Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Mathieson, Trevor' 'Schier, Annette' 'Schmidbaur, Hubert' _publ_contact_author_name 'Prof Hubert Schmidbaur' _publ_contact_author_address ; Prof Hubert Schmidbaur Anorganisch-chemisches Institut der Technischen Universitat Munchen Lichtenbergstrasse 4 D-85747 Garching GERMANY ; data_trev9 _database_code_CSD 155748 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H9 N' _chemical_formula_weight 131.17 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5510(10) _cell_length_b 8.888(2) _cell_length_c 12.820(2) _cell_angle_alpha 83.39(2) _cell_angle_beta 72.870(10) _cell_angle_gamma 64.870(10) _cell_volume 744.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17 _cell_measurement_theta_max 25 _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 280 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Enraf Nonius CAD4' _diffrn_measurement_method omega-2-theta-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600s _diffrn_standards_decay_% ? _diffrn_reflns_number 6437 _diffrn_reflns_av_R_equivalents 0.0924 _diffrn_reflns_av_sigmaI/netI 0.0980 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 26.94 _reflns_number_total 3218 _reflns_number_gt 2199 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf Nonius CAD4' _computing_cell_refinement 'Enraf Nonius CAD4' _computing_data_reduction XCAD4PC _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1098P)^2^+0.0676P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment isotropic _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.021(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3218 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0922 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1832 _refine_ls_wR_factor_gt 0.1676 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 N1 N 0.1643(2) 0.43610(19) 0.67683(13) 0.0279(4) Uani 1 1 d . . . C1 C 0.0837(2) 0.3689(2) 0.61882(15) 0.0242(4) Uani 1 1 d . . . C2 C -0.1267(2) 0.4113(2) 0.65423(15) 0.0264(4) Uani 1 1 d . . . C3 C -0.2028(3) 0.3416(2) 0.59663(16) 0.0287(4) Uani 1 1 d . . . C4 C -0.0776(3) 0.2371(2) 0.50754(17) 0.0312(5) Uani 1 1 d . . . C5 C 0.1305(3) 0.1991(2) 0.47364(16) 0.0284(4) Uani 1 1 d . . . C6 C 0.2139(2) 0.2655(2) 0.52945(15) 0.0255(4) Uani 1 1 d . . . C7 C -0.2612(3) 0.5260(3) 0.74985(17) 0.0326(5) Uani 1 1 d . . . C8 C 0.4378(3) 0.2270(3) 0.49444(18) 0.0329(5) Uani 1 1 d . . . C9 C 0.2323(3) 0.4904(3) 0.7251(2) 0.0414(5) Uani 1 1 d . . . N2 N 0.2777(2) 0.0638(2) 0.82360(13) 0.0294(4) Uani 1 1 d . . . C10 C 0.0713(2) 0.1308(2) 0.88115(15) 0.0235(4) Uani 1 1 d . . . C11 C -0.0609(3) 0.0887(2) 0.84573(15) 0.0258(4) Uani 1 1 d . . . C12 C -0.2653(3) 0.1590(2) 0.90354(16) 0.0292(4) Uani 1 1 d . . . C13 C -0.3328(3) 0.2630(2) 0.99294(17) 0.0300(4) Uani 1 1 d . . . C14 C -0.1968(3) 0.3007(2) 1.02583(16) 0.0272(4) Uani 1 1 d . . . C15 C 0.0088(2) 0.2347(2) 0.97051(15) 0.0245(4) Uani 1 1 d . . . C16 C 0.0145(3) -0.0258(3) 0.75095(17) 0.0324(4) Uani 1 1 d . . . C17 C 0.1588(3) 0.2731(3) 1.00539(18) 0.0328(5) Uani 1 1 d . . . C18 C 0.4478(3) 0.0092(3) 0.77436(19) 0.0407(5) Uani 1 1 d . . . H3 H -0.354(4) 0.375(3) 0.622(2) 0.035(6) Uiso 1 1 d . . . H4 H -0.129(3) 0.187(2) 0.4639(17) 0.021(5) Uiso 1 1 d . . . H5 H 0.219(3) 0.131(3) 0.4140(18) 0.022(5) Uiso 1 1 d . . . H71 H -0.403(5) 0.542(4) 0.764(3) 0.082(10) Uiso 1 1 d . . . H72 H -0.220(4) 0.483(4) 0.816(3) 0.063(8) Uiso 1 1 d . . . H73 H -0.259(4) 0.634(4) 0.742(2) 0.060(8) Uiso 1 1 d . . . H81 H 0.460(4) 0.328(3) 0.472(2) 0.046(7) Uiso 1 1 d . . . H82 H 0.507(3) 0.154(3) 0.429(2) 0.033(6) Uiso 1 1 d . . . H83 H 0.505(4) 0.167(3) 0.547(2) 0.044(6) Uiso 1 1 d . . . H12 H -0.364(4) 0.133(3) 0.880(2) 0.035(6) Uiso 1 1 d . . . H13 H -0.477(3) 0.312(3) 1.0371(19) 0.029(5) Uiso 1 1 d . . . H14 H -0.244(3) 0.366(3) 1.091(2) 0.030(5) Uiso 1 1 d . . . H161 H -0.094(5) -0.046(4) 