Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_compound1 _database_code_CSD 166713 _audit_creation_method SHELXL-97 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Cerrada,E.' 'Diaz, C.' 'Diaz, M. C.' 'Hursthouse,M.B.' 'Laguna,M.' 'Light, M. E.' _publ_contact_author 'Dr. Prof. Mariano Laguna' _publ_contact_author_address ; Departmento Quimica Inorganica Instituto de Ciencia de Materiales Plaza S. Francisco Zaragoza 50009 SPAIN ; _publ_contact_author_email mlaguna@posta.unizar.es _publ_section_title ; Tetrathiafulvalene-functionalized phosphine as a coordinating ligand. X-Ray structures of (PPh2)4TTF and [(AuCI)4{(PPh2)4TTF}] ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H41 Cl3 P4 S4' _chemical_formula_weight 1060.35 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6800(9) _cell_length_b 11.7691(10) _cell_length_c 12.6621(12) _cell_angle_alpha 72.829(6) _cell_angle_beta 69.653(4) _cell_angle_gamma 82.261(5) _cell_volume 1291.4(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(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 0.20 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 546 _exptl_absorpt_coefficient_mu 0.500 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8644 _exptl_absorpt_correction_T_max 0.9950 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9756 _diffrn_reflns_av_R_equivalents 0.0807 _diffrn_reflns_av_sigmaI/netI 0.0995 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 23.26 _reflns_number_total 3687 _reflns_number_gt 2243 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0687P)^2^+0.6414P] 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 SHELXL _refine_ls_extinction_coef 0.008(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3687 _refine_ls_number_parameters 317 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1109 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1614 _refine_ls_wR_factor_gt 0.1356 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.104 _refine_ls_shift/su_mean 0.008 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 C1 C 0.5769(6) 0.6320(5) -0.2288(5) 0.0470(15) Uani 1 1 d . . . H1 H 0.6002 0.5735 -0.1669 0.056 Uiso 1 1 calc R . . C2 C 0.6783(6) 0.6546(5) -0.3395(5) 0.0561(17) Uani 1 1 d . . . H2 H 0.7697 0.6108 -0.3538 0.067 Uiso 1 1 calc R . . C3 C 0.6470(7) 0.7407(6) -0.4294(6) 0.067(2) Uani 1 1 d . . . H3 H 0.7183 0.7576 -0.5053 0.081 Uiso 1 1 calc R . . C4 C 0.5138(7) 0.8026(5) -0.4106(5) 0.0570(17) Uani 1 1 d . . . H4 H 0.4918 0.8608 -0.4733 0.068 Uiso 1 1 calc R . . C5 C 0.4111(6) 0.7790(5) -0.2982(5) 0.0472(15) Uani 1 1 d . . . H5 H 0.3192 0.8222 -0.2844 0.057 Uiso 1 1 calc R . . C6 C 0.4420(6) 0.6926(4) -0.2059(4) 0.0352(13) Uani 1 1 d . . . C7 C 0.1362(5) 