13 1.360(5) . ? C12 H12 0.9500 . ? C13 C14 1.502(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? S21 C21 1.714(3) . ? S21 C22 1.702(4) . ? N21 C21 1.305(4) . ? N21 C23 1.372(4) . ? C22 C23 1.367(5) . ? C22 H22 0.9500 . ? C23 C24 1.493(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? S31 C31 1.719(3) . ? S31 C32 1.701(3) . ? N31 C31 1.320(4) . ? N31 C33 1.375(4) . ? C32 C33 1.366(4) . ? C32 H32 0.9500 . ? C33 C34 1.493(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 167.83(3) . . ? Cl1 Au1 Au1 89.66(2) . 2 ? P1 Au1 Au1 102.50(2) . 2 ? C11 P1 Au1 108.42(10) . . ? C21 P1 Au1 121.44(11) . . ? C31 P1 Au1 113.71(11) . . ? C11 P1 C21 101.54(14) . . ? C11 P1 C31 104.67(14) . . ? C31 P1 C21 105.25(14) . . ? S11 C11 P1 123.28(17) . . ? N11 C11 P1 121.0(2) . . ? N11 C11 S11 115.2(2) . . ? N11 C13 C14 119.6(3) . . ? S11 C12 H12 124.5 . . ? C11 S11 C12 88.70(15) . . ? C11 N11 C13 110.5(3) . . ? C12 C13 N11 114.5(3) . . ? C12 C13 C14 125.9(3) . . ? C13 C12 S11 111.1(2) . . ? C13 C12 H12 124.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? S21 C21 P1 125.46(19) . . ? N21 C21 P1 119.4(2) . . ? N21 C21 S21 115.1(2) . . ? N21 C23 C24 119.3(3) . . ? S21 C22 H22 124.2 . . ? C22 S21 C21 88.74(16) . . ? C21 N21 C23 111.3(3) . . ? C22 C23 N21 113.4(3) . . ? C22 C23 C24 127.3(3) . . ? C23 C22 S21 111.5(2) . . ? C23 C22 H22 124.2 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? S31 C31 P1 124.20(18) . . ? N31 C31 P1 120.6(2) . . ? N31 C31 S31 115.2(2) . . ? N31 C33 C34 120.2(3) . . ? S31 C32 H32 124.4 . . ? C32 S31 C31 88.92(16) . . ? C31 N31 C33 110.1(3) . . ? C32 C33 N31 114.5(3) . . ? C32 C33 C34 125.3(3) . . ? C33 C32 S31 111.3(3) . . ? C33 C32 H32 124.4 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? 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 Au1 Au1 P1 C11 -160.13(10) 2 . . . ? Au1 Au1 P1 C21 -43.34(12) 2 . . . ? Au1 Au1 P1 C31 83.90(11) 2 . . . ? Au1 P1 C11 S11 106.26(18) . . . . ? Au1 P1 C11 N11 -65.7(3) . . . . ? Au1 P1 C21 S21 -1.1(3) . . . . ? Au1 P1 C21 N21 -178.8(2) . . . . ? Au1 P1 C31 S31 169.79(15) . . . . ? Au1 P1 C31 N31 -10.3(3) . . . . ? Cl1 Au1 Au1 Cl1 -74.65(4) . . 2 2 ? Cl1 Au1 P1 C11 16.79(19) . . . . ? Cl1 Au1 P1 C21 133.58(17) . . . . ? Cl1 Au1 P1 C31 -99.18(17) . . . . ? S11 C12 C13 N11 0.4(4) . . . . ? S11 C12 C13 C14 178.2(3) . . . . ? S21 C22 C23 N21 0.4(4) . . . . ? S21 C22 C23 C24 -177.0(3) . . . . ? S31 C32 C33 N31 1.0(4) . . . . ? S31 C32 C33 C34 -179.0(3) . . . . ? C11 S11 C12 C13 -0.1(3) . . . . ? C11 P1 C21 S21 119.1(2) . . . . ? C11 P1 C21 N21 -58.6(3) . . . . ? C11 P1 C31 S31 51.6(2) . . . . ? C11 P1 C31 N31 -128.4(2) . . . . ? C11 N11 C13 C12 -0.5(4) . . . . ? C11 N11 C13 C14 -178.5(3) . . . . ? C12 S11 C11 P1 -172.6(2) . . . . ? C12 S11 C11 N11 -0.2(3) . . . . ? C13 N11 C11 P1 173.0(2) . . . . ? C13 N11 C11 S11 0.4(4) . . . . ? C21 S21 C22 C23 -0.2(3) . . . . ? C21 P1 C11 S11 -22.7(2) . . . . ? C21 P1 C11 N11 165.3(3) . . . . ? C21 P1 C31 S31 -55.0(2) . . . . ? C21 P1 C31 N31 125.0(2) . . . . ? C21 N21 C23 C22 -0.5(4) . . . . ? C21 N21 C23 C24 177.2(3) . . . . ? C22 S21 C21 P1 -177.9(2) . . . . ? C22 S21 C21 N21 -0.1(3) . . . . ? C23 N21 C21 S21 0.3(3) . . . . ? C23 N21 C21 P1 178.3(2) . . . . ? C31 S31 C32 C33 -0.6(3) . . . . ? C31 P1 C11 S11 -132.1(2) . . . . ? C31 P1 C11 N11 56.0(3) . . . . ? C31 P1 C21 S21 -132.0(2) . . . . ? C31 P1 C21 N21 50.3(3) . . . . ? C31 N31 C33 C32 -1.0(4) . . . . ? C31 N31 C33 C34 179.1(3) . . . . ? C32 S31 C31 P1 180.0(2) . . . . ? C32 S31 C31 N31 0.0(3) . . . . ? C33 N31 C31 S31 0.5(3) . . . . ? C33 N31 C31 P1 -179.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.039 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.118 #Compound 2c(i) ends #===END ############ ## 2c(ii) ## ############ data_Compound2c(ii) _database_code_depnum_ccdc_archive 'CCDC 659059' _audit_creation_method SHELXL-97 _chemical_name_systematic chloridotris(4-methylthiazol-2-yl)phosphanegold(I) _chemical_name_common 'tris(4-methylthiazol-2-yl)phosphinegold(I) chloride' _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 Au Cl N3 P S3' _chemical_formula_sum 'C12 H12 Au Cl N3 P S3' _chemical_formula_weight 557.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_int_tables_number 14 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 19.8224(19) _cell_length_b 10.333(1) _cell_length_c 17.5435(17) _cell_angle_alpha 90.00 _cell_angle_beta 109.950(1) _cell_angle_gamma 90.00 _cell_volume 3377.7(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9733 _cell_measurement_theta_min 2.326 _cell_measurement_theta_max 26.452 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.96 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 9.329 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.036 _exptl_absorpt_correction_T_max 0.142 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area detector' _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_% ? _diffrn_reflns_number 35125 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 26.46 _reflns_number_total 6921 _reflns_number_gt 6630 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material X-Seed _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^)+(0.0000P)^2^+19.6917P] 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 6921 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.170 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au -0.077361(9) 0.221203(16) 0.397308(10) 0.01057(5) Uani 1 1 d . . . Cl1 Cl -0.19837(6) 0.20272(11) 0.33350(7) 0.0175(2) Uani 1 1 d . . . P1 P 0.04007(6) 0.23372(11) 0.46020(7) 0.0093(2) Uani 1 1 d . . . Au2 Au 0.428068(9) 0.786271(16) 0.549392(10) 0.01025(5) Uani 1 1 d . . . Cl2 Cl 0.30729(6) 0.80950(12) 0.51702(7) 0.0179(2) Uani 1 1 d . . . P2 P 0.54443(6) 0.76465(11) 0.57305(7) 0.0090(2) Uani 1 1 d . . . S11 S 0.00111(6) 0.16848(12) 0.60928(7) 0.0144(2) Uani 1 1 d . . . N11 N 0.1321(2) 0.1888(4) 0.6162(2) 0.0139(8) Uani 1 1 d . . . C11 C 0.0657(2) 0.1965(4) 0.5663(3) 0.0110(9) Uani 1 1 d . . . C12 C 0.0671(3) 0.1466(5) 0.7004(3) 0.0157(9) Uani 1 1 d . . . H12 H 0.0591 0.1274 0.7496 0.019 Uiso 1 1 calc R . . C13 C 0.1333(3) 0.1603(4) 0.6934(3) 0.0141(9) Uani 1 1 d . . . C14 C 0.2039(3) 0.1501(5) 0.7610(3) 0.0205(11) Uani 1 1 d . . . H14A H 0.1956 0.1435 0.8128 0.031 Uiso 1 1 calc R . . H14B H 0.2328 0.2272 0.7613 0.031 Uiso 1 1 calc R . . H14C H 0.2294 0.0729 0.7530 0.031 Uiso 1 1 calc R . . S21 S 0.14003(7) 0.46729(12) 0.54107(7) 0.0203(3) Uani 1 1 d . . . N21 N 0.0750(2) 0.4436(4) 0.3882(2) 0.0128(8) Uani 1 1 d . . . C21 C 0.0834(2) 0.3869(4) 0.4576(3) 0.0105(9) Uani 1 1 d . . . C22 C 0.1530(3) 0.5832(5) 0.4780(3) 0.0201(10) Uani 1 1 d . . . H22 H 0.1827 0.6571 0.4957 0.024 Uiso 1 1 calc R . . C23 C 0.1148(3) 0.5554(4) 0.3988(3) 0.0140(9) Uani 1 1 d . . . C24 C 0.1138(3) 0.6332(5) 0.3259(3) 0.0212(11) Uani 1 1 d . . . H24A H 0.1449 0.5918 0.3000 0.032 Uiso 1 1 calc R . . H24B H 0.1312 0.7209 0.3430 0.032 Uiso 1 1 calc R . . H24C H 0.0646 0.6374 0.2873 0.032 Uiso 1 1 calc R . . S31 S 0.16114(6) 0.03114(11) 0.47474(7) 0.0148(2) Uani 1 1 d . . . N31 N 0.0704(2) 0.1126(4) 0.3399(2) 0.0118(8) Uani 1 1 d . . . C31 C 0.0891(2) 0.1233(4) 0.4190(3) 0.0116(9) Uani 1 1 d . . . C32 C 0.1667(3) -0.0263(4) 0.3855(3) 0.0148(9) Uani 1 1 d . . . H32 H 0.2012 -0.0876 0.3819 0.018 Uiso 1 1 calc R . . C33 C 0.1155(2) 0.0271(4) 0.3204(3) 0.0135(9) Uani 1 1 d . . . C34 C 0.1051(3) 0.0003(5) 0.2339(3) 0.0193(10) Uani 1 1 d . . . H34A H 0.1375 -0.0694 0.2305 0.029 Uiso 1 1 calc R . . H34B H 0.1156 0.0785 0.2085 0.029 Uiso 1 1 calc R . . H34C H 0.0553 -0.0261 0.2056 0.029 Uiso 1 1 calc R . . S41 S 0.49601(6) 0.85074(12) 0.39788(7) 0.0150(2) Uani 1 1 d . . . N41 N 0.6280(2) 0.7943(4) 0.4751(2) 0.0132(8) Uani 1 1 d . . . C41 C 0.5644(2) 0.8010(4) 0.4830(3) 0.0107(9) Uani 1 1 d . . . C42 C 0.5557(3) 0.8609(5) 0.3477(3) 0.0152(9) Uani 1 1 d . . . H42 H 0.5438 0.8861 0.2926 0.018 Uiso 1 1 calc R . . C43 C 0.6228(2) 0.8279(4) 0.3975(3) 0.0116(9) Uani 1 1 d . . . C44 C 0.6883(3) 0.8276(5) 0.3728(3) 0.0203(11) Uani 1 1 d . . . H44A H 0.7146 0.9088 0.3899 0.030 Uiso 1 1 calc R . . H44B H 0.6737 0.8192 0.3138 0.030 Uiso 1 1 calc R . . H44C H 0.7192 0.7546 0.3987 0.030 Uiso 1 1 calc R . . S51 S 0.63574(7) 0.52044(11) 0.56353(7) 0.0163(2) Uani 1 1 d . . . N51 N 0.5724(2) 0.5514(4) 0.6681(2) 0.0125(8) Uani 1 1 d . . . C51 C 0.5825(2) 0.6064(4) 0.6053(3) 0.0117(9) Uani 1 1 d . . . C52 C 0.6446(3) 0.4033(5) 0.6350(3) 0.0163(10) Uani 1 1 d . . . H52 H 0.6713 0.3257 0.6388 0.020 Uiso 1 1 calc R . . C53 C 0.6086(2) 0.4356(4) 0.6858(3) 0.0136(9) Uani 1 1 d . . . C54 C 0.6050(3) 0.3591(5) 0.7569(3) 0.0176(10) Uani 1 1 d . . . H54A H 0.6358 0.3997 0.8072 0.026 Uiso 1 1 calc R . . H54B H 0.6216 0.2706 0.7537 0.026 Uiso 1 1 calc R . . H54C H 0.5554 0.3570 0.7562 0.026 Uiso 1 1 calc R . . S61 S 0.67422(6) 0.95096(12) 0.64486(8) 0.0172(2) Uani 1 1 d . . . N61 N 0.5843(2) 0.8935(4) 0.7158(2) 0.0136(8) Uani 1 1 d . . . C61 C 0.6001(2) 0.8714(4) 0.6509(3) 0.0104(9) Uani 1 1 d . . . C62 C 0.6858(3) 1.0178(5) 0.7377(3) 0.0176(10) Uani 1 1 d . . . H62 H 0.7235 1.0755 0.7654 0.021 Uiso 1 1 calc R . . C63 C 0.6333(3) 0.9769(4) 0.7666(3) 0.0154(10) Uani 1 1 d . . . C64 C 0.6266(3) 1.0155(5) 0.8454(3) 0.0251(12) Uani 1 1 d . . . H64A H 0.6337 0.9395 0.8806 0.038 Uiso 1 1 calc R . . H64B H 0.5787 1.0516 0.8359 0.038 Uiso 1 1 calc R . . H64C H 0.6630 1.0808 0.8714 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.00877(9) 0.01002(9) 0.01146(9) 0.00064(6) 0.00158(7) 0.00015(6) Cl1 0.0102(5) 0.0197(6) 0.0196(6) 0.0003(4) 0.0012(4) 0.0001(4) P1 0.0101(5) 0.0082(5) 0.0087(5) 0.0006(4) 0.0022(4) -0.0007(4) Au2 0.00827(9) 0.01018(9) 0.01117(9) 0.00089(6) 0.00184(7) 0.00013(6) Cl2 0.0087(5) 0.0232(6) 0.0204(6) 0.0044(5) 0.0032(4) 0.0023(4) P2 0.0083(5) 0.0088(5) 0.0084(5) 0.0010(4) 0.0009(4) -0.0001(4) S11 0.0111(5) 0.0189(6) 0.0131(5) 0.0024(4) 0.0040(4) -0.0016(4) N11 0.014(2) 0.0126(19) 0.0123(19) 0.0001(15) 0.0012(16) -0.0022(15) C11 0.012(2) 0.008(2) 0.013(2) -0.0018(17) 0.0048(18) -0.0014(17) C12 0.018(2) 0.017(2) 0.011(2) 0.0024(18) 0.0039(19) -0.0015(19) C13 0.015(2) 0.010(2) 0.015(2) 0.0017(17) 0.0030(19) -0.0003(18) C14 0.016(2) 0.027(3) 0.014(2) 0.004(2) -0.0001(19) -0.001(2) S21 0.0286(7) 0.0158(6) 0.0126(6) -0.0019(5) 0.0019(5) -0.0100(5) N21 0.017(2) 0.0102(19) 0.0122(19) 0.0004(15) 0.0062(16) -0.0014(15) C21 0.009(2) 0.009(2) 0.015(2) -0.0009(17) 0.0054(17) 0.0000(16) C22 0.027(3) 0.012(2) 0.021(3) -0.0027(19) 0.009(2) -0.007(2) C23 0.020(2) 0.008(2) 0.016(2) -0.0007(17) 0.0088(19) -0.0003(18) C24 0.036(3) 0.009(2) 0.022(3) -0.0005(19) 0.015(2) -0.005(2) S31 0.0114(5) 0.0146(6) 0.0139(5) -0.0012(4) -0.0016(4) 0.0021(4) N31 0.0145(19) 0.0087(18) 0.0122(18) -0.0006(14) 0.0045(15) -0.0007(15) C31 0.011(2) 0.010(2) 0.014(2) -0.0033(17) 0.0030(18) -0.0032(17) C32 0.015(2) 0.009(2) 0.022(2) -0.0048(18) 0.0075(19) -0.0024(18) C33 0.013(2) 0.010(2) 0.018(2) 0.0001(18) 0.0045(19) -0.0010(17) C34 0.023(3) 0.016(2) 0.019(2) -0.0017(19) 0.007(2) 0.003(2) S41 0.0107(5) 0.0202(6) 0.0127(5) 0.0053(4) 0.0020(4) 0.0024(4) N41 0.012(2) 0.013(2) 0.0139(19) 0.0002(15) 0.0046(16) 0.0014(15) C41 0.013(2) 0.007(2) 0.011(2) 0.0005(16) 0.0032(18) 0.0010(16) C42 0.015(2) 0.020(2) 0.011(2) 0.0000(18) 0.0039(18) -0.0013(19) C43 0.014(2) 0.010(2) 0.012(2) -0.0016(17) 0.0039(18) 0.0000(17) C44 0.015(2) 0.028(3) 0.016(2) -0.003(2) 0.004(2) -0.006(2) S51 0.0217(6) 0.0136(6) 0.0163(6) 0.0011(4) 0.0100(5) 0.0043(5) N51 0.0133(19) 0.0093(18) 0.0139(19) -0.0004(15) 0.0031(16) 0.0006(15) C51 0.011(2) 0.008(2) 0.013(2) -0.0031(16) -0.0003(17) -0.0003(16) C52 0.020(2) 0.012(2) 0.016(2) 0.0012(18) 0.0042(19) 0.0036(19) C53 0.014(2) 0.011(2) 0.013(2) -0.0014(17) 0.0013(18) -0.0019(17) C54 0.025(3) 0.010(2) 0.016(2) 0.0021(18) 0.004(2) 0.0002(19) S61 0.0129(6) 0.0162(6) 0.0229(6) -0.0038(5) 0.0065(5) -0.0043(4) N61 0.018(2) 0.0102(19) 0.0107(18) 0.0010(15) 0.0023(16) 0.0000(15) C61 0.011(2) 0.008(2) 0.011(2) 0.0054(16) 0.0006(17) -0.0004(16) C62 0.015(2) 0.011(2) 0.022(2) -0.0065(19) -0.0011(19) -0.0023(18) C63 0.018(2) 0.009(2) 0.015(2) 0.0006(17) -0.0006(19) 0.0022(18) C64 0.037(3) 0.020(3) 0.016(2) -0.001(2) 0.004(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.2137(12) . ? Au1 Cl1 2.2828(12) . ? P1 C11 1.796(5) . ? P1 C31 1.803(5) . ? P1 C21 1.809(5) . ? Au2 P2 2.2112(12) . ? Au2 Cl2 2.2769(11) . ? P2 C41 1.795(5) . ? P2 C61 1.808(5) . ? P2 C51 1.809(5) . ? S11 C12 1.701(5) . ? S11 C11 1.717(5) . ? N11 C11 1.311(6) . ? N11 C13 1.378(6) . ? C12 C13 1.366(7) . ? C12 H12 0.9500 . ? C13 C14 1.497(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? S21 C22 1.708(5) . ? S21 C21 1.724(5) . ? N21 C21 1.311(6) . ? N21 C23 1.376(6) . ? C22 C23 1.368(7) . ? C22 H22 0.9500 . ? C23 C24 1.505(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? S31 C32 1.713(5) . ? S31 C31 1.717(5) . ? N31 C31 1.312(6) . ? N31 C33 1.381(6) . ? C32 C33 1.360(7) . ? C32 H32 0.9500 . ? C33 C34 1.486(6) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? S41 C42 1.701(5) . ? S41 C41 1.718(5) . ? N41 C41 1.316(6) . ? N41 C43 1.374(6) . ? C42 C43 1.363(7) . ? C42 H42 0.9500 . ? C43 C44 1.502(6) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? S51 C52 1.708(5) . ? S51 C51 1.723(5) . ? N51 C51 1.313(6) . ? N51 C53 1.375(6) . ? C52 C53 1.361(7) . ? C52 H52 0.9500 . ? C53 C54 1.498(6) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? S61 C62 1.710(5) . ? S61 C61 1.718(5) . ? N61 C61 1.301(6) . ? N61 C63 1.374(6) . ? C62 C63 1.371(7) . ? C62 H62 0.9500 . ? C63 C64 1.487(7) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 178.49(4) . . ? C11 P1 C31 106.3(2) . . ? C11 P1 C21 104.1(2) . . ? C31 P1 C21 102.6(2) . . ? C11 P1 Au1 112.41(15) . . ? C31 P1 Au1 112.49(15) . . ? C21 P1 Au1 117.79(15) . . ? P2 Au2 Cl2 176.59(4) . . ? C41 P2 C61 106.0(2) . . ? C41 P2 C51 105.7(2) . . ? C61 P2 C51 103.5(2) . . ? C41 P2 Au2 110.05(15) . . ? C61 P2 Au2 114.14(15) . . ? C51 P2 Au2 116.55(15) . . ? C12 S11 C11 89.2(2) . . ? C11 N11 C13 110.3(4) . . ? N11 C11 S11 115.2(3) . . ? N11 C11 P1 124.7(4) . . ? S11 C11 P1 120.1(3) . . ? C13 C12 S11 110.8(3) . . ? C13 C12 H12 124.6 . . ? S11 C12 H12 124.6 . . ? C12 C13 N11 114.6(4) . . ? C12 C13 C14 126.0(4) . . ? N11 C13 C14 119.5(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C22 S21 C21 89.2(2) . . ? C21 N21 C23 111.3(4) . . ? N21 C21 S21 114.5(3) . . ? N21 C21 P1 120.2(3) . . ? S21 C21 P1 125.3(3) . . ? C23 C22 S21 111.0(4) . . ? C23 C22 H22 124.5 . . ? S21 C22 H22 124.5 . . ? C22 C23 N21 114.0(4) . . ? C22 C23 C24 126.4(4) . . ? N21 C23 C24 119.5(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C32 S31 C31 88.4(2) . . ? C31 N31 C33 110.0(4) . . ? N31 C31 S31 115.9(3) . . ? N31 C31 P1 118.7(3) . . ? S31 C31 P1 125.4(3) . . ? C33 C32 S31 111.4(4) . . ? C33 C32 H32 124.3 . . ? S31 C32 H32 124.3 . . ? C32 C33 N31 114.3(4) . . ? C32 C33 C34 125.9(4) . . ? N31 C33 C34 119.8(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C42 S41 C41 89.2(2) . . ? C41 N41 C43 109.9(4) . . ? N41 C41 S41 115.1(3) . . ? N41 C41 P2 126.0(3) . . ? S41 C41 P2 118.8(3) . . ? C43 C42 S41 110.6(3) . . ? C43 C42 H42 124.7 . . ? S41 C42 H42 124.7 . . ? C42 C43 N41 115.1(4) . . ? C42 C43 C44 124.5(4) . . ? N41 C43 C44 120.4(4) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C52 S51 C51 88.7(2) . . ? C51 N51 C53 110.4(4) . . ? N51 C51 S51 115.1(3) . . ? N51 C51 P2 119.1(3) . . ? S51 C51 P2 125.7(3) . . ? C53 C52 S51 111.2(4) . . ? C53 C52 H52 124.4 . . ? S51 C52 H52 124.4 . . ? C52 C53 N51 114.5(4) . . ? C52 C53 C54 126.9(4) . . ? N51 C53 C54 118.6(4) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C62 S61 C61 88.6(2) . . ? C61 N61 C63 110.5(4) . . ? N61 C61 S61 115.8(3) . . ? N61 C61 P2 120.1(3) . . ? S61 C61 P2 124.1(3) . . ? C63 C62 S61 110.8(4) . . ? C63 C62 H62 124.6 . . ? S61 C62 H62 124.6 . . ? C62 C63 N61 114.3(4) . . ? C62 C63 C64 125.5(4) . . ? N61 C63 C64 120.2(4) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? 