# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name _publ_author_address A.Molter ; Max-Planck-Institut f\"ur Kohlenforschung Kaiser-Wilhelm-Platz 1 45470 M\"ulheim an der Ruhr Germany ; C.Lehmann ; Max-Planck-Institut f\"ur Kohlenforschung Kaiser-Wilhelm-Platz 1 45470 M\"ulheim an der Ruhr Germany ; G.Deepa '' P.Chiba '' F.Mohr '' _publ_contact_author_name 'Mohr, Fabian' _publ_contact_author_email fmohr@uni-wuppertal.de _publ_section_title ; Synthesis, structures and anti-malaria activity of some gold(I) phosphine complexes containing seleno- and thiosemicarbazone ligands ; _publ_contact_author_address ? _publ_contact_author_phone ? data_7010SADABS _database_code_depnum_ccdc_archive 'CCDC 803631' _audit_creation_date 2010-06-21 _audit_block_code ACA-MS-122-F2 _audit_creation_method SHELXL-97 _chemical_compound_source 'see paper' _chemical_absolute_configuration ? _chemical_formula_moiety 'C14 H20 N4 S' _chemical_formula_sum 'C14 H20 N4 S' _chemical_formula_weight 276.40 _chemical_melting_point ? _chemical_name_common Title _chemical_name_systematic ; Title ; 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' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'p 2yb' _symmetry_Int_Tables_number 4 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1.00 0.00 0.00 0.0300 1.00 0.00 0.00 0.0300 1.00 -1.00 0.00 0.2000 -3.00 -1.00 0.00 0.1200 0.00 1.00 0.00 0.3000 0.00 0.00 -1.00 0.0300 0.00 0.00 1.00 0.0300 0.00 -1.00 5.00 0.1400 0.00 -1.00 -5.00 0.1400 _cell_angle_alpha 90.00 _cell_angle_beta 92.275(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 8.4059(4) _cell_length_b 4.8128(4) _cell_length_c 17.6696(10) _cell_measurement_reflns_used 15678 _cell_measurement_temperature 100 _cell_measurement_theta_max 33.0941 _cell_measurement_theta_min 2.6393 _cell_volume 714.28(8) _exptl_absorpt_coefficient_mu 0.219 _exptl_absorpt_correction_T_max 0.98805 _exptl_absorpt_correction_T_min 0.94272 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2008)' _exptl_crystal_F_000 296 _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_special_details ; Crystal mounted on a MiTeGen loop using Perfluoropolyether PFO-XR75 ; _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean 18.02 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker AXS Enraf-Nonius KappaCCD' _diffrn_measurement_method 'CCD \f- and \w-scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source '0.2 x 2mm^2^ focus rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 14810 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 33.15 _diffrn_reflns_theta_min 2.64 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4950 _reflns_number_total 5436 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'DENZO (Bruker AXS, 2006)' _computing_data_collection 'DATCOL (Bruker AXS, 2006)' _computing_data_reduction 'DENZO (Bruker AXS, 2006)' _computing_molecular_graphics 'DIAMOND (Crystal Impact GbR, 2005)' _computing_publication_material ; OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341 ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 0.643 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.056 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0407 _refine_ls_abs_structure_Flack 0.00(19) _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 179 _refine_ls_number_reflns 5436 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_wR_factor_gt 0.0978 _refine_ls_wR_factor_ref 0.1025 _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+0.1945P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _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. The minimum and maximum estimated transmissions from the multi-scan scaling are 0.7513 and 1.0000 (SADABS). Highest peak ? Deepest hole ? ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 S1 S 0.29208(4) 0.56637(8) 0.831012(18) 0.01723(8) Uani 1 1 d . . . N4 N 0.38392(14) 0.2585(3) 0.71226(7) 0.0171(2) Uani 1 1 d . . . N3 N 0.56969(12) 0.5676(3) 0.75597(6) 0.01435(18) Uani 1 1 d . . . N2 N 0.60606(13) 0.7639(3) 0.80828(6) 0.01301(19) Uani 1 1 d . . . N1 N 0.63554(14) 1.1304(2) 0.91970(7) 0.0154(2) Uani 1 1 d . . . C1 C 0.42116(15) 0.4607(3) 0.76392(7) 0.0141(2) Uani 1 1 d . . . C2 C 0.73909(16) 0.9040(3) 0.81154(7) 0.0136(2) Uani 1 1 d . . . C3 C 0.75815(15) 1.1110(3) 0.87273(7) 0.0137(2) Uani 1 1 d . . . C4 C 0.89538(16) 1.2741(3) 0.88097(8) 0.0155(2) Uani 1 1 d . . . H4 H 0.9786 1.2532 0.8483 0.019 Uiso 1 1 calc R . . C5 C 0.90424(17) 1.4695(3) 0.93958(8) 0.0177(2) Uani 1 1 d . . . H5 H 0.9935 1.5823 0.9463 0.021 Uiso 1 1 calc R . . C6 C 0.77826(18) 1.4932(3) 0.98766(8) 0.0184(3) Uani 1 1 d . . . H6 H 0.7811 1.6219 1.0269 0.022 Uiso 1 1 calc R . . C7 C 0.64664(17) 1.3175(3) 0.97530(8) 0.0170(2) Uani 1 1 d . . . H7 H 0.5625 1.3324 1.0077 0.020 Uiso 1 1 calc R . . C8 C 0.86351(17) 0.8550(3) 0.75521(8) 0.0200(3) Uani 1 1 d . . . H8A H 0.8333 0.6995 0.7238 0.030 Uiso 1 1 calc R . . H8B H 0.9634 0.8164 0.7813 0.030 Uiso 1 1 calc R . . H8C H 0.8739 1.0175 0.7243 0.030 Uiso 1 1 calc R . . C9 C 0.49209(16) 0.1753(3) 0.65354(8) 0.0171(2) Uani 1 1 d . . . H9A H 0.4993 -0.0257 0.6518 0.021 Uiso 1 1 calc R . . H9B H 0.5977 0.2486 0.6654 0.021 Uiso 1 1 calc R . . C10 C 0.43141(16) 0.2852(3) 0.57647(7) 0.0161(2) Uani 1 1 d . . . H10A H 0.5014 0.2225 0.5376 0.019 Uiso 1 1 calc R . . H10B H 0.4331 0.4867 0.5770 0.019 Uiso 1 1 calc R . . C11 C 0.26108(17) 0.1839(3) 0.55742(8) 0.0179(3) Uani 1 1 d . . . H11 H 0.2639 -0.0192 0.5540 0.021 Uiso 1 1 calc R . . C12 C 0.15386(17) 0.2613(3) 0.62215(8) 0.0185(3) Uani 1 1 d . . . H12A H 0.0489 0.1824 0.6124 0.022 Uiso 1 1 calc R . . H12B H 0.1428 0.4618 0.6242 0.022 Uiso 1 1 calc R . . C13 C 0.22191(17) 0.1550(3) 0.69872(8) 0.0207(3) Uani 1 1 d . . . H13A H 0.1552 0.2175 0.7389 0.025 Uiso 1 1 calc R . . H13B H 0.2225 -0.0465 0.6988 0.025 Uiso 1 1 calc R . . C14 C 0.1979(2) 0.2966(4) 0.48070(9) 0.0256(3) Uani 1 1 d . . . H14A H 0.1938 0.4958 0.4826 0.038 Uiso 1 1 calc R . . H14B H 0.0929 0.2247 0.4698 0.038 Uiso 1 1 calc R . . H14C H 0.2673 0.2397 0.4418 0.038 Uiso 1 1 calc R . . H2 H 0.529(3) 0.813(5) 0.8404(13) 0.023(5) 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 S1 0.01209(13) 0.02519(16) 0.01455(13) 0.00008(13) 0.00212(9) -0.00346(13) N4 0.0149(5) 0.0239(6) 0.0125(5) -0.0009(4) -0.0005(4) -0.0061(4) N3 0.0123(4) 0.0187(5) 0.0120(4) -0.0009(5) -0.0005(3) -0.0026(5) N2 0.0106(4) 0.0175(5) 0.0108(4) 0.0012(4) 0.0000(3) -0.0013(4) N1 0.0134(5) 0.0189(5) 0.0141(5) 0.0010(4) 0.0019(4) -0.0005(4) C1 0.0131(5) 0.0182(5) 0.0108(5) 0.0030(4) -0.0009(4) -0.0017(4) C2 0.0107(5) 0.0173(6) 0.0127(5) 0.0007(4) 0.0000(4) -0.0015(4) C3 0.0115(5) 0.0178(6) 0.0117(5) 0.0014(4) -0.0001(4) -0.0003(4) C4 0.0136(5) 0.0191(6) 0.0138(5) 0.0003(5) 0.0002(4) -0.0020(5) C5 0.0164(6) 0.0197(6) 0.0168(6) -0.0003(5) -0.0028(5) -0.0025(5) C6 0.0225(6) 0.0175(6) 0.0150(6) -0.0007(4) -0.0023(5) 0.0015(5) C7 0.0166(6) 0.0203(6) 0.0143(6) 0.0004(5) 0.0025(4) 0.0017(5) C8 0.0146(6) 0.0294(7) 0.0162(6) -0.0042(5) 0.0041(4) -0.0058(5) C9 0.0167(6) 0.0192(6) 0.0153(6) -0.0012(5) -0.0009(4) 0.0002(5) C10 0.0173(6) 0.0188(6) 0.0123(5) -0.0004(4) 0.0007(4) 0.0002(5) C11 0.0195(6) 0.0210(6) 0.0131(6) -0.0007(5) -0.0020(4) -0.0020(5) C12 0.0145(6) 0.0249(6) 0.0161(6) -0.0004(5) -0.0009(4) -0.0044(5) C13 0.0190(6) 0.0291(7) 0.0139(6) 0.0011(5) -0.0012(5) -0.0124(5) C14 0.0239(7) 0.0372(9) 0.0151(6) 0.0031(6) -0.0044(5) -0.0021(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 S1 C1 