0.739(3) 0.069(9) Uiso 1 1 d . . . H162 H 0.080(4) 0.018(3) 0.686(2) 0.049(7) Uiso 1 1 d . . . H163 H 0.115(4) -0.137(4) 0.766(2) 0.055(7) Uiso 1 1 d . . . H171 H 0.093(3) 0.344(3) 1.075(2) 0.038(6) Uiso 1 1 d . . . H172 H 0.230(3) 0.322(3) 0.946(2) 0.040(6) Uiso 1 1 d . . . H173 H 0.263(4) 0.172(3) 1.029(2) 0.045(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0247(7) 0.0314(8) 0.0280(8) -0.0028(6) -0.0069(6) -0.0114(6) C1 0.0184(8) 0.0276(9) 0.0287(10) -0.0001(7) -0.0074(6) -0.0108(6) C2 0.0191(8) 0.0284(9) 0.0289(10) 0.0002(7) -0.0038(7) -0.0088(6) C3 0.0203(8) 0.0353(10) 0.0322(10) 0.0006(8) -0.0066(7) -0.0133(7) C4 0.0232(9) 0.0389(11) 0.0362(11) -0.0026(8) -0.0089(7) -0.0159(8) C5 0.0203(8) 0.0314(9) 0.0314(10) -0.0051(8) -0.0040(7) -0.0093(7) C6 0.0186(8) 0.0283(9) 0.0282(9) 0.0006(7) -0.0050(7) -0.0093(6) C7 0.0258(9) 0.0358(11) 0.0307(11) -0.0058(8) -0.0019(7) -0.0099(8) C8 0.0173(8) 0.0403(11) 0.0389(12) -0.0075(9) -0.0032(7) -0.0108(7) C9 0.0341(10) 0.0506(13) 0.0451(13) -0.0110(10) -0.0112(9) -0.0194(9) N2 0.0213(7) 0.0332(9) 0.0314(9) -0.0072(7) -0.0007(6) -0.0114(6) C10 0.0165(8) 0.0274(9) 0.0256(9) -0.0014(7) -0.0027(6) -0.0096(6) C11 0.0242(8) 0.0279(9) 0.0270(9) 0.0001(7) -0.0072(7) -0.0121(7) C12 0.0209(8) 0.0357(10) 0.0346(10) -0.0038(8) -0.0067(7) -0.0146(7) C13 0.0187(8) 0.0347(10) 0.0346(11) 0.0002(8) -0.0040(7) -0.0112(7) C14 0.0235(9) 0.0294(9) 0.0265(10) -0.0051(7) -0.0022(7) -0.0104(7) C15 0.0204(8) 0.0290(9) 0.0256(9) -0.0024(7) -0.0049(6) -0.0117(6) C16 0.0332(10) 0.0368(11) 0.0296(11) -0.0066(8) -0.0074(8) -0.0158(8) C17 0.0255(9) 0.0391(11) 0.0395(12) -0.0063(9) -0.0084(8) -0.0174(8) C18 0.0263(9) 0.0483(12) 0.0435(12) -0.0148(9) 0.0003(8) -0.0145(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 N1 C9 1.160(3) . ? N1 C1 1.399(2) . ? C1 C6 1.391(3) . ? C1 C2 1.406(2) . ? C2 C3 1.385(3) . ? C2 C7 1.499(3) . ? C3 C4 1.387(3) . ? C3 H3 1.01(2) . ? C4 C5 1.398(2) . ? C4 H4 1.00(2) . ? C5 C6 1.391(3) . ? C5 H5 0.93(2) . ? C6 C8 1.508(2) . ? C7 H71 0.98(3) . ? C7 H72 0.97(3) . ? C7 H73 0.96(3) . ? C8 H81 0.98(3) . ? C8 H82 0.99(2) . ? C8 H83 0.94(3) . ? N2 C18 1.161(2) . ? N2 C10 1.401(2) . ? C10 C15 1.394(3) . ? C10 C11 1.402(2) . ? C11 C12 1.391(2) . ? C11 C16 1.491(3) . ? C12 C13 1.388(3) . ? C12 H12 0.99(2) . ? C13 C14 1.387(3) . ? C13 H13 0.99(2) . ? C14 C15 1.390(2) . ? C14 H14 0.96(2) . ? C15 C17 1.503(2) . ? C16 H161 0.96(3) . ? C16 H162 0.97(3) . ? C16 H163 1.00(3) . ? C17 H171 1.02(3) . ? C17 H172 0.97(2) . ? C17 H173 1.00(3) . ? 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 C9 N1 C1 179.4(2) . . ? C6 C1 N1 118.78(14) . . ? C6 C1 C2 123.55(16) . . ? N1 C1 C2 117.67(16) . . ? C3 C2 C1 116.71(16) . . ? C3 C2 C7 121.85(15) . . ? C1 C2 C7 121.44(17) . . ? C2 C3 C4 121.43(16) . . ? C2 C3 H3 116.0(15) . . ? C4 C3 H3 122.5(15) . . ? C3 C4 C5 120.42(17) . . ? C3 C4 H4 122.9(11) . . ? C5 C4 H4 116.7(11) . . ? C6 C5 C4 120.14(17) . . ? C6 C5 H5 117.0(12) . . ? C4 C5 H5 122.9(12) . . ? C5 C6 C1 117.74(15) . . ? C5 C6 C8 121.23(17) . . ? C1 C6 C8 121.03(16) . . ? C2 C7 H71 111(2) . . ? C2 C7 H72 111.8(18) . . ? H71 C7 H72 107(3) . . ? C2 C7 H73 114.4(17) . . ? H71 C7 H73 107(3) . . ? H72 C7 H73 104(2) . . ? C6 C8 H81 110.8(14) . . ? C6 C8 H82 110.6(12) . . ? H81 C8 H82 105(2) . . ? C6 C8 H83 113.0(15) . . ? H81 C8 H83 112(2) . . ? H82 C8 H83 104(2) . . ? C18 N2 C10 178.9(2) . . ? C15 C10 N2 118.37(15) . . ? C15 C10 C11 123.65(15) . . ? N2 C10 C11 117.99(16) . . ? C12 C11 C10 116.65(17) . . ? C12 C11 C16 121.85(16) . . ? C10 C11 C16 121.50(16) . . ? C13 C12 C11 121.22(16) . . ? C13 C12 H12 119.9(14) . . ? C11 C12 H12 118.9(14) . . ? C14 C13 C12 120.33(16) . . ? C14 C13 H13 116.7(13) . . ? C12 C13 H13 122.9(13) . . ? C13 C14 C15 120.77(17) . . ? C13 C14 H14 119.1(12) . . ? C15 C14 H14 120.0(12) . . ? C14 C15 C10 117.36(15) . . ? C14 C15 C17 121.57(17) . . ? C10 C15 C17 121.07(16) . . ? C11 C16 H161 111(2) . . ? C11 C16 H162 110.7(16) . . ? H161 C16 H162 111(2) . . ? C11 C16 H163 109.8(16) . . ? H161 C16 H163 106(2) . . ? H162 C16 H163 109(2) . . ? C15 C17 H171 112.3(12) . . ? C15 C17 H172 110.8(14) . . ? H171 C17 H172 112.4(19) . . ? C15 C17 H173 112.3(14) . . ? H171 C17 H173 100.9(19) . . ? H172 C17 H173 107.7(19) . . ? 