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 C13 N11 C11 S11 -0.6(5) . . . . ? C13 N11 C11 P1 179.2(3) . . . . ? C12 S11 C11 N11 0.7(4) . . . . ? C12 S11 C11 P1 -179.2(3) . . . . ? C31 P1 C11 N11 51.9(4) . . . . ? C21 P1 C11 N11 -56.0(4) . . . . ? Au1 P1 C11 N11 175.4(3) . . . . ? C31 P1 C11 S11 -128.2(3) . . . . ? C21 P1 C11 S11 123.9(3) . . . . ? Au1 P1 C11 S11 -4.8(3) . . . . ? C11 S11 C12 C13 -0.5(4) . . . . ? S11 C12 C13 N11 0.3(5) . . . . ? S11 C12 C13 C14 178.9(4) . . . . ? C11 N11 C13 C12 0.2(6) . . . . ? C11 N11 C13 C14 -178.5(4) . . . . ? C23 N21 C21 S21 0.6(5) . . . . ? C23 N21 C21 P1 -177.1(3) . . . . ? C22 S21 C21 N21 -0.2(4) . . . . ? C22 S21 C21 P1 177.3(3) . . . . ? C11 P1 C21 N21 -179.1(4) . . . . ? C31 P1 C21 N21 70.2(4) . . . . ? Au1 P1 C21 N21 -53.9(4) . . . . ? C11 P1 C21 S21 3.4(3) . . . . ? C31 P1 C21 S21 -107.2(3) . . . . ? Au1 P1 C21 S21 128.7(2) . . . . ? C21 S21 C22 C23 -0.2(4) . . . . ? S21 C22 C23 N21 0.6(6) . . . . ? S21 C22 C23 C24 -178.7(4) . . . . ? C21 N21 C23 C22 -0.8(6) . . . . ? C21 N21 C23 C24 178.6(4) . . . . ? C33 N31 C31 S31 -0.6(5) . . . . ? C33 N31 C31 P1 178.0(3) . . . . ? C32 S31 C31 N31 0.1(4) . . . . ? C32 S31 C31 P1 -178.5(3) . . . . ? C11 P1 C31 N31 167.1(4) . . . . ? C21 P1 C31 N31 -83.9(4) . . . . ? Au1 P1 C31 N31 43.7(4) . . . . ? C11 P1 C31 S31 -14.4(4) . . . . ? C21 P1 C31 S31 94.6(3) . . . . ? Au1 P1 C31 S31 -137.8(2) . . . . ? C31 S31 C32 C33 0.5(4) . . . . ? S31 C32 C33 N31 -1.0(5) . . . . ? S31 C32 C33 C34 179.5(4) . . . . ? C31 N31 C33 C32 1.0(6) . . . . ? C31 N31 C33 C34 -179.4(4) . . . . ? C43 N41 C41 S41 -1.1(5) . . . . ? C43 N41 C41 P2 179.5(3) . . . . ? C42 S41 C41 N41 1.0(4) . . . . ? C42 S41 C41 P2 -179.5(3) . . . . ? C61 P2 C41 N41 58.1(4) . . . . ? C51 P2 C41 N41 -51.4(4) . . . . ? Au2 P2 C41 N41 -178.0(4) . . . . ? C61 P2 C41 S41 -121.3(3) . . . . ? C51 P2 C41 S41 129.2(3) . . . . ? Au2 P2 C41 S41 2.6(3) . . . . ? C41 S41 C42 C43 -0.6(4) . . . . ? S41 C42 C43 N41 0.1(5) . . . . ? S41 C42 C43 C44 -179.4(4) . . . . ? C41 N41 C43 C42 0.6(6) . . . . ? C41 N41 C43 C44 -179.8(4) . . . . ? C53 N51 C51 S51 0.5(5) . . . . ? C53 N51 C51 P2 -176.7(3) . . . . ? C52 S51 C51 N51 0.2(4) . . . . ? C52 S51 C51 P2 177.1(3) . . . . ? C41 P2 C51 N51 -176.2(4) . . . . ? C61 P2 C51 N51 72.6(4) . . . . ? Au2 P2 C51 N51 -53.6(4) . . . . ? C41 P2 C51 S51 7.0(4) . . . . ? C61 P2 C51 S51 -104.3(3) . . . . ? Au2 P2 C51 S51 129.6(2) . . . . ? C51 S51 C52 C53 -0.8(4) . . . . ? S51 C52 C53 N51 1.2(5) . . . . ? S51 C52 C53 C54 -178.6(4) . . . . ? C51 N51 C53 C52 -1.1(6) . . . . ? C51 N51 C53 C54 178.7(4) . . . . ? C63 N61 C61 S61 -0.9(5) . . . . ? C63 N61 C61 P2 -179.9(3) . . . . ? C62 S61 C61 N61 0.8(4) . . . . ? C62 S61 C61 P2 179.8(3) . . . . ? C41 P2 C61 N61 161.2(4) . . . . ? C51 P2 C61 N61 -87.7(4) . . . . ? Au2 P2 C61 N61 39.9(4) . . . . ? C41 P2 C61 S61 -17.7(3) . . . . ? C51 P2 C61 S61 93.3(3) . . . . ? Au2 P2 C61 S61 -139.0(2) . . . . ? C61 S61 C62 C63 -0.4(4) . . . . ? S61 C62 C63 N61 0.0(5) . . . . ? S61 C62 C63 C64 180.0(4) . . . . ? C61 N61 C63 C62 0.6(6) . . . . ? C61 N61 C63 C64 -179.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.46 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.029 _refine_diff_density_min -1.001 _refine_diff_density_rms 0.142 #Compound 2c(ii) ends #===END ############## ## 2c . thf ## ############## data_compound2cTHF _database_code_depnum_ccdc_archive 'CCDC 659060' _audit_creation_method SHELXL-97 _chemical_name_systematic ;chlorido[tris(4-methylthiazol-2-yl)phosphane]gold(I) tetrahydrofuran solvate ; _chemical_name_common ;tris(4-methylthiazol-2-yl)phosphanegold(I) chloride tetrahydrofuran solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 Au Cl N3 P S3, C4 H8 O' _chemical_formula_sum 'C16 H20 Au Cl N3 O P S3' _chemical_formula_weight 629.94 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_int_tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.0405(9) _cell_length_b 9.6531(10) _cell_length_c 24.273(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2118.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6075 _cell_measurement_theta_min 2.271 _cell_measurement_theta_max 26.711 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.975 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 7.454 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.655 _exptl_absorpt_correction_T_max 0.925 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _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_% ? _diffrn_reflns_number 12563 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 26.73 _reflns_number_total 4472 _reflns_number_gt 4210 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material X-Seed _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881; 1897 Friedel Pairs' _refine_ls_abs_structure_Flack 0.015(5) _refine_ls_number_reflns 4472 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0495 _refine_ls_wR_factor_gt 0.0489 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.906 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.62623(2) 0.225946(17) 0.097583(7) 0.01331(5) Uani 1 1 d . . . Cl1 Cl 0.77529(14) 0.03668(12) 0.09590(6) 0.0232(3) Uani 1 1 d . . . P1 P 0.48182(13) 0.41066(12) 0.10091(6) 0.0122(2) Uani 1 1 d . . . S11 S 0.32186(15) 0.59806(15) 0.18691(5) 0.0249(3) Uani 1 1 d . . . S21 S 0.59065(14) 0.71540(13) 0.08374(5) 0.0197(3) Uani 1 1 d . . . S31 S 0.24357(13) 0.21594(14) 0.05473(5) 0.0162(2) Uani 1 1 d . . . N11 N 0.5468(5) 0.4449(4) 0.20876(16) 0.0163(9) Uani 1 1 d . . . N21 N 0.5720(5) 0.5338(4) 0.00715(15) 0.0142(9) Uani 1 1 d . . . N31 N 0.1914(5) 0.4692(4) 0.07912(16) 0.0167(10) Uani 1 1 d . . . C11 C 0.4575(5) 0.4804(5) 0.16925(18) 0.0135(10) Uani 1 1 d . . . C12 C 0.3927(7) 0.6015(5) 0.25193(19) 0.0241(12) Uani 1 1 d . . . H12 H 0.3551 0.6575 0.2809 0.029 Uiso 1 1 calc R . . C13 C 0.5103(6) 0.5137(5) 0.2572(2) 0.0160(11) Uani 1 1 d . . . C14 C 0.5954(6) 0.4841(5) 0.3084(2) 0.0254(13) Uani 1 1 d . . . H14A H 0.6067 0.5697 0.3297 0.038 Uiso 1 1 calc R . . H14B H 0.6932 0.4479 0.2987 0.038 Uiso 1 1 calc R . . H14C H 0.5421 0.4154 0.3306 0.038 Uiso 1 1 calc R . . C21 C 0.5454(5) 0.5533(5) 0.05887(19) 0.0123(10) Uani 1 1 d . . . C22 C 0.6479(5) 0.7593(5) 0.01884(19) 0.0199(11) Uani 1 1 d . . . H22 H 0.6878 0.8469 0.0091 0.024 Uiso 1 1 calc R . . C23 C 0.6288(6) 0.6522(5) -0.01692(19) 0.0180(10) Uani 1 1 d . . . C24 C 0.6684(6) 0.6508(5) -0.07698(19) 0.0242(13) Uani 1 1 d . . . H24A H 0.6840 0.7460 -0.0898 0.036 Uiso 1 1 calc R . . H24B H 0.5878 0.6084 -0.0981 0.036 Uiso 1 1 calc R . . H24C H 0.7593 0.5971 -0.0823 0.036 Uiso 1 1 calc R . . C31 C 0.2968(5) 0.3773(5) 0.07678(19) 0.0129(10) Uani 1 1 d . . . C32 C 0.0667(5) 0.2756(5) 0.04894(18) 0.0160(10) Uani 1 1 d . . . H32 H -0.0151 0.2212 0.0373 0.019 Uiso 1 1 calc R . . C33 C 0.0588(6) 0.4119(5) 0.06331(19) 0.0156(11) Uani 1 1 d . . . C34 C -0.0786(6) 0.4972(5) 0.0654(2) 0.0252(13) Uani 1 1 d . . . H34A H -0.0947 0.5297 0.1032 0.038 Uiso 1 1 calc R . . H34B H -0.1631 0.4409 0.0537 0.038 Uiso 1 1 calc R . . H34C H -0.0681 0.5770 0.0408 0.038 Uiso 1 1 calc R . . O1 O -0.0833(5) 0.3090(5) 0.26802(17) 0.0505(13) Uani 1 1 d . . . C2 C 0.0469(6) 0.2781(7) 0.2983(2) 0.0371(14) Uani 1 1 d . . . H2A H 0.0256 0.2066 0.3264 0.045 Uiso 1 1 calc R . . H2B H 0.0830 0.3624 0.3173 0.045 Uiso 1 1 calc R . . C3 C 0.1617(7) 0.2265(7) 0.2591(2) 0.0445(16) Uani 1 1 d . . . H3A H 0.1950 0.1322 0.2692 0.053 Uiso 1 1 calc R . . H3B H 0.2484 0.2892 0.2582 0.053 Uiso 1 1 calc R . . C4 C 0.0803(7) 0.2261(7) 0.2036(2) 0.0501(18) Uani 1 1 d . . . H4A H 0.0410 0.1329 0.1949 0.060 Uiso 1 1 calc R . . H4B H 0.1464 0.2564 0.1734 0.060 Uiso 1 1 calc R . . C5 C -0.0410(7) 0.3267(7) 0.2124(2) 0.0403(16) Uani 1 1 d . . . H5A H -0.1249 0.3072 0.1874 0.048 Uiso 1 1 calc R . . H5B H -0.0062 0.4225 0.2058 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01183(8) 0.01349(8) 0.01460(8) 0.00055(7) 0.00052(9) 0.00084(8) Cl1 0.0202(6) 0.0163(6) 0.0331(7) -0.0006(6) 0.0004(7) 0.0042(5) P1 0.0104(6) 0.0138(6) 0.0125(6) 0.0002(5) 0.0000(6) 0.0008(5) S11 0.0255(8) 0.0324(8) 0.0169(7) -0.0038(5) -0.0023(6) 0.0148(6) S21 0.0234(7) 0.0150(6) 0.0207(6) -0.0018(5) 0.0021(5) -0.0018(5) S31 0.0137(6) 0.0166(6) 0.0182(6) -0.0027(5) 0.0023(5) -0.0020(6) N11 0.017(2) 0.016(2) 0.015(2) 0.0018(17) 0.0009(19) -0.0022(18) N21 0.014(2) 0.015(2) 0.014(2) 0.0003(16) 0.0000(17) -0.0013(17) N31 0.017(2) 0.018(2) 0.016(2) -0.0004(17) -0.0032(18) -0.0010(18) C11 0.012(3) 0.017(3) 0.011(2) -0.0004(18) 0.000(2) -0.001(2) C12 0.029(3) 0.028(3) 0.016(3) 0.000(2) 0.002(3) 0.006(3) C13 0.017(3) 0.015(3) 0.016(3) 0.000(2) -0.001(2) -0.004(2) C14 0.023(3) 0.034(3) 0.019(3) 0.001(2) -0.002(2) 0.004(2) C21 0.007(2) 0.014(2) 0.016(3) -0.0003(19) -0.002(2) -0.001(2) C22 0.020(3) 0.018(3) 0.022(2) 0.0025(19) 0.002(2) 0.000(2) C23 0.015(2) 0.024(3) 0.014(2) 0.0025(18) -0.001(3) 0.001(3) C24 0.031(3) 0.022(3) 0.019(3) 0.004(2) 0.002(2) -0.008(2) C31 0.014(3) 0.016(3) 0.009(2) 0.0032(18) 0.001(2) 0.002(2) C32 0.011(2) 0.022(2) 0.015(2) -0.001(2) -0.0020(19) -0.002(2) C33 0.015(3) 0.021(3) 0.011(3) 0.001(2) -0.003(2) -0.002(2) C34 0.015(3) 0.022(3) 0.038(3) 0.001(2) -0.003(3) 0.002(2) O1 0.030(3) 0.082(4) 0.040(3) 0.013(2) 0.006(2) 0.011(2) C2 0.037(3) 0.048(4) 0.027(3) -0.006(3) -0.002(3) -0.001(3) C3 0.033(4) 0.058(4) 0.042(4) -0.002(3) 0.002(3) 0.004(3) C4 0.060(5) 0.069(5) 0.021(3) -0.001(3) 0.004(3) 0.009(4) C5 0.035(4) 0.057(4) 0.029(3) 0.011(3) -0.005(3) -0.004(3) _geom_special_details ;All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 Cl1 2.2706(12) . ? Au1 P1 2.2114(12) . ? Cl1 S21 3.5344(18) 1_545 ? P1 C11 1.804(5) . ? P1 C21 1.807(5) . ? P1 C31 1.801(5) . ? S11 C11 1.725(5) . ? S11 C12 1.704(5) . ? S21 C21 1.727(5) . ? S21 C22 1.711(5) . ? S31 C31 1.716(5) . ? S31 C32 1.705(5) . ? N11 C11 1.300(6) . ? N11 C13 1.390(6) . ? N21 C21 1.292(6) . ? N21 C23 1.382(6) . ? N31 C31 1.303(6) . ? N31 C33 1.376(6) . ? C12 C13 1.366(7) . ? C12 H12 0.9500 . ? C13 C14 1.490(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C22 C23 1.361(6) . ? C22 H22 0.9500 . ? C23 C24 1.501(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C32 C33 1.363(7) . ? C32 H32 0.9500 . ? C33 C34 1.491(7) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O1 C2 1.419(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O1 C5 1.413(7) . ? C2 C3 1.493(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.535(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C5 1.480(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Au1 P1 178.92(6) . . ? Au1 Cl1 S21 115.29(5) . 1_545 ? C11 P1 Au1 114.01(16) . . ? C21 P1 Au1 113.94(16) . . ? C31 P1 Au1 113.09(16) . . ? C11 P1 C21 105.9(2) . . ? C11 P1 C31 104.6(2) . . ? C21 P1 C31 104.3(2) . . ? C12 S11 C11 88.6(2) . . ? C22 S21 C21 88.5(2) . . ? C32 S31 C31 89.0(2) . . ? S11 C11 P1 124.1(3) . . ? S21 C21 P1 124.6(3) . . ? S31 C31 P1 121.6(3) . . ? N11 C11 S11 115.6(3) . . ? N21 C21 S21 115.3(4) . . ? N31 C31 S31 115.3(4) . . ? N11 C11 P1 120.3(4) . . ? N21 C21 P1 119.8(4) . . ? N31 C31 P1 122.9(4) . . ? S11 C12 H12 124.2 . . ? S21 C22 H22 124.4 . . ? S31 C32 H32 124.6 . . ? N11 C13 C14 119.5(5) . . ? N21 C23 C24 119.5(4) . . ? N31 C33 C34 119.6(4) . . ? C11 N11 C13 110.5(4) . . ? C21 N21 C23 111.1(4) . . ? C31 N31 C33 110.5(4) . . ? C13 C12 S11 111.6(4) . . ? C23 C22 S21 111.1(4) . . ? C33 C32 S31 110.8(4) . . ? C12 C13 N11 113.7(4) . . ? C22 C23 N21 113.9(4) . . ? C32 C33 N31 114.5(4) . . ? C22 C23 C24 126.6(5) . . ? C23 C22 H22 124.4 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C33 C32 H32 124.6 . . ? C32 C33 C34 125.9(5) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C12 C13 C14 126.8(5) . . ? C13 C12 H12 124.2 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C2 O1 C5 107.1(4) . . ? O1 C2 C3 108.5(5) . . ? O1 C2 H2A 110.0 . . ? O1 C2 H2B 110.0 . . ? C3 C2 H2A 110.0 . . ? C3 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? C5 C4 C3 103.1(5) . . ? C5 C4 H4A 111.1 . . ? C5 C4 H4B 111.1 . . ? C3 C4 H4A 111.1 . . ? C3 C4 H4B 111.1 . . ? H4B C4 H4A 109.1 . . ? C2 C3 C4 103.1(5) . . ? C2 C3 H3A 111.1 . . ? C2 C3 H3B 111.1 . . ? C4 C3 H3A 111.1 . . ? C4 C3 H3B 111.1 . . ? H3A C3 H3B 109.1 . . ? O1 C5 C4 105.0(5) . . ? O1 C5 H5A 110.7 . . ? O1 C5 H5B 110.7 . . ? C4 C5 H5A 110.7 . . ? C4 C5 H5B 110.7 . . ? H5B C5 H5A 108.8 . . ? 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 Au1 P1 C11 S11 -165.2(2) . . . . ? Au1 P1 C11 N11 16.2(4) . . . . ? Au1 P1 C21 S21 -119.7(3) . . . . ? Au1 P1 C21 N21 54.1(4) . . . . ? Au1 P1 C31 S31 0.8(3) . . . . ? Au1 P1 C31 N31 174.8(3) . . . . ? S11 C11 N11 C13 -0.4(5) . . . . ? S21 C21 N21 C23 -1.5(6) . . . . ? S21 C22 C23 N21 -1.4(6) . . . . ? S21 C22 C23 C24 -178.9(4) . . . . ? S31 C31 N31 C33 0.6(5) . . . . ? S31 C32 C33 N31 -0.3(5) . . . . ? S31 C32 C33 C34 -177.5(4) . . . . ? P1 C11 S11 C12 -177.7(3) . . . . ? P1 C11 N11 C13 178.3(3) . . . . ? P1 C21 N21 C23 -175.9(4) . . . . ? P1 C31 N31 C33 -173.8(3) . . . . ? N11 C11 S11 C12 1.0(4) . . . . ? N11 C13 C12 S11 1.3(6) . . . . ? C11 S11 C12 C13 -1.2(4) . . . . ? C11 P1 C21 S21 6.4(4) . . . . ? C11 P1 C21 N21 -179.8(4) . . . . ? C11 P1 C31 S31 -123.9(3) . . . . ? C11 P1 C31 N31 50.2(5) . . . . ? C11 N11 C13 C12 -0.6(6) . . . . ? C11 N11 C13 C14 177.7(4) . . . . ? C14 C13 C12 S11 -176.9(4) . . . . ? C21 S21 C22 C23 0.5(4) . . . . ? C21 P1 C11 S11 68.7(4) . . . . ? C21 P1 C31 S31 125.1(3) . . . . ? C21 P1 C11 N11 -109.9(4) . . . . ? C21 P1 C31 N31 -60.9(4) . . . . ? C22 S21 C21 P1 174.7(3) . . . . ? C22 S21 C21 N21 0.6(4) . . . . ? C22 C23 N21 C21 1.9(7) . . . . ? C24 C23 N21 C21 179.6(4) . . . . ? C31 P1 C21 S21 116.5(3) . . . . ? C31 P1 C21 N21 -69.7(4) . . . . ? C32 S31 C31 P1 173.8(3) . . . . ? C32 S31 C31 N31 -0.7(4) . . . . ? C31 S31 C32 C33 0.5(4) . . . . ? C31 N31 C33 C32 -0.2(6) . . . . ? C31 N31 C33 C34 177.2(4) . . . . ? C31 P1 C11 N11 140.2(4) . . . . ? C31 P1 C11 S11 -41.2(4) . . . . ? O1 C2 C3 C4 -2.1(7) . . . . ? C2 O1 C5 C4 35.3(7) . . . . ? C3 C4 C5 O1 -35.4(7) . . . . ? C5 O1 C2 C3 -20.4(7) . . . . ? C5 C4 C3 C2 22.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.429 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.124 #Compound 2cTHF ends #===END ######## ## 2d ## ######## data_Compound2d _database_code_depnum_ccdc_archive 'CCDC 659061' _audit_creation_method SHELXL-97 _chemical_name_systematic chlorido[tris(4,5-dimethylthiazol-2-yl)phosphane]gold(I) _chemical_name_common 'tris(4,5-dimethylthiazol-2-yl)phosphanegold(I) chloride' _chemical_melting_point 359 _chemical_formula_moiety 'C15 H18 Au Cl N3 P S3' _chemical_formula_sum 'C15 H18 Au Cl N3 P S3' _chemical_formula_weight 599.91 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_int_tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 12.9541(15) _cell_length_b 11.2941(13) _cell_length_c 13.3664(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1955.