1.7158(14) . ? N4 C1 1.3620(18) . ? N4 C9 1.4625(18) . ? N4 C13 1.4608(18) . ? N3 N2 1.3483(17) . ? N3 C1 1.3628(16) . ? N2 C2 1.3051(17) . ? N1 C3 1.3520(16) . ? N1 C7 1.3332(18) . ? C2 C3 1.4741(18) . ? C2 C8 1.4909(19) . ? C3 C4 1.3981(18) . ? C4 C5 1.399(2) . ? C5 C6 1.388(2) . ? C6 C7 1.403(2) . ? C9 C10 1.5293(19) . ? C10 C11 1.537(2) . ? C11 C12 1.530(2) . ? C11 C14 1.535(2) . ? C12 C13 1.535(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N4 C9 122.56(11) . . ? C1 N4 C13 122.77(12) . . ? C13 N4 C9 113.09(11) . . ? N2 N3 C1 112.19(11) . . ? C2 N2 N3 124.25(11) . . ? C7 N1 C3 117.80(12) . . ? N4 C1 S1 122.69(10) . . ? N4 C1 N3 112.82(12) . . ? N3 C1 S1 124.49(10) . . ? N2 C2 C3 116.70(12) . . ? N2 C2 C8 120.75(12) . . ? C3 C2 C8 122.54(11) . . ? N1 C3 C2 115.71(11) . . ? N1 C3 C4 122.90(12) . . ? C4 C3 C2 121.40(12) . . ? C3 C4 C5 118.30(12) . . ? C6 C5 C4 119.26(13) . . ? C5 C6 C7 118.12(13) . . ? N1 C7 C6 123.61(13) . . ? N4 C9 C10 110.02(11) . . ? C9 C10 C11 111.11(11) . . ? C12 C11 C10 109.29(11) . . ? C12 C11 C14 112.37(12) . . ? C14 C11 C10 111.60(12) . . ? C11 C12 C13 111.57(12) . . ? N4 C13 C12 110.06(11) . . ? # Attachment '- Cifs_all.cif' data_AMSE3_4 _database_code_depnum_ccdc_archive 'CCDC 803632' _audit_creation_method SHELXL-97 _chemical_formula_moiety ? _chemical_formula_sum 'C14 H20 N4 Se' _chemical_formula_weight 323.30 _chemical_melting_point ? _chemical_name_common ? _chemical_name_systematic ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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 Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, z' 'x-1/2, y, -z-1/2' 'x+1/2, -y+1/2, -z' '-x-1/2, y-1/2, z' '-x+1/2, -y, z+1/2' 'x, -y-1/2, z-1/2' _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 12.7398(4) _cell_length_b 9.0666(4) _cell_length_c 26.1314(12) _cell_measurement_reflns_used 3419 _cell_measurement_temperature 200 _cell_measurement_theta_max 29.3135 _cell_measurement_theta_min 2.7492 _cell_volume 3018.3(2) _exptl_absorpt_coefficient_mu 2.481 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_T_min 0.77933 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_F_000 1328 _exptl_crystal_colour ? _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_special_details ? _diffrn_ambient_temperature 199.85 _diffrn_detector_area_resol_mean 16.2705 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.841 _diffrn_measurement_details ; 1 omega -4.00 60.00 1.0000 25.9600 omega____ theta____ kappa____ phi______ frames - 17.9787 36.0000 -43.0000 64 2 omega -93.00 -50.00 1.0000 25.9600 omega____ theta____ kappa____ phi______ frames - -19.6975 0.0000 -120.0000 43 3 omega 12.00 53.00 1.0000 25.9600 omega____ theta____ kappa____ phi______ frames - -19.6975 0.0000 -120.0000 41 4 omega -82.00 -43.00 1.0000 25.9600 omega____ theta____ kappa____ phi______ frames - -19.6975 179.0000 -30.0000 39 ; _diffrn_measurement_device_type ; Goniometer Xcalibur, detector: Eos (Gemini ultra Mo) ; _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0187473771 _diffrn_orient_matrix_UB_12 0.02589159 _diffrn_orient_matrix_UB_13 -0.0231145934 _diffrn_orient_matrix_UB_21 0.0306914393 _diffrn_orient_matrix_UB_22 -0.0473004923 _diffrn_orient_matrix_UB_23 -0.0095869433 _diffrn_orient_matrix_UB_31 -0.0695594315 _diffrn_orient_matrix_UB_32 -0.0138726404 _diffrn_orient_matrix_UB_33 -0.0105012798 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 9738 _diffrn_reflns_theta_full 25.05 _diffrn_reflns_theta_max 29.39 _diffrn_reflns_theta_min 2.87 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 1985 _reflns_number_total 3507 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_molecular_graphics ; OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341 ; _computing_publication_material ; OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341 ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)/Bruker' _refine_diff_density_max 0.655 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.049 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_gt 0.0347 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.888 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 178 _refine_ls_number_reflns 3507 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.888 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_wR_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.0866 _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Se1 Se 0.494601(19) 0.30254(3) 0.375007(11) 0.06051(12) Uani 1 1 d . . . N3 N 0.27036(14) 0.30737(19) 0.37004(7) 0.0401(5) Uani 1 1 d . . . N2 N 0.28394(16) 0.2097(2) 0.40885(8) 0.0411(5) Uani 1 1 d . . . C8 C 0.36126(16) 0.3595(2) 0.35128(9) 0.0390(5) Uani 1 1 d . . . N4 N 0.34961(14) 0.4589(2) 0.31373(7) 0.0440(5) Uani 1 1 d . . . C7 C 0.09724(18) 0.1896(3) 0.42195(10) 0.0568(7) Uani 1 1 d . . . H7A H 0.0620 0.1042 0.4067 0.085 Uiso 1 1 calc R . . H7B H 0.0964 0.2720 0.3977 0.085 Uiso 1 1 calc R . . H7C H 0.0605 0.2184 0.4533 0.085 Uiso 1 1 calc R . . N1 N 0.33875(15) 0.0331(2) 0.48481(7) 0.0439(5) Uani 1 1 d . . . C1 C 0.23634(18) 0.0477(2) 0.47542(9) 0.0409(6) Uani 1 1 d . . . C6 C 0.20761(18) 0.1505(3) 0.43434(9) 0.0415(6) Uani 1 1 d . . . C13 C 0.24856(17) 0.4862(3) 0.28875(9) 0.0490(7) Uani 1 1 d . . . H13B H 0.2361 0.5937 0.2860 0.059 Uiso 1 1 calc R . . H13A H 0.1912 0.4427 0.3094 0.059 Uiso 1 1 calc R . . C9 C 0.43609(19) 0.5247(3) 0.28544(9) 0.0530(7) Uani 1 1 d . . . H9B H 0.5025 0.5098 0.3044 0.064 Uiso 1 1 calc R . . H9A H 0.4243 0.6321 0.2818 0.064 Uiso 1 1 calc R . . C4 C 0.2955(2) -0.1353(3) 0.55186(9) 0.0538(7) Uani 1 1 d . . . H4 H 0.3189 -0.1978 0.5787 0.065 Uiso 1 1 calc R . . C11 C 0.3420(2) 0.4674(2) 0.20283(9) 0.0481(6) Uani 1 1 d . . . H11 H 0.3313 0.5739 0.1943 0.058 Uiso 1 1 calc R . . C3 C 0.1911(2) -0.1200(3) 0.54155(10) 0.0628(8) Uani 1 1 d . . . H3 H 0.1402 -0.1723 0.5610 0.075 Uiso 1 1 calc R . . C5 C 0.36618(19) -0.0581(3) 0.52245(9) 0.0514(7) Uani 1 1 d . . . H5 H 0.4388 -0.0706 0.5294 0.062 Uiso 1 1 calc R . . C12 C 0.24970(19) 0.4177(3) 0.23596(9) 0.0552(7) Uani 1 1 d . . . H12A H 0.1834 0.4432 0.2183 0.066 Uiso 1 1 calc R . . H12B H 0.2522 0.3091 0.2396 0.066 Uiso 1 1 calc R . . C2 C 0.1606(2) -0.0279(3) 0.50252(10) 0.0598(8) Uani 1 1 d . . . H2A H 0.0885 -0.0163 0.4943 0.072 Uiso 1 1 calc R . . C10 C 0.4440(2) 0.4542(3) 0.23305(10) 0.0569(7) Uani 1 1 d . . . H10A H 0.4621 0.3486 0.2370 0.068 Uiso 1 1 calc R . . H10B H 0.5014 0.5021 0.2136 0.068 Uiso 1 1 calc R . . C14 C 0.3465(3) 0.3822(3) 0.15288(11) 0.0923(11) Uani 1 1 d . . . H14C H 0.4056 0.4179 0.1323 0.138 Uiso 1 1 calc R . . H14A H 0.2809 0.3968 0.1339 0.138 Uiso 1 1 calc R . . H14B H 0.3559 0.2770 0.1601 0.138 Uiso 1 1 calc R . . H2 H 0.3509(16) 0.187(2) 0.4158(9) 0.047(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 Se1 0.03506(15) 0.0827(2) 0.0638(2) 0.02517(15) -0.00141(13) 0.00977(13) N3 0.0362(10) 0.0433(11) 0.0408(11) 0.0097(10) -0.0016(9) 0.0010(9) N2 0.0364(12) 0.0470(12) 0.0400(11) 0.0067(10) -0.0042(10) 0.0042(10) C8 0.0357(13) 0.0424(12) 0.0388(13) 0.0000(12) -0.0035(11) 0.0027(11) N4 0.0348(10) 0.0528(12) 0.0444(12) 0.0144(10) -0.0025(9) -0.0019(10) C7 0.0385(14) 0.0614(16) 0.0705(19) 0.0184(14) -0.0038(13) -0.0020(13) N1 0.0387(11) 0.0500(12) 0.0430(11) 0.0078(10) 0.0018(10) 0.0012(10) C1 0.0387(13) 0.0436(14) 0.0405(14) 0.0037(12) -0.0005(11) -0.0002(12) C6 0.0389(13) 0.0408(13) 0.0447(13) 0.0032(12) 0.0008(12) -0.0017(11) C13 0.0378(13) 0.0547(15) 0.0546(17) 0.0187(13) -0.0001(12) 