0.7046(5) -0.0771(4) 0.0348(13) Uani 1 1 d . . . C8 C 0.0636(6) 0.8143(5) -0.0653(4) 0.0403(13) Uani 1 1 d . . . H8 H 0.1100 0.8698 -0.0483 0.048 Uiso 1 1 calc R . . C9 C -0.0727(6) 0.8423(6) -0.0778(5) 0.0556(16) Uani 1 1 d . . . H9 H -0.1211 0.9162 -0.0686 0.067 Uiso 1 1 calc R . . C10 C -0.1401(7) 0.7617(7) -0.1040(5) 0.0649(18) Uani 1 1 d . . . H10 H -0.2341 0.7811 -0.1139 0.078 Uiso 1 1 calc R . . C11 C -0.0707(7) 0.6545(6) -0.1156(5) 0.0558(17) Uani 1 1 d . . . H11 H -0.1175 0.5991 -0.1323 0.067 Uiso 1 1 calc R . . C12 C 0.0656(6) 0.6270(5) -0.1032(5) 0.0462(15) Uani 1 1 d . . . H12 H 0.1129 0.5528 -0.1128 0.055 Uiso 1 1 calc R . . C13 C 0.3499(5) 0.7682(4) 0.0002(4) 0.0309(12) Uani 1 1 d . . . C14 C 0.4595(5) 0.9532(4) 0.0115(4) 0.0318(12) Uani 1 1 d . . . C15 C 0.2935(5) 0.7681(4) 0.1137(4) 0.0301(12) Uani 1 1 d . . . C16 C 0.1974(5) 0.6523(4) 0.3550(4) 0.0333(13) Uani 1 1 d . . . C17 C 0.3384(6) 0.6357(5) 0.3616(5) 0.0470(15) Uani 1 1 d . . . H17 H 0.4189 0.6311 0.2934 0.056 Uiso 1 1 calc R . . C18 C 0.3665(7) 0.6258(5) 0.4629(5) 0.0570(17) Uani 1 1 d . . . H18 H 0.4650 0.6173 0.4641 0.068 Uiso 1 1 calc R . . C19 C 0.2500(8) 0.6285(6) 0.5630(6) 0.069(2) Uani 1 1 d . . . H19 H 0.2679 0.6214 0.6339 0.083 Uiso 1 1 calc R . . C20 C 0.1089(7) 0.6412(6) 0.5603(5) 0.0659(19) Uani 1 1 d . . . H20 H 0.0289 0.6421 0.6297 0.079 Uiso 1 1 calc R . . C21 C 0.0809(6) 0.6530(5) 0.4562(5) 0.0497(16) Uani 1 1 d . . . H21 H -0.0176 0.6615 0.4551 0.060 Uiso 1 1 calc R . . C22 C -0.0113(5) 0.7236(5) 0.2307(4) 0.0376(13) Uani 1 1 d . . . C23 C -0.0533(6) 0.8370(5) 0.2411(5) 0.0488(15) Uani 1 1 d . . . H23 H 0.0149 0.8852 0.2453 0.059 Uiso 1 1 calc R . . C24 C -0.1954(7) 0.8817(6) 0.2456(5) 0.0653(19) Uani 1 1 d . . . H24 H -0.2246 0.9599 0.2534 0.078 Uiso 1 1 calc R . . C25 C -0.2924(6) 0.8125(6) 0.2387(5) 0.0622(18) Uani 1 1 d . . . H25 H -0.3891 0.8433 0.2412 0.075 Uiso 1 1 calc R . . C26 C -0.2529(7) 0.6999(7) 0.2282(6) 0.072(2) Uani 1 1 d . . . H26 H -0.3213 0.6522 0.2236 0.086 Uiso 1 1 calc R . . C27 C -0.1124(6) 0.6560(6) 0.2242(5) 0.0567(17) Uani 1 1 d . . . H27 H -0.0846 0.5775 0.2168 0.068 Uiso 1 1 calc R . . C28 C -0.0299(8) 0.0672(6) 0.5209(4) 0.167(10) Uani 0.50 1 d PDU . . H28 H -0.0375 0.1449 0.5400 0.201 Uiso 0.50 1 calc PR . . P1 P 0.31320(14) 0.65308(11) -0.05631(12) 0.0339(4) Uani 1 1 d . . . P2 P 0.17045(14) 0.65277(11) 0.21950(11) 0.0342(4) Uani 1 1 d . . . S1 S 0.46261(14) 0.88638(11) -0.09697(11) 0.0350(4) Uani 1 1 d . . . S2 S 0.34087(14) 0.88632(11) 0.15227(11) 0.0346(4) Uani 1 1 d . . . Cl1 Cl -0.1875(7) -0.0147(9) 0.5861(7) 0.219(4) Uani 0.50 1 d PDU . . Cl2 Cl 0.1034(10) -0.0333(9) 0.5594(9) 0.246(5) Uani 0.50 1 d PDU . . Cl3 Cl 0.0118(11) 0.0763(5) 0.3744(4) 0.168(3) Uani 0.50 1 d PDU . . 