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6785 _cell_measurement_theta_min 2.361 _cell_measurement_theta_max 26.768 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.038 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 8.064 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.653 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area detector' _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_% ? _diffrn_reflns_number 11189 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 26.81 _reflns_number_total 3661 _reflns_number_gt 3469 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material X-Seed _refine_special_details ;The thiazole ring containing C11 was found to be disordered in two positions rotated around 180\% in a 3:1 ratio. The respective parts were constrained to lie on a plane and both N11A and N11B were constrained to have the same anisotropic displacement parameters using the EADP command. 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^)+(0.0384P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.519(7) _refine_ls_number_reflns 3661 _refine_ls_number_parameters 236 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0591 _refine_ls_wR_factor_gt 0.0581 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.964089(11) 0.043971(12) 0.57066(3) 0.01617(6) Uani 1 1 d . . . Cl1 Cl 1.04883(9) -0.13252(10) 0.55878(15) 0.0241(3) Uani 1 1 d . . . P1 P 0.88009(8) 0.21447(10) 0.58284(13) 0.0167(3) Uani 1 1 d . A . C32 C 0.6552(5) 0.2937(5) 0.3659(5) 0.0240(13) Uani 1 1 d . . . S31 S 0.69238(11) 0.34058(12) 0.48285(11) 0.0261(3) Uani 1 1 d . . . S21 S 0.81264(10) 0.13013(12) 0.79312(11) 0.0234(3) Uani 1 1 d . A . C33 C 0.7178(4) 0.2034(5) 0.3342(4) 0.0203(12) Uani 1 1 d . . . N31 N 0.7955(3) 0.1723(4) 0.4013(3) 0.0192(9) Uani 1 1 d . . . N21 N 0.7377(3) 0.3136(4) 0.7078(3) 0.0206(9) Uani 1 1 d . A . C22 C 0.7178(4) 0.2062(5) 0.8556(5) 0.0241(13) Uani 1 1 d . . . C23 C 0.6869(4) 0.3010(5) 0.7969(4) 0.0207(12) Uani 1 1 d . . . C35 C 0.5608(5) 0.3429(6) 0.3176(5) 0.0305(14) Uani 1 1 d . . . H16A H 0.5039 0.2864 0.3246 0.046 Uiso 1 1 calc R . . H16B H 0.5745 0.3569 0.2465 0.046 Uiso 1 1 calc R . . H16C H 0.5421 0.4177 0.3500 0.046 Uiso 1 1 calc R . . C25 C 0.6789(5) 0.1679(6) 0.9549(5) 0.0361(15) Uani 1 1 d . . . H36A H 0.6331 0.2290 0.9822 0.054 Uiso 1 1 calc R . . H36B H 0.7373 0.1558 1.0004 0.054 Uiso 1 1 calc R . . H36C H 0.6405 0.0936 0.9477 0.054 Uiso 1 1 calc R . . C34 C 0.7099(5) 0.1379(5) 0.2369(4) 0.0275(12) Uani 1 1 d . . . H17A H 0.7768 0.1401 0.2026 0.041 Uiso 1 1 calc R . . H17B H 0.6574 0.1754 0.1947 0.041 Uiso 1 1 calc R . . H17C H 0.6905 0.0555 0.2498 0.041 Uiso 1 1 calc R . . C24 C 0.6039(4) 0.3889(5) 0.8230(4) 0.0242(11) Uani 1 1 d . . . H37A H 0.6329 0.4510 0.8657 0.036 Uiso 1 1 calc R . . H37B H 0.5480 0.3484 0.8586 0.036 Uiso 1 1 calc R . . H37C H 0.5768 0.4245 0.7615 0.036 Uiso 1 1 calc R . . C31 C 0.7903(4) 0.2355(5) 0.4830(5) 0.0190(13) Uani 1 1 d . . . C11 C 0.9613(3) 0.3452(4) 0.5852(5) 0.0199(14) Uani 1 1 d D . . N11A N 0.9980(10) 0.3968(10) 0.5075(9) 0.027(3) Uani 0.75 1 d PD A 2 S11B S 1.0066(13) 0.3991(11) 0.4720(9) 0.033(3) Uani 0.25 1 d PD A 1 N11B N 0.9997(16) 0.4018(15) 0.6557(16) 0.027(3) Uani 0.25 1 d PD A 1 S11A S 1.0060(2) 0.39925(19) 0.6979(2) 0.0259(5) Uani 0.75 1 d PD A 2 C21 C 0.8045(4) 0.2291(5) 0.6952(4) 0.0195(12) Uani 1 1 d . . . C12 C 1.0745(5) 0.4980(6) 0.6346(5) 0.0309(15) Uani 1 1 d D . . C13 C 1.0692(5) 0.4923(7) 0.5357(5) 0.0326(16) Uani 1 1 d D A . C15 C 1.1405(9) 0.5903(8) 0.6876(11) 0.084(4) Uani 1 1 d . A . H14A H 1.2137 0.5733 0.6757 0.127 Uiso 1 1 calc R . . H14B H 1.1265 0.5879 0.7596 0.127 Uiso 1 1 calc R . . H14C H 1.1239 0.6692 0.6616 0.127 Uiso 1 1 calc R . . C14 C 1.1174(9) 0.5658(8) 0.4546(9) 0.067(3) Uani 1 1 d . . . H15A H 1.0933 0.6478 0.4603 0.101 Uiso 1 1 calc R A . H15B H 1.0977 0.5340 0.3892 0.101 Uiso 1 1 calc R . . H15C H 1.1927 0.5637 0.4615 0.101 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01546(9) 0.01447(9) 0.01857(10) -0.00092(11) 0.00002(11) 0.00246(5) Cl1 0.0255(5) 0.0186(5) 0.0284(10) -0.0038(6) -0.0035(6) 0.0077(4) P1 0.0135(5) 0.0144(5) 0.0221(8) -0.0014(6) 0.0004(6) 0.0014(4) C32 0.021(3) 0.023(3) 0.028(3) 0.001(2) -0.004(2) -0.003(2) S31 0.0231(6) 0.0235(6) 0.0316(8) -0.0072(6) -0.0075(6) 0.0106(5) S21 0.0189(6) 0.0231(6) 0.0284(7) 0.0058(5) 0.0030(5) 0.0044(5) C33 0.016(2) 0.019(3) 0.025(3) 0.005(2) 0.006(2) -0.007(2) N31 0.016(2) 0.021(2) 0.021(2) 0.0024(19) 0.0014(17) -0.0003(17) N21 0.020(2) 0.020(2) 0.021(2) -0.0020(18) -0.0005(18) 0.0007(18) C22 0.014(3) 0.030(3) 0.028(3) 0.000(3) -0.003(2) 0.001(2) C23 0.016(3) 0.026(3) 0.019(3) -0.003(2) 0.001(2) -0.002(2) C35 0.028(3) 0.033(4) 0.031(3) 0.001(3) -0.010(3) 0.007(3) C25 0.030(3) 0.043(4) 0.035(4) 0.014(3) 0.004(3) 0.012(3) C34 0.030(3) 0.033(3) 0.019(3) -0.004(2) -0.003(2) -0.001(2) C24 0.019(3) 0.028(3) 0.026(3) -0.001(2) -0.001(2) 0.004(2) C31 0.016(3) 0.019(3) 0.022(3) -0.002(2) -0.003(2) 0.004(2) C11 0.017(2) 0.014(2) 0.028(4) -0.001(3) 0.003(2) 0.0053(16) N11A 0.041(5) 0.016(4) 0.024(8) -0.008(5) -0.003(5) 0.001(3) S11B 0.055(5) 0.015(4) 0.030(8) -0.006(5) 0.009(6) -0.006(4) N11B 0.041(5) 0.016(4) 0.024(8) -0.008(5) -0.003(5) 0.001(3) S11A 0.0327(11) 0.0183(10) 0.0269(12) 0.0007(9) -0.0089(10) -0.0044(9) C21 0.018(3) 0.019(3) 0.021(3) -0.005(2) 0.000(2) -0.005(2) C12 0.034(4) 0.017(3) 0.042(4) 0.005(3) -0.010(3) 0.008(3) C13 0.029(3) 0.025(3) 0.044(4) 0.003(3) 0.010(3) 0.008(3) C15 0.087(7) 0.031(4) 0.136(10) -0.011(5) -0.073(7) 0.015(5) C14 0.080(7) 0.044(5) 0.078(7) 0.008(4) 0.059(6) 0.008(4) _geom_special_details ;All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.2178(11) . ? Au1 Cl1 2.2812(11) . ? P1 C31 1.786(6) . ? P1 C21 1.800(6) . ? P1 C11 1.813(5) . ? C32 C33 1.370(8) . ? C32 C35 1.490(8) . ? C32 S31 1.718(6) . ? S31 C31 1.738(5) . ? S21 C22 1.716(6) . ? S21 C21 1.725(6) . ? C33 N31 1.394(7) . ? C33 C34 1.499(8) . ? N31 C31 1.306(7) . ? N21 C21 1.299(7) . ? N21 C23 1.368(7) . ? C22 C23 1.386(8) . ? C22 C25 1.484(8) . ? C23 C24 1.504(8) . ? C35 H16A 0.9800 . ? C35 H16B 0.9800 . ? C35 H16C 0.9800 . ? C25 H36A 0.9800 . ? C25 H36B 0.9800 . ? C25 H36C 0.9800 . ? C34 H17A 0.9800 . ? C34 H17B 0.9800 . ? C34 H17C 0.9800 . ? C24 H37A 0.9800 . ? C24 H37B 0.9800 . ? C24 H37C 0.9800 . ? C11 N11B 1.243(17) . ? C11 N11A 1.282(12) . ? C11 S11A 1.725(7) . ? C11 S11B 1.734(11) . ? N11A C13 1.469(15) . ? S11B C13 1.579(14) . ? N11B C12 1.483(19) . ? S11A C12 1.657(7) . ? C12 C13 1.325(9) . ? C12 C15 1.523(12) . ? C13 C14 1.501(11) . ? C15 H14A 0.9800 . ? C15 H14B 0.9800 . ? C15 H14C 0.9800 . ? C14 H15A 0.9800 . ? C14 H15B 0.9800 . ? C14 H15C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 179.34(5) . . ? C31 P1 C21 104.9(3) . . ? C31 P1 C11 106.4(2) . . ? C21 P1 C11 103.1(2) . . ? C31 P1 Au1 112.33(18) . . ? C21 P1 Au1 114.1(2) . . ? C11 P1 Au1 115.07(14) . . ? C33 C32 C35 128.9(6) . . ? C33 C32 S31 110.2(4) . . ? C35 C32 S31 120.6(5) . . ? C32 S31 C31 89.7(3) . . ? C22 S21 C21 90.1(3) . . ? C32 C33 N31 114.6(5) . . ? C32 C33 C34 126.6(5) . . ? N31 C33 C34 118.9(5) . . ? C31 N31 C33 111.3(5) . . ? C21 N21 C23 111.0(5) . . ? C23 C22 C25 129.3(5) . . ? C23 C22 S21 108.5(5) . . ? C25 C22 S21 122.2(5) . . ? N21 C23 C22 115.7(5) . . ? N21 C23 C24 118.5(5) . . ? C22 C23 C24 125.8(5) . . ? C32 C35 H16A 109.5 . . ? C32 C35 H16B 109.5 . . ? H16A C35 H16B 109.5 . . ? C32 C35 H16C 109.5 . . ? H16A C35 H16C 109.5 . . ? H16B C35 H16C 109.5 . . ? C22 C25 H36A 109.5 . . ? C22 C25 H36B 109.5 . . ? H36A C25 H36B 109.5 . . ? C22 C25 H36C 109.5 . . ? H36A C25 H36C 109.5 . . ? H36B C25 H36C 109.5 . . ? C33 C34 H17A 109.5 . . ? C33 C34 H17B 109.5 . . ? H17A C34 H17B 109.5 . . ? C33 C34 H17C 109.5 . . ? H17A C34 H17C 109.5 . . ? H17B C34 H17C 109.5 . . ? C23 C24 H37A 109.5 . . ? C23 C24 H37B 109.5 . . ? H37A C24 H37B 109.5 . . ? C23 C24 H37C 109.5 . . ? H37A C24 H37C 109.5 . . ? H37B C24 H37C 109.5 . . ? N31 C31 S31 114.2(4) . . ? N31 C31 P1 121.3(4) . . ? S31 C31 P1 124.5(3) . . ? N11A C11 S11A 114.9(6) . . ? N11B C11 S11B 110.2(10) . . ? N11B C11 P1 131.7(10) . . ? N11A C11 P1 124.8(7) . . ? S11A C11 P1 119.9(3) . . ? S11B C11 P1 117.8(5) . . ? C11 N11A C13 111.0(9) . . ? C13 S11B C11 86.4(7) . . ? C11 N11B C12 119.6(16) . . ? C12 S11A C11 88.4(3) . . ? N21 C21 S21 114.7(4) . . ? N21 C21 P1 122.6(4) . . ? S21 C21 P1 122.7(3) . . ? C13 C12 C15 121.8(9) . . ? C13 C12 N11B 96.9(10) . . ? C15 C12 N11B 141.3(11) . . ? C13 C12 S11A 116.6(7) . . ? C15 C12 S11A 121.6(7) . . ? C12 C13 N11A 108.9(8) . . ? C12 C13 C14 132.2(8) . . ? N11A C13 C14 118.9(8) . . ? C12 C13 S11B 126.7(8) . . ? C14 C13 S11B 101.1(7) . . ? C12 C15 H14A 109.5 . . ? C12 C15 H14B 109.5 . . ? H14A C15 H14B 109.5 . . ? C12 C15 H14C 109.5 . . ? H14A C15 H14C 109.5 . . ? H14B C15 H14C 109.5 . . ? C13 C14 H15A 109.5 . . ? C13 C14 H15B 109.5 . . ? H15A C14 H15B 109.5 . . ? C13 C14 H15C 109.5 . . ? H15A C14 H15C 109.5 . . ? H15B C14 H15C 109.5 . . ? 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 C33 C32 S31 C31 -0.1(5) . . . . ? C35 C32 S31 C31 174.5(5) . . . . ? C35 C32 C33 N31 -174.9(6) . . . . ? S31 C32 C33 N31 -0.8(6) . . . . ? C35 C32 C33 C34 5.3(10) . . . . ? S31 C32 C33 C34 179.3(4) . . . . ? C32 C33 N31 C31 1.6(6) . . . . ? C34 C33 N31 C31 -178.5(5) . . . . ? C21 S21 C22 C23 0.2(4) . . . . ? C21 S21 C22 C25 178.9(5) . . . . ? C21 N21 C23 C22 1.9(7) . . . . ? C21 N21 C23 C24 -178.1(5) . . . . ? C25 C22 C23 N21 -179.8(6) . . . . ? S21 C22 C23 N21 -1.2(6) . . . . ? C25 C22 C23 C24 0.1(10) . . . . ? S21 C22 C23 C24 178.8(5) . . . . ? C33 N31 C31 S31 -1.7(5) . . . . ? C33 N31 C31 P1 179.7(4) . . . . ? C32 S31 C31 N31 1.1(4) . . . . ? C32 S31 C31 P1 179.6(4) . . . . ? C21 P1 C31 N31 -141.0(5) . . . . ? C11 P1 C31 N31 110.2(4) . . . . ? Au1 P1 C31 N31 -16.6(5) . . . . ? C21 P1 C31 S31 40.6(4) . . . . ? C11 P1 C31 S31 -68.3(4) . . . . ? Au1 P1 C31 S31 165.0(3) . . . . ? C31 P1 C11 N11B 142.8(12) . . . . ? C21 P1 C11 N11B 32.7(12) . . . . ? Au1 P1 C11 N11B -92.1(12) . . . . ? C31 P1 C11 N11A -42.0(8) . . . . ? C21 P1 C11 N11A -152.0(8) . . . . ? Au1 P1 C11 N11A 83.1(8) . . . . ? C31 P1 C11 S11A 145.2(3) . . . . ? C21 P1 C11 S11A 35.2(3) . . . . ? Au1 P1 C11 S11A -89.7(3) . . . . ? C31 P1 C11 S11B -43.9(7) . . . . ? C21 P1 C11 S11B -154.0(7) . . . . ? Au1 P1 C11 S11B 81.2(7) . . . . ? N11B C11 N11A C13 2.2(13) . . . . ? S11A C11 N11A C13 -1.0(10) . . . . ? S11B C11 N11A C13 -160(9) . . . . ? P1 C11 N11A C13 -174.1(5) . . . . ? N11B C11 S11B C13 -1.1(10) . . . . ? N11A C11 S11B C13 17(8) . . . . ? S11A C11 S11B C13 -5.1(10) . . . . ? P1 C11 S11B C13 -175.8(5) . . . . ? N11A C11 N11B C12 -3.6(18) . . . . ? S11A C11 N11B C12 162(6) . . . . ? S11B C11 N11B C12 -1.2(16) . . . . ? P1 C11 N11B C12 172.4(7) . . . . ? N11B C11 S11A C12 -14(5) . . . . ? N11A C11 S11A C12 1.5(7) . . . . ? S11B C11 S11A C12 4.6(7) . . . . ? P1 C11 S11A C12 175.0(3) . . . . ? C23 N21 C21 S21 -1.7(6) . . . . ? C23 N21 C21 P1 176.8(4) . . . . ? C22 S21 C21 N21 0.9(5) . . . . ? C22 S21 C21 P1 -177.6(4) . . . . ? C31 P1 C21 N21 -45.4(5) . . . . ? C11 P1 C21 N21 65.8(5) . . . . ? Au1 P1 C21 N21 -168.7(4) . . . . ? C31 P1 C21 S21 133.0(4) . . . . ? C11 P1 C21 S21 -115.8(3) . . . . ? Au1 P1 C21 S21 9.7(4) . . . . ? C11 N11B C12 C13 3.3(17) . . . . ? C11 N11B C12 C15 179.6(10) . . . . ? C11 N11B C12 S11A -169(4) . . . . ? C11 S11A C12 C13 -1.8(7) . . . . ? C11 S11A C12 C15 178.5(7) . . . . ? C11 S11A C12 N11B 7(2) . . . . ? C15 C12 C13 N11A -178.7(8) . . . . ? N11B C12 C13 N11A -1.4(11) . . . . ? S11A C12 C13 N11A 1.6(10) . . . . ? C15 C12 C13 C14 -1.4(16) . . . . ? N11B C12 C13 C14 175.8(11) . . . . ? S11A C12 C13 C14 178.8(7) . . . . ? C15 C12 C13 S11B 178.1(10) . . . . ? N11B C12 C13 S11B -4.7(16) . . . . ? S11A C12 C13 S11B -1.7(15) . . . . ? C11 N11A C13 C12 -0.3(12) . . . . ? C11 N11A C13 C14 -178.0(8) . . . . ? C11 N11A C13 S11B 171(4) . . . . ? C11 S11B C13 C12 3.9(13) . . . . ? C11 S11B C13 N11A -6(3) . . . . ? C11 S11B C13 C14 -176.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.81 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.831 _refine_diff_density_min -0.680 _refine_diff_density_rms 0.143 #Compound 2d ends #===END #################### ## 3b . 0.5hexane ## #################### data_Compound3bHexane _database_code_depnum_ccdc_archive 'CCDC 659062' _audit_creation_method SHELXL-97 _chemical_name_systematic ;(thiobenzoato)[tris(4-methylthiazol-2-yl)phosphane]gold(I) hemi hexane solvate ; _chemical_name_common ;tris(4-methylthiazol-2-yl)phosphanegold(I) thiobenzoate hemi hexane solvate ; _chemical_melting_point 345 _chemical_formula_moiety 'C19 H17 Au N3 O P S4, 0.5(C6 H14)' _chemical_formula_sum 'C22 H24 Au N3 O P S4' _chemical_formula_weight 702.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_int_tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6209(8) _cell_length_b 17.6637(14) _cell_length_c 27.839(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5222.7(7) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9517 _cell_measurement_theta_min 2.354 _cell_measurement_theta_max 26.697 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.787 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2744 _exptl_absorpt_coefficient_mu 6.035 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.750 _exptl_absorpt_correction_T_max 0.937 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area detector' _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_% ? _diffrn_reflns_number 29548 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 26.73 _reflns_number_total 5534 _reflns_number_gt 4937 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material X-Seed _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^)+(0.0400P)^2^+31.6052P] 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 5534 _refine_ls_number_parameters 266 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.1051 _refine_ls_goodness_of_fit_ref 1.207 _refine_ls_restrained_S_all 1.206 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.30862(2) 0.080824(13) 0.553949(9) 0.02270(9) Uani 1 1 d . . . P1 P 0.27084(14) 0.05665(8) 0.47590(6) 0.0190(3) Uani 1 1 d . . . S1 S 0.3558(2) 0.11618(11) 0.63131(7) 0.0390(4) Uani 1 1 d . A . C21 C 0.3017(5) -0.0399(3) 0.4597(2) 0.0224(13) Uani 1 1 d . . . C11 C 0.1131(6) 0.0733(3) 0.4546(2) 0.0189(12) Uani 1 1 d . . . C31 C 0.3686(5) 0.1130(4) 0.4360(2) 0.0228(13) Uani 1 1 d . . . S11 S 0.01795(14) 0.00501(8) 0.42957(6) 0.0226(3) Uani 1 1 d . . . S21 S 0.35887(16) -0.10170(9) 0.50172(7) 0.0303(4) Uani 1 1 d . . . S31 S 0.4350(2) 0.07922(12) 0.38487(9) 0.0564(7) Uani 1 1 d . . . N31 N 0.3994(5) 0.1821(3) 0.44789(19) 0.0230(11) Uani 1 1 d . . . N21 N 0.2828(5) -0.0689(3) 0.4169(2) 0.0259(12) Uani 1 1 d . . . N11 N 0.0617(5) 0.1406(3) 0.45730(19) 0.0234(11) Uani 1 1 d . . . C13 C -0.0573(6) 0.1403(3) 0.4383(2) 0.0236(13) Uani 1 1 d . . . C12 C -0.0968(6) 0.0713(3) 0.4219(2) 0.0240(13) Uani 1 1 d . . . H12 H -0.1771 0.0616 0.4082 0.029 Uiso 1 1 calc R . . C23 C 0.3140(6) -0.1450(4) 