0.0028(12) C9 0.0405(14) 0.0633(16) 0.0553(16) 0.0196(14) -0.0046(13) -0.0107(13) C4 0.0506(15) 0.0628(16) 0.0479(15) 0.0170(14) 0.0020(13) 0.0001(14) C11 0.0614(16) 0.0388(14) 0.0440(14) 0.0068(12) -0.0017(13) 0.0069(13) C3 0.0487(16) 0.0753(19) 0.0645(18) 0.0312(17) 0.0064(14) -0.0054(15) C5 0.0408(14) 0.0641(16) 0.0493(16) 0.0125(14) 0.0003(12) 0.0032(13) C12 0.0560(17) 0.0485(15) 0.0611(17) 0.0155(13) -0.0164(15) -0.0098(12) C2 0.0378(14) 0.074(2) 0.0681(19) 0.0237(16) 0.0013(13) -0.0016(13) C10 0.0478(16) 0.0620(16) 0.0608(17) 0.0184(14) 0.0105(14) 0.0127(14) C14 0.149(3) 0.078(2) 0.0506(18) -0.0062(17) -0.005(2) 0.018(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 Se1 C8 1.881(2) . ? N3 N2 1.358(2) . ? N3 C8 1.344(3) . ? N2 C6 1.295(3) . ? N2 H2 0.90(2) . ? C8 N4 1.340(3) . ? N4 C13 1.464(3) . ? N4 C9 1.455(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C7 C6 1.486(3) . ? N1 C1 1.334(3) . ? N1 C5 1.332(3) . ? C1 C6 1.468(3) . ? C1 C2 1.379(3) . ? C13 H13B 0.9900 . ? C13 H13A 0.9900 . ? C13 C12 1.513(3) . ? C9 H9B 0.9900 . ? C9 H9A 0.9900 . ? C9 C10 1.514(3) . ? C4 H4 0.9500 . ? C4 C3 1.365(3) . ? C4 C5 1.375(3) . ? C11 H11 1.0000 . ? C11 C12 1.528(3) . ? C11 C10 1.526(3) . ? C11 C14 1.517(3) . ? C3 H3 0.9500 . ? C3 C2 1.374(3) . ? C5 H5 0.9500 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C2 H2A 0.9500 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C14 H14C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 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 N3 N2 H2 115.0(15) . . ? N3 C8 Se1 124.16(17) . . ? N2 C6 C7 120.0(2) . . ? N2 C6 C1 116.9(2) . . ? C8 N3 N2 113.11(18) . . ? C8 N4 C13 122.51(19) . . ? C8 N4 C9 124.32(19) . . ? N4 C8 Se1 121.75(16) . . ? N4 C8 N3 114.10(19) . . ? N4 C13 H13B 109.8 . . ? N4 C13 H13A 109.8 . . ? N4 C13 C12 109.18(19) . . ? N4 C9 H9B 109.7 . . ? N4 C9 H9A 109.7 . . ? N4 C9 C10 109.69(19) . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C1 C6 116.2(2) . . ? N1 C1 C2 122.7(2) . . ? N1 C5 C4 123.9(2) . . ? N1 C5 H5 118.1 . . ? C1 C6 C7 123.1(2) . . ? C1 C2 H2A 120.5 . . ? C6 N2 N3 124.0(2) . . ? C6 N2 H2 121.0(14) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? C13 C12 C11 113.8(2) . . ? C13 C12 H12A 108.8 . . ? C13 C12 H12B 108.8 . . ? H13B C13 H13A 108.3 . . ? C9 N4 C13 111.71(18) . . ? C9 C10 C11 112.2(2) . . ? C9 C10 H10A 109.2 . . ? C9 C10 H10B 109.2 . . ? H9B C9 H9A 108.2 . . ? C4 C3 H3 120.6 . . ? C4 C3 C2 118.9(2) . . ? C4 C5 H5 118.1 . . ? C11 C12 H12A 108.8 . . ? C11 C12 H12B 108.8 . . ? C11 C10 H10A 109.2 . . ? C11 C10 H10B 109.2 . . ? C11 C14 H14C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? C3 C4 H4 120.8 . . ? C3 C4 C5 118.5(2) . . ? C3 C2 C1 119.1(2) . . ? C3 C2 H2A 120.5 . . ? C5 N1 C1 117.0(2) . . ? C5 C4 H4 120.8 . . ? C12 C13 H13B 109.8 . . ? C12 C13 H13A 109.8 . . ? C12 C11 H11 107.8 . . ? H12A C12 H12B 107.7 . . ? C2 C1 C6 121.1(2) . . ? C2 C3 H3 120.6 . . ? C10 C9 H9B 109.7 . . ? C10 C9 H9A 109.7 . . ? C10 C11 H11 107.8 . . ? C10 C11 C12 109.83(19) . . ? H10A C10 H10B 107.9 . . ? C14 C11 H11 107.8 . . ? C14 C11 C12 111.5(2) . . ? C14 C11 C10 111.9(2) . . ? H14C C14 H14A 109.5 . . ? H14C C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? data_ams79m _database_code_depnum_ccdc_archive 'CCDC 803633' #TrackingRef '- Cifs_all.cif' _audit_creation_date 2011-07-07 _audit_creation_method ; Olex2 1.1 (compiled Feb 15 2011 20:38:53, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C23 H24 Au N4 P S)' _chemical_formula_sum 'C46 H48 Au2 N8 P2 S2' _chemical_formula_weight 1232.92 _chemical_melting_point ? _chemical_oxdiff_formula C46H48N8P2S2Au1 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.6538(2) _cell_length_b 18.3046(3) _cell_length_c 21.4734(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.6764(15) _cell_angle_gamma 90.00 _cell_volume 4575.69(14) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8995 _cell_measurement_temperature 150.15 _cell_measurement_theta_max 32.7797 _cell_measurement_theta_min 3.5767 _exptl_absorpt_coefficient_mu 6.609 _exptl_absorpt_correction_T_max 0.352 _exptl_absorpt_correction_T_min 0.068 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.790 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2400 _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.18 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_unetI/netI 0.0426 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 14697 _diffrn_reflns_theta_full 25.05 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_theta_min 3.59 _diffrn_ambient_temperature 150.15 _diffrn_detector_area_resol_mean 16.2705 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 70.00 96.00 1.0000 7.6000 omega____ theta____ kappa____ phi______ frames - 26.2288 179.0000 120.0000 26 #__ type_ start__ end____ width___ exp.time_ 2 omega -36.00 -10.00 1.0000 7.6000 omega____ theta____ kappa____ phi______ frames - 26.2288 0.0000 -120.0000 26 #__ type_ start__ end____ width___ exp.time_ 3 omega 32.00 95.00 1.0000 7.6000 omega____ theta____ kappa____ phi______ frames - 26.2288 0.0000 -120.0000 63 #__ type_ start__ end____ width___ exp.time_ 4 omega -99.00 -31.00 1.0000 7.6000 omega____ theta____ kappa____ phi______ frames - -27.9476 -37.0000 30.0000 68 #__ type_ start__ end____ width___ exp.time_ 5 omega -100.00 -11.00 1.0000 7.6000 omega____ theta____ kappa____ phi______ frames - -27.9476 -37.0000 -60.0000 89 #__ type_ start__ end____ width___ exp.time_ 6 omega -65.00 -39.00 1.0000 7.6000 omega____ theta____ kappa____ phi______ frames - -27.9476 179.0000 150.0000 26 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0368088000 _diffrn_orient_matrix_UB_12 -0.0135458000 _diffrn_orient_matrix_UB_13 -0.0227397000 _diffrn_orient_matrix_UB_21 0.0394893000 _diffrn_orient_matrix_UB_22 -0.0119335000 _diffrn_orient_matrix_UB_23 0.0239805000 _diffrn_orient_matrix_UB_31 -0.0282803000 _diffrn_orient_matrix_UB_32 -0.0342969000 _diffrn_orient_matrix_UB_33 0.0006045000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 5182 _reflns_number_total 6675 _reflns_odcompleteness_completeness 99.81 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 30.44 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 3.357 _refine_diff_density_min -3.063 _refine_diff_density_rms 0.145 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 274 _refine_ls_number_reflns 6675 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0339 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0767 _refine_ls_wR_factor_ref 0.0794 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.749300(13) 0.065434(9) 0.296380(6) 0.02205(5) Uani 1 1 d . . . P1 P 0.84674(8) 0.11083(6) 0.21713(4) 0.01680(19) Uani 1 1 d . . . S1 S 0.63563(11) 0.00529(6) 0.36524(5) 0.0329(3) Uani 1 1 d . . . N3 N 0.7334(3) 0.1510(2) 0.39934(15) 0.0266(8) Uani 1 1 d . . . N2 N 0.7262(3) 0.1070(2) 0.45022(15) 0.0277(8) Uani 1 1 d . . . C3 C 0.6773(4) 0.0440(2) 0.43870(19) 0.0265(9) Uani 1 1 d . . . N1 N 0.6553(4) 0.0036(2) 0.48909(18) 0.0409(10) Uani 1 1 d . . . C11 C 0.9468(3) 0.1834(2) 0.23839(16) 0.0183(7) Uani 1 1 d . . . H11 H 0.9162 0.2310 0.2314 0.022 Uiso 1 1 calc R . . C30 C 0.9236(3) 0.0451(2) 0.17078(17) 0.0186(7) Uani 1 1 d . . . C20 C 0.7510(3) 0.1590(2) 0.16190(17) 0.0212(8) Uani 1 1 d . . . C4 C 0.8013(4) 0.2088(2) 0.40796(19) 0.0255(8) Uani 1 1 d . . . C21 C 0.6342(3) 0.1418(2) 0.15924(18) 0.0256(9) Uani 1 1 d . . . H21 H 0.6062 0.1036 0.1844 0.031 Uiso 1 1 calc R . . C35 C 0.9847(4) 