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 C9 N1 C1 C6 -59(20) . . . . ? C9 N1 C1 C2 122(20) . . . . ? C6 C1 C2 C3 1.3(3) . . . . ? N1 C1 C2 C3 -179.11(16) . . . . ? C6 C1 C2 C7 -178.80(18) . . . . ? N1 C1 C2 C7 0.7(3) . . . . ? C1 C2 C3 C4 -0.9(3) . . . . ? C7 C2 C3 C4 179.26(19) . . . . ? C2 C3 C4 C5 0.1(3) . . . . ? C3 C4 C5 C6 0.2(3) . . . . ? C4 C5 C6 C1 0.2(3) . . . . ? C4 C5 C6 C8 -179.82(18) . . . . ? N1 C1 C6 C5 179.45(16) . . . . ? C2 C1 C6 C5 -1.0(3) . . . . ? N1 C1 C6 C8 -0.5(3) . . . . ? C2 C1 C6 C8 179.01(17) . . . . ? C18 N2 C10 C15 -129(10) . . . . ? C18 N2 C10 C11 51(10) . . . . ? C15 C10 C11 C12 1.2(3) . . . . ? N2 C10 C11 C12 -179.11(16) . . . . ? C15 C10 C11 C16 -178.75(18) . . . . ? N2 C10 C11 C16 1.0(3) . . . . ? C10 C11 C12 C13 -1.1(3) . . . . ? C16 C11 C12 C13 178.77(19) . . . . ? C11 C12 C13 C14 0.8(3) . . . . ? C12 C13 C14 C15 -0.3(3) . . . . ? C13 C14 C15 C10 0.3(3) . . . . ? C13 C14 C15 C17 -179.53(19) . . . . ? N2 C10 C15 C14 179.51(16) . . . . ? C11 C10 C15 C14 -0.8(3) . . . . ? N2 C10 C15 C17 -0.6(3) . . . . ? C11 C10 C15 C17 179.09(17) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.94 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.281 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.074 data_trev11 _database_code_CSD 155749 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H9 Au N2 S' _chemical_formula_weight 386.22 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' '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.0765(3) _cell_length_b 8.3241(4) _cell_length_c 11.0001(6) _cell_angle_alpha 98.626(2) _cell_angle_beta 95.504(2) _cell_angle_gamma 97.452(4) _cell_volume 541.67(5) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 356 _exptl_absorpt_coefficient_mu 13.732 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius DIP2020' _diffrn_measurement_method phi-rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2647 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 29.13 _reflns_number_total 2647 _reflns_number_gt 2532 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XPRESS' _computing_cell_refinement 'SCALEPACK' _computing_data_reduction 'SCALEPACK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0907P)^2^+1.5877P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.029(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2647 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1248 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 0.38192(5) 0.02999(3) 0.33092(2) 0.03435(18) Uani 1 1 d . . . S1 S 0.7148(4) 0.1757(3) 0.4242(2) 0.0436(5) Uani 1 1 d . . . N1 N -0.0818(13) -0.1682(8) 0.2307(6) 0.0371(14) Uani 1 1 d . . . N2 N 0.9203(15) 0.2748(10) 0.2219(8) 0.0490(17) Uani 1 1 d . . . C1 C 0.8288(14) 0.2323(10) 0.3019(7) 0.0344(15) Uani 1 1 d . . . C2 C 0.0885(15) -0.0968(10) 0.2621(7) 0.0343(15) Uani 1 1 d . . . C3 C -0.2986(13) -0.2588(9) 0.1942(7) 0.0348(15) Uani 1 1 d . . . C4 C -0.3860(13) -0.3552(8) 0.2787(7) 0.0335(14) Uani 1 1 d . . . C5 C -0.5963(14) -0.4412(10) 0.2434(8) 0.0381(16) Uani 1 1 d . . . H5A H -0.6611 -0.5092 0.2965 0.046 Uiso 1 1 calc R . . C6 C -0.7169(15) -0.4308(11) 0.1313(8) 0.0395(16) Uani 1 1 d . . . H6A H -0.8630 -0.4906 0.1096 0.047 Uiso 1 1 calc R . . C7 C -0.6261(17) -0.3340(10) 0.0509(8) 0.0402(17) Uani 1 1 d . . . H7A H -0.7110 -0.3274 -0.0249 0.048 Uiso 1 1 calc R . . C8 C -0.4117(15) -0.2465(9) 0.0806(7) 0.0358(16) Uani 1 1 d . . . C9 C -0.2519(16) -0.3609(11) 0.3989(8) 0.0414(18) Uani 1 1 d . . . H9A H -0.3426 -0.4258 0.4484 0.062 Uiso 1 1 calc R . . H9B H -0.2067 -0.2490 0.4444 0.062 Uiso 1 1 calc R . . H9C H -0.1185 -0.4116 0.3828 0.062 Uiso 1 1 calc R . . C10 C -0.2976(18) -0.1402(11) -0.0045(8) 0.046(2) Uani 1 1 d . . . H10A H -0.1503 -0.0871 0.0364 0.069 Uiso 1 1 calc R . . H10B H -0.3895 -0.0561 -0.0220 0.069 Uiso 1 1 calc R . . H10C H -0.2803 -0.2096 -0.0822 0.069 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 0.0347(3) 0.0309(2) 0.0379(2) 0.00893(12) 0.00717(12) 0.00102(13) S1 0.0423(13) 0.0495(11) 0.0356(9) 0.0104(8) 0.0021(8) -0.0075(9) N1 0.036(4) 0.030(3) 0.045(3) 0.009(2) 0.011(3) 0.000(3) N2 0.046(5) 0.046(4) 0.054(4) 0.013(3) 0.009(3) -0.001(3) C1 0.030(4) 0.035(3) 0.037(4) 0.008(3) 0.002(3) 0.000(3) C2 0.035(4) 0.035(3) 0.036(3) 0.010(3) 0.011(3) 0.005(3) C3 0.028(4) 0.032(3) 0.045(4) 0.004(3) 0.011(3) 0.003(3) C4 0.036(4) 0.025(3) 0.040(4) 0.003(3) 0.011(3) 0.003(3) C5 0.035(4) 0.036(4) 0.044(4) 0.007(3) 0.006(3) 0.004(3) C6 0.031(4) 0.041(4) 0.047(4) 0.008(3) 0.011(3) 0.000(3) C7 0.043(5) 0.035(4) 0.042(4) 0.006(3) 0.004(3) 0.006(3) C8 0.043(5) 0.027(3) 0.040(4) 0.007(3) 0.010(3) 0.008(3) C9 0.041(5) 0.040(4) 0.044(4) 0.013(3) 0.002(3) 0.005(3) C10 0.060(6) 0.037(4) 0.045(4) 0.013(3) 0.017(4) 0.006(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 C2 1.970(9) . ? Au1 S1 2.282(2) . ? S1 C1 1.672(8) . ? N1 C2 1.119(12) . ? N1 C3 1.420(11) . ? N2 C1 1.160(12) . ? C3 C8 1.392(11) . ? C3 C4 1.413(10) . ? C4 C5 1.371(12) . ? C4 C9 1.496(12) . ? C5 C6 1.393(12) . ? C5 H5A 0.9500 . ? C6 C7 1.388(12) . ? C6 H6A 0.9500 . ? C7 C8 1.391(13) . ? C7 H7A 0.9500 . ? C8 C10 1.534(11) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 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 C2 Au1 S1 176.0(2) . . ? C1 S1 Au1 100.9(3) . . ? C2 N1 C3 178.4(8) . . ? N2 C1 S1 175.7(8) . . ? N1 C2 Au1 175.5(7) . . ? C8 C3 C4 124.4(8) . . ? C8 C3 N1 119.1(7) . . ? C4 C3 N1 116.6(7) . . ? C5 C4 C3 116.3(7) . . ? C5 C4 C9 123.1(7) . . ? C3 C4 C9 120.6(8) . . ? C4 C5 C6 121.3(8) . . ? C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? C7 C6 C5 120.8(9) . . ? C7 C6 H6A 119.6 . . ? C5 C6 H6A 119.6 . . ? C6 C7 C8 120.5(8) . . ? C6 C7 H7A 119.8 . . ? C8 C7 H7A 119.8 . . ? C7 C8 C3 116.8(8) . . ? C7 C8 C10 123.6(8) . . ? C3 C8 C10 119.6(8) . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 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 C2 Au1 S1 C1 -173(3) . . . . ? Au1 S1 C1 N2 -170(11) . . . . ? C3 N1 C2 Au1 -7(38) . . . . ? S1 Au1 C2 N1 5(12) . . . . ? C2 N1 C3 C8 155(30) . . . . ? C2 N1 C3 C4 -24(30) . . . . ? C8 C3 C4 C5 0.2(11) . . . . ? N1 C3 C4 C5 179.4(6) . . . . ? C8 C3 C4 C9 180.0(8) . . . . ? N1 C3 C4 C9 -0.8(10) . . . . ? C3 C4 C5 C6 -1.1(11) . . . . ? C9 C4 C5 C6 179.1(8) . . . . ? C4 C5 C6 C7 0.8(13) . . . . ? C5 C6 C7 C8 0.6(13) . . . . ? C6 C7 C8 C3 -1.4(12) . . . . ? C6 C7 C8 C10 178.5(8) . . . . ? C4 C3 C8 C7 1.0(11) . . . . ? N1 C3 C8 C7 -178.2(7) . . . . ? C4 C3 C8 C10 -178.9(7) . . . . ? N1 C3 C8 C10 1.9(10) . . . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 2.220 _refine_diff_density_min -3.211 _refine_diff_density_rms 0.295 data_t12 _database_code_CSD 155750 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H9 Au N P S' _chemical_formula_weight 331.12 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' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.625(1) _cell_length_b 9.438(1) _cell_length_c 18.677(1) _cell_angle_alpha 90.00 _cell_angle_beta 103.78(1) _cell_angle_gamma 90.00 _cell_volume 1649.9(7) _cell_formula_units_Z 8 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 18.190 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.0736 _exptl_absorpt_correction_T_max 0.1217 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'ENRAF NONIUS CAD4' _diffrn_measurement_method omega-theta-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600s _diffrn_standards_decay_% ? _diffrn_reflns_number 7022 _diffrn_reflns_av_R_equivalents 0.0731 _diffrn_reflns_av_sigmaI/netI 0.0735 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.02 _reflns_number_total 3533 _reflns_number_gt 3010 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ENRAF NONIUS CAD4' _computing_cell_refinement 'ENRAF NONIUS CAD4' _computing_data_reduction 'Xcad4 (Harms, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0725P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3533 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1144 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 0.39218(3) 0.03917(3) 0.096229(18) 0.02108(13) Uani 1 1 d . . . P1 P 0.5454(2) 0.1950(2) 0.16573(12) 0.0214(4) Uani 1 1 d . . . S1 S 0.2379(2) -0.1137(3) 0.01686(14) 0.0332(5) Uani 1 1 d . . . C1 C 0.2788(9) -0.2714(11) 0.0571(6) 0.034(2) Uani 1 1 d . . . N1 N 0.3005(10) -0.3852(11) 0.0815(6) 0.055(3) Uani 1 1 d . . . Au2 Au 0.13733(3) 0.24826(3) 0.057422(18) 0.02021(13) Uani 1 1 d . . . P2 P 0.1531(2) 0.2803(2) -0.05993(13) 0.0222(4) Uani 1 1 d . . . S2 S 0.0879(2) 0.2516(2) 0.17365(14) 0.0285(5) Uani 1 1 d . . . C2 C 0.1621(8) 0.1020(10) 0.2124(5) 0.0260(17) Uani 1 1 d . . . N2 N 0.2127(9) 0.0003(10) 0.2424(4) 0.0329(17) Uani 1 1 d . . . C11 C 0.5653(11) 0.3502(10) 0.1140(5) 0.035(2) Uani 1 1 d . . . H11A H 0.6319 0.4157 0.1453 0.052 Uiso 1 1 calc R . . H11B H 0.4721 0.3963 0.0969 0.052 Uiso 1 1 calc R . . H11C H 0.6026 0.3235 0.0714 0.052 Uiso 1 1 calc R . . C12 C 0.7214(9) 0.1269(11) 0.1996(7) 0.040(2) Uani 1 1 d . . . H12A H 0.7816 0.1996 0.2291 0.059 Uiso 1 1 calc R . . H12B H 0.7618 0.1002 0.1580 0.059 Uiso 1 1 calc R . . H12C H 0.7176 0.0435 0.2303 0.059 Uiso 1 1 calc R . . C13 C 0.4927(11) 0.2626(12) 0.2448(6) 0.039(3) Uani 1 1 d . . . H13A H 0.5655 0.3288 0.2712 0.059 Uiso 1 1 calc R . . H13B H 0.4828 0.1841 0.2776 0.059 Uiso 1 1 calc R . . H13C H 0.4010 0.3120 0.2291 0.059 Uiso 1 1 calc R . . C21 C 0.3274(10) 0.2722(12) -0.0785(6) 0.035(2) Uani 1 1 d . . . H21A H 0.3195 0.2875 -0.1312 0.053 Uiso 1 1 calc R . . H21B H 0.3697 0.1790 -0.0643 0.053 Uiso 1 1 calc R . . H21C H 0.3884 0.3457 -0.0501 0.053 Uiso 1 1 calc R . . C22 C 0.0816(11) 0.4515(10) -0.0951(6) 0.035(2) Uani 1 1 d . . . H22A H 0.0899 0.4623 -0.1461 0.053 Uiso 1 1 calc R . . H22B H 0.1357 0.5269 -0.0647 0.053 Uiso 1 1 calc R . . H22C H -0.0192 0.4575 -0.0934 0.053 Uiso 1 1 calc R . . C23 C 0.0508(10) 0.1557(10) -0.1242(5) 0.034(2) Uani 1 1 d . . . H23A H 0.0629 0.1759 -0.1738 0.051 Uiso 1 1 calc R . . H23B H -0.0505 0.1637 -0.1238 0.051 Uiso 1 1 calc R . . H23C H 0.0842 0.0594 -0.1099 0.051 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 0.02245(18) 0.01852(19) 0.0220(2) -0.00196(12) 0.00485(13) -0.00057(10) P1 0.0222(9) 0.0215(10) 0.0206(11) -0.0026(9) 0.0053(8) -0.0017(8) S1 0.0366(11) 0.0305(11) 0.0273(13) -0.0042(10) -0.0030(9) -0.0067(9) C1 0.021(4) 0.036(5) 0.044(7) -0.007(5) 0.005(4) -0.004(3) N1 0.054(5) 0.034(5) 0.070(8) -0.001(5) -0.001(5) -0.003(4) Au2 0.02242(18) 0.0219(2) 0.0167(2) 0.00214(11) 0.00546(13) 0.00336(10) P2 0.0219(9) 0.0231(10) 0.0223(12) 0.0012(9) 0.0068(8) 0.0036(8) S2 0.0347(11) 0.0328(12) 0.0199(12) 0.0032(9) 0.0106(9) 0.0101(8) C2 0.021(3) 0.038(5) 0.017(4) 0.004(4) 0.002(3) -0.001(3) N2 0.042(4) 0.043(5) 0.012(4) 0.007(4) 0.001(3) 0.001(4) C11 0.051(5) 0.024(4) 0.029(5) 0.004(4) 0.010(4) -0.006(4) C12 0.025(4) 0.035(5) 0.055(7) 0.003(5) 0.002(4) 0.006(4) C13 0.035(5) 0.060(7) 0.027(6) -0.022(5) 0.015(4) -0.015(4) C21 0.031(4) 0.052(6) 0.027(5) 0.014(5) 0.015(4) 0.008(4) C22 0.040(5) 0.029(5) 0.042(7) 0.007(4) 0.017(4) 0.008(4) C23 0.042(5) 0.038(5) 0.024(5) -0.008(4) 0.012(4) -0.004(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 2.263(2) . ? Au1 S1 2.334(2) . ? Au1 Au2 3.0994(5) . ? P1 C12 1.783(9) . ? P1 C13 1.789(10) . ? P1 C11 1.791(9) . ? S1 C1 1.673(11) . ? C1 N1 