0.4172(3) 0.0314(16) Uani 1 1 d . . . C33 C 0.4780(6) 0.2127(4) 0.4135(3) 0.0281(14) Uani 1 1 d . . . C34 C 0.5256(6) 0.2927(4) 0.4200(3) 0.0316(15) Uani 1 1 d . . . H34A H 0.5821 0.3057 0.3934 0.047 Uiso 1 1 calc R . . H34B H 0.5713 0.2965 0.4505 0.047 Uiso 1 1 calc R . . H34C H 0.4541 0.3277 0.4203 0.047 Uiso 1 1 calc R . . C22 C 0.3559(6) -0.1718(4) 0.4598(3) 0.0331(16) Uani 1 1 d . . . H22 H 0.3803 -0.2228 0.4656 0.040 Uiso 1 1 calc R . . C14 C -0.1302(6) 0.2131(4) 0.4361(3) 0.0340(16) Uani 1 1 d . . . H14A H -0.2134 0.2035 0.4222 0.051 Uiso 1 1 calc R . . H14B H -0.0847 0.2497 0.4162 0.051 Uiso 1 1 calc R . . H14C H -0.1401 0.2335 0.4686 0.051 Uiso 1 1 calc R . . C24 C 0.3015(7) -0.1903(4) 0.3716(3) 0.043(2) Uani 1 1 d . . . H24A H 0.3733 -0.1796 0.3506 0.064 Uiso 1 1 calc R . . H24B H 0.2232 -0.1762 0.3552 0.064 Uiso 1 1 calc R . . H24C H 0.2997 -0.2444 0.3794 0.064 Uiso 1 1 calc R . . C32 C 0.5058(8) 0.1646(5) 0.3780(3) 0.051(2) Uani 1 1 d . . . H32 H 0.5594 0.1768 0.3518 0.062 Uiso 1 1 calc R . . O1 O 0.3033(5) -0.0242(3) 0.6563(2) 0.0436(13) Uani 1 1 d . A . C1 C 0.3472(6) 0.0358(4) 0.6683(3) 0.0315(15) Uani 1 1 d . . . C41A C 0.3965(11) 0.0451(8) 0.7171(3) 0.055(8) Uani 0.593(13) 1 d PG A 1 C42A C 0.5106(12) 0.0821(9) 0.7239(4) 0.081(7) Uani 0.593(13) 1 d PGU A 1 H42A H 0.5568 0.1001 0.6970 0.097 Uiso 0.593(13) 1 calc PR A 1 C43A C 0.5570(12) 0.0929(9) 0.7700(5) 0.119(12) Uani 0.593(13) 1 d PGU A 1 H43A H 0.6350 0.1183 0.7747 0.143 Uiso 0.593(13) 1 calc PR A 1 C44A C 0.4894(14) 0.0667(9) 0.8094(3) 0.091(10) Uani 0.593(13) 1 d PG A 1 H44A H 0.5212 0.0741 0.8410 0.110 Uiso 0.593(13) 1 calc PR A 1 C45A C 0.3753(13) 0.0297(7) 0.8026(3) 0.069(6) Uani 0.593(13) 1 d PG A 1 H45A H 0.3291 0.0117 0.8295 0.082 Uiso 0.593(13) 1 calc PR A 1 C46A C 0.3289(9) 0.0189(7) 0.7564(4) 0.056(5) Uani 0.593(13) 1 d PG A 1 H46A H 0.2509 -0.0065 0.7518 0.068 Uiso 0.593(13) 1 calc PR A 1 C41B C 0.4094(13) 0.0508(7) 0.7182(3) 0.016(6) Uiso 0.407(13) 1 d PG A 2 C42B C 0.4429(13) 0.1219(6) 0.7354(4) 0.034(4) Uiso 0.407(13) 1 d PG A 2 H42B H 0.4275 0.1657 0.7165 0.041 Uiso 0.407(13) 1 calc PR A 2 C43B C 0.4991(14) 0.1290(6) 0.7803(5) 0.045(6) Uiso 0.407(13) 1 d PG A 2 H43B H 0.5220 0.1775 0.7920 0.055 Uiso 0.407(13) 1 calc PR A 2 C44B C 0.5217(15) 0.0649(8) 0.8080(4) 0.028(5) Uiso 0.407(13) 1 d PG A 2 H44B H 0.5600 0.0698 0.8387 0.033 Uiso 0.407(13) 1 calc PR A 2 C45B C 0.4881(14) -0.0062(6) 0.7908(4) 0.052(6) Uiso 0.407(13) 1 d PG A 2 H45B H 0.5036 -0.0499 0.8098 0.062 Uiso 0.407(13) 1 calc PR A 2 C46B C 0.4320(13) -0.0132(6) 0.7460(4) 0.044(5) Uiso 0.407(13) 1 d PG A 2 H46B H 0.4091 -0.0618 0.7342 0.052 Uiso 0.407(13) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.02172(14) 0.01634(13) 0.03003(15) 0.00399(10) -0.00616(9) -0.00322(9) P1 0.0161(7) 0.0107(7) 0.0304(8) 0.0024(6) -0.0025(6) -0.0005(5) S1 0.0538(12) 0.0311(10) 0.0321(9) 0.0061(8) -0.0096(8) -0.0167(9) C21 0.012(3) 0.014(3) 0.042(4) 0.007(3) 0.001(2) 0.000(2) C11 0.019(3) 0.013(3) 0.025(3) 0.005(2) -0.003(2) -0.004(2) C31 0.012(3) 0.021(3) 0.035(4) 0.000(3) 0.000(2) -0.001(2) S11 0.0188(7) 0.0129(7) 0.0361(8) -0.0037(6) -0.0044(6) -0.0006(6) S21 0.0254(8) 0.0172(7) 0.0481(10) 0.0083(7) 0.0015(7) 0.0080(6) S31 0.0712(16) 0.0333(10) 0.0647(14) -0.0194(10) 0.0393(12) -0.0256(10) N31 0.019(3) 0.016(2) 0.034(3) 0.003(2) -0.007(2) -0.0016(19) N21 0.020(3) 0.014(3) 0.044(3) -0.001(2) 0.001(2) -0.002(2) N11 0.019(3) 0.013(2) 0.038(3) 0.003(2) -0.003(2) -0.004(2) C13 0.019(3) 0.018(3) 0.034(3) 0.003(2) -0.002(2) 0.001(2) C12 0.016(3) 0.018(3) 0.038(4) -0.001(3) -0.002(3) -0.002(2) C23 0.014(3) 0.017(3) 0.063(5) -0.011(3) 0.008(3) 0.000(2) C33 0.020(3) 0.024(3) 0.040(4) 0.005(3) -0.005(3) 0.000(3) C34 0.022(3) 0.018(3) 0.055(5) 0.007(3) -0.001(3) -0.002(3) C22 0.025(3) 0.012(3) 0.062(5) 0.004(3) 0.012(3) 0.006(3) C14 0.024(3) 0.020(3) 0.058(5) 0.006(3) -0.006(3) 0.003(3) C24 0.036(4) 0.021(4) 0.072(6) -0.023(4) 0.010(4) 0.002(3) C32 0.059(6) 0.036(4) 0.059(5) -0.005(4) 0.030(4) -0.023(4) O1 0.062(4) 0.027(3) 0.042(3) 0.000(2) -0.008(3) -0.003(2) C1 0.024(3) 0.031(4) 0.040(4) 0.000(3) 0.004(3) 0.004(3) C41A 0.072(14) 0.046(11) 0.048(11) 0.005(7) -0.004(8) -0.008(8) C42A 0.085(14) 0.104(16) 0.054(10) 0.033(10) -0.023(10) -0.053(13) C43A 0.16(3) 0.14(2) 0.056(12) 0.034(13) -0.058(14) -0.11(2) C44A 0.15(3) 0.078(15) 0.048(11) 0.001(9) -0.045(14) -0.024(15) C45A 0.113(16) 0.071(12) 0.022(7) 0.012(7) -0.004(8) -0.025(11) C46A 0.058(10) 0.063(11) 0.048(9) 0.007(8) 0.008(7) -0.018(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.2504(16) . ? Au1 S1 2.2976(19) . ? P1 C21 1.793(6) . ? P1 C11 1.801(6) . ? P1 C31 1.818(6) . ? S1 C1 1.755(7) . ? C21 N21 1.312(9) . ? C21 S21 1.711(6) . ? C11 N11 1.310(8) . ? C11 S11 1.721(6) . ? C31 N31 1.307(8) . ? C31 S31 1.696(7) . ? S11 C12 1.703(6) . ? S21 C22 1.701(7) . ? S31 C32 1.696(8) . ? N31 C33 1.381(8) . ? N21 C23 1.386(8) . ? N11 C13 1.371(8) . ? C13 C12 1.368(8) . ? C13 C14 1.502(9) . ? C12 H12 0.9500 . ? C23 C22 1.352(11) . ? C23 C24 1.506(10) . ? C33 C32 1.335(10) . ? C33 C34 1.511(9) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C22 H22 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C32 H32 0.9500 . ? O1 C1 1.205(9) . ? C1 C41A 1.465(10) . ? C1 C41B 1.563(12) . ? C41A C42A 1.3900 . ? C41A C46A 1.3900 . ? C42A C43A 1.3900 . ? C42A H42A 0.9500 . ? C43A C44A 1.3900 . ? C43A H43A 0.9500 . ? C44A C45A 1.3900 . ? C44A H44A 0.9500 . ? C45A C46A 1.3900 . ? C45A H45A 0.9500 . ? C46A H46A 0.9500 . ? C41B C42B 1.3900 . ? C41B C46B 1.3900 . ? C42B C43B 1.3900 . ? C42B H42B 0.9500 . ? C43B C44B 1.3900 . ? C43B H43B 0.9500 . ? C44B C45B 1.3900 . ? C44B H44B 0.9500 . ? C45B C46B 1.3900 . ? C45B H45B 0.9500 . ? C46B H46B 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 S1 174.53(6) . . ? C21 P1 C11 104.0(3) . . ? C21 P1 C31 105.2(3) . . ? C11 P1 C31 103.9(3) . . ? C21 P1 Au1 113.0(2) . . ? C11 P1 Au1 116.9(2) . . ? C31 P1 Au1 112.6(2) . . ? C1 S1 Au1 108.6(3) . . ? N21 C21 S21 115.2(5) . . ? N21 C21 P1 124.8(5) . . ? S21 C21 P1 120.0(4) . . ? N11 C11 S11 114.5(4) . . ? N11 C11 P1 121.1(4) . . ? S11 C11 P1 124.4(3) . . ? N31 C31 S31 116.0(5) . . ? N31 C31 P1 119.9(5) . . ? S31 C31 P1 123.9(4) . . ? C12 S11 C11 89.4(3) . . ? C22 S21 C21 89.4(3) . . ? C31 S31 C32 88.0(4) . . ? C31 N31 C33 109.9(6) . . ? C21 N21 C23 109.7(6) . . ? C11 N11 C13 111.0(5) . . ? C12 C13 N11 114.5(5) . . ? C12 C13 C14 126.3(6) . . ? N11 C13 C14 119.2(6) . . ? C13 C12 S11 110.6(5) . . ? C13 C12 H12 124.7 . . ? S11 C12 H12 124.7 . . ? C22 C23 N21 115.1(6) . . ? C22 C23 C24 125.7(6) . . ? N21 C23 C24 119.2(7) . . ? C32 C33 N31 113.4(6) . . ? C32 C33 C34 127.6(7) . . ? N31 C33 C34 119.0(6) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C23 C22 S21 110.7(5) . . ? C23 C22 H22 124.7 . . ? S21 C22 H22 124.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C33 C32 S31 112.6(6) . . ? C33 C32 H32 123.7 . . ? S31 C32 H32 123.7 . . ? O1 C1 C41A 119.6(8) . . ? O1 C1 C41B 124.0(8) . . ? O1 C1 S1 124.7(6) . . ? C41A C1 S1 115.8(7) . . ? C41B C1 S1 111.3(6) . . ? C42A C41A C46A 120.0 . . ? C42A C41A C1 119.4(8) . . ? C46A C41A C1 120.6(8) . . ? C41A C42A C43A 120.0 . . ? C41A C42A H42A 120.0 . . ? C43A C42A H42A 120.0 . . ? C44A C43A C42A 120.0 . . ? C44A C43A H43A 120.0 . . ? C42A C43A H43A 120.0 . . ? C43A C44A C45A 120.0 . . ? C43A C44A H44A 120.0 . . ? C45A C44A H44A 120.0 . . ? C46A C45A C44A 120.0 . . ? C46A C45A H45A 120.0 . . ? C44A C45A H45A 120.0 . . ? C45A C46A C41A 120.0 . . ? C45A C46A H46A 120.0 . . ? C41A C46A H46A 120.0 . . ? C42B C41B C46B 120.0 . . ? C42B C41B C1 124.6(8) . . ? C46B C41B C1 115.4(8) . . ? C41B C42B C43B 120.0 . . ? C41B C42B H42B 120.0 . . ? C43B C42B H42B 120.0 . . ? C42B C43B C44B 120.0 . . ? C42B C43B H43B 120.0 . . ? C44B C43B H43B 120.0 . . ? C45B C44B C43B 120.0 . . ? C45B C44B H44B 120.0 . . ? C43B C44B H44B 120.0 . . ? C44B C45B C46B 120.0 . . ? C44B C45B H45B 120.0 . . ? C46B C45B H45B 120.0 . . ? C45B C46B C41B 120.0 . . ? C45B C46B H46B 120.0 . . ? C41B C46B H46B 120.0 . . ? 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 C11 P1 C21 N21 49.6(6) . . . . ? C31 P1 C21 N21 -59.3(6) . . . . ? Au1 P1 C21 N21 177.4(4) . . . . ? C11 P1 C21 S21 -129.8(4) . . . . ? C31 P1 C21 S21 121.2(4) . . . . ? Au1 P1 C21 S21 -2.1(4) . . . . ? C21 P1 C11 N11 -175.2(5) . . . . ? C31 P1 C11 N11 -65.3(6) . . . . ? Au1 P1 C11 N11 59.5(5) . . . . ? C21 P1 C11 S11 4.9(5) . . . . ? C31 P1 C11 S11 114.8(4) . . . . ? Au1 P1 C11 S11 -120.4(3) . . . . ? C21 P1 C31 N31 -158.0(5) . . . . ? C11 P1 C31 N31 93.0(5) . . . . ? Au1 P1 C31 N31 -34.5(6) . . . . ? C21 P1 C31 S31 16.6(5) . . . . ? C11 P1 C31 S31 -92.4(4) . . . . ? Au1 P1 C31 S31 140.1(3) . . . . ? N11 C11 S11 C12 0.5(5) . . . . ? P1 C11 S11 C12 -179.5(4) . . . . ? N21 C21 S21 C22 -0.8(5) . . . . ? P1 C21 S21 C22 178.7(4) . . . . ? N31 C31 S31 C32 -1.7(6) . . . . ? P1 C31 S31 C32 -176.5(5) . . . . ? S31 C31 N31 C33 2.3(7) . . . . ? P1 C31 N31 C33 177.3(4) . . . . ? S21 C21 N21 C23 0.7(6) . . . . ? P1 C21 N21 C23 -178.8(4) . . . . ? S11 C11 N11 C13 -1.1(7) . . . . ? P1 C11 N11 C13 179.0(4) . . . . ? C11 N11 C13 C12 1.3(8) . . . . ? C11 N11 C13 C14 -177.5(6) . . . . ? N11 C13 C12 S11 -0.9(7) . . . . ? C14 C13 C12 S11 177.7(6) . . . . ? C11 S11 C12 C13 0.2(5) . . . . ? C21 N21 C23 C22 -0.2(8) . . . . ? C21 N21 C23 C24 -179.2(6) . . . . ? C31 N31 C33 C32 -1.9(9) . . . . ? C31 N31 C33 C34 180.0(6) . . . . ? N21 C23 C22 S21 -0.4(7) . . . . ? C24 C23 C22 S21 178.6(5) . . . . ? C21 S21 C22 C23 0.6(5) . . . . ? N31 C33 C32 S31 0.7(10) . . . . ? C34 C33 C32 S31 178.6(6) . . . . ? C31 S31 C32 C33 0.5(7) . . . . ? Au1 S1 C1 O1 -11.5(7) . . . . ? Au1 S1 C1 C41A 169.3(6) . . . . ? Au1 S1 C1 C41B 166.0(6) . . . . ? O1 C1 C41A C42A 136.2(9) . . . . ? C41B C1 C41A C42A -10(9) . . . . ? S1 C1 C41A C42A -44.5(10) . . . . ? O1 C1 C41A C46A -45.4(13) . . . . ? C41B C1 C41A C46A 169(10) . . . . ? S1 C1 C41A C46A 133.9(8) . . . . ? C46A C41A C42A C43A 0.0 . . . . ? C1 C41A C42A C43A 178.4(12) . . . . ? C41A C42A C43A C44A 0.0 . . . . ? C42A C43A C44A C45A 0.0 . . . . ? C43A C44A C45A C46A 0.0 . . . . ? C44A C45A C46A C41A 0.0 . . . . ? C42A C41A C46A C45A 0.0 . . . . ? C1 C41A C46A C45A -178.4(12) . . . . ? O1 C1 C41B C42B -169.7(8) . . . . ? C41A C1 C41B C42B -134(10) . . . . ? S1 C1 C41B C42B 12.8(11) . . . . ? O1 C1 C41B C46B 11.0(12) . . . . ? C41A C1 C41B C46B 47(9) . . . . ? S1 C1 C41B C46B -166.5(6) . . . . ? C46B C41B C42B C43B 0.0 . . . . ? C1 C41B C42B C43B -179.3(12) . . . . ? C41B C42B C43B C44B 0.0 . . . . ? C42B C43B C44B C45B 0.0 . . . . ? C43B C44B C45B C46B 0.0 . . . . ? C44B C45B C46B C41B 0.0 . . . . ? C42B C41B C46B C45B 0.0 . . . . ? C1 C41B C46B C45B 179.4(11) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.370 _refine_diff_density_min -1.154 _refine_diff_density_rms 0.170 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.025 0.691 0.250 206.4 54.6 2 0.001 0.191 0.250 206.4 54.1 3 -0.024 0.809 0.750 206.4 52.1 4 0.001 0.309 0.750 206.4 52.6 _platon_squeeze_details 'Spek (2003)' #Compound 3bHexane ends #===END ################# ## 4 . acetone ## ################# data_Compound4Acetone _database_code_depnum_ccdc_archive 'CCDC 659063' _audit_creation_method SHELXL-97 _chemical_name_systematic ;Bis(pentafluorophenyl)-\m-[tris(1-methylimidazol-2-yl) phosphane-\kP:\kN]digold(I) acetone solvate ; _chemical_name_common ;Bis(pentafluorophenyl)-\m-[tris(1-methylimidazolyl)phosphine] digold(I) acetone solvate ; _chemical_melting_point 447 _chemical_formula_moiety 'C24 H15 Au2 F10 N6 P, 0.77(C3 H6 O)' _chemical_formula_sum 'C26.31 H19.62 Au2 F10 N6 O0.77 P' _chemical_formula_weight 1047.04 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2802(15) _cell_length_b 12.7070(18) _cell_length_c 13.1407(19) _cell_angle_alpha 81.504(2) _cell_angle_beta 81.244(3) _cell_angle_gamma 72.231(2) _cell_volume 1606.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3508 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 28.17 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 977.3 _exptl_absorpt_coefficient_mu 9.262 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.318 _exptl_absorpt_correction_T_max 0.628 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _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_% ? _diffrn_reflns_number 9403 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.73 _reflns_number_total 6595 _reflns_number_gt 5084 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material X-Seed _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^)+(0.0676P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6595 _refine_ls_number_parameters 408 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1130 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.73486(3) 0.38461(3) 0.15662(3) 0.01853(11) Uani 1 1 d . . . P1 P 0.8398(2) 0.40865(18) 0.28716(18) 0.0182(5) Uani 1 1 d . . . Au2 Au 0.98644(3) 0.19924(3) 0.11463(3) 0.02026(11) Uani 1 1 d . . . N11 N 1.1234(7) 0.3771(6) 0.3008(6) 0.0207(16) Uani 1 1 d . . . C11 C 1.0244(8) 0.3526(7) 0.2610(7) 0.0181(17) Uani 1 1 d . . . N12 N 1.0824(7) 0.2773(6) 0.1952(6) 0.0230(17) Uani 1 1 d . . . C12 C 1.2484(9) 0.3155(7) 0.2602(8) 0.028(2) Uani 1 1 d . . . H12 H 1.3359 0.3157 0.2751 0.033 Uiso 1 1 calc R . . C13 C 1.2224(9) 0.2533(8) 0.1933(8) 0.033(2) Uani 1 1 d . . . H13 H 1.2897 0.2022 0.1526 0.040 Uiso 1 1 calc R . . C14 C 1.1077(9) 0.4549(8) 0.3772(7) 0.027(2) Uani 1 1 d . . . H14A H 1.0357 0.4457 0.4330 0.041 Uiso 1 1 calc R . . H14B H 1.0821 0.5313 0.3435 0.041 Uiso 1 1 calc R . . H14C H 1.1948 0.4396 0.4062 0.041 Uiso 1 1 calc R . . N21 N 0.6798(9) 0.3396(9) 0.4601(7) 0.049(3) Uani 1 1 d . . . C21 C 0.8062(10) 0.3477(7) 0.4159(7) 0.027(2) Uani 1 1 d . . . N22 N 0.8995(10) 0.3033(8) 0.4793(7) 0.049(2) Uani 1 1 d . . . C22 C 0.6940(13) 0.2933(12) 0.5590(9) 0.059(4) Uani 1 1 d . . . H22 H 0.6242 0.2787 0.6104 0.071 Uiso 1 1 calc R . . C23 C 0.8279(14) 0.2726(10) 0.5691(8) 0.050(3) Uani 1 1 d . . . H23 H 0.8679 0.2404 0.6312 0.060 Uiso 1 1 calc R . . C24 C 0.5513(14) 0.381(2) 0.4132(12) 0.131(9) Uani 1 1 d . . . H24A H 0.4750 0.4075 0.4665 0.196 Uiso 1 1 calc R . . H24B H 0.5360 0.3212 0.3819 0.196 Uiso 1 1 calc R . . H24C H 0.5568 0.4426 0.3596 0.196 Uiso 1 1 calc R . . N31 N 0.8350(7) 0.6310(6) 0.2289(5) 0.0189(15) Uani 1 1 d . . . C31 C 0.8107(8) 0.5529(7) 0.3053(7) 0.0178(17) Uani 1 1 d . . . N32 N 0.7573(7) 0.5943(6) 0.3942(6) 0.0262(17) Uani 1 1 d . . . C32 C 0.7987(9) 0.7278(7) 0.2738(8) 0.028(2) Uani 1 1 d . . . H32 H 0.8058 0.7979 0.2410 0.034 Uiso 1 1 calc R . . C33 C 0.7506(10) 0.7050(8) 0.3741(8) 0.033(2) Uani 1 1 d . . . H33 H 0.7172 0.7577 0.4232 0.040 Uiso 1 1 calc R . . C34 C 0.8892(9) 0.6175(7) 0.1203(7) 0.024(2) Uani 1 1 d . . . H34A H 0.8420 0.5735 0.0925 0.037 Uiso 1 1 calc R . . H34B H 0.9880 0.5792 0.1156 0.037 Uiso 1 1 calc R . . H34C H 0.8737 0.6907 0.0801 0.037 Uiso 1 1 calc R . . C41 C 0.6424(8) 0.3736(6) 0.0343(7) 0.0197(19) Uani 1 1 d . . . F42 F 0.7528(5) 0.4913(4) -0.0784(4) 0.0290(12) Uani 1 1 d . . . C42 C 0.6676(8) 0.4258(7) -0.0629(7) 0.0206(19) Uani 1 1 d . . . F43 F 0.6425(5) 0.4673(5) -0.2428(4) 0.0339(13) Uani 1 1 d . . . C43 C 0.6150(9) 0.4143(7) -0.1505(8) 0.026(2) Uani 1 1 d . . . F44 F 0.4739(5) 0.3353(5) -0.2221(4) 0.0343(14) Uani 1 1 d . . . C44 C 