0.0682(2) 0.11994(18) 0.0252(8) Uani 1 1 d . . . H35 H 0.9908 0.1189 0.1111 0.030 Uiso 1 1 calc R . . C6 C 0.8019(4) 0.2605(2) 0.3553(2) 0.0271(9) Uani 1 1 d . . . C7 C 0.7149(4) 0.2597(3) 0.3075(2) 0.0321(10) Uani 1 1 d . . . H7 H 0.6537 0.2255 0.3082 0.038 Uiso 1 1 calc R . . C22 C 0.5589(4) 0.1808(3) 0.1196(2) 0.0381(12) Uani 1 1 d . . . H22 H 0.4796 0.1686 0.1173 0.046 Uiso 1 1 calc R . . C31 C 0.9156(4) -0.0288(2) 0.1834(2) 0.0290(9) Uani 1 1 d . . . H31 H 0.8735 -0.0453 0.2176 0.035 Uiso 1 1 calc R . . N4 N 0.8878(4) 0.3091(2) 0.35576(19) 0.0400(10) Uani 1 1 d . . . C34 C 1.0358(4) 0.0181(3) 0.0827(2) 0.0329(10) Uani 1 1 d . . . H34 H 1.0767 0.0340 0.0479 0.040 Uiso 1 1 calc R . . C32 C 0.9686(5) -0.0782(2) 0.1464(2) 0.0382(11) Uani 1 1 d . . . H32 H 0.9647 -0.1288 0.1556 0.046 Uiso 1 1 calc R . . C25 C 0.7900(4) 0.2145(2) 0.12388(19) 0.0293(9) Uani 1 1 d . . . H25 H 0.8695 0.2260 0.1241 0.035 Uiso 1 1 calc R . . C33 C 1.0278(4) -0.0550(2) 0.0958(2) 0.0353(11) Uani 1 1 d . . . H33 H 1.0630 -0.0898 0.0700 0.042 Uiso 1 1 calc R . . C5 C 0.8755(4) 0.2249(3) 0.4640(2) 0.0404(12) Uani 1 1 d . . . H5A H 0.8587 0.1902 0.4971 0.061 Uiso 1 1 calc R . . H5B H 0.8605 0.2747 0.4782 0.061 Uiso 1 1 calc R . . H5C H 0.9563 0.2204 0.4539 0.061 Uiso 1 1 calc R . . C24 C 0.7112(5) 0.2533(3) 0.0852(2) 0.0390(12) Uani 1 1 d . . . H24 H 0.7373 0.2917 0.0597 0.047 Uiso 1 1 calc R . . C23 C 0.5974(5) 0.2363(3) 0.0842(2) 0.0435(13) Uani 1 1 d . . . H23 H 0.5445 0.2634 0.0584 0.052 Uiso 1 1 calc R . . C2 C 0.6263(6) -0.0725(3) 0.4878(3) 0.0541(16) Uani 1 1 d . . . H2A H 0.6211 -0.0896 0.4445 0.081 Uiso 1 1 calc R . . H2B H 0.5522 -0.0797 0.5067 0.081 Uiso 1 1 calc R . . H2C H 0.6858 -0.1002 0.5113 0.081 Uiso 1 1 calc R . . C8 C 0.7207(5) 0.3096(3) 0.2595(3) 0.0488(15) Uani 1 1 d . . . H8 H 0.6637 0.3097 0.2264 0.059 Uiso 1 1 calc R . . C9 C 0.8093(6) 0.3590(3) 0.2600(3) 0.0505(15) Uani 1 1 d . . . H9 H 0.8157 0.3934 0.2273 0.061 Uiso 1 1 calc R . . C10 C 0.8872(5) 0.3571(3) 0.3086(3) 0.0503(15) Uani 1 1 d . . . H10 H 0.9464 0.3928 0.3095 0.060 Uiso 1 1 calc R . . C1 C 0.6815(5) 0.0319(4) 0.5514(2) 0.0547(16) Uani 1 1 d . . . H1A H 0.7627 0.0232 0.5629 0.082 Uiso 1 1 calc R . . H1B H 0.6336 0.0070 0.5812 0.082 Uiso 1 1 calc R . . H1C H 0.6657 0.0845 0.5522 0.082 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 0.02265(8) 0.02426(8) 0.01973(8) 0.00316(6) 0.00634(5) -0.00353(7) P1 0.0134(4) 0.0199(5) 0.0171(4) 0.0015(4) 0.0017(3) -0.0013(4) S1 0.0426(7) 0.0323(6) 0.0248(5) -0.0001(4) 0.0136(4) -0.0150(5) N3 0.0232(18) 0.037(2) 0.0197(16) -0.0013(15) 0.0008(13) 0.0037(17) N2 0.0278(19) 0.035(2) 0.0209(16) 0.0041(15) 0.0031(13) 0.0033(17) C3 0.026(2) 0.024(2) 0.030(2) -0.0024(16) 0.0041(16) 0.0052(18) N1 0.057(3) 0.043(2) 0.0231(19) 0.0014(17) 0.0097(17) 0.004(2) C11 0.0178(19) 0.0152(17) 0.0219(18) 0.0008(14) 0.0015(13) 0.0035(15) C30 0.0153(18) 0.0204(18) 0.0202(17) -0.0018(14) 0.0016(13) -0.0009(15) C20 0.0170(19) 0.026(2) 0.0201(17) -0.0032(15) -0.0012(14) 0.0030(17) C4 0.021(2) 0.024(2) 0.031(2) -0.0024(17) 0.0062(15) 0.0010(18) C21 0.017(2) 0.033(2) 0.026(2) -0.0069(17) -0.0020(15) 0.0017(18) C35 0.026(2) 0.025(2) 0.0251(19) -0.0015(17) 0.0058(15) -0.0082(19) C6 0.029(2) 0.019(2) 0.035(2) -0.0088(17) 0.0138(17) -0.0028(18) C7 0.030(2) 0.028(2) 0.039(2) -0.0035(19) 0.0088(19) 0.004(2) C22 0.021(2) 0.047(3) 0.044(3) -0.020(2) -0.0110(18) 0.009(2) C31 0.031(2) 0.025(2) 0.031(2) 0.0034(17) 0.0082(17) -0.002(2) N4 0.044(2) 0.032(2) 0.046(2) -0.0169(18) 0.0223(18) -0.019(2) C34 0.029(2) 0.039(3) 0.031(2) -0.011(2) 0.0104(18) -0.007(2) C32 0.047(3) 0.020(2) 0.048(3) -0.0027(19) 0.010(2) 0.003(2) C25 0.030(2) 0.035(2) 0.023(2) 0.0054(17) -0.0020(16) 0.003(2) C33 0.032(3) 0.027(2) 0.048(3) -0.015(2) 0.012(2) 0.000(2) C5 0.029(3) 0.057(3) 0.036(2) -0.012(2) 0.0030(19) 0.002(2) C24 0.056(3) 0.031(2) 0.029(2) 0.0079(19) -0.007(2) 0.007(2) C23 0.045(3) 0.044(3) 0.039(3) -0.006(2) -0.019(2) 0.022(3) C2 0.079(5) 0.043(3) 0.042(3) 0.016(2) 0.023(3) 0.016(3) C8 0.054(3) 0.043(3) 0.052(3) 0.017(3) 0.026(2) 0.030(3) C9 0.075(4) 0.027(3) 0.052(3) 0.004(2) 0.032(3) 0.012(3) C10 0.068(4) 0.027(3) 0.059(3) -0.014(2) 0.036(3) -0.019(3) C1 0.067(4) 0.069(4) 0.029(3) 0.005(3) 0.009(2) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.2486(9) . ? Au1 S1 2.3100(10) . ? P1 C11 1.812(4) . ? P1 C30 1.823(4) . ? P1 C20 1.818(4) . ? S1 C3 1.776(4) . ? N3 N2 1.363(5) . ? N3 C4 1.328(5) . ? N2 C3 1.305(6) . ? C3 N1 1.345(6) . ? N1 C2 1.434(7) . ? N1 C1 1.454(7) . ? C11 C11 1.315(7) 2_755 ? C11 H11 0.9500 . ? C30 C35 1.396(5) . ? C30 C31 1.384(6) . ? C20 C21 1.395(5) . ? C20 C25 1.393(6) . ? C4 C6 1.475(6) . ? C4 C5 1.478(6) . ? C21 H21 0.9500 . ? C21 C22 1.391(6) . ? C35 H35 0.9500 . ? C35 C34 1.372(6) . ? C6 C7 1.410(6) . ? C6 N4 1.339(6) . ? C7 H7 0.9500 . ? C7 C8 1.381(7) . ? C22 H22 0.9500 . ? C22 C23 1.357(7) . ? C31 H31 0.9500 . ? C31 C32 1.369(6) . ? N4 C10 1.339(7) . ? C34 H34 0.9500 . ? C34 C33 1.371(6) . ? C32 H32 0.9500 . ? C32 C33 1.380(7) . ? C25 H25 0.9500 . ? C25 C24 1.402(6) . ? C33 H33 0.9500 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C24 H24 0.9500 . ? C24 C23 1.362(7) . ? C23 H23 0.9500 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C8 H8 0.9500 . ? C8 C9 1.373(8) . ? C9 H9 0.9500 . ? C9 C10 1.351(8) . ? C10 H10 0.9500 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 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 170.23(4) . . ? C11 P1 Au1 114.97(12) . . ? C11 P1 C30 107.12(17) . . ? C11 P1 C20 100.19(18) . . ? C30 P1 Au1 116.60(13) . . ? C20 P1 Au1 110.88(13) . . ? C20 P1 C30 105.44(17) . . ? C3 S1 Au1 103.72(15) . . ? C4 N3 N2 114.7(3) . . ? C3 N2 N3 114.4(3) . . ? N2 C3 S1 128.3(3) . . ? N2 C3 N1 115.5(4) . . ? N1 C3 S1 116.2(3) . . ? C3 N1 C2 124.9(4) . . ? C3 N1 C1 120.4(4) . . ? C2 N1 C1 113.7(4) . . ? P1 C11 H11 113.6 . . ? C11 C11 P1 132.83(12) 2_755 . ? C11 C11 H11 113.6 2_755 . ? C35 C30 P1 120.6(3) . . ? C31 C30 P1 119.9(3) . . ? C31 C30 C35 119.4(4) . . ? C21 C20 P1 119.0(3) . . ? C25 C20 P1 121.9(3) . . ? C25 C20 C21 119.0(4) . . ? N3 C4 C6 115.4(4) . . ? N3 C4 C5 126.4(4) . . ? C6 C4 C5 118.2(4) . . ? C20 C21 H21 120.2 . . ? C22 C21 C20 119.7(4) . . ? C22 C21 H21 120.2 . . ? C30 C35 H35 119.8 . . ? C34 C35 C30 120.3(4) . . ? C34 C35 H35 119.8 . . ? C7 C6 C4 121.5(4) . . ? N4 C6 C4 116.9(4) . . ? N4 C6 C7 121.6(4) . . ? C6 C7 H7 120.7 . . ? C8 C7 C6 118.6(5) . . ? C8 C7 H7 120.7 . . ? C21 C22 H22 119.6 . . ? C23 C22 C21 120.7(4) . . ? C23 C22 H22 119.6 . . ? C30 C31 H31 120.2 . . ? C32 C31 C30 119.7(4) . . ? C32 C31 H31 120.2 . . ? C6 N4 C10 116.9(5) . . ? C35 C34 H34 120.1 . . ? C33 C34 C35 119.8(4) . . ? C33 C34 H34 120.1 . . ? C31 C32 H32 119.7 . . ? C31 C32 C33 120.7(4) . . ? C33 C32 H32 119.7 . . ? C20 C25 H25 120.2 . . ? C20 C25 C24 119.6(4) . . ? C24 C25 H25 120.2 . . ? C34 C33 C32 120.2(4) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C25 C24 H24 119.9 . . ? C23 C24 C25 120.3(5) . . ? C23 C24 H24 119.9 . . ? C22 C23 C24 120.6(4) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C7 C8 H8 120.3 . . ? C9 C8 C7 119.5(6) . . ? C9 C8 H8 120.3 . . ? C8 C9 H9 121.1 . . ? C10 C9 C8 117.9(5) . . ? C10 C9 H9 121.1 . . ? N4 C10 C9 125.5(5) . . ? N4 C10 H10 117.3 . . ? C9 C10 H10 117.3 . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -1 1 0 0.0399 -1.0009 1.0002 0.0010 -0.0504 -0.0514 -0.0060 1 -1 0 0.1370 1.0009 -1.0002 -0.0010 0.0504 0.0514 0.0060 -1 -1 0 0.2236 -0.9993 -1.0020 -0.0007 -0.0233 -0.0276 0.0626 1 1 0 0.2358 0.9993 1.0020 0.0007 0.0233 0.0276 -0.0626 0 0 1 0.2413 -0.0000 -0.0004 1.0005 -0.0227 0.0240 0.0006 0 0 -1 0.1857 0.0000 0.0004 -1.0005 0.0227 -0.0240 -0.0006 data_ams113c _database_code_depnum_ccdc_archive 'CCDC 803634' #TrackingRef '- Cifs_all.cif' _audit_creation_date 2011-07-07 _audit_creation_method ; Olex2 1.1 (compiled Feb 15 2011 20:38:53, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C23 H24 Au N3 P S2)' _chemical_formula_sum 'C46 H48 Au2 N6 P2 S4' _chemical_formula_weight 1269.02 _chemical_melting_point ? 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 8.1598(3) _cell_length_b 11.3329(6) _cell_length_c 13.6971(6) _cell_angle_alpha 104.614(4) _cell_angle_beta 100.524(3) _cell_angle_gamma 101.158(4) _cell_volume 1166.19(9) _cell_formula_units_Z 1 _cell_measurement_reflns_used 7113 _cell_measurement_temperature 150.0 _cell_measurement_theta_max 29.3554 _cell_measurement_theta_min 2.8240 _exptl_absorpt_coefficient_mu 6.570 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.44468 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.807 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 618 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.1 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_unetI/netI 0.0427 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 9583 _diffrn_reflns_theta_full 25.05 _diffrn_reflns_theta_max 29.3554 _diffrn_reflns_theta_min 2.8240 _diffrn_ambient_temperature 150.0 _diffrn_detector_area_resol_mean 16.2705 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.833 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -8.00 54.00 1.0000 1.5100 omega____ theta____ kappa____ phi______ frames - 17.9787 77.0000 -60.0000 62 #__ type_ start__ end____ width___ exp.time_ 2 omega 27.00 78.00 1.0000 1.5100 omega____ theta____ kappa____ phi______ frames - 17.9787 -129.0000 -153.0000 51 #__ type_ start__ end____ width___ exp.time_ 3 omega -42.00 48.00 1.0000 1.5100 omega____ theta____ kappa____ phi______ frames - -19.6975 37.0000 -120.0000 90 #__ type_ start__ end____ width___ exp.time_ 4 omega -71.00 -3.00 1.0000 1.5100 omega____ theta____ kappa____ phi______ frames - -19.6975 129.0000 -26.0000 68 #__ type_ start__ end____ width___ exp.time_ 5 omega -96.00 -67.00 1.0000 1.5100 omega____ theta____ kappa____ phi______ frames - -19.6975 179.0000 -30.0000 29 #__ type_ start__ end____ width___ exp.time_ 6 omega -92.00 22.00 1.0000 1.5100 omega____ theta____ kappa____ phi______ frames - -19.6975 0.0000 30.0000 114 ; _diffrn_measurement_device_type 'Goniometer Xcalibur, detector: Eos (Gemini ultra Mo)' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0344838635 _diffrn_orient_matrix_UB_12 0.0411826182 _diffrn_orient_matrix_UB_13 -0.0242967861 _diffrn_orient_matrix_UB_21 -0.0034050813 _diffrn_orient_matrix_UB_22 -0.0407163604 _diffrn_orient_matrix_UB_23 -0.0494865218 _diffrn_orient_matrix_UB_31 -0.0844723515 _diffrn_orient_matrix_UB_32 -0.0333235195 _diffrn_orient_matrix_UB_33 -0.0025942692 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4745 _reflns_number_total 5374 _reflns_odcompleteness_completeness 99.81 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)/Bruker' _refine_diff_density_max 0.898 _refine_diff_density_min -0.973 _refine_diff_density_rms 0.119 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 273 _refine_ls_number_reflns 5374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0288 _refine_ls_R_factor_gt 0.0234 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.0492 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 -0.027286(15) 0.016865(12) -0.321871(10) 0.01788(4) Uani 1 1 d . . . P1 P -0.19719(10) -0.12123(8) -0.26699(6) 0.01550(17) Uani 1 1 d . . . S2 S 0.42328(11) 0.36130(9) -0.32697(7) 0.0290(2) Uani 1 1 d . . . C20 C -0.4243(4) -0.1480(3) -0.3283(3) 0.0168(7) Uani 1 1 d . . . C21 C -0.4722(4) -0.1248(3) -0.4219(3) 0.0243(8) Uani 1 1 d . . . H21 H -0.3862 -0.0929 -0.4535 0.029 Uiso 1 1 calc R . . C30 C -0.1600(4) -0.2788(3) -0.2989(2) 0.0161(6) Uani 1 1 d . . . C35 C -0.0743(4) -0.3238(3) -0.2242(3) 0.0202(7) Uani 1 1 d . . . H35 H -0.0353 -0.2722 -0.1539 0.024 Uiso 1 1 calc R . . C31 C -0.2154(5) -0.3542(3) -0.4012(3) 0.0308(9) Uani 1 1 d . . . H31 H -0.2726 -0.3237 -0.4529 0.037 Uiso 1 1 calc R . . C34 C -0.0452(4) -0.4424(3) -0.2511(3) 0.0256(8) Uani 1 1 d . . . H34 H 0.0139 -0.4720 -0.1995 0.031 Uiso 1 1 calc R . . C23 C -0.7694(4) -0.1915(3) -0.4233(3) 0.0302(9) Uani 1 1 d . . . H23 H -0.8878 -0.2046 -0.4551 0.036 Uiso 1 1 calc R . . C22 C -0.6446(4) -0.1474(3) -0.4704(3) 0.0298(8) Uani 1 1 d . . . H22 H -0.6768 -0.1327 -0.5357 0.036 Uiso 1 1 calc R . . C25 C -0.5513(4) -0.1960(4) -0.2834(3) 0.0317(9) Uani 1 1 d . . . H25 H -0.5202 -0.2149 -0.2198 0.038 Uiso 1 1 calc R . . C24 C -0.7228(4) -0.2162(4) -0.3315(3) 0.0364(10) Uani 1 1 d . . . H24 H -0.8093 -0.2477 -0.3000 0.044 Uiso 1 1 calc R . . C33 C -0.1023(5) -0.5183(4) -0.3536(3) 0.0362(9) Uani 1 1 d . . . H33 H -0.0832 -0.6002 -0.3724 0.043 Uiso 1 1 calc R . . C32 C -0.1883(5) -0.4731(4) -0.4289(3) 0.0420(11) Uani 1 1 d . . . H32 H -0.2280 -0.5246 -0.4992 0.050 Uiso 1 1 calc R . . C10 C -0.1825(4) -0.0758(3) -0.1267(2) 0.0184(7) Uani 1 1 d . . . H10A H -0.2580 -0.0184 -0.1116 0.022 Uiso 1 1 calc R . . H10B H -0.2277 -0.1524 -0.1078 0.022 Uiso 1 1 calc R . . C11 C -0.0024(4) -0.0116(3) -0.0579(2) 0.0178(7) Uani 1 1 d . . . H11A H 0.0390 0.0699 -0.0706 0.021 Uiso 1 1 calc R . . H11B H 0.0766 -0.0650 -0.0768 0.021 Uiso 1 1 calc R . . N1 N 0.1884(3) 0.3350(3) -0.2213(2) 0.0256(7) Uani 1 1 d . . . S1 S 0.14860(11) 0.13477(8) -0.39603(7) 0.02523(19) Uani 1 1 d . . . N2 N 0.0279(3) 0.2736(3) -0.2126(2) 0.0232(6) Uani 1 1 d . . . N3 N -0.1822(4) 0.2601(3) -0.0101(2) 0.0302(7) Uani 1 1 d . . . C5 C -0.1688(4) 0.2508(3) -0.1087(3) 0.0210(7) Uani 1 1 d . . . C2 C 0.2351(4) 0.2809(3) -0.3019(3) 0.0203(7) Uani 1 1 d . . . C3 C 0.0058(4) 0.3041(3) -0.1194(3) 0.0226(7) Uani 1 1 d . . . C4 C 0.1438(5) 0.3865(4) -0.0257(3) 0.0349(9) Uani 1 1 d . . . H4A H 0.1917 0.4662 -0.0381 0.052 Uiso 1 1 calc R . . H4B H 0.2355 0.3438 -0.0128 0.052 Uiso 1 1 calc R . . H4C H 0.0946 0.4036 0.0350 0.052 Uiso 1 1 calc R . . C9 C -0.3379(5) 0.2124(4) 0.0017(3) 0.0404(10) Uani 1 1 d . . . H9 H -0.3496 0.2173 0.0703 0.049 Uiso 1 1 calc R . . C8 C -0.4828(5) 0.1564(4) -0.0794(4) 0.0420(11) Uani 1 1 d . . . H8 H -0.5904 0.1236 -0.0665 0.050 Uiso 1 1 calc R . . C1 C 0.4795(6) 0.5067(4) -0.2249(5) 0.0682(17) Uani 1 1 d . . . H1A H 0.3877 0.5504 -0.2330 0.102 Uiso 1 1 calc R . . H1B H 0.5874 0.5597 -0.2281 0.102 Uiso 1 1 calc R . . H1C H 0.4944 0.4897 -0.1575 0.102 Uiso 1 1 calc R . . C6 C -0.3089(4) 0.1974(3) -0.1939(3) 0.0269(8) Uani 1 1 d . . . H6 H -0.2951 0.1941 -0.2618 0.032 Uiso 1 1 calc R . . C7 C -0.4683(5) 0.1490(4) -0.1794(3) 0.0348(9) Uani 1 1 d . . . H7 H -0.5656 0.1115 -0.2369 0.042 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 0.01684(7) 0.01841(7) 0.01595(7) 0.00388(5) 0.00412(4) 0.00032(4) P1 0.0145(4) 0.0173(4) 0.0133(4) 0.0038(3) 0.0030(3) 0.0025(3) S2 0.0248(4) 0.0312(5) 0.0285(5) 0.0118(4) 0.0064(4) -0.0028(4) C20 0.0145(15) 0.0161(16) 0.0174(17) 0.0023(13) 0.0028(12) 0.0029(12) C21 0.0219(17) 0.0299(19) 0.0212(19) 0.0089(16) 0.0059(14) 0.0043(14) C30 0.0151(15) 0.0136(15) 0.0178(17) 0.0012(13) 0.0066(12) 0.0018(12) C35 0.0210(16) 0.0196(17) 0.0178(17) 0.0032(14) 0.0051(13) 0.0028(13) C31 0.042(2) 0.031(2) 0.0158(19) 0.0005(16) 0.0005(16) 0.0166(17) C34 