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 C1 0.043(4) 0.039(3) 0.049(4) -0.005(3) -0.007(3) -0.002(3) C2 0.035(3) 0.062(4) 0.056(4) -0.013(3) 0.002(3) 0.000(3) C3 0.055(4) 0.088(5) 0.044(4) -0.022(4) 0.008(3) -0.009(4) C4 0.060(4) 0.067(4) 0.033(4) -0.003(3) -0.009(3) -0.007(3) C5 0.042(3) 0.059(4) 0.037(3) -0.014(3) -0.006(3) -0.004(3) C6 0.037(3) 0.038(3) 0.036(3) -0.015(3) -0.012(3) -0.009(2) C7 0.024(3) 0.049(3) 0.031(3) -0.006(2) -0.008(2) -0.011(2) C8 0.038(3) 0.040(3) 0.040(3) -0.003(2) -0.013(3) -0.006(3) C9 0.036(4) 0.069(4) 0.057(4) -0.008(3) -0.017(3) 0.001(3) C10 0.038(4) 0.094(5) 0.059(4) 0.000(4) -0.024(3) -0.011(4) C11 0.042(4) 0.076(5) 0.052(4) -0.008(3) -0.020(3) -0.019(3) C12 0.039(4) 0.061(4) 0.043(3) -0.015(3) -0.013(3) -0.016(3) C13 0.022(3) 0.034(3) 0.036(3) -0.010(2) -0.006(2) -0.005(2) C14 0.026(3) 0.037(3) 0.029(3) -0.007(2) -0.006(2) -0.004(2) C15 0.022(3) 0.034(3) 0.034(3) -0.008(2) -0.009(2) -0.005(2) C16 0.029(3) 0.032(3) 0.036(3) -0.006(2) -0.008(3) -0.008(2) C17 0.041(4) 0.054(4) 0.045(4) -0.008(3) -0.014(3) -0.007(3) C18 0.051(4) 0.061(4) 0.059(4) -0.001(3) -0.027(4) -0.016(3) C19 0.070(5) 0.084(5) 0.057(4) 0.005(4) -0.035(4) -0.033(4) C20 0.057(4) 0.098(5) 0.034(4) -0.007(3) -0.008(3) -0.019(4) C21 0.043(4) 0.068(4) 0.034(3) -0.005(3) -0.009(3) -0.018(3) C22 0.028(3) 0.048(3) 0.027(3) -0.001(2) -0.002(2) -0.009(2) C23 0.024(3) 0.047(4) 0.061(4) -0.005(3) -0.003(3) -0.004(3) C24 0.049(4) 0.055(4) 0.062(4) 0.007(3) -0.003(3) 0.004(3) C25 0.024(3) 0.086(5) 0.062(4) 0.006(4) -0.017(3) -0.006(3) C26 0.042(4) 0.086(5) 0.092(6) -0.019(4) -0.025(4) -0.020(4) C27 0.029(3) 0.081(5) 0.059(4) -0.018(3) -0.007(3) -0.019(3) C28 0.213(18) 0.182(18) 0.162(16) -0.031(13) -0.138(15) -0.015(15) P1 0.0317(8) 0.0359(8) 0.0365(8) -0.0117(6) -0.0106(6) -0.0059(6) P2 0.0287(8) 0.0372(8) 0.0348(8) -0.0085(6) -0.0056(6) -0.0101(6) S1 0.0336(8) 0.0394(8) 0.0314(8) -0.0096(6) -0.0057(6) -0.0117(6) S2 0.0327(8) 0.0384(8) 0.0323(8) -0.0111(6) -0.0048(6) -0.0120(6) Cl1 0.252(9) 0.230(8) 0.136(6) -0.035(6) -0.005(6) -0.067(7) Cl2 0.289(12) 0.223(9) 0.231(11) -0.038(8) -0.089(9) -0.066(8) Cl3 0.290(10) 0.129(5) 0.080(4) -0.028(3) -0.058(5) 0.006(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 C1 C2 1.375(7) . ? C1 C6 1.381(7) . ? C2 C3 1.375(9) . ? C3 C4 1.373(9) . ? C4 C5 1.395(7) . ? C5 C6 1.397(8) . ? C6 P1 1.831(5) . ? C7 C12 1.384(6) . ? C7 C8 1.407(7) . ? C7 P1 1.820(5) . ? C8 C9 1.369(8) . ? C9 C10 1.392(8) . ? C10 C11 1.370(9) . ? C11 C12 1.367(8) . ? C13 C15 1.347(6) . ? C13 S1 1.761(4) . ? C13 P1 1.832(4) . ? C14 C14 1.340(8) 2_675 ? C14 S1 1.763(4) . ? C14 S2 1.763(4) . ? C15 S2 1.764(4) . ? C15 P2 