0.5269(9) 0.3486(7) -0.1406(8) 0.025(2) Uani 1 1 d . . . F45 F 0.4149(5) 0.2274(4) -0.0351(5) 0.0336(14) Uani 1 1 d . . . C45 C 0.4988(8) 0.2942(7) -0.0453(8) 0.026(2) Uani 1 1 d . . . F46 F 0.5251(5) 0.2498(4) 0.1312(4) 0.0278(12) Uani 1 1 d . . . C46 C 0.5556(8) 0.3071(7) 0.0388(7) 0.0218(19) Uani 1 1 d . . . C51 C 0.8894(8) 0.1232(7) 0.0394(7) 0.0221(19) Uani 1 1 d . . . F52 F 0.9366(6) 0.2195(5) -0.1244(4) 0.0367(14) Uani 1 1 d . . . C52 C 0.8734(9) 0.1476(7) -0.0641(8) 0.025(2) Uani 1 1 d . . . F53 F 0.7853(6) 0.1308(5) -0.2151(5) 0.0408(15) Uani 1 1 d . . . C53 C 0.7972(8) 0.1039(7) -0.1136(7) 0.024(2) Uani 1 1 d . . . F54 F 0.6508(5) -0.0097(4) -0.1035(5) 0.0352(14) Uani 1 1 d . . . C54 C 0.7295(9) 0.0335(7) -0.0579(8) 0.023(2) Uani 1 1 d . . . F55 F 0.6761(6) -0.0662(5) 0.1014(5) 0.0489(17) Uani 1 1 d . . . C55 C 0.7414(9) 0.0055(7) 0.0466(8) 0.030(2) Uani 1 1 d . . . F56 F 0.8306(7) 0.0189(5) 0.1941(5) 0.0469(16) Uani 1 1 d . . . C56 C 0.8207(9) 0.0510(7) 0.0928(8) 0.028(2) Uani 1 1 d . . . C97 C 0.759(3) -0.055(2) 0.565(3) 0.160(14) Uiso 0.770(18) 1 d PD . . H97A H 0.8067 -0.1018 0.5097 0.240 Uiso 0.770(18) 1 calc PR . . H97B H 0.8097 -0.0782 0.6255 0.240 Uiso 0.770(18) 1 calc PR . . H97C H 0.7517 0.0228 0.5405 0.240 Uiso 0.770(18) 1 calc PR . . C98 C 0.6131(17) -0.069(2) 0.5949(19) 0.111(9) Uiso 0.770(18) 1 d PD . . O99 O 0.5806(15) -0.1438(14) 0.5639(13) 0.105(6) Uiso 0.770(18) 1 d PD . . C99 C 0.508(2) 0.0085(19) 0.6695(19) 0.107(9) Uiso 0.770(18) 1 d PD . . H99A H 0.4163 0.0013 0.6682 0.160 Uiso 0.770(18) 1 calc PR . . H99B H 0.5077 0.0857 0.6475 0.160 Uiso 0.770(18) 1 calc PR . . H99C H 0.5343 -0.0128 0.7400 0.160 Uiso 0.770(18) 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01499(16) 0.02113(18) 0.0239(2) -0.00847(14) -0.00047(14) -0.00971(13) P1 0.0163(10) 0.0215(11) 0.0195(12) -0.0034(9) 0.0004(9) -0.0103(9) Au2 0.01755(17) 0.01898(18) 0.0290(2) -0.01085(15) -0.00012(14) -0.00968(13) N11 0.021(3) 0.023(4) 0.024(4) -0.009(3) -0.002(3) -0.012(3) C11 0.018(4) 0.018(4) 0.022(5) -0.004(3) 0.002(4) -0.012(3) N12 0.022(4) 0.019(4) 0.031(5) -0.012(3) -0.003(3) -0.006(3) C12 0.017(4) 0.027(5) 0.044(6) -0.004(4) -0.005(4) -0.013(4) C13 0.022(5) 0.035(5) 0.045(7) -0.016(5) 0.000(4) -0.009(4) C14 0.027(5) 0.034(5) 0.028(5) -0.016(4) -0.003(4) -0.013(4) N21 0.034(5) 0.077(7) 0.033(5) 0.009(5) 0.017(4) -0.028(5) C21 0.033(5) 0.027(5) 0.022(5) -0.009(4) 0.004(4) -0.012(4) N22 0.063(6) 0.061(6) 0.033(5) 0.015(5) -0.016(5) -0.036(5) C22 0.062(8) 0.092(10) 0.029(7) 0.009(7) 0.012(6) -0.047(8) C23 0.084(9) 0.055(7) 0.018(6) 0.017(5) -0.016(6) -0.036(7) C24 0.046(9) 0.28(3) 0.057(11) 0.049(14) 0.007(8) -0.067(13) N31 0.022(3) 0.022(4) 0.019(4) -0.006(3) 0.000(3) -0.014(3) C31 0.016(4) 0.018(4) 0.021(5) -0.010(4) -0.005(3) -0.003(3) N32 0.028(4) 0.020(4) 0.032(5) -0.007(3) -0.005(4) -0.006(3) C32 0.027(5) 0.021(4) 0.039(6) -0.008(4) -0.001(4) -0.010(4) C33 0.039(5) 0.031(5) 0.033(6) -0.013(5) 0.000(5) -0.013(4) C34 0.027(5) 0.023(4) 0.024(5) -0.002(4) 0.002(4) -0.013(4) C41 0.019(4) 0.008(4) 0.035(5) -0.005(4) -0.013(4) -0.003(3) F42 0.027(3) 0.029(3) 0.037(3) -0.003(2) -0.005(2) -0.018(2) C42 0.015(4) 0.016(4) 0.034(5) -0.009(4) -0.004(4) -0.005(3) F43 0.035(3) 0.044(3) 0.031(3) -0.008(3) -0.009(3) -0.018(3) C43 0.028(5) 0.020(4) 0.029(5) -0.010(4) 0.004(4) -0.007(4) F44 0.023(3) 0.048(3) 0.040(4) -0.017(3) -0.008(3) -0.013(2) C44 0.021(4) 0.026(5) 0.033(6) -0.015(4) -0.007(4) -0.008(4) F45 0.028(3) 0.037(3) 0.048(4) -0.020(3) -0.001(3) -0.022(2) C45 0.014(4) 0.023(5) 0.043(6) -0.017(4) 0.002(4) -0.007(4) F46 0.022(3) 0.034(3) 0.032(3) -0.007(2) 0.001(2) -0.016(2) C46 0.010(4) 0.032(5) 0.025(5) -0.013(4) -0.002(4) -0.004(4) C51 0.018(4) 0.022(4) 0.030(5) -0.010(4) 0.002(4) -0.010(4) F52 0.039(3) 0.050(4) 0.032(3) -0.005(3) 0.003(3) -0.032(3) C52 0.023(4) 0.018(4) 0.036(6) -0.008(4) 0.006(4) -0.014(4) F53 0.049(4) 0.055(4) 0.030(3) -0.014(3) -0.005(3) -0.027(3) C53 0.018(4) 0.026(5) 0.028(5) -0.010(4) -0.009(4) 0.002(4) F54 0.037(3) 0.031(3) 0.052(4) -0.011(3) -0.015(3) -0.023(2) C54 0.022(4) 0.013(4) 0.036(6) -0.016(4) -0.005(4) -0.002(3) F55 0.062(4) 0.047(4) 0.057(4) 0.014(3) -0.023(4) -0.046(3) C55 0.028(5) 0.018(4) 0.050(7) 0.001(4) -0.011(5) -0.012(4) F56 0.069(4) 0.046(4) 0.044(4) 0.015(3) -0.027(3) -0.041(3) C56 0.027(5) 0.025(5) 0.036(6) -0.008(4) -0.005(4) -0.012(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C41 2.029(8) . ? Au1 P1 2.263(2) . ? Au1 Au2 2.9620(5) . ? P1 C21 1.783(10) . ? P1 C11 1.810(8) . ? P1 C31 1.811(8) . ? Au2 C51 2.019(8) . ? Au2 N12 2.074(7) . ? N11 C11 1.345(10) . ? N11 C12 1.361(10) . ? N11 C14 1.469(10) . ? C11 N12 1.326(10) . ? N12 C13 1.374(11) . ? C12 C13 1.369(13) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? N21 C22 1.356(15) . ? N21 C21 1.368(12) . ? N21 C24 1.458(16) . ? C21 N22 1.307(13) . ? N22 C23 1.364(14) . ? C22 C23 1.343(17) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? N31 C31 1.355(11) . ? N31 C32 1.366(10) . ? N31 C34 1.466(11) . ? C31 N32 1.324(10) . ? N32 C33 1.375(12) . ? C32 C33 1.358(14) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C41 C42 1.376(13) . ? C41 C46 1.394(11) . ? F42 C42 1.357(9) . ? C42 C43 1.387(13) . ? F43 C43 1.333(11) . ? C43 C44 1.388(12) . ? F44 C44 1.326(10) . ? C44 C45 1.373(14) . ? F45 C45 1.364(10) . ? C45 C46 1.377(12) . ? F46 C46 1.365(11) . ? C51 C52 1.373(13) . ? C51 C56 1.375(13) . ? F52 C52 1.369(10) . ? C52 C53 1.368(12) . ? F53 C53 1.342(11) . ? C53 C54 1.360(13) . ? F54 C54 1.353(9) . ? C54 C55 1.381(14) . ? F55 C55 1.354(11) . ? C55 C56 1.382(12) . ? F56 C56 1.343(11) . ? C97 C98 1.54(2) . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C98 O99 1.24(3) . ? C98 C99 1.55(2) . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 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 C41 Au1 P1 175.9(2) . . ? C41 Au1 Au2 96.2(2) . . ? P1 Au1 Au2 85.26(6) . . ? C21 P1 C11 102.4(4) . . ? C21 P1 C31 102.4(4) . . ? C11 P1 C31 105.3(4) . . ? C21 P1 Au1 120.9(3) . . ? C11 P1 Au1 110.4(3) . . ? C31 P1 Au1 113.9(3) . . ? C51 Au2 N12 178.5(3) . . ? C51 Au2 Au1 93.0(2) . . ? N12 Au2 Au1 86.16(19) . . ? C11 N11 C12 109.1(7) . . ? C11 N11 C14 128.4(7) . . ? C12 N11 C14 122.6(7) . . ? N12 C11 N11 109.2(7) . . ? N12 C11 P1 122.4(6) . . ? N11 C11 P1 128.5(6) . . ? C11 N12 C13 107.4(7) . . ? C11 N12 Au2 128.0(6) . . ? C13 N12 Au2 124.4(6) . . ? N11 C12 C13 105.9(7) . . ? N11 C12 H12 127.0 . . ? C13 C12 H12 127.0 . . ? C12 C13 N12 108.4(8) . . ? C12 C13 H13 125.8 . . ? N12 C13 H13 125.8 . . ? N11 C14 H14A 109.5 . . ? N11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C22 N21 C21 106.9(10) . . ? C22 N21 C24 126.1(10) . . ? C21 N21 C24 126.8(10) . . ? N22 C21 N21 111.4(9) . . ? N22 C21 P1 124.4(8) . . ? N21 C21 P1 124.2(8) . . ? C21 N22 C23 104.4(10) . . ? C23 C22 N21 105.4(10) . . ? C23 C22 H22 127.3 . . ? N21 C22 H22 127.3 . . ? C22 C23 N22 111.8(10) . . ? C22 C23 H23 124.1 . . ? N22 C23 H23 124.1 . . ? N21 C24 H24A 109.5 . . ? N21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C31 N31 C32 105.6(7) . . ? C31 N31 C34 128.4(7) . . ? C32 N31 C34 126.0(8) . . ? N32 C31 N31 112.8(7) . . ? N32 C31 P1 123.2(7) . . ? N31 C31 P1 124.0(6) . . ? C31 N32 C33 104.4(8) . . ? C33 C32 N31 107.2(8) . . ? C33 C32 H32 126.4 . . ? N31 C32 H32 126.4 . . ? C32 C33 N32 109.9(8) . . ? C32 C33 H33 125.0 . . ? N32 C33 H33 125.0 . . ? N31 C34 H34A 109.5 . . ? N31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C42 C41 C46 113.8(8) . . ? C42 C41 Au1 122.5(6) . . ? C46 C41 Au1 123.6(7) . . ? F42 C42 C41 119.7(7) . . ? F42 C42 C43 115.6(8) . . ? C41 C42 C43 124.7(8) . . ? F43 C43 C42 122.0(8) . . ? F43 C43 C44 119.1(8) . . ? C42 C43 C44 118.8(9) . . ? F44 C44 C45 120.2(8) . . ? F44 C44 C43 120.9(9) . . ? C45 C44 C43 118.8(8) . . ? F45 C45 C44 119.4(8) . . ? F45 C45 C46 120.6(9) . . ? C44 C45 C46 120.0(8) . . ? F46 C46 C45 117.2(8) . . ? F46 C46 C41 118.9(7) . . ? C45 C46 C41 123.9(9) . . ? C52 C51 C56 115.0(8) . . ? C52 C51 Au2 123.9(6) . . ? C56 C51 Au2 120.8(7) . . ? C53 C52 F52 116.1(9) . . ? C53 C52 C51 124.2(8) . . ? F52 C52 C51 119.8(8) . . ? F53 C53 C54 119.4(8) . . ? F53 C53 C52 121.5(9) . . ? C54 C53 C52 119.1(9) . . ? F54 C54 C53 120.9(9) . . ? F54 C54 C55 119.5(8) . . ? C53 C54 C55 119.6(8) . . ? F55 C55 C54 119.5(8) . . ? F55 C55 C56 121.4(10) . . ? C54 C55 C56 119.1(9) . . ? F56 C56 C51 120.7(8) . . ? F56 C56 C55 116.4(9) . . ? C51 C56 C55 123.0(10) . . ? C98 C97 H97A 109.5 . . ? C98 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C98 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? O99 C98 C97 120.8(14) . . ? O99 C98 C99 119.3(13) . . ? C97 C98 C99 120(2) . . ? C98 C99 H99A 109.5 . . ? C98 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? C98 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? 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 Au2 Au1 P1 C21 -95.3(4) . . . . ? Au2 Au1 P1 C11 23.9(3) . . . . ? Au2 Au1 P1 C31 142.0(3) . . . . ? C41 Au1 Au2 C51 -26.0(4) . . . . ? P1 Au1 Au2 C51 157.8(3) . . . . ? C41 Au1 Au2 N12 155.2(3) . . . . ? P1 Au1 Au2 N12 -20.9(2) . . . . ? C12 N11 C11 N12 -0.4(10) . . . . ? C14 N11 C11 N12 -179.3(8) . . . . ? C12 N11 C11 P1 179.9(7) . . . . ? C14 N11 C11 P1 1.0(14) . . . . ? C21 P1 C11 N12 109.1(8) . . . . ? C31 P1 C11 N12 -144.2(7) . . . . ? Au1 P1 C11 N12 -20.9(8) . . . . ? C21 P1 C11 N11 -71.2(9) . . . . ? C31 P1 C11 N11 35.5(9) . . . . ? Au1 P1 C11 N11 158.8(7) . . . . ? N11 C11 N12 C13 0.0(10) . . . . ? P1 C11 N12 C13 179.8(7) . . . . ? N11 C11 N12 Au2 176.5(6) . . . . ? P1 C11 N12 Au2 -3.8(12) . . . . ? Au1 Au2 N12 C11 19.1(8) . . . . ? Au1 Au2 N12 C13 -165.0(8) . . . . ? C11 N11 C12 C13 0.6(11) . . . . ? C14 N11 C12 C13 179.6(9) . . . . ? N11 C12 C13 N12 -0.6(11) . . . . ? C11 N12 C13 C12 0.3(11) . . . . ? Au2 N12 C13 C12 -176.3(7) . . . . ? C22 N21 C21 N22 3.8(13) . . . . ? C24 N21 C21 N22 179.1(15) . . . . ? C22 N21 C21 P1 -177.4(8) . . . . ? C24 N21 C21 P1 -2.1(19) . . . . ? C11 P1 C21 N22 17.6(9) . . . . ? C31 P1 C21 N22 -91.3(9) . . . . ? Au1 P1 C21 N22 140.7(8) . . . . ? C11 P1 C21 N21 -161.1(8) . . . . ? C31 P1 C21 N21 90.0(9) . . . . ? Au1 P1 C21 N21 -38.0(9) . . . . ? N21 C21 N22 C23 -4.0(12) . . . . ? P1 C21 N22 C23 177.2(8) . . . . ? C21 N21 C22 C23 -1.8(14) . . . . ? C24 N21 C22 C23 -177.2(16) . . . . ? N21 C22 C23 N22 -0.5(16) . . . . ? C21 N22 C23 C22 2.8(14) . . . . ? C32 N31 C31 N32 2.2(9) . . . . ? C34 N31 C31 N32 -178.0(8) . . . . ? C32 N31 C31 P1 179.3(6) . . . . ? C34 N31 C31 P1 -0.9(12) . . . . ? C21 P1 C31 N32 -8.8(8) . . . . ? C11 P1 C31 N32 -115.5(7) . . . . ? Au1 P1 C31 N32 123.5(6) . . . . ? C21 P1 C31 N31 174.4(7) . . . . ? C11 P1 C31 N31 67.7(8) . . . . ? Au1 P1 C31 N31 -53.4(7) . . . . ? N31 C31 N32 C33 -1.7(10) . . . . ? P1 C31 N32 C33 -178.9(6) . . . . ? C31 N31 C32 C33 -1.7(10) . . . . ? C34 N31 C32 C33 178.5(8) . . . . ? N31 C32 C33 N32 0.7(11) . . . . ? C31 N32 C33 C32 0.6(11) . . . . ? Au2 Au1 C41 C42 -85.8(7) . . . . ? Au2 Au1 C41 C46 89.7(7) . . . . ? C46 C41 C42 F42 -178.7(7) . . . . ? Au1 C41 C42 F42 -2.8(11) . . . . ? C46 C41 C42 C43 -0.8(12) . . . . ? Au1 C41 C42 C43 175.0(6) . . . . ? F42 C42 C43 F43 -2.3(12) . . . . ? C41 C42 C43 F43 179.8(8) . . . . ? F42 C42 C43 C44 -179.9(7) . . . . ? C41 C42 C43 C44 2.1(13) . . . . ? F43 C43 C44 F44 2.2(12) . . . . ? C42 C43 C44 F44 179.9(7) . . . . ? F43 C43 C44 C45 -179.9(8) . . . . ? C42 C43 C44 C45 -2.2(12) . . . . ? F44 C44 C45 F45 -0.6(12) . . . . ? C43 C44 C45 F45 -178.5(7) . . . . ? F44 C44 C45 C46 179.1(7) . . . . ? C43 C44 C45 C46 1.2(13) . . . . ? F45 C45 C46 F46 0.5(11) . . . . ? C44 C45 C46 F46 -179.2(7) . . . . ? F45 C45 C46 C41 179.8(7) . . . . ? C44 C45 C46 C41 0.1(13) . . . . ? C42 C41 C46 F46 178.9(7) . . . . ? Au1 C41 C46 F46 3.1(11) . . . . ? C42 C41 C46 C45 -0.3(12) . . . . ? Au1 C41 C46 C45 -176.1(6) . . . . ? Au1 Au2 C51 C52 86.0(7) . . . . ? Au1 Au2 C51 C56 -86.5(7) . . . . ? C56 C51 C52 C53 -0.9(13) . . . . ? Au2 C51 C52 C53 -173.8(6) . . . . ? C56 C51 C52 F52 179.5(8) . . . . ? Au2 C51 C52 F52 6.6(12) . . . . ? F52 C52 C53 F53 -0.3(12) . . . . ? C51 C52 C53 F53 -179.9(8) . . . . ? F52 C52 C53 C54 -178.8(7) . . . . ? C51 C52 C53 C54 1.6(13) . . . . ? F53 C53 C54 F54 0.1(12) . . . . ? C52 C53 C54 F54 178.6(7) . . . . ? F53 C53 C54 C55 179.9(8) . . . . ? C52 C53 C54 C55 -1.6(12) . . . . ? F54 C54 C55 F55 1.1(13) . . . . ? C53 C54 C55 F55 -178.7(8) . . . . ? F54 C54 C55 C56 -179.3(7) . . . . ? C53 C54 C55 C56 0.9(13) . . . . ? C52 C51 C56 F56 178.6(8) . . . . ? Au2 C51 C56 F56 -8.2(12) . . . . ? C52 C51 C56 C55 0.2(13) . . . . ? Au2 C51 C56 C55 173.4(7) . . . . ? F55 C55 C56 F56 0.9(13) . . . . ? C54 C55 C56 F56 -178.7(8) . . . . ? F55 C55 C56 C51 179.4(8) . . . . ? C54 C55 C56 C51 -0.2(14) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.946 _refine_diff_density_min -1.770 _refine_diff_density_rms 0.244 #Compound 4Acetone ends #===END ###################################### ## 4 . 5/6 deuteriotrichloromethane ## ###################################### data_Compound4CDCl3 _database_code_depnum_ccdc_archive 'CCDC 659064' _audit_creation_method SHELXL-97 _chemical_name_systematic ;bis(pentafluorophenyl)-\m-[tris(1-methylimidazol-2-yl)phosphane-\k^2^P:N] digold(I) 5/6 deuteriotrichloromethane solvate ; _chemical_name_common ;bis(pentafluorophenyl)-\m-[tris(1-methylimidazol-2-yl)phosphine]digold(I) 5/6 deuteriochloroform solvate ; _chemical_melting_point ? _chemical_formula_moiety '(C24 H15 Au2 F10 N6 P), 0.83(C D Cl3)' _chemical_formula_sum 'C24.83 H15 Au2 Cl2.5 D0.83 F10 N6 P' _chemical_formula_weight 1103 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' D D 0.0000 0.0000 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3247(12) _cell_length_b 19.1230(19) _cell_length_c 20.242(2) _cell_angle_alpha 101.251(2) _cell_angle_beta 98.052(2) _cell_angle_gamma 100.106(2) _cell_volume 4530.7(8) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9212 _cell_measurement_theta_min 2.221 _cell_measurement_theta_max 26.427 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3074 _exptl_absorpt_coefficient_mu 10.