1.167(14) . ? Au2 P2 2.252(2) . ? Au2 S2 2.329(2) . ? P2 C21 1.794(9) . ? P2 C23 1.799(9) . ? P2 C22 1.818(9) . ? S2 C2 1.669(9) . ? C2 N2 1.160(12) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 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 S1 175.76(8) . . ? P1 Au1 Au2 95.30(5) . . ? S1 Au1 Au2 84.04(6) . . ? C12 P1 C13 105.5(6) . . ? C12 P1 C11 105.8(5) . . ? C13 P1 C11 103.9(5) . . ? C12 P1 Au1 113.9(4) . . ? C13 P1 Au1 115.6(3) . . ? C11 P1 Au1 111.2(3) . . ? C1 S1 Au1 102.7(3) . . ? N1 C1 S1 175.6(10) . . ? P2 Au2 S2 168.57(8) . . ? P2 Au2 Au1 94.67(5) . . ? S2 Au2 Au1 96.64(6) . . ? C21 P2 C23 103.5(5) . . ? C21 P2 C22 105.1(5) . . ? C23 P2 C22 103.9(5) . . ? C21 P2 Au2 117.6(4) . . ? C23 P2 Au2 114.1(3) . . ? C22 P2 Au2 111.3(4) . . ? C2 S2 Au2 103.4(3) . . ? N2 C2 S2 176.8(9) . . ? P1 C11 H11A 109.5 . . ? P1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P1 C12 H12A 109.5 . . ? P1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P2 C21 H21A 109.5 . . ? P2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? P2 C22 H22A 109.5 . . ? P2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P2 C23 H23A 109.5 . . ? P2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 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 S1 Au1 P1 C12 -96.0(11) . . . . ? Au2 Au1 P1 C12 -176.8(4) . . . . ? S1 Au1 P1 C13 141.6(11) . . . . ? Au2 Au1 P1 C13 60.8(5) . . . . ? S1 Au1 P1 C11 23.5(12) . . . . ? Au2 Au1 P1 C11 -57.3(4) . . . . ? P1 Au1 S1 C1 134.8(11) . . . . ? Au2 Au1 S1 C1 -143.9(4) . . . . ? Au1 S1 C1 N1 178(100) . . . . ? P1 Au1 Au2 P2 106.28(8) . . . . ? S1 Au1 Au2 P2 -69.51(9) . . . . ? P1 Au1 Au2 S2 -72.05(8) . . . . ? S1 Au1 Au2 S2 112.16(9) . . . . ? S2 Au2 P2 C21 139.1(5) . . . . ? Au1 Au2 P2 C21 -32.5(4) . . . . ? S2 Au2 P2 C23 -99.4(5) . . . . ? Au1 Au2 P2 C23 89.0(3) . . . . ? S2 Au2 P2 C22 17.9(6) . . . . ? Au1 Au2 P2 C22 -153.8(4) . . . . ? P2 Au2 S2 C2 167.3(4) . . . . ? Au1 Au2 S2 C2 -21.1(3) . . . . ? Au2 S2 C2 N2 169(14) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.02 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 3.271 _refine_diff_density_min -2.986 _refine_diff_density_rms 0.362 _database_code_CSD 159216 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H11 Au N2 S' _chemical_formula_weight 400.24 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4885(2) _cell_length_b 11.6095(3) _cell_length_c 14.1815(4) _cell_angle_alpha 102.144(1) _cell_angle_beta 106.554(2) _cell_angle_gamma 110.128(2) _cell_volume 1181.65(5) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 12.594 _exptl_absorpt_correction_type DELABS _exptl_absorpt_correction_T_min 0.0813 _exptl_absorpt_correction_T_max 0.5716 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius DIP2020HU' _diffrn_measurement_method phi-rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26554 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 31.03 _reflns_number_total 6843 _reflns_number_gt 5905 _reflns_threshold_expression >2sigma(I) _computing_data_collection XPRESS _computing_cell_refinement SCALEPACK _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+2.6290P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0008(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6843 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1229 _refine_ls_wR_factor_gt 0.1172 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 0.79142(3) 0.38119(2) 0.415712(19) 0.04318(9) Uani 1 1 d . . . S1 S 0.8402(3) 0.4807(2) 0.29677(17) 0.0616(6) Uani 1 1 d . . . N11 N 0.7312(7) 0.2190(5) 0.5626(4) 0.0387(10) Uani 1 1 d . . . N12 N 0.4894(10) 0.4001(8) 0.1458(6) 0.0601(17) Uani 1 1 d . . . C11 C 0.7529(8) 0.2829(6) 0.5095(5) 0.0400(12) Uani 1 1 d . . . C12 C 0.6275(9) 0.4316(7) 0.2094(6) 0.0448(14) Uani 1 1 d . . . C13 C 0.7033(8) 0.1405(6) 0.6221(4) 0.0354(11) Uani 1 1 d . . . C14 C 0.5361(8) 0.0972(6) 0.6339(5) 