1.819(4) . ? C16 C21 1.383(7) . ? C16 C17 1.381(7) . ? C16 P2 1.821(5) . ? C17 C18 1.371(8) . ? C18 C19 1.378(8) . ? C19 C20 1.365(9) . ? C20 C21 1.400(8) . ? C22 C23 1.373(7) . ? C22 C27 1.379(7) . ? C22 P2 1.820(5) . ? C23 C24 1.393(8) . ? C24 C25 1.363(8) . ? C25 C26 1.361(9) . ? C26 C27 1.377(9) . ? C28 Cl3 1.729(2) . ? C28 Cl1 1.729(2) . ? C28 Cl2 1.729(2) . ? Cl1 Cl2 1.685(9) 2_556 ? Cl1 Cl3 1.928(12) 2_556 ? Cl1 C28 2.192(11) 2_556 ? Cl2 Cl3 1.206(9) 2_556 ? Cl2 C28 1.586(11) 2_556 ? Cl2 Cl1 1.685(9) 2_556 ? Cl3 Cl2 1.206(9) 2_556 ? Cl3 C28 1.845(10) 2_556 ? Cl3 Cl1 1.928(12) 2_556 ? 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 C1 C6 121.4(6) . . ? C1 C2 C3 119.8(6) . . ? C4 C3 C2 120.7(6) . . ? C3 C4 C5 119.2(6) . . ? C6 C5 C4 120.7(6) . . ? C1 C6 C5 118.2(5) . . ? C1 C6 P1 117.9(4) . . ? C5 C6 P1 123.9(4) . . ? C12 C7 C8 117.6(5) . . ? C12 C7 P1 116.7(4) . . ? C8 C7 P1 125.7(4) . . ? C9 C8 C7 121.0(5) . . ? C8 C9 C10 119.6(6) . . ? C11 C10 C9 120.0(6) . . ? C12 C11 C10 120.2(5) . . ? C11 C12 C7 121.5(6) . . ? C15 C13 S1 117.6(3) . . ? C15 C13 P1 123.1(3) . . ? S1 C13 P1 119.3(3) . . ? C14 C14 S1 122.8(5) 2_675 . ? C14 C14 S2 123.1(5) 2_675 . ? S1 C14 S2 114.2(2) . . ? C13 C15 S2 116.8(3) . . ? C13 C15 P2 120.7(3) . . ? S2 C15 P2 122.4(3) . . ? C21 C16 C17 118.1(5) . . ? C21 C16 P2 122.5(4) . . ? C17 C16 P2 118.9(4) . . ? C18 C17 C16 122.3(5) . . ? C17 C18 C19 119.2(6) . . ? C20 C19 C18 120.0(6) . . ? C19 C20 C21 120.6(6) . . ? C16 C21 C20 119.7(6) . . ? C23 C22 C27 118.5(5) . . ? C23 C22 P2 126.1(4) . . ? C27 C22 P2 115.4(4) . . ? C22 C23 C24 120.3(5) . . ? C25 C24 C23 119.6(6) . . ? C26 C25 C24 121.0(6) . . ? C25 C26 C27 119.1(6) . . ? C26 C27 C22 121.5(6) . . ? Cl3 C28 Cl1 102.99(17) . . ? Cl3 C28 Cl2 102.69(17) . . ? Cl1 C28 Cl2 102.85(17) . . ? C7 P1 C13 102.1(2) . . ? C7 P1 C6 102.5(2) . . ? C13 P1 C6 100.6(2) . . ? C22 P2 C15 102.9(2) . . ? C22 P2 C16 104.0(2) . . ? C15 P2 C16 101.7(2) . . ? C14 S1 C13 95.4(2) . . ? C15 S2 C14 95.7(2) . . ? Cl2 Cl1 C28 55.4(4) 2_556 . ? Cl2 Cl1 Cl3 96.5(5) 2_556 2_556 ? C28 Cl1 Cl3 60.3(3) . 2_556 ? Cl2 Cl1 C28 50.9(3) 2_556 2_556 ? C28 Cl1 C28 52.2(3) . 2_556 ? Cl3 Cl1 C28 49.1(3) 2_556 2_556 ? Cl3 Cl2 C28 75.1(5) 2_556 2_556 ? Cl3 Cl2 Cl1 138.1(8) 2_556 2_556 ? C28 Cl2 Cl1 63.7(4) 2_556 2_556 ? Cl3 Cl2 C28 75.6(6) 2_556 . ? C28 Cl2 C28 64.6(5) 2_556 . ? Cl1 Cl2 C28 79.9(4) 2_556 . ? Cl2 Cl3 C28 62.5(5) 2_556 . ? Cl2 Cl3 C28 65.2(4) 2_556 2_556 ? C28 Cl3 C28 59.5(4) . 2_556 ? Cl2 Cl3 Cl1 117.4(7) 2_556 2_556 ? C28 Cl3 Cl1 73.5(3) . 2_556 ? C28 Cl3 Cl1 54.5(3) 2_556 2_556 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.571 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.067 # data for compound 2 data_compound2 _database_code_CSD 166714 _audit_creation_method SHELXL-97 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Cerrada,E.' 