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.240 _exptl_absorpt_correction_T_max 0.331 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area detector' _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_% ? _diffrn_reflns_number 47479 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.47 _reflns_number_total 18211 _reflns_number_gt 14419 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material X-Seed _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^)+(0.0324P)^2^+5.4135P] 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 18211 _refine_ls_number_parameters 1270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0622 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.705083(19) 0.010434(12) 0.638503(12) 0.01722(6) Uani 1 1 d . . . Au2 Au 0.722697(19) 0.060164(12) 0.791603(12) 0.01797(6) Uani 1 1 d . . . Au3 Au 0.635380(19) 0.420708(12) 0.100117(12) 0.01734(6) Uani 1 1 d . . . Au4 Au 0.76453(2) 0.367458(12) -0.008751(12) 0.01745(6) Uani 1 1 d . . . Au5 Au 0.566704(19) 0.321232(12) 0.270285(12) 0.01647(6) Uani 1 1 d . . . Au6 Au 0.587107(19) 0.368865(12) 0.422053(12) 0.01739(6) Uani 1 1 d . . . Cl11 Cl 0.90331(16) 0.97286(9) 0.05626(9) 0.0374(4) Uani 1 1 d . . . Cl12 Cl 0.74536(19) 0.87868(14) 0.10917(11) 0.0640(7) Uani 1 1 d . . . Cl13 Cl 0.9745(2) 0.85957(11) 0.11455(13) 0.0621(7) Uani 1 1 d . . . Cl21 Cl 1.1163(3) 0.71884(14) 0.3644(2) 0.147(2) Uani 1 1 d . . . Cl22 Cl 1.02398(18) 0.80437(11) 0.27915(11) 0.0488(5) Uani 1 1 d . . . Cl23 Cl 0.8886(3) 0.73526(14) 0.36244(13) 0.0926(11) Uani 1 1 d . . . Cl31 Cl 0.9559(4) 0.6012(2) 0.47155(19) 0.0452(10) Uani 0.50 1 d P . . Cl32 Cl 0.8882(2) 0.45911(16) 0.47003(16) 0.0905(10) Uani 1 1 d . . . P1 P 0.85082(13) -0.04105(8) 0.66925(8) 0.0167(3) Uani 1 1 d . . . P3 P 0.77261(13) 0.52337(8) 0.12553(8) 0.0170(3) Uani 1 1 d . . . P5 P 0.70557(13) 0.26226(8) 0.29630(8) 0.0155(3) Uani 1 1 d . . . F12 F 0.4515(3) -0.07091(18) 0.58932(19) 0.0264(9) Uani 1 1 d . . . F13 F 0.2671(3) -0.0284(2) 0.53781(19) 0.0280(9) Uani 1 1 d . . . F14 F 0.2786(3) 0.1103(2) 0.52280(19) 0.0308(9) Uani 1 1 d . . . F15 F 0.4792(3) 0.2064(2) 0.5574(2) 0.0341(10) Uani 1 1 d . . . F16 F 0.6660(3) 0.1650(2) 0.6067(2) 0.0307(9) Uani 1 1 d . . . F22 F 0.4708(3) 0.07283(18) 0.73726(19) 0.0266(9) Uani 1 1 d . . . F23 F 0.3903(3) 0.1860(2) 0.7064(2) 0.0359(10) Uani 1 1 d . . . F24 F 0.5253(4) 0.3218(2) 0.7371(2) 0.0440(11) Uani 1 1 d . . . F25 F 0.7417(4) 0.3424(2) 0.8017(2) 0.0439(11) Uani 1 1 d . . . F26 F 0.8243(3) 0.2296(2) 0.8305(2) 0.0319(9) Uani 1 1 d . . . F32 F 0.6111(3) 0.25209(19) 0.11072(18) 0.0256(8) Uani 1 1 d . . . F33 F 0.4316(3) 0.14274(19) 0.08881(19) 0.0307(9) Uani 1 1 d . . . F34 F 0.2233(3) 0.1656(2) 0.04756(19) 0.0326(10) Uani 1 1 d . . . F35 F 0.1968(3) 0.2976(2) 0.0261(2) 0.0310(9) Uani 1 1 d . . . F36 F 0.3743(3) 0.40755(19) 0.04749(19) 0.0277(9) Uani 1 1 d . . . F42 F 0.9194(3) 0.2660(2) 0.0405(2) 0.0352(10) Uani 1 1 d . . . F43 F 0.8831(3) 0.1226(2) 0.0319(2) 0.0471(12) Uani 1 1 d . . . F44 F 0.6785(4) 0.0361(2) -0.0280(2) 0.0458(12) Uani 1 1 d . . . F45 F 0.5116(4) 0.0967(2) -0.0796(2) 0.0451(11) Uani 1 1 d . . . F46 F 0.5464(3) 0.2399(2) -0.07258(19) 0.0327(9) Uani 1 1 d . . . F52 F 0.3158(3) 0.23784(18) 0.22420(18) 0.0248(8) Uani 1 1 d . . . F53 F 0.1270(3) 0.27722(19) 0.17564(19) 0.0288(9) Uani 1 1 d . . . F54 F 0.1296(3) 0.41645(19) 0.16683(18) 0.0250(8) Uani 1 1 d . . . F55 F 0.3257(3) 0.51743(19) 0.2023(2) 0.0290(9) Uani 1 1 d . . . F56 F 0.5169(3) 0.47937(19) 0.24761(18) 0.0258(8) Uani 1 1 d . . . F62 F 0.3293(3) 0.37382(19) 0.3897(2) 0.0304(9) Uani 1 1 d . . . F63 F 0.2261(3) 0.4819(2) 0.3693(2) 0.0372(10) Uani 1 1 d . . . F64 F 0.3465(3) 0.6190(2) 0.3832(2) 0.0362(10) Uani 1 1 d . . . F65 F 0.5742(3) 0.6471(2) 0.4209(2) 0.0392(10) Uani 1 1 d . . . F66 F 0.6792(3) 0.5399(2) 0.4401(2) 0.0297(9) Uani 1 1 d . . . N11 N 0.7987(4) -0.0264(3) 0.7991(2) 0.0161(11) Uani 1 1 d . . . N12 N 0.9019(4) -0.1081(3) 0.7801(3) 0.0176(11) Uani 1 1 d . . . N13 N 1.0769(4) 0.0093(3) 0.7214(3) 0.0222(12) Uani 1 1 d . . . N14 N 1.0234(4) 0.0449(3) 0.6259(3) 0.0208(12) Uani 1 1 d . . . N15 N 0.9319(4) -0.1388(3) 0.5803(3) 0.0223(12) Uani 1 1 d . . . N16 N 0.7609(4) -0.1850(3) 0.5939(3) 0.0206(12) Uani 1 1 d . . . N31 N 0.8154(4) 0.4772(2) -0.0041(2) 0.0146(11) Uani 1 1 d . . . N32 N 0.9074(4) 0.5899(3) 0.0410(3) 0.0173(11) Uani 1 1 d . . . N33 N 0.7954(5) 0.6646(3) 0.1938(3) 0.0348(15) Uani 1 1 d . . . N34 N 0.6292(4) 0.6242(3) 0.1266(3) 0.0233(12) Uani 1 1 d . . . N35 N 0.9944(4) 0.5425(3) 0.1855(3) 0.0223(12) Uani 1 1 d . . . N36 N 0.8767(4) 0.5275(3) 0.2591(3) 0.0214(12) Uani 1 1 d . . . N51 N 0.6636(4) 0.2824(3) 0.4291(2) 0.0154(11) Uani 1 1 d . . . N52 N 0.7477(4) 0.1905(3) 0.4047(3) 0.0177(11) Uani 1 1 d . . . N53 N 0.7702(4) 0.1633(3) 0.2005(3) 0.0229(12) Uani 1 1 d . . . N54 N 0.5999(4) 0.1213(3) 0.2194(3) 0.0215(12) Uani 1 1 d . . . N55 N 0.9241(4) 0.3015(3) 0.3608(3) 0.0241(12) Uani 1 1 d . . . N56 N 0.9008(4) 0.3375(3) 0.2625(3) 0.0199(12) Uani 1 1 d . . . C11 C 0.5670(5) 0.0452(3) 0.5995(3) 0.0197(14) Uani 1 1 d . . . C12 C 0.4632(5) -0.0009(3) 0.5814(3) 0.0202(14) Uani 1 1 d . . . C13 C 0.3664(5) 0.0196(3) 0.5555(3) 0.0183(13) Uani 1 1 d . . . C14 C 0.3727(5) 0.0885(4) 0.5470(3) 0.0228(15) Uani 1 1 d . . . C15 C 0.4731(6) 0.1370(4) 0.5646(3) 0.0253(15) Uani 1 1 d . . . C16 C 0.5672(5) 0.1145(3) 0.5895(3) 0.0214(14) Uani 1 1 d . . . C21 C 0.6520(5) 0.1455(3) 0.7832(3) 0.0205(14) Uani 1 1 d . . . C22 C 0.5422(5) 0.1389(3) 0.7538(3) 0.0212(14) Uani 1 1 d . . . C23 C 0.4987(5) 0.1960(4) 0.7375(3) 0.0254(15) Uani 1 1 d . . . C24 C 0.5676(6) 0.2654(4) 0.7528(4) 0.0310(17) Uani 1 1 d . . . C25 C 0.6757(6) 0.2750(3) 0.7847(3) 0.0261(15) Uani 1 1 d . . . C26 C 0.7158(5) 0.2161(3) 0.7989(3) 0.0205(14) Uani 1 1 d . . . C31 C 0.5018(5) 0.3346(3) 0.0801(3) 0.0184(13) Uani 1 1 d . . . C32 C 0.5098(5) 0.2662(3) 0.0893(3) 0.0171(13) Uani 1 1 d . . . C33 C 0.4201(5) 0.2088(3) 0.0782(3) 0.0223(14) Uani 1 1 d . . . C34 C 0.3139(5) 0.2203(3) 0.0571(3) 0.0216(14) Uani 1 1 d . . . C35 C 0.3002(5) 0.2872(4) 0.0460(3) 0.0220(14) Uani 1 1 d . . . C36 C 0.3938(5) 0.3419(3) 0.0576(3) 0.0222(14) Uani 1 1 d . . . C41 C 0.7338(5) 0.2597(3) -0.0155(3) 0.0188(13) Uani 1 1 d . . . C42 C 0.8153(6) 0.2261(3) 0.0096(3) 0.0248(15) Uani 1 1 d . . . C43 C 0.8003(6) 0.1524(4) 0.0062(4) 0.0325(17) Uani 1 1 d . . . C44 C 0.6976(7) 0.1093(3) -0.0231(4) 0.0320(17) Uani 1 1 d . . . C45 C 0.6131(6) 0.1396(4) -0.0493(3) 0.0285(16) Uani 1 1 d . . . C46 C 0.6333(6) 0.2133(3) -0.0455(3) 0.0237(15) Uani 1 1 d . . . C51 C 0.4255(5) 0.3569(3) 0.2383(3) 0.0194(14) Uani 1 1 d . . . C52 C 0.3227(5) 0.3090(3) 0.2193(3) 0.0192(14) Uani 1 1 d . . . C53 C 0.2251(5) 0.3265(3) 0.1951(3) 0.0197(14) Uani 1 1 d . . . C54 C 0.2250(5) 0.3974(3) 0.1890(3) 0.0176(13) Uani 1 1 d . . . C55 C 0.3248(5) 0.4479(3) 0.2076(3) 0.0228(14) Uani 1 1 d . . . C56 C 0.4212(5) 0.4269(3) 0.2307(3) 0.0180(13) Uani 1 1 d . . . C61 C 0.5098(5) 0.4519(3) 0.4149(3) 0.0160(13) Uani 1 1 d . . . C62 C 0.3938(5) 0.4411(3) 0.3979(3) 0.0206(14) Uani 1 1 d . . . C63 C 0.3391(5) 0.4957(4) 0.3880(3) 0.0227(15) Uani 1 1 d . . . C64 C 0.3992(6) 0.5653(4) 0.3949(3) 0.0264(16) Uani 1 1 d . . . C65 C 0.5144(5) 0.5787(3) 0.4125(3) 0.0235(15) Uani 1 1 d . . . C66 C 0.5659(5) 0.5226(3) 0.4227(3) 0.0210(14) Uani 1 1 d . . . C111 C 0.8533(5) -0.0601(3) 0.7534(3) 0.0192(14) Uani 1 1 d . . . C112 C 0.8156(5) -0.0545(3) 0.8557(3) 0.0185(13) Uani 1 1 d . . . H112 H 0.7872 -0.0408 0.8966 0.022 Uiso 1 1 calc R . . C113 C 0.8797(5) -0.1056(3) 0.8446(3) 0.0224(14) Uani 1 1 d . . . H113 H 0.9040 -0.1336 0.8754 0.027 Uiso 1 1 calc R . . C114 C 0.9691(6) -0.1568(4) 0.7473(4) 0.0309(17) Uani 1 1 d . . . H11A H 0.9193 -0.1974 0.7131 0.046 Uiso 1 1 calc R . . H11B H 1.0107 -0.1760 0.7821 0.046 Uiso 1 1 calc R . . H11C H 1.0220 -0.1295 0.7248 0.046 Uiso 1 1 calc R . . C121 C 0.9910(5) 0.0074(3) 0.6728(3) 0.0182(13) Uani 1 1 d . . . C122 C 1.1667(5) 0.0504(4) 0.7041(4) 0.0283(16) Uani 1 1 d . . . H122 H 1.2410 0.0617 0.7293 0.034 Uiso 1 1 calc R . . C123 C 1.1354(5) 0.0727(3) 0.6466(3) 0.0217(14) Uani 1 1 d . . . H123 H 1.1823 0.1020 0.6246 0.026 Uiso 1 1 calc R . . C124 C 0.9528(6) 0.0572(4) 0.5673(3) 0.0304(16) Uani 1 1 d . . . H12A H 0.9083 0.0104 0.5397 0.046 Uiso 1 1 calc R . . H12B H 0.9998 0.0809 0.5394 0.046 Uiso 1 1 calc R . . H12C H 0.9025 0.0886 0.5834 0.046 Uiso 1 1 calc R . . C131 C 0.8490(5) -0.1265(3) 0.6119(3) 0.0191(14) Uani 1 1 d . . . C132 C 0.8978(6) -0.2076(3) 0.5414(3) 0.0265(15) Uani 1 1 d . . . H132 H 0.9409 -0.2319 0.5128 0.032 Uiso 1 1 calc R . . C133 C 0.7916(6) -0.2370(3) 0.5494(3) 0.0268(16) Uani 1 1 d . . . H133 H 0.7486 -0.2844 0.5280 0.032 Uiso 1 1 calc R . . C134 C 0.6529(5) -0.1915(4) 0.6171(3) 0.0241(15) Uani 1 1 d . . . H13A H 0.6126 -0.1563 0.6014 0.036 Uiso 1 1 calc R . . H13B H 0.6656 -0.1818 0.6672 0.036 Uiso 1 1 calc R . . H13C H 0.6084 -0.2410 0.5981 0.036 Uiso 1 1 calc R . . C311 C 0.8393(5) 0.5315(3) 0.0533(3) 0.0162(13) Uani 1 1 d . . . C312 C 0.8710(5) 0.5017(3) -0.0509(3) 0.0217(14) Uani 1 1 d . . . H312 H 0.8707 0.4745 -0.0955 0.026 Uiso 1 1 calc R . . C313 C 0.9277(5) 0.5717(3) -0.0237(3) 0.0219(14) Uani 1 1 d . . . H313 H 0.9728 0.6020 -0.0459 0.026 Uiso 1 1 calc R . . C314 C 0.9593(6) 0.6602(3) 0.0884(3) 0.0289(16) Uani 1 1 d . . . H31A H 1.0176 0.6866 0.0687 0.043 Uiso 1 1 calc R . . H31B H 0.9929 0.6517 0.1322 0.043 Uiso 1 1 calc R . . H31C H 0.9021 0.6892 0.0958 0.043 Uiso 1 1 calc R . . C321 C 0.7280(5) 0.6074(3) 0.1512(3) 0.0196(14) Uani 1 1 d . . . C322 C 0.7391(6) 0.7201(4) 0.1962(5) 0.049(2) Uani 1 1 d . . . H322 H 0.7675 0.7686 0.2221 0.059 Uiso 1 1 calc R . . C323 C 0.6359(6) 0.6954(4) 0.1555(4) 0.0363(18) Uani 1 1 d . . . H323 H 0.5796 0.7228 0.1488 0.044 Uiso 1 1 calc R . . C324 C 0.5267(5) 0.5760(4) 0.0855(3) 0.0280(16) Uani 1 1 d . . . H32A H 0.4815 0.5547 0.1156 0.042 Uiso 1 1 calc R . . H32B H 0.5461 0.5370 0.0531 0.042 Uiso 1 1 calc R . . H32C H 0.4837 0.6040 0.0602 0.042 Uiso 1 1 calc R . . C331 C 0.8880(5) 0.5314(3) 0.1936(3) 0.0172(13) Uani 1 1 d . . . C332 C 1.0541(5) 0.5457(3) 0.2494(3) 0.0209(14) Uani 1 1 d . . . H332 H 1.1334 0.5535 0.2604 0.025 Uiso 1 1 calc R . . C333 C 0.9846(5) 0.5363(4) 0.2934(3) 0.0264(16) Uani 1 1 d . . . H333 H 1.0058 0.5358 0.3403 0.032 Uiso 1 1 calc R . . C334 C 0.7748(6) 0.5185(4) 0.2877(4) 0.0393(19) Uani 1 1 d . . . H33A H 0.7479 0.5642 0.2939 0.059 Uiso 1 1 calc R . . H33B H 0.7903 0.5055 0.3321 0.059 Uiso 1 1 calc R . . H33C H 0.7174 0.4796 0.2564 0.059 Uiso 1 1 calc R . . C511 C 0.7027(5) 0.2416(3) 0.3794(3) 0.0179(13) Uani 1 1 d . . . C512 C 0.6865(5) 0.2563(3) 0.4860(3) 0.0235(15) Uani 1 1 d . . . H512 H 0.6686 0.2748 0.5293 0.028 Uiso 1 1 calc R . . C513 C 0.7384(5) 0.2001(3) 0.4720(3) 0.0233(14) Uani 1 1 d . . . H513 H 0.7636 0.1725 0.5030 0.028 Uiso 1 1 calc R . . C514 C 0.7999(5) 0.1351(3) 0.3680(3) 0.0220(14) Uani 1 1 d . . . H51A H 0.7415 0.0956 0.3384 0.033 Uiso 1 1 calc R . . H51B H 0.8446 0.1155 0.4011 0.033 Uiso 1 1 calc R . . H51C H 0.8485 0.1573 0.3400 0.033 Uiso 1 1 calc R . . C521 C 0.6913(5) 0.1771(3) 0.2361(3) 0.0201(14) Uani 1 1 d . . . C522 C 0.7264(6) 0.0955(3) 0.1589(4) 0.0303(16) Uani 1 1 d . . . H522 H 0.7631 0.0710 0.1261 0.036 Uiso 1 1 calc R . . C523 C 0.6235(6) 0.0684(4) 0.1709(4) 0.0298(16) Uani 1 1 d . . . H523 H 0.5773 0.0219 0.1499 0.036 Uiso 1 1 calc R . . C524 C 0.4978(5) 0.1174(3) 0.2483(4) 0.0263(16) Uani 1 1 d . . . H52A H 0.5168 0.1246 0.2982 0.040 Uiso 1 1 calc R . . H52B H 0.4484 0.0696 0.2290 0.040 Uiso 1 1 calc R . . H52C H 0.4595 0.1556 0.2372 0.040 Uiso 1 1 calc R . . C531 C 0.8515(5) 0.3017(3) 0.3063(3) 0.0190(14) Uani 1 1 d . . . C532 C 1.0244(5) 0.3385(3) 0.3513(4) 0.0247(15) Uani 1 1 d . . . H532 H 1.0934 0.3468 0.3821 0.030 Uiso 1 1 calc R . . C533 C 1.0116(5) 0.3614(3) 0.2921(3) 0.0237(15) Uani 1 1 d . . . H533 H 1.0682 0.3887 0.2745 0.028 Uiso 1 1 calc R . . C534 C 0.8506(5) 0.3430(4) 0.1952(3) 0.0268(15) Uani 1 1 d . . . H53A H 0.8400 0.2958 0.1630 0.040 Uiso 1 1 calc R . . H53B H 0.8999 0.3802 0.1799 0.040 Uiso 1 1 calc R . . H53C H 0.7779 0.3566 0.1972 0.040 Uiso 1 1 calc R . . C1 C 0.8868(6) 0.9220(4) 0.1188(4) 0.0356(18) Uani 1 1 d . . . D1 D 0.9089 0.9563 0.1648 0.043 Uiso 1 1 calc R . . C2 C 0.9955(7) 0.7282(4) 0.3143(4) 0.052(2) Uani 1 1 d . . . D2 D 0.9696 0.6839 0.2761 0.063 Uiso 1 1 calc R . . C3 C 0.9738(12) 0.5351(8) 0.5188(7) 0.036(4) Uani 0.50 1 d P . . D3 D 0.9498 0.5482 0.5640 0.044 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01758(12) 0.01698(12) 0.01815(13) 0.00526(10) 0.00339(10) 0.00480(10) Au2 0.01945(12) 0.01567(12) 0.01815(13) 0.00241(10) 0.00474(10) 0.00244(10) Au3 0.01652(12) 0.01732(13) 0.01666(13) 0.00313(10) 0.00292(9) 0.00029(9) Au4 0.02213(13) 0.01298(12) 0.01758(13) 0.00322(9) 0.00526(10) 0.00348(9) Au5 0.01712(12) 0.01654(12) 0.01691(13) 0.00461(9) 0.00237(10) 0.00621(9) Au6 0.02033(13) 0.01526(12) 0.01706(13) 0.00295(10) 0.00429(10) 0.00506(10) Cl11 0.0439(11) 0.0250(9) 0.0357(10) 0.0092(8) -0.0098(8) -0.0026(8) Cl12 0.0533(13) 0.0835(17) 0.0334(12) -0.0040(11) 0.0115(10) -0.0271(12) Cl13 0.0806(17) 0.0324(11) 0.0712(16) 0.0167(11) -0.0097(13) 0.0192(11) Cl21 0.141(3) 0.0393(15) 0.194(4) 0.0138(19) -0.137(3) -0.0103(17) Cl22 0.0588(13) 0.0382(11) 0.0506(13) 0.0053(10) 0.0176(11) 0.0121(10) Cl23 0.179(3) 0.0574(16) 0.0419(15) 0.0110(12) 0.0508(18) 0.0026(18) Cl31 0.062(3) 0.042(2) 0.031(2) 0.0054(17) 0.0021(19) 0.017(2) Cl32 0.0527(15) 0.085(2) 0.104(2) -0.0256(17) 0.0103(15) -0.0087(14) P1 0.0153(8) 0.0162(8) 0.0185(8) 0.0045(7) 0.0037(6) 0.0019(6) P3 0.0162(8) 0.0160(8) 0.0179(8) 0.0025(7) 0.0021(7) 0.0032(6) P5 0.0148(8) 0.0131(8) 0.0197(8) 0.0048(6) 0.0045(6) 0.0030(6) F12 0.029(2) 0.0143(18) 0.037(2) 0.0094(16) 0.0018(17) 0.0048(16) F13 0.0200(19) 0.030(2) 0.036(2) 0.0150(18) 0.0022(17) 0.0044(16) F14 0.031(2) 0.038(2) 0.033(2) 0.0201(19) 0.0091(18) 0.0182(19) F15 0.041(2) 0.021(2) 0.048(3) 0.0194(19) 0.010(2) 0.0106(18) F16 0.031(2) 0.028(2) 0.037(2) 0.0156(18) 0.0081(18) 0.0049(17) F22 0.0201(19) 0.0181(19) 0.037(2) -0.0013(16) 0.0063(17) -0.0007(15) F23 0.033(2) 0.037(2) 0.039(2) 0.0036(19) 0.0038(19) 0.0177(19) F24 0.058(3) 0.029(2) 0.055(3) 0.019(2) 0.016(2) 0.022(2) F25 0.051(3) 0.018(2) 0.060(3) 0.006(2) 0.010(2) -0.0006(19) F26 0.025(2) 0.026(2) 0.039(2) 0.0036(18) -0.0006(18) -0.0033(17) F32 0.025(2) 0.028(2) 0.023(2) 0.0070(16) 0.0016(16) 0.0063(17) F33 0.040(2) 0.018(2) 0.034(2) 0.0105(17) 0.0044(19) 0.0030(17) F34 0.032(2) 0.031(2) 0.030(2) 0.0081(18) 0.0059(18) -0.0095(18) F35 0.0186(19) 0.035(2) 0.039(2) 0.0105(19) 0.0033(17) 0.0035(17) F36 0.028(2) 0.022(2) 0.036(2) 0.0100(17) 0.0055(17) 0.0073(16) F42 0.030(2) 0.031(2) 0.049(3) 0.019(2) 0.008(2) 0.0049(18) F43 0.042(3) 0.037(3) 0.081(4) 0.035(2) 0.026(2) 0.023(2) F44 0.066(3) 0.015(2) 0.066(3) 0.013(2) 0.033(3) 0.012(2) F45 0.052(3) 0.025(2) 0.047(3) -0.003(2) 0.007(2) -0.009(2) F46 0.035(2) 0.029(2) 0.031(2) 0.0035(18) 0.0002(18) 0.0050(18) F52 0.030(2) 0.0163(19) 0.031(2) 0.0096(16) 0.0043(17) 0.0094(16) F53 0.0191(19) 0.026(2) 0.039(2) 0.0107(18) -0.0015(17) 0.0010(16) F54 0.025(2) 0.031(2) 0.027(2) 0.0164(17) 0.0051(16) 0.0158(17) F55 0.032(2) 0.019(2) 0.041(2) 0.0132(17) 0.0069(18) 0.0103(17) F56 0.0215(19) 0.023(2) 0.031(2) 0.0048(17) 0.0033(16) 0.0032(16) F62 0.025(2) 0.021(2) 0.042(2) 0.0059(18) 0.0046(18) -0.0010(16) F63 0.025(2) 0.037(2) 0.049(3) 0.005(2) 0.0016(19) 0.0122(19) F64 0.045(2) 0.026(2) 0.038(2) 0.0021(18) -0.001(2) 0.0210(19) F65 0.041(2) 0.020(2) 0.053(3) 0.0079(19) 0.002(2) 0.0029(18) F66 0.0194(19) 0.027(2) 0.039(2) 0.0043(18) 0.0002(17) 0.0019(16) N11 0.015(3) 0.016(3) 0.018(3) 0.004(2) 0.002(2) 0.006(2) N12 0.013(2) 0.020(3) 0.021(3) 0.006(2) 0.004(2) 0.003(2) N13 0.015(3) 0.027(3) 0.023(3) 0.005(2) 0.005(2) 0.001(2) N14 0.019(3) 0.021(3) 0.022(3) 0.004(2) 0.006(2) 0.003(2) N15 0.019(3) 0.025(3) 0.026(3) 0.006(2) 0.008(2) 0.010(2) N16 0.019(3) 0.019(3) 0.024(3) 0.008(2) 0.004(2) 0.002(2) N31 0.018(3) 0.010(2) 0.020(3) 0.009(2) 0.005(2) 0.008(2) N32 0.015(3) 0.015(3) 0.019(3) 0.002(2) 0.003(2) -0.003(2) N33 0.026(3) 0.028(3) 0.043(4) -0.011(3) 0.000(3) 0.011(3) N34 0.020(3) 0.022(3) 0.028(3) 0.002(2) 0.004(2) 0.008(2) N35 0.019(3) 0.020(3) 0.027(3) 0.005(2) 0.004(2) 0.003(2) N36 0.024(3) 0.023(3) 0.017(3) 0.008(2) 0.002(2) -0.001(2) N51 0.022(3) 0.012(2) 0.014(3) 0.002(2) 0.007(2) 0.006(2) N52 0.017(3) 0.020(3) 0.019(3) 0.009(2) 0.005(2) 0.008(2) N53 0.021(3) 0.025(3) 0.024(3) 0.006(2) 0.005(2) 0.008(2) N54 0.016(3) 