0.0365(11) Uani 1 1 d . . . C15 C 0.5124(9) 0.0180(6) 0.6939(5) 0.0408(13) Uani 1 1 d . . . H15A H 0.3999 -0.0140 0.7022 0.049 Uiso 1 1 calc R . . C16 C 0.6490(9) -0.0168(6) 0.7430(5) 0.0404(12) Uani 1 1 d . . . C17 C 0.8121(8) 0.0299(6) 0.7287(5) 0.0383(12) Uani 1 1 d . . . H17A H 0.9059 0.0079 0.7623 0.046 Uiso 1 1 calc R . . C18 C 0.8430(8) 0.1063(6) 0.6680(5) 0.0370(12) Uani 1 1 d . . . C19 C 0.3898(9) 0.1341(7) 0.5810(5) 0.0427(13) Uani 1 1 d . . . H19A H 0.2831 0.0949 0.5973 0.064 Uiso 1 1 calc R . . H19B H 0.3554 0.1021 0.5051 0.064 Uiso 1 1 calc R . . H19C H 0.4356 0.2294 0.6062 0.064 Uiso 1 1 calc R . . C110 C 1.0155(8) 0.1494(7) 0.6484(5) 0.0439(14) Uani 1 1 d . . . H11A H 1.0972 0.1178 0.6872 0.066 Uiso 1 1 calc R . . H11B H 1.0753 0.2450 0.6720 0.066 Uiso 1 1 calc R . . H11C H 0.9864 0.1136 0.5734 0.066 Uiso 1 1 calc R . . C111 C 0.6191(11) -0.1043(8) 0.8059(6) 0.0509(16) Uani 1 1 d . . . H11D H 0.4985 -0.1260 0.8085 0.076 Uiso 1 1 calc R . . H11E H 0.7128 -0.0597 0.8772 0.076 Uiso 1 1 calc R . . H11F H 0.6264 -0.1846 0.7734 0.076 Uiso 1 1 calc R . . Au2 Au 0.73153(3) 0.54625(2) 0.681113(19) 0.04207(9) Uani 1 1 d . . . S2 S 0.6762(3) 0.6537(2) 0.56691(16) 0.0540(4) Uani 1 1 d . . . N21 N 0.7805(7) 0.3929(5) 0.8340(4) 0.0398(11) Uani 1 1 d . . . N22 N 1.0274(9) 0.8489(7) 0.6134(6) 0.0547(15) Uani 1 1 d . . . C21 C 0.7650(9) 0.4520(6) 0.7782(5) 0.0404(13) Uani 1 1 d . . . C22 C 0.8885(10) 0.7660(7) 0.5969(5) 0.0447(14) Uani 1 1 d . . . C23 C 0.8002(8) 0.3268(6) 0.9050(5) 0.0377(12) Uani 1 1 d . . . C24 C 0.6532(8) 0.2671(7) 0.9298(5) 0.0406(13) Uani 1 1 d . . . C25 C 0.6783(10) 0.2065(7) 1.0015(5) 0.0458(14) Uani 1 1 d . . . H25A H 0.5804 0.1684 1.0217 0.055 Uiso 1 1 calc R . . C26 C 0.8417(10) 0.1979(8) 1.0470(5) 0.0481(15) Uani 1 1 d . . . C27 C 0.9841(9) 0.2578(7) 1.0174(5) 0.0432(13) Uani 1 1 d . . . H27A H 1.0963 0.2533 1.0473 0.052 Uiso 1 1 calc R . . C28 C 0.9698(9) 0.3229(6) 0.9471(5) 0.0396(12) Uani 1 1 d . . . C29 C 0.4767(9) 0.2766(8) 0.8839(6) 0.0501(16) Uani 1 1 d . . . H29A H 0.3889 0.2289 0.9101 0.075 Uiso 1 1 calc R . . H29B H 0.4279 0.2385 0.8074 0.075 Uiso 1 1 calc R . . H29C H 0.4986 0.3685 0.9043 0.075 Uiso 1 1 calc R . . C210 C 1.1259(9) 0.3882(7) 0.9179(5) 0.0421(13) Uani 1 1 d . . . H21A H 1.2314 0.3757 0.9558 0.063 Uiso 1 1 calc R . . H21B H 1.1576 0.4818 0.9365 0.063 Uiso 1 1 calc R . . H21C H 1.0905 0.3498 0.8423 0.063 Uiso 1 1 calc R . . C211 C 0.8607(12) 0.1278(10) 1.1241(7) 0.062(2) Uani 1 1 d . . . H21D H 0.9831 0.1313 1.1472 0.093 Uiso 1 1 calc R . . H21E H 0.7699 0.0364 1.0907 0.093 Uiso 1 1 calc R . . H21F H 0.8414 0.1697 1.1846 0.093 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 0.04206(14) 0.04600(15) 0.04295(14) 0.01844(10) 0.01707(10) 0.01829(11) S1 0.0456(9) 0.0705(12) 0.0589(11) 0.0357(10) 0.0147(8) 0.0107(9) N11 0.039(2) 0.041(2) 0.038(2) 0.010(2) 0.019(2) 0.018(2) N12 0.055(3) 0.080(5) 0.064(4) 0.038(4) 0.028(3) 0.039(4) C11 0.038(3) 0.044(3) 0.043(3) 0.015(2) 0.019(2) 0.021(2) C12 0.042(3) 0.049(3) 0.050(3) 0.021(3) 0.022(3) 0.022(3) C13 0.036(2) 0.039(3) 0.031(2) 0.011(2) 0.014(2) 0.016(2) C14 0.033(2) 0.041(3) 0.039(3) 0.009(2) 0.018(2) 0.019(2) C15 0.038(3) 0.040(3) 0.044(3) 0.008(2) 0.020(2) 0.016(2) C16 0.045(3) 0.043(3) 0.039(3) 0.014(2) 0.022(3) 0.021(3) C17 0.039(3) 0.038(3) 0.038(3) 0.015(2) 0.012(2) 0.018(2) C18 0.035(3) 0.042(3) 0.037(3) 0.011(2) 0.016(2) 0.020(2) C19 0.040(3) 0.051(3) 0.045(3) 0.013(3) 0.022(3) 0.027(3) C110 0.034(3) 0.054(4) 0.047(3) 0.016(3) 0.021(3) 0.021(3) C111 0.057(4) 0.050(4) 0.055(4) 0.023(3) 0.030(3) 0.025(3) Au2 0.04277(14) 0.04134(14) 0.04551(14) 0.01570(10) 0.01832(11) 0.02049(10) S2 0.0451(8) 0.0547(10) 0.0581(10) 0.0267(8) 0.0134(8) 0.0183(8) N21 0.039(2) 0.039(2) 0.036(2) 0.0063(19) 0.012(2) 0.016(2) N22 0.053(3) 0.062(4) 0.062(4) 0.027(3) 0.031(3) 0.029(3) C21 0.042(3) 0.038(3) 0.046(3) 0.016(2) 