'Diaz, C.' 'Diaz, M. C.' 'Hursthouse,M.B.' 'Laguna,M.' 'Light, M. E.' _publ_contact_author 'Dr. Prof. Mariano Laguna' _publ_contact_author_address ; Departmento Quimica Inorganica Instituto de Ciencia de Materiales Plaza S. Francisco Zaragoza 50009 SPAIN ; _publ_contact_author_email mlaguna@posta.unizar.es _publ_section_title ; Tetrathiafulvalene-functionalized phosphine as a coordinating ligand. X-Ray structures of (PPh2)4TTF and [(AuCI)4{(PPh2)4TTF}] ; _chemical_name_systematic ; Dichlorine-Tetrakis(bisdiphenylphosphino)tetrathiafulvalene-gold(I) ; _chemical_formula_sum 'C56 H42 Au4 Cl8 P4 S4' _chemical_formula_weight 2038.48 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' '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 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.362(2) _cell_length_b 17.624(4) _cell_length_c 15.911(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.99(3) _cell_angle_gamma 90.00 _cell_volume 3077.7(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1908 _exptl_absorpt_coefficient_mu 10.129 _exptl_absorpt_correction_type 'SORTAV' _exptl_absorpt_correction_T_min 0.32 _exptl_absorpt_correction_T_max 0.61 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Crysta (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_fileds are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 10 degree phi range. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Phi+Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 21144 _diffrn_reflns_av_R_equivalents 0.0869 _diffrn_reflns_av_sigmaI/netI 0.0642 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5428 _reflns_number_gt 4252 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinoski and Monir, 1997' 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO and COLLECT' _computing_data_reduction 'DENZO and COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v5 (Siemens)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0860P)^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 5428 _refine_ls_number_parameters 343 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1349 _refine_ls_wR_factor_gt 0.1237 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.012 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.70448(3) 0.31259(2) 0.38653(2) 0.03470(15) Uani 1 d . . . Au2 Au 0.79935(3) 0.29149(2) 0.22823(2) 0.03447(15) Uani 1 d . . . Cl1 Cl 0.7171(3) 0.44000(17) 0.41150(19) 0.0587(8) Uani 1 d . . . Cl2 Cl 0.6619(2) 0.37436(17) 0.14565(17) 0.0486(7) Uani 1 d . . . S1 S 0.8217(2) 0.05639(15) 0.47068(16) 0.0367(6) Uani 1 d . . . S2 S 1.0330(2) 