0.0313(19) 0.0217(18) 0.026(2) 0.0087(16) 0.0071(15) 0.0097(15) C23 0.0176(17) 0.028(2) 0.034(2) -0.0018(17) -0.0025(15) 0.0058(15) C22 0.034(2) 0.033(2) 0.021(2) 0.0094(17) -0.0020(15) 0.0108(16) C25 0.0266(19) 0.045(2) 0.027(2) 0.0174(18) 0.0094(16) 0.0047(17) C24 0.0186(18) 0.052(3) 0.039(2) 0.016(2) 0.0134(17) 0.0024(17) C33 0.048(2) 0.024(2) 0.034(2) -0.0001(18) 0.0071(18) 0.0170(17) C32 0.058(3) 0.034(2) 0.024(2) -0.0074(19) 0.0033(19) 0.018(2) C10 0.0189(15) 0.0200(17) 0.0152(17) 0.0011(14) 0.0057(13) 0.0064(13) C11 0.0213(16) 0.0157(16) 0.0138(17) 0.0001(13) 0.0023(13) 0.0061(13) N1 0.0276(15) 0.0212(15) 0.0270(17) 0.0078(13) 0.0082(13) 0.0014(12) S1 0.0265(4) 0.0263(5) 0.0180(4) 0.0027(4) 0.0090(4) -0.0030(4) N2 0.0272(15) 0.0179(14) 0.0240(16) 0.0040(12) 0.0094(12) 0.0047(12) N3 0.0325(17) 0.0377(19) 0.0249(17) 0.0108(15) 0.0137(14) 0.0114(14) C5 0.0292(18) 0.0199(17) 0.0194(18) 0.0077(14) 0.0106(14) 0.0116(14) C2 0.0207(16) 0.0211(17) 0.0182(17) 0.0086(14) 0.0011(13) 0.0031(13) C3 0.0304(18) 0.0189(17) 0.0222(19) 0.0074(15) 0.0079(15) 0.0119(14) C4 0.038(2) 0.037(2) 0.023(2) 0.0037(18) 0.0051(17) 0.0022(17) C9 0.044(2) 0.057(3) 0.029(2) 0.016(2) 0.0202(19) 0.018(2) C8 0.031(2) 0.055(3) 0.053(3) 0.024(2) 0.024(2) 0.019(2) C1 0.064(3) 0.033(3) 0.083(4) -0.009(3) 0.030(3) -0.022(2) C6 0.0315(19) 0.033(2) 0.0230(19) 0.0119(16) 0.0104(15) 0.0152(16) C7 0.0248(19) 0.043(2) 0.040(2) 0.017(2) 0.0050(17) 0.0136(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.2519(8) . ? Au1 S1 2.3135(8) . ? P1 C20 1.821(3) . ? P1 C30 1.827(3) . ? P1 C10 1.834(3) . ? S2 C2 1.765(3) . ? S2 C1 1.786(4) . ? C20 C21 1.375(5) . ? C20 C25 1.390(5) . ? C21 H21 0.9500 . ? C21 C22 1.386(5) . ? C30 C35 1.391(5) . ? C30 C31 1.383(5) . ? C35 H35 0.9500 . ? C35 C34 1.380(5) . ? C31 H31 0.9500 . ? C31 C32 1.377(5) . ? C34 H34 0.9500 . ? C34 C33 1.387(5) . ? C23 H23 0.9500 . ? C23 C22 1.381(5) . ? C23 C24 1.360(6) . ? C22 H22 0.9500 . ? C25 H25 0.9500 . ? C25 C24 1.382(5) . ? C24 H24 0.9500 . ? C33 H33 0.9500 . ? C33 C32 1.400(6) . ? C32 H32 0.9500 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.521(4) . ? C11 C11 1.532(6) 2 ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? N1 N2 1.400(4) . ? N1 C2 1.282(4) . ? S1 C2 1.744(3) . ? N2 C3 1.292(4) . ? N3 C5 1.353(4) . ? N3 C9 1.337(5) . ? C5 C3 1.485(5) . ? C5 C6 1.387(5) . ? C3 C4 1.499(5) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C9 H9 0.9500 . ? C9 C8 1.382(6) . ? C8 H8 0.9500 . ? C8 C7 1.380(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C6 H6 0.9500 . ? C6 C7 1.381(5) . ? C7 H7 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 172.09(3) . . ? C20 P1 Au1 112.03(11) . . ? C20 P1 C30 103.72(14) . . ? C20 P1 C10 105.19(14) . . ? C30 P1 Au1 113.97(10) . . ? C30 P1 C10 105.35(15) . . ? C10 P1 Au1 115.51(11) . . ? C2 S2 C1 101.22(19) . . ? C21 C20 P1 120.1(2) . . ? C21 C20 C25 119.1(3) . . ? C25 C20 P1 120.7(3) . . ? C20 C21 H21 119.7 . . ? C20 C21 C22 120.6(3) . . ? C22 C21 H21 119.7 . . ? C35 C30 P1 122.1(2) . . ? C31 C30 P1 118.7(3) . . ? C31 C30 C35 119.2(3) . . ? C30 C35 H35 119.6 . . ? C34 C35 C30 120.8(3) . . ? C34 C35 H35 119.6 . . ? C30 C31 H31 119.7 . . ? C32 C31 C30 120.6(4) . . ? C32 C31 H31 119.7 . . ? C35 C34 H34 120.0 . . ? C35 C34 C33 119.9(3) . . ? C33 C34 H34 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C24 C23 C22 120.0(3) . . ? C21 C22 H22 120.2 . . ? C23 C22 C21 119.6(3) . . ? C23 C22 H22 120.2 . . ? C20 C25 H25 120.1 . . ? C24 C25 C20 119.8(4) . . ? C24 C25 H25 120.1 . . ? C23 C24 C25 120.8(3) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C34 C33 H33 120.3 . . ? C34 C33 C32 119.4(3) . . ? C32 C33 H33 120.3 . . ? C31 C32 C33 120.1(4) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? P1 C10 H10A 108.5 . . ? P1 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? C11 C10 P1 115.2(2) . . ? C11 C10 H10A 108.5 . . ? C11 C10 H10B 108.5 . . ? C10 C11 C11 112.1(3) . 2 ? C10 C11 H11A 109.2 . . ? C10 C11 H11B 109.2 . . ? C11 C11 H11A 109.2 2 . ? C11 C11 H11B 109.2 2 . ? H11A C11 H11B 107.9 . . ? C2 N1 N2 114.9(3) . . ? C2 S1 Au1 105.19(12) . . ? C3 N2 N1 113.9(3) . . ? C9 N3 C5 116.6(3) . . ? N3 C5 C3 115.4(3) . . ? N3 C5 C6 122.5(3) . . ? C6 C5 C3 122.1(3) . . ? N1 C2 S2 117.8(2) . . ? N1 C2 S1 132.0(3) . . ? S1 C2 S2 110.22(19) . . ? N2 C3 C5 115.6(3) . . ? N2 C3 C4 124.0(3) . . ? C5 C3 C4 120.4(3) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C9 H9 117.9 . . ? N3 C9 C8 124.2(4) . . ? C8 C9 H9 117.9 . . ? C9 C8 H8 120.7 . . ? C7 C8 C9 118.7(4) . . ? C7 C8 H8 120.7 . . ? S2 C1 H1A 109.5 . . ? S2 C1 H1B 109.5 . . ? S2 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C5 C6 H6 120.2 . . ? C7 C6 C5 119.6(3) . . ? C7 C6 H6 120.2 . . ? C8 C7 C6 118.3(4) . . ? C8 C7 H7 120.8 . . ? C6 C7 H7 120.8 . . ? data_ams60 _database_code_depnum_ccdc_archive 'CCDC 803635' #TrackingRef '- Cifs_all.cif' _audit_creation_date 2011-07-07 _audit_creation_method ; Olex2 1.1-alpha (compiled Jun 27 2011 15:38:31, GUI svn.r3676) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H28 Au N4 P S' _chemical_formula_sum 'C28 H28 Au N4 P S' _chemical_formula_weight 680.54 _chemical_melting_point ? _chemical_oxdiff_formula C28H28N4S1Au1 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.6881(5) _cell_length_b 12.9308(3) _cell_length_c 18.0223(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.015(2) _cell_angle_gamma 90.00 _cell_volume 5452.1(2) _cell_formula_units_Z 8 _cell_measurement_reflns_used 7248 _cell_measurement_temperature 150.15 _cell_measurement_theta_max 32.8354 _cell_measurement_theta_min 3.0111 _exptl_absorpt_coefficient_mu 5.555 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.73785 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 2672 _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_unetI/netI 0.0857 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 19703 _diffrn_reflns_theta_full 25.05 _diffrn_reflns_theta_max 32.91 _diffrn_reflns_theta_min 3.02 _diffrn_ambient_temperature 150.15 _diffrn_detector_area_resol_mean 16.2705 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.884 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 56.00 81.00 1.0000 110.0000 omega____ theta____ kappa____ phi______ frames - 26.2288 179.0000 120.0000 25 #__ type_ start__ end____ width___ exp.time_ 2 omega 39.00 96.00 1.0000 110.0000 omega____ theta____ kappa____ phi______ frames - 26.2288 0.0000 -180.0000 57 #__ type_ start__ end____ width___ exp.time_ 3 omega -30.00 -3.00 1.0000 110.0000 omega____ theta____ kappa____ phi______ frames - 26.2288 0.0000 -180.0000 27 #__ type_ start__ end____ width___ exp.time_ 4 omega -58.00 38.00 1.0000 110.0000 omega____ theta____ kappa____ phi______ frames - -27.7913 77.0000 30.0000 96 #__ type_ start__ end____ width___ exp.time_ 5 omega -98.00 -2.00 1.0000 110.0000 omega____ theta____ kappa____ phi______ frames - -27.7913 -77.0000 -90.0000 96 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0113611000 _diffrn_orient_matrix_UB_12 -0.0478720000 _diffrn_orient_matrix_UB_13 -0.0099321000 _diffrn_orient_matrix_UB_21 0.0167508000 _diffrn_orient_matrix_UB_22 0.0263772000 _diffrn_orient_matrix_UB_23 -0.0233518000 _diffrn_orient_matrix_UB_31 0.0225718000 _diffrn_orient_matrix_UB_32 0.0045129000 _diffrn_orient_matrix_UB_33 0.0307351000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 5316 _reflns_number_total 9033 _reflns_odcompleteness_completeness 99.80 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 