0.020(3) 0.025(3) 0.002(2) 0.001(2) -0.002(2) N55 0.019(3) 0.029(3) 0.025(3) 0.014(2) -0.001(2) 0.001(2) N56 0.024(3) 0.016(3) 0.021(3) 0.008(2) 0.004(2) 0.002(2) C11 0.020(3) 0.023(3) 0.019(3) 0.007(3) 0.006(3) 0.008(3) C12 0.024(3) 0.019(3) 0.021(3) 0.008(3) 0.008(3) 0.007(3) C13 0.018(3) 0.025(3) 0.010(3) 0.004(3) 0.000(2) 0.002(3) C14 0.027(4) 0.030(4) 0.020(3) 0.015(3) 0.007(3) 0.016(3) C15 0.037(4) 0.023(4) 0.025(4) 0.016(3) 0.011(3) 0.015(3) C16 0.024(3) 0.021(3) 0.020(3) 0.007(3) 0.007(3) 0.003(3) C21 0.030(4) 0.017(3) 0.016(3) 0.003(3) 0.010(3) 0.006(3) C22 0.024(3) 0.018(3) 0.021(3) 0.000(3) 0.009(3) 0.004(3) C23 0.024(4) 0.031(4) 0.019(4) 0.003(3) -0.002(3) 0.008(3) C24 0.046(5) 0.021(4) 0.033(4) 0.012(3) 0.015(4) 0.011(3) C25 0.029(4) 0.019(3) 0.028(4) 0.001(3) 0.006(3) 0.000(3) C26 0.020(3) 0.018(3) 0.021(3) -0.001(3) 0.002(3) 0.003(3) C31 0.021(3) 0.018(3) 0.010(3) 0.000(2) -0.002(3) -0.004(3) C32 0.019(3) 0.020(3) 0.010(3) -0.003(2) 0.006(2) 0.003(3) C33 0.029(4) 0.022(3) 0.019(3) 0.004(3) 0.013(3) 0.008(3) C34 0.022(3) 0.024(4) 0.014(3) 0.001(3) 0.006(3) -0.007(3) C35 0.017(3) 0.028(4) 0.020(3) 0.010(3) 0.001(3) 0.000(3) C36 0.029(4) 0.020(3) 0.020(3) 0.010(3) 0.008(3) 0.004(3) C41 0.029(4) 0.011(3) 0.018(3) 0.006(3) 0.005(3) 0.005(3) C42 0.032(4) 0.020(3) 0.025(4) 0.006(3) 0.009(3) 0.004(3) C43 0.047(5) 0.017(4) 0.043(5) 0.012(3) 0.021(4) 0.016(3) C44 0.054(5) 0.007(3) 0.036(4) 0.002(3) 0.018(4) 0.006(3) C45 0.031(4) 0.029(4) 0.020(4) 0.005(3) 0.002(3) -0.007(3) C46 0.036(4) 0.016(3) 0.018(3) 0.000(3) 0.008(3) 0.003(3) C51 0.014(3) 0.020(3) 0.021(3) -0.001(3) 0.000(3) 0.005(3) C52 0.024(3) 0.013(3) 0.022(3) 0.003(3) 0.008(3) 0.004(3) C53 0.023(3) 0.023(3) 0.015(3) 0.006(3) 0.002(3) 0.008(3) C54 0.013(3) 0.026(3) 0.015(3) 0.007(3) 0.002(2) 0.006(3) C55 0.030(4) 0.020(3) 0.023(4) 0.007(3) 0.009(3) 0.010(3) C56 0.021(3) 0.021(3) 0.014(3) 0.006(3) 0.006(3) 0.006(3) C61 0.025(3) 0.010(3) 0.012(3) -0.002(2) -0.001(3) 0.011(3) C62 0.033(4) 0.020(3) 0.011(3) 0.006(3) 0.004(3) 0.009(3) C63 0.017(3) 0.032(4) 0.017(3) 0.000(3) -0.001(3) 0.009(3) C64 0.041(4) 0.024(4) 0.019(4) 0.007(3) 0.004(3) 0.020(3) C65 0.031(4) 0.012(3) 0.025(4) 0.001(3) 0.000(3) 0.004(3) C66 0.026(4) 0.024(4) 0.015(3) 0.006(3) 0.006(3) 0.008(3) C111 0.018(3) 0.016(3) 0.024(3) 0.007(3) -0.001(3) 0.004(3) C112 0.017(3) 0.016(3) 0.020(3) 0.001(3) 0.004(3) -0.001(3) C113 0.022(3) 0.026(4) 0.018(3) 0.008(3) 0.005(3) 0.000(3) C114 0.026(4) 0.043(4) 0.034(4) 0.017(3) 0.012(3) 0.020(3) C121 0.018(3) 0.017(3) 0.020(3) 0.004(3) 0.005(3) 0.006(3) C122 0.015(3) 0.031(4) 0.035(4) 0.000(3) 0.002(3) 0.005(3) C123 0.019(3) 0.018(3) 0.024(4) -0.002(3) 0.008(3) -0.002(3) C124 0.031(4) 0.035(4) 0.027(4) 0.013(3) 0.002(3) 0.006(3) C131 0.016(3) 0.018(3) 0.022(3) 0.007(3) -0.002(3) 0.000(3) C132 0.039(4) 0.020(4) 0.025(4) 0.004(3) 0.012(3) 0.012(3) C133 0.034(4) 0.012(3) 0.028(4) -0.002(3) -0.001(3) 0.002(3) C134 0.019(3) 0.025(4) 0.026(4) 0.003(3) 0.006(3) 0.001(3) C311 0.020(3) 0.007(3) 0.018(3) 0.001(2) -0.006(3) 0.000(2) C312 0.030(4) 0.027(4) 0.009(3) 0.004(3) 0.002(3) 0.008(3) C313 0.020(3) 0.024(4) 0.026(4) 0.013(3) 0.006(3) 0.005(3) C314 0.039(4) 0.015(3) 0.028(4) 0.005(3) -0.001(3) -0.003(3) C321 0.017(3) 0.021(3) 0.016(3) -0.002(3) 0.003(3) 0.001(3) C322 0.040(5) 0.024(4) 0.073(6) -0.014(4) 0.002(4) 0.017(4) C323 0.027(4) 0.029(4) 0.047(5) -0.005(3) 0.002(3) 0.010(3) C324 0.025(4) 0.028(4) 0.027(4) 0.004(3) -0.006(3) 0.006(3) C331 0.020(3) 0.007(3) 0.021(3) -0.001(2) 0.004(3) -0.004(2) C332 0.014(3) 0.026(4) 0.018(3) 0.003(3) -0.003(3) 0.001(3) C333 0.030(4) 0.029(4) 0.015(3) 0.007(3) -0.009(3) 0.000(3) C334 0.033(4) 0.055(5) 0.032(4) 0.012(4) 0.017(3) 0.001(4) C511 0.014(3) 0.017(3) 0.022(3) 0.007(3) 0.003(3) 0.000(2) C512 0.027(4) 0.023(4) 0.021(4) 0.002(3) 0.010(3) 0.006(3) C513 0.029(4) 0.022(4) 0.018(3) 0.008(3) 0.002(3) 0.004(3) C514 0.024(3) 0.028(4) 0.025(4) 0.015(3) 0.012(3) 0.018(3) C521 0.018(3) 0.021(3) 0.025(4) 0.008(3) 0.007(3) 0.006(3) C522 0.042(4) 0.016(3) 0.031(4) 0.000(3) 0.006(3) 0.007(3) C523 0.033(4) 0.016(3) 0.032(4) -0.003(3) -0.002(3) 0.001(3) C524 0.019(3) 0.018(3) 0.043(4) 0.004(3) 0.013(3) 0.002(3) C531 0.015(3) 0.013(3) 0.022(3) 0.002(3) -0.002(3) -0.006(2) C532 0.010(3) 0.026(4) 0.038(4) 0.011(3) 0.000(3) 0.003(3) C533 0.018(3) 0.015(3) 0.036(4) 0.008(3) -0.002(3) 0.000(3) C534 0.024(4) 0.028(4) 0.025(4) 0.009(3) 0.002(3) -0.002(3) C1 0.044(5) 0.032(4) 0.026(4) 0.006(3) 0.005(3) -0.005(3) C2 0.072(6) 0.025(4) 0.042(5) 0.001(4) -0.027(4) 0.002(4) C3 0.034(8) 0.047(10) 0.019(8) 0.000(7) -0.010(6) 0.006(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C11 2.047(6) . ? Au1 P1 2.2648(16) . ? Au1 Au2 3.0240(4) . ? Au2 C21 2.004(6) . ? Au2 N11 2.060(5) . ? Au3 C31 2.046(6) . ? Au3 P3 2.2752(16) . ? Au3 Au4 3.0170(4) . ? Au4 C41 2.003(6) . ? Au4 N31 2.062(5) . ? Au5 C51 2.045(6) . ? Au5 P5 2.2660(16) . ? Au5 Au6 2.9903(4) . ? Au6 C61 2.008(6) . ? Au6 N51 2.060(5) . ? Cl11 C1 1.754(7) . ? Cl12 C1 1.759(7) . ? Cl13 C1 1.743(8) . ? Cl21 C2 1.737(8) . ? Cl22 C2 1.746(8) . ? Cl23 C2 1.753(10) . ? Cl31 C3 1.753(15) . ? Cl32 C3 1.665(14) 2_766 ? Cl32 C3 1.676(14) . ? P1 C121 1.797(6) . ? P1 C131 1.805(6) . ? P1 C111 1.808(6) . ? P3 C311 1.793(6) . ? P3 C321 1.794(6) . ? P3 C331 1.799(6) . ? P5 C531 1.791(6) . ? P5 C521 1.797(6) . ? P5 C511 1.804(6) . ? F12 C12 1.364(7) . ? F13 C13 1.351(7) . ? F14 C14 1.360(7) . ? F15 C15 1.353(7) . ? F16 C16 1.369(7) . ? F22 C22 1.357(7) . ? F23 C23 1.359(7) . ? F24 C24 1.349(7) . ? F25 C25 1.350(7) . ? F26 C26 1.356(7) . ? F32 C32 1.353(7) . ? F33 C33 1.349(7) . ? F34 C34 1.352(7) . ? F35 C35 1.342(7) . ? F36 C36 1.367(7) . ? F42 C42 1.366(7) . ? F43 C43 1.344(8) . ? F44 C44 1.360(7) . ? F45 C45 1.357(7) . ? F46 C46 1.357(7) . ? F52 C52 1.372(7) . ? F53 C53 1.351(7) . ? F54 C54 1.335(7) . ? F55 C55 1.353(7) . ? F56 C56 1.361(7) . ? F62 C62 1.354(7) . ? F63 C63 1.355(7) . ? F64 C64 1.349(7) . ? F65 C65 1.350(7) . ? F66 C66 1.355(7) . ? N11 C111 1.349(8) . ? N11 C112 1.363(8) . ? N12 C111 1.337(7) . ? N12 C113 1.365(8) . ? N12 C114 1.476(8) . ? N13 C121 1.331(7) . ? N13 C122 1.369(8) . ? N14 C121 1.360(8) . ? N14 C123 1.362(8) . ? N14 C124 1.452(8) . ? N15 C131 1.310(8) . ? N15 C132 1.355(8) . ? N16 C133 1.350(8) . ? N16 C131 1.366(7) . ? N16 C134 1.465(8) . ? N31 C312 1.352(8) . ? N31 C311 1.357(7) . ? N32 C313 1.359(8) . ? N32 C311 1.361(7) . ? N32 C314 1.470(8) . ? N33 C321 1.321(8) . ? N33 C322 1.364(9) . ? N34 C323 1.357(8) . ? N34 C321 1.364(8) . ? N34 C324 1.462(8) . ? N35 C331 1.331(8) . ? N35 C332 1.379(8) . ? N36 C331 1.366(8) . ? N36 C333 1.377(8) . ? N36 C334 1.452(8) . ? N51 C511 1.348(7) . ? N51 C512 1.356(8) . ? N52 C511 1.353(7) . ? N52 C513 1.362(8) . ? N52 C514 1.469(7) . ? N53 C521 1.323(8) . ? N53 C522 1.371(8) . ? N54 C521 1.361(7) . ? N54 C523 1.368(8) . ? N54 C524 1.456(8) . ? N55 C531 1.320(7) . ? N55 C532 1.370(8) . ? N56 C531 1.365(8) . ? N56 C533 1.369(8) . ? N56 C534 1.446(8) . ? C11 C12 1.377(9) . ? C11 C16 1.377(8) . ? C12 C13 1.386(8) . ? C13 C14 1.351(9) . ? C14 C15 1.366(9) . ? C15 C16 1.373(9) . ? C21 C22 1.374(9) . ? C21 C26 1.390(8) . ? C22 C23 1.374(9) . ? C23 C24 1.397(9) . ? C24 C25 1.362(10) . ? C25 C26 1.370(9) . ? C31 C32 1.376(8) . ? C31 C36 1.384(9) . ? C32 C33 1.374(8) . ? C33 C34 1.387(9) . ? C34 C35 1.376(9) . ? C35 C36 1.373(8) . ? C41 C46 1.372(9) . ? C41 C42 1.374(9) . ? C42 C43 1.377(9) . ? C43 C44 1.366(10) . ? C44 C45 1.370(10) . ? C45 C46 1.373(9) . ? C51 C52 1.383(8) . ? C51 C56 1.386(8) . ? C52 C53 1.356(8) . ? C53 C54 1.386(8) . ? C54 C55 1.377(8) . ? C55 C56 1.371(9) . ? C61 C66 1.374(8) . ? C61 C62 1.392(9) . ? C62 C63 1.370(9) . ? C63 C64 1.375(9) . ? C64 C65 1.379(9) . ? C65 C66 1.373(9) . ? C112 C113 1.365(9) . ? C112 H112 0.9500 . ? C113 H113 0.9500 . ? C114 H11A 0.9800 . ? C114 H11B 0.9800 . ? C114 H11C 0.9800 . ? C122 C123 1.347(9) . ? C122 H122 0.9500 . ? C123 H123 0.9500 . ? C124 H12A 0.9800 . ? C124 H12B 0.9800 . ? C124 H12C 0.9800 . ? C132 C133 1.376(9) . ? C132 H132 0.9500 . ? C133 H133 0.9500 . ? C134 H13A 0.9800 . ? C134 H13B 0.9800 . ? C134 H13C 0.9800 . ? C312 C313 1.364(9) . ? C312 H312 0.9500 . ? C313 H313 0.9500 . ? C314 H31A 0.9800 . ? C314 H31B 0.9800 . ? C314 H31C 0.9800 . ? C322 C323 1.364(10) . ? C322 H322 0.9500 . ? C323 H323 0.9500 . ? C324 H32A 0.9800 . ? C324 H32B 0.9800 . ? C324 H32C 0.9800 . ? C332 C333 1.336(9) . ? C332 H332 0.9500 . ? C333 H333 0.9500 . ? C334 H33A 0.9800 . ? C334 H33B 0.9800 . ? C334 H33C 0.9800 . ? C512 C513 1.348(9) . ? C512 H512 0.9500 . ? C513 H513 0.9500 . ? C514 H51A 0.9800 . ? C514 H51B 0.9800 . ? C514 H51C 0.9800 . ? C522 C523 1.357(10) . ? C522 H522 0.9500 . ? C523 H523 0.9500 . ? C524 H52A 0.9800 . ? C524 H52B 0.9800 . ? C524 H52C 0.9800 . ? C532 C533 1.354(9) . ? C532 H532 0.9500 . ? C533 H533 0.9500 . ? C534 H53A 0.9800 . ? C534 H53B 0.9800 . ? C534 H53C 0.9800 . ? C1 D1 1.0000 . ? C2 D2 1.0000 . ? C3 D3 1.0000 . ? 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 C11 Au1 P1 172.24(18) . . ? C11 Au1 Au2 103.23(17) . . ? P1 Au1 Au2 83.28(4) . . ? C21 Au2 N11 178.5(2) . . ? C21 Au2 Au1 93.27(17) . . ? N11 Au2 Au1 86.04(14) . . ? C31 Au3 P3 174.54(18) . . ? C31 Au3 Au4 100.20(17) . . ? P3 Au3 Au4 84.43(4) . . ? C41 Au4 N31 173.0(2) . . ? C41 Au4 Au3 102.46(17) . . ? N31 Au4 Au3 83.28(13) . . ? C51 Au5 P5 170.07(17) . . ? C51 Au5 Au6 100.16(17) . . ? P5 Au5 Au6 84.71(4) . . ? C61 Au6 N51 179.0(2) . . ? C61 Au6 Au5 93.18(16) . . ? N51 Au6 Au5 86.73(13) . . ? C3 Cl32 C3 60.6(9) 2_766 . ? C121 P1 C131 101.1(3) . . ? C121 P1 C111 103.7(3) . . ? C131 P1 C111 106.1(3) . . ? C121 P1 Au1 119.0(2) . . ? C131 P1 Au1 113.5(2) . . ? C111 P1 Au1 112.0(2) . . ? C311 P3 C321 106.4(3) . . ? C311 P3 C331 103.4(3) . . ? C321 P3 C331 101.6(3) . . ? C311 P3 Au3 110.75(19) . . ? C321 P3 Au3 115.5(2) . . ? C331 P3 Au3 117.8(2) . . ? C531 P5 C521 102.5(3) . . ? C531 P5 C511 99.8(3) . . ? C521 P5 C511 107.0(3) . . ? C531 P5 Au5 123.7(2) . . ? C521 P5 Au5 112.4(2) . . ? C511 P5 Au5 109.9(2) . . ? C111 N11 C112 106.5(5) . . ? C111 N11 Au2 127.3(4) . . ? C112 N11 Au2 125.7(4) . . ? C111 N12 C113 108.8(5) . . ? C111 N12 C114 127.3(5) . . ? C113 N12 C114 123.9(5) . . ? C121 N13 C122 104.4(5) . . ? C121 N14 C123 106.4(5) . . ? C121 N14 C124 127.4(5) . . ? C123 N14 C124 126.1(5) . . ? C131 N15 C132 105.6(5) . . ? C133 N16 C131 106.7(5) . . ? C133 N16 C134 125.5(5) . . ? C131 N16 C134 127.8(5) . . ? C312 N31 C311 107.4(5) . . ? C312 N31 Au4 121.9(4) . . ? C311 N31 Au4 126.1(4) . . ? C313 N32 C311 108.4(5) . . ? C313 N32 C314 123.1(5) . . ? C311 N32 C314 128.4(5) . . ? C321 N33 C322 105.9(6) . . ? C323 N34 C321 106.7(5) . . ? C323 N34 C324 123.4(5) . . ? C321 N34 C324 129.3(5) . . ? C331 N35 C332 104.3(5) . . ? C331 N36 C333 104.8(5) . . ? C331 N36 C334 128.4(5) . . ? C333 N36 C334 126.9(6) . . ? C511 N51 C512 106.3(5) . . ? C511 N51 Au6 127.5(4) . . ? C512 N51 Au6 126.2(4) . . ? C511 N52 C513 107.8(5) . . ? C511 N52 C514 127.1(5) . . ? C513 N52 C514 125.0(5) . . ? C521 N53 C522 104.6(5) . . ? C521 N54 C523 106.4(5) . . ? C521 N54 C524 127.2(5) . . ? C523 N54 C524 126.4(5) . . ? C531 N55 C532 104.8(5) . . ? C531 N56 C533 106.1(5) . . ? C531 N56 C534 127.6(5) . . ? C533 N56 C534 126.0(5) . . ? C12 C11 C16 114.2(6) . . ? C12 C11 Au1 120.9(5) . . ? C16 C11 Au1 124.9(5) . . ? F12 C12 C11 120.0(5) . . ? F12 C12 C13 116.4(5) . . ? C11 C12 C13 123.6(6) . . ? F13 C13 C14 120.0(5) . . ? F13 C13 C12 121.0(5) . . ? C14 C13 C12 119.1(6) . . ? C13 C14 F14 120.2(6) . . ? C13 C14 C15 120.1(6) . . ? F14 C14 C15 119.7(6) . . ? F15 C15 C14 120.2(6) . . ? F15 C15 C16 120.7(6) . . ? C14 C15 C16 119.1(6) . . ? F16 C16 C15 117.2(6) . . ? F16 C16 C11 118.9(5) . . ? C15 C16 C11 123.9(6) . . ? C22 C21 C26 114.7(6) . . ? C22 C21 Au2 123.6(5) . . ? C26 C21 Au2 121.3(5) . . ? F22 C22 C23 116.2(6) . . ? F22 C22 C21 120.3(6) . . ? C23 C22 C21 123.5(6) . . ? F23 C23 C22 121.2(6) . . ? F23 C23 C24 119.6(6) . . ? C22 C23 C24 119.3(6) . . ? F24 C24 C25 121.4(6) . . ? F24 C24 C23 119.5(6) . . ? C25 C24 C23 119.1(6) . . ? F25 C25 C24 119.3(6) . . ? F25 C25 C26 121.2(6) . . ? C24 C25 C26 119.5(6) . . ? F26 C26 C25 116.3(5) . . ? F26 C26 C21 119.8(6) . . ? C25 C26 C21 123.9(6) . . ? C32 C31 C36 114.4(5) . . ? C32 C31 Au3 123.9(4) . . ? C36 C31 Au3 121.7(5) . . ? F32 C32 C33 115.7(5) . . ? F32 C32 C31 120.0(5) . . ? C33 C32 C31 124.4(6) . . ? F33 C33 C32 122.4(6) . . ? F33 C33 C34 119.4(6) . . ? C32 C33 C34 118.2(6) . . ? F34 C34 C35 119.7(6) . . ? F34 C34 C33 119.9(6) . . ? C35 C34 C33 120.4(6) . . ? F35 C35 C36 122.3(6) . . ? F35 C35 C34 119.6(5) . . ? C36 C35 C34 118.1(6) . . ? F36 C36 C35 115.3(6) . . ? F36 C36 C31 120.1(5) . . ? C35 C36 C31 124.5(6) . . ? C46 C41 C42 114.5(6) . . ? C46 C41 Au4 124.3(5) . . ? C42 C41 Au4 121.2(5) . . ? F42 C42 C41 120.4(6) . . ? F42 C42 C43 115.3(6) . . ? C41 C42 C43 124.3(6) . . ? F43 C43 C44 119.9(6) . . ? F43 C43 C42 121.7(7) . . ? C44 C43 C42 118.4(7) . . ? F44 C44 C43 120.7(7) . . ? F44 C44 C45 119.3(7) . . ? C43 C44 C45 120.0(6) . . ? F45 C45 C44 120.1(6) . . ? F45 C45 C46 120.7(6) . . ? C44 C45 C46 119.1(6) . . ? F46 C46 C41 120.0(5) . . ? F46 C46 C45 116.3(6) . . ? C41 C46 C45 123.7(6) . . ? C52 C51 C56 113.6(5) . . ? C52 C51 Au5 120.3(5) . . ? C56 C51 Au5 126.0(4) . . ? C53 C52 F52 115.8(5) . . ? C53 C52 C51 124.9(6) . . ? F52 C52 C51 119.3(5) . . ? F53 C53 C52 122.7(5) . . ? F53 C53 C54 118.0(5) . . ? C52 C53 C54 119.2(6) . . ? F54 C54 C55 120.9(5) . . ? F54 C54 C53 120.4(5) . . ? C55 C54 C53 118.6(5) . . ? F55 C55 C56 121.2(6) . . ? F55 C55 C54 119.2(6) . . ? C56 C55 C54 119.6(6) . . ? F56 C56 C55 116.5(5) . . ? F56 C56 C51 119.5(5) . . ? C55 C56 C51 123.9(6) . . ? C66 C61 C62 114.6(5) . . ? C66 C61 Au6 123.5(5) . . ? C62 C61 Au6 121.8(4) . . ? F62 C62 C63 116.8(6) . . ? F62 C62 C61 120.0(5) . . ? C63 C62 C61 123.2(6) . . ? F63 C63 C62 120.9(6) . . ? F63 C63 C64 119.1(6) . . ? C62 C63 C64 120.0(6) . . ? F64 C64 C63 120.5(6) . . ? F64 C64 C65 120.7(6) . . ? C63 C64 C65 118.8(6) . . ? F65 C65 C66 121.2(6) . . ? F65 C65 C64 119.3(6) . . ? C66 C65 C64 119.4(6) . . ? F66 C66 C65 116.1(6) . . ? F66 C66 C61 120.0(6) . . ? C65 C66 C61 123.9(6) . . ? N12 C111 N11 109.4(5) . . ? N12 C111 P1 128.8(5) . . ? N11 C111 P1 121.8(4) . . ? N11 C112 C113 109.3(5) . . ? N11 C112 H112 125.3 . . ? C113 C112 H112 125.3 . . ? N12 C113 C112 106.0(6) . . ? N12 C113 H113 127.0 . . ? C112 C113 H113 127.0 . . ? N12 C114 H11A 109.5 . . ? N12 C114 H11B 109.5 . . ? H11A C114 H11B 109.5 . . ? N12 C114 H11C 109.5 . . ? H11A C114 H11C 109.5 . . ? H11B C114 H11C 109.5 . . ? N13 C121 N14 111.6(5) . . ? N13 C121 P1 123.6(5) . . ? N14 C121 P1 124.7(5) . . ? C123 C122 N13 110.8(6) . . ? C123 C122 H122 124.6 . . ? N13 C122 H122 124.6 . . ? C122 C123 N14 106.7(6) . . ? C122 C123 H123 126.6 . . ? N14 C123 H123 126.6 . . ? N14 C124 H12A 109.5 . . ? N14 C124 H12B 109.5 . . ? H12A C124 H12B 109.5 . . ? N14 C124 H12C 109.5 . . ? H12A C124 H12C 109.5 . . ? H12B C124 H12C 109.5 . . ? N15 C131 N16 111.6(5) . . ? N15 C131 P1 123.4(5) . . ? N16 C131 P1 124.9(5) . . ? N15 C132 C133 110.1(6) . . ? N15 C132 H132 124.9 . . ? C133 C132 H132 124.9 . . ? N16 C133 C132 106.0(5) . . ? N16 C133 H133 127.0 . . ? C132 C133 H133 127.0 . . ? N16 C134 H13A 109.5 . . ? N16 C134 H13B 109.5 . . ? H13A C134 H13B 109.5 . . ? N16 