0.023(3) 0.018(2) C22 0.053(3) 0.044(3) 0.046(3) 0.019(3) 0.025(3) 0.024(3) C23 0.037(3) 0.041(3) 0.035(2) 0.008(2) 0.013(2) 0.020(2) C24 0.035(3) 0.048(3) 0.040(3) 0.010(2) 0.017(2) 0.021(2) C25 0.047(3) 0.051(3) 0.041(3) 0.014(3) 0.019(3) 0.021(3) C26 0.046(3) 0.055(4) 0.042(3) 0.017(3) 0.016(3) 0.021(3) C27 0.038(3) 0.047(3) 0.040(3) 0.009(2) 0.013(2) 0.019(3) C28 0.042(3) 0.039(3) 0.037(3) 0.006(2) 0.015(2) 0.020(2) C29 0.041(3) 0.061(4) 0.050(3) 0.016(3) 0.017(3) 0.026(3) C210 0.039(3) 0.046(3) 0.040(3) 0.013(2) 0.018(2) 0.016(2) C211 0.061(4) 0.078(6) 0.054(4) 0.037(4) 0.020(4) 0.031(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 C11 1.951(7) . ? Au1 S1 2.289(2) . ? S1 C12 1.685(7) . ? N11 C11 1.172(9) . ? N11 C13 1.374(8) . ? N12 C12 1.134(9) . ? C13 C14 1.405(8) . ? C13 C18 1.407(8) . ? C14 C15 1.381(9) . ? C14 C19 1.503(9) . ? C15 C16 1.405(9) . ? C15 H15A 0.9500 . ? C16 C17 1.393(9) . ? C16 C111 1.492(10) . ? C17 C18 1.373(9) . ? C17 H17A 0.9500 . ? C18 C110 1.502(9) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C110 H11A 0.9800 . ? C110 H11B 0.9800 . ? C110 H11C 0.9800 . ? C111 H11D 0.9800 . ? C111 H11E 0.9800 . ? C111 H11F 0.9800 . ? Au2 C21 1.949(7) . ? Au2 S2 2.284(2) . ? S2 C22 1.685(7) . ? N21 C21 1.160(9) . ? N21 C23 1.397(9) . ? N22 C22 1.156(10) . ? C23 C24 1.385(9) . ? C23 C28 1.414(9) . ? C24 C25 1.362(10) . ? C24 C29 1.506(9) . ? C25 C26 1.401(10) . ? C25 H25A 0.9500 . ? C26 C27 1.399(10) . ? C26 C211 1.499(11) . ? C27 C28 1.375(10) . ? C27 H27A 0.9500 . ? C28 C210 1.501(9) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C210 H21A 0.9800 . ? C210 H21B 0.9800 . ? C210 H21C 0.9800 . ? C211 H21D 0.9800 . ? C211 H21E 0.9800 . ? C211 H21F 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 Au1 S1 174.6(2) . . ? C12 S1 Au1 102.9(3) . . ? C11 N11 C13 178.2(6) . . ? N11 C11 Au1 176.4(6) . . ? N12 C12 S1 175.3(7) . . ? N11 C13 C14 118.6(6) . . ? N11 C13 C18 118.6(6) . . ? C14 C13 C18 122.9(6) . . ? C15 C14 C13 117.0(6) . . ? C15 C14 C19 122.3(6) . . ? C13 C14 C19 120.7(6) . . ? C14 C15 C16 122.2(6) . . ? C14 C15 H15A 118.9 . . ? C16 C15 H15A 118.9 . . ? C17 C16 C15 117.9(6) . . ? C17 C16 C111 120.8(6) . . ? C15 C16 C111 121.2(6) . . ? C18 C17 C16 122.9(6) . . ? C18 C17 H17A 118.6 . . ? C16 C17 H17A 118.6 . . ? C17 C18 C13 117.0(6) . . ? C17 C18 C110 122.2(6) . . ? C13 C18 C110 120.8(6) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C110 H11A 109.5 . . ? C18 C110 H11B 109.5 . . ? H11A C110 H11B 109.5 . . ? C18 C110 H11C 109.5 . . ? H11A C110 H11C 109.5 . . ? H11B C110 H11C 109.5 . . ? C16 C111 H11D 109.5 . . ? C16 C111 H11E 109.5 . . ? H11D C111 H11E 109.5 . . ? C16 C111 H11F 109.5 . . ? H11D C111 H11F 109.5 . . ? H11E C111 H11F 109.5 . . ? C21 Au2 S2 176.8(2) . . ? C22 S2 Au2 101.2(3) . . ? C21 N21 C23 177.3(6) . . ? N21 C21 Au2 178.1(6) . . ? N22 C22 S2 174.2(7) . . ? C24 C23 N21 118.9(6) . . ? C24 C23 C28 123.3(6) . . ? N21 C23 C28 117.9(6) . . ? C25 C24 C23 117.4(6) . . ? C25 C24 C29 121.7(6) . . ? C23 C24 C29 120.8(6) . . ? C24 C25 C26 123.1(7) . . ? C24 C25 H25A 118.5 . . ? C26 C25 H25A 118.5 . . ? C27 C26 C25 116.9(7) . . ? C27 C26 C211 122.3(7) . . ? C25 C26 C211 120.8(7) . . ? C28 C27 C26 123.3(6) . . ? C28 C27 H27A 118.4 . . ? C26 C27 H27A 118.4 . . ? C27 C28 C23 116.1(6) . . ? C27 C28 C210 122.2(6) . . ? C23 C28 C210 121.7(6) . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C210 H21A 109.5 . . ? C28 C210 H21B 109.5 . . ? H21A C210 H21B 109.5 . . ? C28 C210 H21C 109.5 . . ? H21A C210 H21C 109.5 . . ? H21B C210 H21C 109.5 . . ? C26 C211 H21D 109.5 . . ? C26 C211 H21E 109.5 . . ? H21D C211 H21E 109.5 . . ? C26 C211 H21F 109.5 . . ? H21D C211 H21F 109.5 . . ? H21E C211 H21F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 31.03 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 1.397 _refine_diff_density_min -1.478 _refine_diff_density_rms 0.197