0.07367(15) 0.39767(15) 0.0333(6) Uani 1 d . . . P1 P 0.6796(2) 0.18828(14) 0.37035(17) 0.0298(5) Uani 1 d . . . P2 P 0.9532(2) 0.22166(15) 0.30611(15) 0.0291(5) Uani 1 d . . . C1 C 0.9715(8) 0.0263(6) 0.4733(5) 0.030(2) Uani 1 d . . . C2 C 0.9206(8) 0.1446(6) 0.3721(5) 0.031(2) Uani 1 d . . . C3 C 0.8205(8) 0.1335(5) 0.4024(6) 0.028(2) Uani 1 d . . . C11 C 0.6119(8) 0.1548(6) 0.2606(6) 0.035(2) Uani 1 d . . . C12 C 0.5382(8) 0.2033(7) 0.2016(7) 0.043(3) Uani 1 d . . . H12 H 0.5269 0.2531 0.2171 0.052 Uiso 1 calc R . . C13 C 0.4814(10) 0.1771(9) 0.1192(8) 0.058(3) Uani 1 d . . . H13 H 0.4302 0.2098 0.0805 0.069 Uiso 1 calc R . . C14 C 0.4971(11) 0.1062(10) 0.0927(8) 0.072(5) Uani 1 d . . . H14 H 0.4576 0.0900 0.0369 0.087 Uiso 1 calc R . . C15 C 0.5738(12) 0.0576(9) 0.1508(10) 0.073(4) Uani 1 d . . . H15 H 0.5872 0.0089 0.1328 0.088 Uiso 1 calc R . . C16 C 0.6314(9) 0.0803(8) 0.2359(8) 0.055(3) Uani 1 d . . . H16 H 0.6810 0.0470 0.2748 0.066 Uiso 1 calc R . . C21 C 0.5829(8) 0.1525(6) 0.4363(6) 0.034(2) Uani 1 d . . . C22 C 0.4950(12) 0.0995(9) 0.4065(10) 0.078(5) Uani 1 d . . . H22 H 0.4873 0.0776 0.3521 0.094 Uiso 1 calc R . . C23 C 0.4165(14) 0.0777(11) 0.4563(11) 0.098(6) Uani 1 d . . . H23 H 0.3574 0.0408 0.4360 0.118 Uiso 1 calc R . . C24 C 0.4273(13) 0.1112(9) 0.5359(11) 0.078(5) Uani 1 d . . . H24 H 0.3751 0.0972 0.5695 0.094 Uiso 1 calc R . . C25 C 0.5125(16) 0.1638(8) 0.5652(10) 0.087(5) Uani 1 d . . . H25 H 0.5189 0.1869 0.6187 0.104 Uiso 1 calc R . . C26 C 0.5912(13) 0.1839(7) 0.5158(10) 0.071(4) Uani 1 d . . . H26 H 0.6515 0.2198 0.5373 0.085 Uiso 1 calc R . . C31 C 1.0597(8) 0.2826(6) 0.3804(6) 0.036(2) Uani 1 d . . . C32 C 1.0627(10) 0.3579(7) 0.3576(7) 0.048(3) Uani 1 d . . . H32 H 1.0071 0.3763 0.3082 0.058 Uiso 1 calc R . . C33 C 1.1491(10) 0.4061(7) 0.4085(8) 0.055(3) Uani 1 d . . . H33 H 1.1533 0.4563 0.3917 0.066 Uiso 1 calc R . . C34 C 1.2269(9) 0.3806(7) 0.4822(7) 0.047(3) Uani 1 d . . . H34 H 1.2826 0.4137 0.5170 0.056 Uiso 1 calc R . . C35 C 1.2238(12) 0.3063(7) 0.5059(7) 0.058(3) Uani 1 d . . . H35 H 1.2781 0.2889 0.5564 0.070 Uiso 1 calc R . . C36 C 1.1411(10) 0.2571(7) 0.4557(7) 0.051(3) Uani 1 d . . . H36 H 1.1399 0.2065 0.4723 0.062 Uiso 1 calc R . . C41 C 1.0396(8) 0.1748(6) 0.2400(6) 0.036(2) Uani 1 d . . . C42 C 0.9812(9) 0.1227(7) 0.1771(7) 0.049(3) Uani 1 d . . . H42 H 0.9011 0.1086 0.1731 0.058 Uiso 1 calc R . . C43 C 1.0418(10) 0.0926(8) 0.1214(7) 0.057(3) Uani 1 d . . . H43 H 1.0001 0.0611 0.0767 0.068 Uiso 1 calc R . . C44 C 1.1623(11) 0.1075(8) 0.1296(8) 0.061(4) Uani 1 d . . . H44 H 1.2036 0.0850 0.0927 0.073 Uiso 1 calc R . . C45 C 1.2215(14) 0.1573(12) 0.1948(10) 0.092(6) Uani 1 d . . . C46 C 1.1593(11) 0.1895(9) 0.2491(7) 0.069(4) Uani 1 d . . . H46 H 1.2001 0.2220 0.2931 0.083 Uiso 1 calc R . . Cl4 Cl 0.3973(5) 0.3381(4) 0.3307(5) 0.157(3) Uani 1 d DU . . Cl3 Cl 0.2693(5) 0.4446(8) 0.2002(4) 0.274(7) Uani 1 d DU . . C99 C 0.4060(16) 0.4130(11) 0.2565(16) 0.129(8) Uani 1 d DU . . 