C134 H13C 109.5 . . ? H13A C134 H13C 109.5 . . ? H13B C134 H13C 109.5 . . ? N31 C311 N32 108.2(5) . . ? N31 C311 P3 121.4(4) . . ? N32 C311 P3 130.0(4) . . ? N31 C312 C313 109.1(5) . . ? N31 C312 H312 125.4 . . ? C313 C312 H312 125.4 . . ? N32 C313 C312 106.9(5) . . ? N32 C313 H313 126.6 . . ? C312 C313 H313 126.6 . . ? N32 C314 H31A 109.5 . . ? N32 C314 H31B 109.5 . . ? H31A C314 H31B 109.5 . . ? N32 C314 H31C 109.5 . . ? H31A C314 H31C 109.5 . . ? H31B C314 H31C 109.5 . . ? N33 C321 N34 111.0(5) . . ? N33 C321 P3 121.7(5) . . ? N34 C321 P3 127.1(4) . . ? N33 C322 C323 109.6(6) . . ? N33 C322 H322 125.2 . . ? C323 C322 H322 125.2 . . ? N34 C323 C322 106.8(6) . . ? N34 C323 H323 126.6 . . ? C322 C323 H323 126.6 . . ? N34 C324 H32A 109.5 . . ? N34 C324 H32B 109.5 . . ? H32A C324 H32B 109.5 . . ? N34 C324 H32C 109.5 . . ? H32A C324 H32C 109.5 . . ? H32B C324 H32C 109.5 . . ? N35 C331 N36 112.6(5) . . ? N35 C331 P3 123.2(5) . . ? N36 C331 P3 124.2(4) . . ? C333 C332 N35 110.4(5) . . ? C333 C332 H332 124.8 . . ? N35 C332 H332 124.8 . . ? C332 C333 N36 108.0(6) . . ? C332 C333 H333 126.0 . . ? N36 C333 H333 126.0 . . ? N36 C334 H33A 109.5 . . ? N36 C334 H33B 109.5 . . ? H33A C334 H33B 109.5 . . ? N36 C334 H33C 109.5 . . ? H33A C334 H33C 109.5 . . ? H33B C334 H33C 109.5 . . ? N51 C511 N52 109.2(5) . . ? N51 C511 P5 122.7(5) . . ? N52 C511 P5 127.7(5) . . ? C513 C512 N51 109.9(6) . . ? C513 C512 H512 125.1 . . ? N51 C512 H512 125.1 . . ? C512 C513 N52 106.8(6) . . ? C512 C513 H513 126.6 . . ? N52 C513 H513 126.6 . . ? N52 C514 H51A 109.5 . . ? N52 C514 H51B 109.5 . . ? H51A C514 H51B 109.5 . . ? N52 C514 H51C 109.5 . . ? H51A C514 H51C 109.5 . . ? H51B C514 H51C 109.5 . . ? N53 C521 N54 112.0(5) . . ? N53 C521 P5 122.1(5) . . ? N54 C521 P5 125.8(4) . . ? C523 C522 N53 110.7(6) . . ? C523 C522 H522 124.6 . . ? N53 C522 H522 124.6 . . ? C522 C523 N54 106.2(6) . . ? C522 C523 H523 126.9 . . ? N54 C523 H523 126.9 . . ? N54 C524 H52A 109.5 . . ? N54 C524 H52B 109.5 . . ? H52A C524 H52B 109.5 . . ? N54 C524 H52C 109.5 . . ? H52A C524 H52C 109.5 . . ? H52B C524 H52C 109.5 . . ? N55 C531 N56 112.0(5) . . ? N55 C531 P5 121.8(5) . . ? N56 C531 P5 126.2(5) . . ? C533 C532 N55 110.6(6) . . ? C533 C532 H532 124.7 . . ? N55 C532 H532 124.7 . . ? C532 C533 N56 106.5(6) . . ? C532 C533 H533 126.8 . . ? N56 C533 H533 126.8 . . ? N56 C534 H53A 109.5 . . ? N56 C534 H53B 109.5 . . ? H53A C534 H53B 109.5 . . ? N56 C534 H53C 109.5 . . ? H53A C534 H53C 109.5 . . ? H53B C534 H53C 109.5 . . ? Cl13 C1 Cl11 110.3(4) . . ? Cl13 C1 Cl12 111.8(4) . . ? Cl11 C1 Cl12 110.1(4) . . ? Cl13 C1 D1 108.2 . . ? Cl11 C1 D1 108.2 . . ? Cl12 C1 D1 108.2 . . ? Cl21 C2 Cl22 110.1(5) . . ? Cl21 C2 Cl23 110.9(5) . . ? Cl22 C2 Cl23 110.4(5) . . ? Cl21 C2 D2 108.4 . . ? Cl22 C2 D2 108.4 . . ? Cl23 C2 D2 108.4 . . ? Cl32 C3 Cl32 119.4(9) 2_766 . ? Cl32 C3 Cl31 102.3(8) 2_766 . ? Cl32 C3 Cl31 103.4(7) . . ? Cl32 C3 D3 110.3 2_766 . ? Cl32 C3 D3 110.3 . . ? Cl31 C3 D3 110.3 . . ? 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 C11 Au1 Au2 C21 -29.1(3) . . . . ? P1 Au1 Au2 C21 155.17(19) . . . . ? C11 Au1 Au2 N11 152.2(2) . . . . ? P1 Au1 Au2 N11 -23.53(14) . . . . ? C31 Au3 Au4 C41 -34.1(3) . . . . ? P3 Au3 Au4 C41 148.88(19) . . . . ? C31 Au3 Au4 N31 150.0(2) . . . . ? P3 Au3 Au4 N31 -27.05(14) . . . . ? C51 Au5 Au6 C61 -27.8(3) . . . . ? P5 Au5 Au6 C61 160.95(18) . . . . ? C51 Au5 Au6 N51 151.2(2) . . . . ? P5 Au5 Au6 N51 -20.09(14) . . . . ? Au2 Au1 P1 C121 -95.8(2) . . . . ? Au2 Au1 P1 C131 145.5(2) . . . . ? Au2 Au1 P1 C111 25.4(2) . . . . ? Au4 Au3 P3 C311 22.7(2) . . . . ? Au4 Au3 P3 C321 143.8(2) . . . . ? Au4 Au3 P3 C331 -95.9(2) . . . . ? Au6 Au5 P5 C531 -91.4(3) . . . . ? Au6 Au5 P5 C521 144.9(2) . . . . ? Au6 Au5 P5 C511 25.9(2) . . . . ? Au1 Au2 N11 C111 24.1(5) . . . . ? Au1 Au2 N11 C112 -165.0(5) . . . . ? Au3 Au4 N31 C312 -169.3(4) . . . . ? Au3 Au4 N31 C311 37.8(4) . . . . ? Au5 Au6 N51 C511 13.0(5) . . . . ? Au5 Au6 N51 C512 -168.4(5) . . . . ? Au2 Au1 C11 C12 -95.7(5) . . . . ? Au2 Au1 C11 C16 83.6(5) . . . . ? C16 C11 C12 F12 -179.5(5) . . . . ? Au1 C11 C12 F12 -0.1(8) . . . . ? C16 C11 C12 C13 -0.2(9) . . . . ? Au1 C11 C12 C13 179.3(5) . . . . ? F12 C12 C13 F13 -1.5(8) . . . . ? C11 C12 C13 F13 179.2(6) . . . . ? F12 C12 C13 C14 179.5(5) . . . . ? C11 C12 C13 C14 0.2(10) . . . . ? F13 C13 C14 F14 2.2(9) . . . . ? C12 C13 C14 F14 -178.8(5) . . . . ? F13 C13 C14 C15 -179.7(6) . . . . ? C12 C13 C14 C15 -0.7(9) . . . . ? C13 C14 C15 F15 -178.6(6) . . . . ? F14 C14 C15 F15 -0.5(9) . . . . ? C13 C14 C15 C16 1.3(10) . . . . ? F14 C14 C15 C16 179.4(6) . . . . ? F15 C15 C16 F16 0.1(9) . . . . ? C14 C15 C16 F16 -179.8(5) . . . . ? F15 C15 C16 C11 178.6(6) . . . . ? C14 C15 C16 C11 -1.4(10) . . . . ? C12 C11 C16 F16 179.2(5) . . . . ? Au1 C11 C16 F16 -0.2(8) . . . . ? C12 C11 C16 C15 0.8(9) . . . . ? Au1 C11 C16 C15 -178.6(5) . . . . ? Au1 Au2 C21 C22 66.8(5) . . . . ? Au1 Au2 C21 C26 -104.7(5) . . . . ? C26 C21 C22 F22 -178.8(5) . . . . ? Au2 C21 C22 F22 9.3(8) . . . . ? C26 C21 C22 C23 3.4(9) . . . . ? Au2 C21 C22 C23 -168.5(5) . . . . ? F22 C22 C23 F23 -0.2(9) . . . . ? C21 C22 C23 F23 177.8(6) . . . . ? F22 C22 C23 C24 -179.8(6) . . . . ? C21 C22 C23 C24 -1.9(10) . . . . ? F23 C23 C24 F24 0.5(10) . . . . ? C22 C23 C24 F24 -179.8(6) . . . . ? F23 C23 C24 C25 179.3(6) . . . . ? C22 C23 C24 C25 -1.1(10) . . . . ? F24 C24 C25 F25 0.8(10) . . . . ? C23 C24 C25 F25 -177.9(6) . . . . ? F24 C24 C25 C26 -179.1(6) . . . . ? C23 C24 C25 C26 2.2(10) . . . . ? F25 C25 C26 F26 -0.1(9) . . . . ? C24 C25 C26 F26 179.8(6) . . . . ? F25 C25 C26 C21 179.6(6) . . . . ? C24 C25 C26 C21 -0.6(10) . . . . ? C22 C21 C26 F26 177.5(5) . . . . ? Au2 C21 C26 F26 -10.4(8) . . . . ? C22 C21 C26 C25 -2.2(9) . . . . ? Au2 C21 C26 C25 170.0(5) . . . . ? Au4 Au3 C31 C32 66.7(5) . . . . ? Au4 Au3 C31 C36 -115.0(5) . . . . ? C36 C31 C32 F32 179.5(5) . . . . ? Au3 C31 C32 F32 -2.1(8) . . . . ? C36 C31 C32 C33 -0.7(9) . . . . ? Au3 C31 C32 C33 177.7(5) . . . . ? F32 C32 C33 F33 0.8(8) . . . . ? C31 C32 C33 F33 -179.0(5) . . . . ? F32 C32 C33 C34 179.1(5) . . . . ? C31 C32 C33 C34 -0.7(9) . . . . ? F33 C33 C34 F34 0.2(9) . . . . ? C32 C33 C34 F34 -178.2(5) . . . . ? F33 C33 C34 C35 -180.0(5) . . . . ? C32 C33 C34 C35 1.6(9) . . . . ? F34 C34 C35 F35 0.3(9) . . . . ? C33 C34 C35 F35 -179.5(5) . . . . ? F34 C34 C35 C36 178.6(5) . . . . ? C33 C34 C35 C36 -1.2(9) . . . . ? F35 C35 C36 F36 0.1(9) . . . . ? C34 C35 C36 F36 -178.2(5) . . . . ? F35 C35 C36 C31 178.0(6) . . . . ? C34 C35 C36 C31 -0.3(10) . . . . ? C32 C31 C36 F36 179.0(5) . . . . ? Au3 C31 C36 F36 0.6(8) . . . . ? C32 C31 C36 C35 1.2(9) . . . . ? Au3 C31 C36 C35 -177.2(5) . . . . ? Au3 Au4 C41 C46 73.4(5) . . . . ? Au3 Au4 C41 C42 -107.7(5) . . . . ? C46 C41 C42 F42 179.8(5) . . . . ? Au4 C41 C42 F42 0.8(8) . . . . ? C46 C41 C42 C43 -0.5(10) . . . . ? Au4 C41 C42 C43 -179.5(5) . . . . ? F42 C42 C43 F43 0.1(10) . . . . ? C41 C42 C43 F43 -179.7(6) . . . . ? F42 C42 C43 C44 179.0(6) . . . . ? C41 C42 C43 C44 -0.8(11) . . . . ? F43 C43 C44 F44 -1.4(10) . . . . ? C42 C43 C44 F44 179.7(6) . . . . ? F43 C43 C44 C45 179.9(6) . . . . ? C42 C43 C44 C45 1.0(11) . . . . ? F44 C44 C45 F45 0.1(10) . . . . ? C43 C44 C45 F45 178.8(6) . . . . ? F44 C44 C45 C46 -178.7(6) . . . . ? C43 C44 C45 C46 -0.1(11) . . . . ? C42 C41 C46 F46 -179.5(5) . . . . ? Au4 C41 C46 F46 -0.5(9) . . . . ? C42 C41 C46 C45 1.5(10) . . . . ? Au4 C41 C46 C45 -179.5(5) . . . . ? F45 C45 C46 F46 0.9(9) . . . . ? C44 C45 C46 F46 179.7(6) . . . . ? F45 C45 C46 C41 179.9(6) . . . . ? C44 C45 C46 C41 -1.3(10) . . . . ? Au6 Au5 C51 C52 -99.0(5) . . . . ? Au6 Au5 C51 C56 83.7(5) . . . . ? C56 C51 C52 C53 0.1(9) . . . . ? Au5 C51 C52 C53 -177.5(5) . . . . ? C56 C51 C52 F52 179.8(5) . . . . ? Au5 C51 C52 F52 2.1(8) . . . . ? F52 C52 C53 F53 -1.2(9) . . . . ? C51 C52 C53 F53 178.4(6) . . . . ? F52 C52 C53 C54 179.6(5) . . . . ? C51 C52 C53 C54 -0.7(10) . . . . ? F53 C53 C54 F54 2.3(9) . . . . ? C52 C53 C54 F54 -178.4(5) . . . . ? F53 C53 C54 C55 -178.9(5) . . . . ? C52 C53 C54 C55 0.3(9) . . . . ? F54 C54 C55 F55 -0.8(9) . . . . ? C53 C54 C55 F55 -179.6(5) . . . . ? F54 C54 C55 C56 179.4(5) . . . . ? C53 C54 C55 C56 0.7(9) . . . . ? F55 C55 C56 F56 -0.2(9) . . . . ? C54 C55 C56 F56 179.5(5) . . . . ? F55 C55 C56 C51 178.9(6) . . . . ? C54 C55 C56 C51 -1.4(10) . . . . ? C52 C51 C56 F56 -180.0(5) . . . . ? Au5 C51 C56 F56 -2.5(8) . . . . ? C52 C51 C56 C55 0.9(9) . . . . ? Au5 C51 C56 C55 178.4(5) . . . . ? Au5 Au6 C61 C66 -97.6(5) . . . . ? Au5 Au6 C61 C62 79.0(5) . . . . ? C66 C61 C62 F62 -179.2(5) . . . . ? Au6 C61 C62 F62 3.9(8) . . . . ? C66 C61 C62 C63 1.5(9) . . . . ? Au6 C61 C62 C63 -175.3(5) . . . . ? F62 C62 C63 F63 -1.4(9) . . . . ? C61 C62 C63 F63 177.8(6) . . . . ? F62 C62 C63 C64 -179.4(5) . . . . ? C61 C62 C63 C64 -0.2(10) . . . . ? F63 C63 C64 F64 0.0(9) . . . . ? C62 C63 C64 F64 178.0(6) . . . . ? F63 C63 C64 C65 -178.7(6) . . . . ? C62 C63 C64 C65 -0.7(10) . . . . ? F64 C64 C65 F65 2.7(10) . . . . ? C63 C64 C65 F65 -178.6(6) . . . . ? F64 C64 C65 C66 -178.6(6) . . . . ? C63 C64 C65 C66 0.1(10) . . . . ? F65 C65 C66 F66 -1.1(9) . . . . ? C64 C65 C66 F66 -179.8(6) . . . . ? F65 C65 C66 C61 -179.9(6) . . . . ? C64 C65 C66 C61 1.4(10) . . . . ? C62 C61 C66 F66 179.1(5) . . . . ? Au6 C61 C66 F66 -4.1(8) . . . . ? C62 C61 C66 C65 -2.1(9) . . . . ? Au6 C61 C66 C65 174.6(5) . . . . ? C113 N12 C111 N11 -0.5(7) . . . . ? C114 N12 C111 N11 179.5(5) . . . . ? C113 N12 C111 P1 -178.3(5) . . . . ? C114 N12 C111 P1 1.7(9) . . . . ? C112 N11 C111 N12 0.5(6) . . . . ? Au2 N11 C111 N12 172.9(4) . . . . ? C112 N11 C111 P1 178.5(4) . . . . ? Au2 N11 C111 P1 -9.2(7) . . . . ? C121 P1 C111 N12 -72.7(6) . . . . ? C131 P1 C111 N12 33.3(6) . . . . ? Au1 P1 C111 N12 157.7(5) . . . . ? C121 P1 C111 N11 109.7(5) . . . . ? C131 P1 C111 N11 -144.2(5) . . . . ? Au1 P1 C111 N11 -19.9(5) . . . . ? C111 N11 C112 C113 -0.4(7) . . . . ? Au2 N11 C112 C113 -172.9(4) . . . . ? C111 N12 C113 C112 0.2(7) . . . . ? C114 N12 C113 C112 -179.7(5) . . . . ? N11 C112 C113 N12 0.1(7) . . . . ? C122 N13 C121 N14 0.6(7) . . . . ? C122 N13 C121 P1 178.9(5) . . . . ? C123 N14 C121 N13 -0.9(7) . . . . ? C124 N14 C121 N13 -177.5(6) . . . . ? C123 N14 C121 P1 -179.2(4) . . . . ? C124 N14 C121 P1 4.2(9) . . . . ? C131 P1 C121 N13 -94.9(5) . . . . ? C111 P1 C121 N13 14.9(6) . . . . ? Au1 P1 C121 N13 140.2(4) . . . . ? C131 P1 C121 N14 83.3(5) . . . . ? C111 P1 C121 N14 -166.9(5) . . . . ? Au1 P1 C121 N14 -41.7(6) . . . . ? C121 N13 C122 C123 0.0(7) . . . . ? N13 C122 C123 N14 -0.5(7) . . . . ? C121 N14 C123 C122 0.8(7) . . . . ? C124 N14 C123 C122 177.5(6) . . . . ? C132 N15 C131 N16 -0.9(7) . . . . ? C132 N15 C131 P1 -178.6(5) . . . . ? C133 N16 C131 N15 1.1(7) . . . . ? C134 N16 C131 N15 -178.7(6) . . . . ? C133 N16 C131 P1 178.7(5) . . . . ? C134 N16 C131 P1 -1.0(9) . . . . ? C121 P1 C131 N15 -5.4(6) . . . . ? C111 P1 C131 N15 -113.3(5) . . . . ? Au1 P1 C131 N15 123.3(5) . . . . ? C121 P1 C131 N16 177.3(5) . . . . ? C111 P1 C131 N16 69.3(6) . . . . ? Au1 P1 C131 N16 -54.1(6) . . . . ? C131 N15 C132 C133 0.5(7) . . . . ? C131 N16 C133 C132 -0.7(7) . . . . ? C134 N16 C133 C132 179.1(6) . . . . ? N15 C132 C133 N16 0.1(8) . . . . ? C312 N31 C311 N32 1.5(6) . . . . ? Au4 N31 C311 N32 157.6(4) . . . . ? C312 N31 C311 P3 174.9(4) . . . . ? Au4 N31 C311 P3 -29.1(7) . . . . ? C313 N32 C311 N31 -1.1(6) . . . . ? C314 N32 C311 N31 -177.2(6) . . . . ? C313 N32 C311 P3 -173.7(5) . . . . ? C314 N32 C311 P3 10.2(9) . . . . ? C321 P3 C311 N31 -133.3(5) . . . . ? C331 P3 C311 N31 120.1(5) . . . . ? Au3 P3 C311 N31 -6.9(5) . . . . ? C321 P3 C311 N32 38.5(6) . . . . ? C331 P3 C311 N32 -68.1(6) . . . . ? Au3 P3 C311 N32 164.8(5) . . . . ? C311 N31 C312 C313 -1.4(7) . . . . ? Au4 N31 C312 C313 -158.7(4) . . . . ? C311 N32 C313 C312 0.2(7) . . . . ? C314 N32 C313 C312 176.5(6) . . . . ? N31 C312 C313 N32 0.8(7) . . . . ? C322 N33 C321 N34 -0.8(8) . . . . ? C322 N33 C321 P3 173.7(6) . . . . ? C323 N34 C321 N33 0.0(8) . . . . ? C324 N34 C321 N33 -171.6(6) . . . . ? C323 N34 C321 P3 -174.1(5) . . . . ? C324 N34 C321 P3 14.3(10) . . . . ? C311 P3 C321 N33 -86.5(6) . . . . ? C331 P3 C321 N33 21.4(6) . . . . ? Au3 P3 C321 N33 150.2(5) . . . . ? C311 P3 C321 N34 87.1(6) . . . . ? C331 P3 C321 N34 -165.0(6) . . . . ? Au3 P3 C321 N34 -36.2(6) . . . . ? C321 N33 C322 C323 1.3(9) . . . . ? C321 N34 C323 C322 0.8(8) . . . . ? C324 N34 C323 C322 173.0(7) . . . . ? N33 C322 C323 N34 -1.3(10) . . . . ? C332 N35 C331 N36 0.1(7) . . . . ? C332 N35 C331 P3 179.6(4) . . . . ? C333 N36 C331 N35 -0.5(7) . . . . ? C334 N36 C331 N35 177.7(6) . . . . ? C333 N36 C331 P3 180.0(4) . . . . ? C334 N36 C331 P3 -1.8(9) . . . . ? C311 P3 C331 N35 1.4(6) . . . . ? C321 P3 C331 N35 -108.8(5) . . . . ? Au3 P3 C331 N35 123.9(5) . . . . ? C311 P3 C331 N36 -179.2(5) . . . . ? C321 P3 C331 N36 70.6(5) . . . . ? Au3 P3 C331 N36 -56.7(5) . . . . ? C331 N35 C332 C333 0.4(7) . . . . ? N35 C332 C333 N36 -0.7(8) . . . . ? C331 N36 C333 C332 0.7(7) . . . . ? C334 N36 C333 C332 -177.6(6) . . . . ? C512 N51 C511 N52 0.8(6) . . . . ? Au6 N51 C511 N52 179.6(4) . . . . ? C512 N51 C511 P5 -172.9(4) . . . . ? Au6 N51 C511 P5 5.9(7) . . . . ? C513 N52 C511 N51 -1.0(7) . . . . ? C514 N52 C511 N51 -179.8(5) . . . . ? C513 N52 C511 P5 172.3(5) . . . . ? C514 N52 C511 P5 -6.5(9) . . . . ? C531 P5 C511 N51 103.2(5) . . . . ? C521 P5 C511 N51 -150.4(5) . . . . ? Au5 P5 C511 N51 -28.2(5) . . . . ? C531 P5 C511 N52 -69.3(6) . . . . ? C521 P5 C511 N52 37.1(6) . . . . ? Au5 P5 C511 N52 159.4(5) . . . . ? C511 N51 C512 C513 -0.3(7) . . . . ? Au6 N51 C512 C513 -179.1(4) . . . . ? N51 C512 C513 N52 -0.3(7) . . . . ? C511 N52 C513 C512 0.8(7) . . . . ? C514 N52 C513 C512 179.6(5) . . . . ? C522 N53 C521 N54 0.4(7) . . . . ? C522 N53 C521 P5 -177.3(5) . . . . ? C523 N54 C521 N53 1.0(7) . . . . ? C524 N54 C521 N53 179.6(6) . . . . ? C523 N54 C521 P5 178.6(5) . . . . ? C524 N54 C521 P5 -2.7(9) . . . . ? C531 P5 C521 N53 -13.5(6) . . . . ? C511 P5 C521 N53 -117.9(5) . . . . ? Au5 P5 C521 N53 121.4(5) . . . . ? C531 P5 C521 N54 169.1(5) . . . . ? C511 P5 C521 N54 64.7(6) . . . . ? Au5 P5 C521 N54 -56.0(6) . . . . ? C521 N53 C522 C523 -1.7(8) . . . . ? N53 C522 C523 N54 2.3(8) . . . . ? C521 N54 C523 C522 -2.0(7) . . . . ? C524 N54 C523 C522 179.4(6) . . . . ? C532 N55 C531 N56 -0.3(7) . . . . ? C532 N55 C531 P5 -177.6(5) . . . . ? C533 N56 C531 N55 -0.2(7) . . . . ? C534 N56 C531 N55 173.7(6) . . . . ? C533 N56 C531 P5 176.9(5) . . . . ? C534 N56 C531 P5 -9.1(9) . . . . ? C521 P5 C531 N55 -102.9(6) . . . . ? C511 P5 C531 N55 7.1(6) . . . . ? Au5 P5 C531 N55 129.1(5) . . . . ? C521 P5 C531 N56 80.2(6) . . . . ? C511 P5 C531 N56 -169.8(5) . . . . ? Au5 P5 C531 N56 -47.8(6) . . . . ? C531 N55 C532 C533 0.8(7) . . . . ? N55 C532 C533 N56 -0.9(7) . . . . ? C531 N56 C533 C532 0.7(7) . . . . ? C534 N56 C533 C532 -173.4(6) . . . . ? C3 Cl32 C3 Cl32 0.000(1) 2_766 . . 2_766 ? C3 Cl32 C3 Cl31 112.7(13) 2_766 . . . ? 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 C1 D1 N13 1.00 2.24 3.181(9) 156.0 2_766 _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.525 _refine_diff_density_min -1.451 _refine_diff_density_rms 0.212 #===END #Compound 4CDCl3 ends. End of CIF file.