30.44 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122' _computing_structure_solution 'SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122' _refine_diff_density_max 5.137 _refine_diff_density_min -1.344 _refine_diff_density_rms 0.137 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.873 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 319 _refine_ls_number_reflns 9033 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0405 _refine_ls_restrained_S_all 0.873 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.0857 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.169336(7) 0.376927(15) 0.335526(9) 0.03179(6) Uani 1 1 d . . . S1 S 0.24026(5) 0.36045(10) 0.26192(7) 0.0395(3) Uani 1 1 d . . . P1 P 0.10120(5) 0.42671(10) 0.40171(6) 0.0277(2) Uani 1 1 d . . . N1 N 0.24888(18) 0.2274(3) 0.1519(2) 0.0411(10) Uani 1 1 d . . . N2 N 0.19941(17) 0.1604(3) 0.2383(2) 0.0374(9) Uani 1 1 d . . . N3 N 0.18686(16) 0.1661(3) 0.3094(2) 0.0368(9) Uani 1 1 d . . . C40 C 0.03195(17) 0.3686(4) 0.3711(2) 0.0300(9) Uani 1 1 d . . . C21 C 0.0838(2) 0.6247(4) 0.4591(3) 0.0381(10) Uani 1 1 d . . . H21 H 0.0872 0.5924 0.5070 0.046 Uiso 1 1 calc R . . C30 C 0.11732(17) 0.4001(3) 0.5017(2) 0.0267(9) Uani 1 1 d . . . C41 C -0.01837(19) 0.4223(4) 0.3622(2) 0.0345(10) Uani 1 1 d . . . H41 H -0.0180 0.4951 0.3695 0.041 Uiso 1 1 calc R . . C31 C 0.07849(19) 0.3521(4) 0.5406(3) 0.0344(11) Uani 1 1 d . . . H31 H 0.0419 0.3328 0.5149 0.041 Uiso 1 1 calc R . . C3 C 0.22728(17) 0.2404(4) 0.2176(2) 0.0310(10) Uani 1 1 d . . . C20 C 0.08796(19) 0.5652(4) 0.3963(3) 0.0327(10) Uani 1 1 d . . . C4 C 0.1537(2) 0.0911(4) 0.3269(3) 0.0375(11) Uani 1 1 d . . . C7 C 0.1811(2) 0.1448(4) 0.4612(3) 0.0462(13) Uani 1 1 d . . . H7 H 0.2108 0.1868 0.4478 0.055 Uiso 1 1 calc R . . C35 C 0.17056(19) 0.4287(4) 0.5401(3) 0.0367(11) Uani 1 1 d . . . H35 H 0.1976 0.4610 0.5139 0.044 Uiso 1 1 calc R . . C2 C 0.2424(3) 0.1288(4) 0.1126(3) 0.0674(18) Uani 1 1 d . . . H2A H 0.2455 0.0723 0.1493 0.101 Uiso 1 1 calc R . . H2B H 0.2724 0.1216 0.0812 0.101 Uiso 1 1 calc R . . H2C H 0.2048 0.1261 0.0808 0.101 Uiso 1 1 calc R . . N4 N 0.1036(2) 0.0287(3) 0.4231(3) 0.0545(12) Uani 1 1 d . . . C6 C 0.1460(2) 0.0896(4) 0.4065(3) 0.0410(12) Uani 1 1 d . . . C32 C 0.0928(2) 0.3321(4) 0.6170(3) 0.0432(12) Uani 1 1 d . . . H32 H 0.0663 0.2989 0.6435 0.052 Uiso 1 1 calc R . . C25 C 0.0817(3) 0.6134(4) 0.3270(3) 0.0597(16) Uani 1 1 d . . . H25 H 0.0843 0.5738 0.2832 0.072 Uiso 1 1 calc R . . C42 C -0.07022(19) 0.3709(4) 0.3427(3) 0.0434(12) Uani 1 1 d . . . H42 H -0.1051 0.4086 0.3357 0.052 Uiso 1 1 calc R . . C33 C 0.1457(2) 0.3608(4) 0.6539(3) 0.0475(14) Uani 1 1 d . . . H33 H 0.1558 0.3464 0.7060 0.057 Uiso 1 1 calc R . . C34 C 0.1843(2) 0.4104(4) 0.6161(3) 0.0462(13) Uani 1 1 d . . . H34 H 0.2203 0.4319 0.6424 0.055 Uiso 1 1 calc R . . C22 C 0.0749(2) 0.7297(4) 0.4535(3) 0.0470(13) Uani 1 1 d . . . H22 H 0.0733 0.7695 0.4975 0.056 Uiso 1 1 calc R . . C45 C 0.0302(2) 0.2619(4) 0.3602(4) 0.0557(16) Uani 1 1 d . . . H45 H 0.0649 0.2237 0.3651 0.067 Uiso 1 1 calc R . . C23 C 0.0683(3) 0.7779(4) 0.3835(3) 0.0552(15) Uani 1 1 d . . . H23 H 0.0614 0.8502 0.3789 0.066 Uiso 1 1 calc R . . C5 C 0.1253(2) 0.0124(4) 0.2733(3) 0.0495(13) Uani 1 1 d . . . H5A H 0.1239 0.0376 0.2217 0.074 Uiso 1 1 calc R . . H5B H 0.0864 0.0002 0.2832 0.074 Uiso 1 1 calc R . . H5C H 0.1470 -0.0523 0.2796 0.074 Uiso 1 1 calc R . . C8 C 0.1729(3) 0.1386(4) 0.5359(3) 0.0599(17) Uani 1 1 d . . . H8 H 0.1967 0.1764 0.5739 0.072 Uiso 1 1 calc R . . C43 C -0.0709(2) 0.2653(5) 0.3337(3) 0.0530(15) Uani 1 1 d . . . H43 H -0.1062 0.2298 0.3213 0.064 Uiso 1 1 calc R . . C24 C 0.0719(3) 0.7183(5) 0.3209(3) 0.071(2) Uani 1 1 d . . . H24 H 0.0676 0.7501 0.2729 0.086 Uiso 1 1 calc R . . C9 C 0.1300(4) 0.0771(5) 0.5534(4) 0.074(2) Uani 1 1 d . . . H9 H 0.1236 0.0702 0.6039 0.089 Uiso 1 1 calc R . . C10 C 0.0961(3) 0.0250(5) 0.4956(4) 0.0695(19) Uani 1 1 d . . . H10 H 0.0655 -0.0159 0.5079 0.083 Uiso 1 1 calc R . . C44 C -0.0210(2) 0.2119(5) 0.3423(4) 0.068(2) Uani 1 1 d . . . H44 H -0.0216 0.1389 0.3360 0.081 Uiso 1 1 calc R . . C1 C 0.2641(3) 0.3119(4) 0.1073(3) 0.0563(15) Uani 1 1 d . . . H1A H 0.2988 0.2942 0.0867 0.084 Uiso 1 1 calc R . . H1B H 0.2711 0.3739 0.1386 0.084 Uiso 1 1 calc R . . H1C H 0.2329 0.3252 0.0659 0.084 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 0.02831(8) 0.04567(11) 0.02255(8) -0.00617(9) 0.00763(5) 0.00220(9) S1 0.0325(5) 0.0581(9) 0.0303(6) -0.0121(6) 0.0129(4) -0.0051(6) P1 0.0264(5) 0.0362(6) 0.0212(5) -0.0056(5) 0.0058(4) 0.0020(5) N1 0.055(3) 0.038(2) 0.033(2) -0.0030(18) 0.0163(19) 0.011(2) N2 0.039(2) 0.042(2) 0.032(2) 0.0054(18) 0.0087(17) 0.0159(19) N3 0.037(2) 0.043(2) 0.031(2) 0.0091(18) 0.0081(17) 0.0165(19) C40 0.0248(18) 0.042(3) 0.0223(19) -0.008(2) 0.0018(15) 0.001(2) C21 0.051(3) 0.036(3) 0.030(2) -0.004(2) 0.015(2) -0.002(3) C30 0.0254(19) 0.033(3) 0.0216(19) -0.0052(17) 0.0027(16) 0.0054(17) C41 0.037(2) 0.042(3) 0.025(2) 0.000(2) 0.0067(19) 0.009(2) C31 0.030(2) 0.043(3) 0.031(2) 0.000(2) 0.0084(18) 0.003(2) C3 0.024(2) 0.041(3) 0.027(2) 0.007(2) 0.0023(17) 0.009(2) C20 0.036(2) 0.036(3) 0.028(2) 0.001(2) 0.0111(19) -0.002(2) C4 0.040(2) 0.040(3) 0.035(3) 0.012(2) 0.013(2) 0.020(2) C7 0.056(3) 0.044(3) 0.040(3) 0.003(2) 0.011(2) 0.016(3) C35 0.028(2) 0.046(3) 0.036(3) -0.002(2) 0.003(2) 0.004(2) C2 0.111(5) 0.047(3) 0.054(4) -0.002(3) 0.042(4) 0.019(4) N4 0.074(3) 0.043(3) 0.052(3) 0.000(2) 0.028(3) -0.003(2) C6 0.051(3) 0.035(3) 0.041(3) 0.011(2) 0.017(2) 0.020(2) C32 0.047(3) 0.053(3) 0.033(3) 0.009(2) 0.017(2) 0.013(3) C25 0.108(5) 0.045(4) 0.031(3) -0.002(3) 0.025(3) 0.006(3) C42 0.027(2) 0.075(4) 0.027(2) -0.003(3) 0.0007(17) 0.011(3) C33 0.054(3) 0.065(4) 0.022(2) 0.002(2) 0.002(2) 0.032(3) C34 0.033(2) 0.064(3) 0.036(3) -0.012(3) -0.010(2) 0.014(2) C22 0.063(4) 0.039(3) 0.042(3) -0.011(2) 0.019(3) -0.007(3) C45 0.034(3) 0.045(3) 0.083(4) -0.024(3) -0.007(3) 0.012(2) C23 0.080(4) 0.036(3) 0.056(4) 0.007(3) 0.028(3) -0.002(3) C5 0.059(3) 0.049(3) 0.043(3) 0.004(3) 0.014(3) 0.004(3) C8 0.090(5) 0.052(4) 0.036(3) 0.005(3) 0.005(3) 0.026(3) C43 0.034(3) 0.072(4) 0.050(3) -0.025(3) -0.003(2) -0.008(3) C24 0.134(6) 0.047(4) 0.037(3) 0.011(3) 0.027(4) 0.008(4) C9 0.139(7) 0.051(4) 0.041(3) 0.009(3) 0.043(4) 0.015(4) C10 0.111(6) 0.048(4) 0.061(4) 0.012(3) 0.048(4) 0.003(4) C44 0.042(3) 0.054(4) 0.100(5) -0.039(4) -0.009(3) -0.003(3) C1 0.082(4) 0.061(4) 0.032(3) 0.000(3) 0.025(3) -0.003(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 S1 2.3077(11) . ? Au1 P1 2.2462(11) . ? S1 C3 1.751(5) . ? P1 C40 1.810(4) . ? P1 C30 1.815(4) . ? P1 C20 1.818(5) . ? N1 C3 1.372(6) . ? N1 C2 1.455(7) . ? N1 C1 1.437(6) . ? N2 N3 1.362(5) . ? N2 C3 1.312(6) . ? N3 C4 1.318(7) . ? C40 C41 1.367(6) . ? C40 C45 1.393(7) . ? C21 H21 0.9500 . ? C21 C20 1.385(6) . ? C21 C22 1.375(7) . ? C30 C31 1.388(6) . ? C30 C35 1.391(6) . ? C41 H41 0.9500 . ? C41 C42 1.392(7) . ? C31 H31 0.9500 . ? C31 C32 1.389(6) . ? C20 C25 1.383(7) . ? C4 C6 1.474(7) . ? C4 C5 1.488(7) . ? C7 H7 0.9500 . ? C7 C6 1.384(8) . ? C7 C8 1.393(8) . ? C35 H35 0.9500 . ? C35 C34 1.377(7) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? N4 C6 1.347(7) . ? N4 C10 1.346(7) . ? C32 H32 0.9500 . ? C32 C33 1.375(7) . ? C25 H25 0.9500 . ? C25 C24 1.378(8) . ? C42 H42 0.9500 . ? C42 C43 1.374(7) . ? C33 H33 0.9500 . ? C33 C34 1.381(8) . ? C34 H34 0.9500 . ? C22 H22 0.9500 . ? C22 C23 1.395(8) . ? C45 