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 0.0420(3) 0.0320(3) 0.0299(2) 0.00010(15) 0.00893(17) -0.00140(16) Au2 0.0328(2) 0.0431(3) 0.0269(2) 0.00816(16) 0.00664(16) 0.00222(16) Cl1 0.084(2) 0.0361(17) 0.0520(17) -0.0036(13) 0.0101(15) -0.0045(15) Cl2 0.0459(14) 0.0571(19) 0.0413(14) 0.0192(13) 0.0088(12) 0.0124(13) S1 0.0311(12) 0.0405(16) 0.0430(14) 0.0133(12) 0.0174(11) 0.0018(11) S2 0.0303(12) 0.0379(15) 0.0340(13) 0.0113(11) 0.0123(10) 0.0026(10) P1 0.0271(12) 0.0274(14) 0.0355(14) 0.0002(10) 0.0094(10) 0.0016(10) P2 0.0284(12) 0.0338(14) 0.0240(12) 0.0058(10) 0.0049(9) -0.0037(10) C1 0.029(5) 0.038(6) 0.025(5) 0.002(4) 0.009(4) -0.010(4) C2 0.040(5) 0.034(6) 0.019(4) 0.000(4) 0.008(4) -0.002(4) C3 0.027(5) 0.031(5) 0.026(5) 0.004(4) 0.002(4) 0.000(4) C11 0.025(5) 0.043(6) 0.039(6) -0.009(5) 0.009(4) -0.004(4) C12 0.025(5) 0.062(8) 0.039(6) -0.001(5) 0.003(4) -0.004(5) C13 0.032(6) 0.096(11) 0.041(7) -0.002(7) 0.001(5) -0.001(6) C14 0.040(7) 0.131(15) 0.048(8) -0.033(9) 0.014(6) -0.027(8) C15 0.050(7) 0.087(11) 0.085(10) -0.053(9) 0.021(7) -0.017(7) C16 0.027(5) 0.072(9) 0.062(7) -0.024(7) 0.005(5) -0.003(5) C21 0.031(5) 0.034(6) 0.041(6) 0.005(5) 0.013(4) -0.002(4) C22 0.068(9) 0.100(12) 0.079(10) -0.015(9) 0.040(8) -0.035(9) C23 0.089(11) 0.114(15) 0.109(13) -0.018(11) 0.057(10) -0.052(10) C24 0.073(9) 0.069(11) 0.114(13) 0.029(9) 0.065(9) 0.020(8) C25 0.151(15) 0.056(9) 0.092(11) -0.019(8) 0.099(12) -0.017(10) C26 0.085(10) 0.049(8) 0.099(11) -0.029(8) 0.059(9) -0.030(7) C31 0.032(5) 0.050(7) 0.026(5) 0.006(4) 0.005(4) -0.009(4) C32 0.048(6) 0.040(7) 0.047(6) 0.006(5) -0.003(5) -0.005(5) C33 0.047(7) 0.035(7) 0.075(8) -0.013(6) 0.002(6) -0.008(5) C34 0.032(5) 0.056(8) 0.040(6) -0.014(5) -0.011(5) -0.010(5) C35 0.068(8) 0.065(9) 0.032(6) 0.008(5) -0.004(6) -0.017(7) C36 0.060(7) 0.053(8) 0.036(6) 0.005(5) 0.004(5) -0.015(6) C41 0.032(5) 0.051(7) 0.025(5) 0.016(5) 0.005(4) 0.010(5) C42 0.029(5) 0.068(9) 0.046(6) -0.003(6) 0.006(5) -0.002(5) C43 0.054(7) 0.079(10) 0.032(6) -0.020(6) 0.002(5) 0.003(6) C44 0.056(7) 0.089(10) 0.044(7) 0.002(7) 0.025(6) 0.010(7) C45 0.073(10) 0.145(17) 0.069(10) -0.020(11) 0.042(8) -0.020(11) C46 0.044(7) 0.132(14) 0.032(6) -0.024(7) 0.013(5) -0.025(7) Cl4 0.091(3) 0.129(5) 0.287(9) -0.009(5) 0.117(5) 0.000(3) Cl3 0.108(4) 0.61(2) 0.086(4) 0.100(7) -0.008(3) -0.115(8) C99 0.093(13) 0.079(13) 0.24(2) 0.040(14) 0.083(14) 0.014(10) _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 2.216(3) . ? Au1 Cl1 2.278(3) . ? Au1 Au2 3.0081(8) . ? Au2 P2 2.233(2) . ? Au2 Cl2 2.288(3) . ? S1 C3 1.739(9) . ? S1 C1 1.773(9) . ? S2 C1 1.752(8) . ? S2 C2 1.759(10) . ? P1 C11 1.815(10) . ? P1 C21 1.818(9) . ? P1 C3 1.825(9) . ? P2 C31 1.809(10) . ? P2 C2 1.812(9) . ? P2 C41 1.813(10) . ? C1 C1 1.310(19) 3_756 ? C2 C3 1.358(12) . ? C11 C12 1.381(15) . ? C11 C16 1.404(16) . ? C12 C13 1.382(16) . ? C13 C14 1.346(19) . ? C14 C15 1.39(2) . ? C15 C16 1.401(17) . ? C21 C22 1.359(16) . ? C21 C26 1.361(16) . ? C22 C23 1.393(18) . ? C23 C24 1.37(2) . ? C24 C25 1.33(2) . ? C25 C26 1.381(17) . ? C31 C32 1.379(16) . ? C31 C36 1.386(14) . ? C32 C33 1.389(15) . ? C33 C34 1.350(15) . ? C34 C35 1.365(16) . ? C35 C36 1.373(16) . ? C41 C46 1.354(15) . ? C41 C42 1.394(15) . ? C42 C43 1.363(15) . ? C43 C44 1.367(16) . ? C44 C45 1.39(2) . ? C45 C46 1.373(19) . ? Cl4 C99 1.789(19) . ? Cl3 C99 1.67(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 174.41(10) . . ? P1 Au1 Au2 80.97(6) . . ? Cl1 Au1 Au2 104.35(8) . . ? P2 Au2 Cl2 172.10(10) . . ? P2 Au2 Au1 90.11(6) . . ? Cl2 Au2 Au1 93.59(7) . . ? C3 S1 C1 95.8(4) . . ? C1 S2 C2 95.9(4) . . ? C11 P1 C21 105.9(4) . . ? C11 P1 C3 102.7(4) . . ? C21 P1 C3 105.9(4) . . ? C11 P1 Au1 116.3(4) . . ? C21 P1 Au1 110.7(3) . . ? C3 P1 Au1 114.5(3) . . ? C31 P2 C2 105.5(4) . . ? C31 P2 C41 106.1(5) . . ? C2 P2 C41 102.6(5) . . ? C31 P2 Au2 109.3(4) . . ? C2 P2 Au2 119.1(3) . . ? C41 P2 Au2 113.1(3) . . ? C1 C1 S2 124.4(9) 3_756 . ? C1 C1 S1 122.5(9) 3_756 . ? S2 C1 S1 113.1(5) . . ? C3 C2 S2 116.1(7) . . ? C3 C2 P2 128.9(8) . . ? S2 C2 P2 114.9(5) . . ? C2 C3 S1 117.6(7) . . ? C2 C3 P1 125.4(7) . . ? S1 C3 P1 116.9(5) . . ? C12 C11 C16 120.0(10) . . ? C12 C11 P1 119.0(8) . . ? C16 C11 P1 121.0(8) . . ? C11 C12 C13 119.3(12) . . ? C14 C13 C12 122.7(13) . . ? C13 C14 C15 118.4(12) . . ? C14 C15 C16 121.5(13) . . ? C15 C16 C11 118.0(13) . . ? C22 C21 C26 118.2(10) . . ? C22 C21 P1 122.4(9) . . ? C26 C21 P1 119.2(8) . . ? C21 C22 C23 120.8(14) . . ? C24 C23 C22 119.2(15) . . ? C25 C24 C23 120.3(12) . . ? C24 C25 C26 119.8(14) . . ? C21 C26 C25 121.7(13) . . ? C32 C31 C36 118.9(10) . . ? C32 C31 P2 117.2(7) . . ? C36 C31 P2 123.8(9) . . ? C31 C32 C33 119.8(10) . . ? C34 C33 C32 120.6(11) . . ? C33 C34 C35 120.0(10) . . ? C34 C35 C36 120.6(11) . . ? C35 C36 C31 120.1(11) . . ? C46 C41 C42 118.7(10) . . ? C46 C41 P2 122.1(9) . . ? C42 C41 P2 119.2(7) . . ? C43 C42 C41 119.8(10) . . ? C42 C43 C44 121.7(11) . . ? C43 C44 C45 118.1(11) . . ? C46 C45 C44 120.1(13) . . ? C41 C46 C45 121.3(12) . . ? Cl3 C99 Cl4 113.4(10) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 2.110 _refine_diff_density_min -3.008 _refine_diff_density_rms 0.233