H45 0.9500 . ? C45 C44 1.367(7) . ? C23 H23 0.9500 . ? C23 C24 1.379(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C8 H8 0.9500 . ? C8 C9 1.366(9) . ? C43 H43 0.9500 . ? C43 C44 1.357(7) . ? C24 H24 0.9500 . ? C9 H9 0.9500 . ? C9 C10 1.388(9) . ? C10 H10 0.9500 . ? C44 H44 0.9500 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 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 168.54(5) . . ? C3 S1 Au1 104.61(15) . . ? C40 P1 Au1 114.29(14) . . ? C40 P1 C30 105.27(19) . . ? C40 P1 C20 104.6(2) . . ? C30 P1 Au1 114.57(14) . . ? C30 P1 C20 104.3(2) . . ? C20 P1 Au1 112.71(15) . . ? C3 N1 C2 120.2(4) . . ? C3 N1 C1 123.4(4) . . ? C1 N1 C2 114.2(4) . . ? C3 N2 N3 114.7(4) . . ? C4 N3 N2 114.3(4) . . ? C41 C40 P1 123.8(4) . . ? C41 C40 C45 118.7(4) . . ? C45 C40 P1 117.3(3) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C22 C21 C20 121.2(5) . . ? C31 C30 P1 122.3(3) . . ? C31 C30 C35 119.2(4) . . ? C35 C30 P1 118.5(3) . . ? C40 C41 H41 119.8 . . ? C40 C41 C42 120.4(5) . . ? C42 C41 H41 119.8 . . ? C30 C31 H31 119.8 . . ? C30 C31 C32 120.4(4) . . ? C32 C31 H31 119.8 . . ? N1 C3 S1 116.1(4) . . ? N2 C3 S1 129.0(4) . . ? N2 C3 N1 114.9(4) . . ? C21 C20 P1 122.5(4) . . ? C25 C20 P1 119.1(4) . . ? C25 C20 C21 118.5(4) . . ? N3 C4 C6 114.3(5) . . ? N3 C4 C5 124.9(4) . . ? C6 C4 C5 120.8(5) . . ? C6 C7 H7 120.0 . . ? C6 C7 C8 120.0(6) . . ? C8 C7 H7 120.0 . . ? C30 C35 H35 119.9 . . ? C34 C35 C30 120.3(5) . . ? C34 C35 H35 119.9 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C10 N4 C6 116.9(5) . . ? C7 C6 C4 122.3(5) . . ? N4 C6 C4 115.7(5) . . ? N4 C6 C7 122.0(5) . . ? C31 C32 H32 120.3 . . ? C33 C32 C31 119.5(5) . . ? C33 C32 H32 120.3 . . ? C20 C25 H25 119.7 . . ? C24 C25 C20 120.6(5) . . ? C24 C25 H25 119.7 . . ? C41 C42 H42 120.1 . . ? C43 C42 C41 119.8(5) . . ? C43 C42 H42 120.1 . . ? C32 C33 H33 119.7 . . ? C32 C33 C34 120.6(4) . . ? C34 C33 H33 119.7 . . ? C35 C34 C33 120.0(5) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C21 C22 H22 119.9 . . ? C21 C22 C23 120.2(5) . . ? C23 C22 H22 119.9 . . ? C40 C45 H45 119.8 . . ? C44 C45 C40 120.5(5) . . ? C44 C45 H45 119.8 . . ? C22 C23 H23 120.8 . . ? C24 C23 C22 118.5(5) . . ? C24 C23 H23 120.8 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C8 H8 120.7 . . ? C9 C8 C7 118.5(6) . . ? C9 C8 H8 120.7 . . ? C42 C43 H43 120.0 . . ? C44 C43 C42 119.9(5) . . ? C44 C43 H43 120.0 . . ? C25 C24 C23 121.1(5) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C8 C9 H9 120.9 . . ? C8 C9 C10 118.3(6) . . ? C10 C9 H9 120.9 . . ? N4 C10 C9 124.2(6) . . ? N4 C10 H10 117.9 . . ? C9 C10 H10 117.9 . . ? C45 C44 H44 119.6 . . ? C43 C44 C45 120.7(5) . . ? C43 C44 H44 119.6 . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? ############################################################################ # # # # # ### # # ### ### # ### # # ### # # ### # ### # # # # # # # # # # # # # ## ## # ## # # # # # # # # # # ### # # ### ### # ### # # # ### # ## # ### ### # # # # # # # # # # # # # # # # # # ## # # # ### ### # # ### ### # # ### # # # # # # # # # # # # # # # # # ### ### ### # # # # # ## ## # # # # # # # # # # # # # # # ### # ### ### # ### # # # # # # # # # ## # # # # # # # # # # # ### # # # # # ### # # # # # ############################################################################ ############################################################################ # # # This Supplementary Material is written in the Crystallographic # # Information File (CIF) format. For further details see: S.R. Hall, # # F.H. Allen and I.D. Brown, Acta Cryst. (1991) A47, 655-685. # # # ############################################################################ data_6399 _database_code_depnum_ccdc_archive 'CCDC 833228' # # ############################################################################ _audit_creation_date 2009-03-06 _audit_block_code AMS131 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_compound_source CH2Cl2/Et2O _chemical_formula_moiety 'C62 H66 Au2 Fe N8 P2 Se2' _chemical_formula_sum 'C62 H66 Au2 Fe N8 P2 Se2' _chemical_formula_weight 1592.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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 11.4658(2) _cell_length_b 11.4760(2) _cell_length_c 12.2708(2) _cell_angle_alpha 101.5540(10) _cell_angle_beta 100.5610(10) _cell_angle_gamma 106.8280(10) _cell_volume 1463.18(4) _cell_formula_units_Z 1 _cell_measurement_temperature 100 _cell_measurement_reflns_used 22466 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 33.14 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.808 _exptl_crystal_density_method none _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 6.591 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS, Bruker AXS (2008)' _exptl_absorpt_correction_T_min 0.30 _exptl_absorpt_correction_T_max 0.69 _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '0.3 mm focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'CCD \w-scan' _diffrn_detector_area_resol_mean 18.18 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 34667 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 33.20 _reflns_number_total 11158 _reflns_number_gt 10236 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect software (Nonius, 1998)' _computing_cell_refinement 'Denzo / Scalepack (Otwinowski 1997)' _computing_data_reduction 'Denzo / Scalepack (Otwinowski 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Crystal Impact GbR, 2006)' _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^)+(0.0272P)^2^+1.3162P] 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_number_reflns 11158 _refine_ls_number_parameters 351 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0631 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 C1 C 0.9865(2) 0.1975(2) 0.74455(18) 0.0188(4) Uani 1 1 d . . . C2 C 0.7639(2) 0.3397(2) 0.7501(2) 0.0222(4) Uani 1 1 d . . . C3 C 0.8353(3) 0.4694(3) 0.8295(3) 0.0411(8) Uani 1 1 d . . . H3A H 0.8923 0.4633 0.8943 0.062 Uiso 1 1 calc R . . H3B H 0.7770 0.5065 0.8560 0.062 Uiso 1 1 calc R . . H3C H 0.8823 0.5213 0.7891 0.062 Uiso 1 1 calc R . . C11 C 0.6323(2) 0.3108(2) 0.6818(2) 0.0203(4) Uani 1 1 d . . . C12 C 0.5649(2) 0.1925(2) 0.6043(2) 0.0215(4) Uani 1 1 d . . . H12 H 0.5981 0.1272 0.5997 0.026 Uiso 1 1 calc R . . C13 C 0.4479(2) 0.1736(3) 0.5344(2) 0.0260(5) Uani 1 1 d . . . H13 H 0.4018 0.0956 0.4820 0.031 Uiso 1 1 calc R . . C14 C 0.4008(3) 0.2712(3) 0.5435(3) 0.0300(5) Uani 1 1 d . . . H14 H 0.3225 0.2611 0.4974 0.036 Uiso 1 1 calc R . . C15 C 0.4721(3) 0.3840(3) 0.6222(3) 0.0436(8) Uani 1 1 d . . . H15 H 0.4397 0.4499 0.6278 0.052 Uiso 1 1 calc R . . C21 C 1.1950(2) 0.1870(3) 0.7289(2) 0.0223(4) Uani 1 1 d . . . H21A H 1.2191 0.2510 0.6885 0.027 Uiso 1 1 calc R . . H21B H 1.1500 0.1066 0.6718 0.027 Uiso 1 1 calc R . . C22 C 1.3129(2) 0.1792(3) 0.8029(2) 0.0242(5) Uani 1 1 d . . . H22A H 1.3679 0.1631 0.7548 0.029 Uiso 1 1 calc R . . H22B H 1.2893 0.1090 0.8365 0.029 Uiso 1 1 calc R . . C23 C 1.3841(2) 0.3005(3) 0.8988(2) 0.0263(5) Uani 1 1 d . . . H23 H 1.4096 0.3698 0.8632 0.032 Uiso 1 1 calc R . . C24 C 1.2926(2) 0.3266(3) 0.9686(2) 0.0298(5) Uani 1 1 d . . . H24A H 1.2678 0.2597 1.0059 0.036 Uiso 1 1 calc R . . H24B H 1.3349 0.4055 1.0282 0.036 Uiso 1 1 calc R . . C25 C 1.1748(2) 0.3348(3) 0.8939(2) 0.0275(5) Uani 1 1 d . . . H25A H 1.1177 0.3476 0.9407 0.033 Uiso 1 1 calc R . . H25B H 1.1983 0.4067 0.8623 0.033 Uiso 1 1 calc R . . C26 C 1.5027(3) 0.2925(3) 0.9718(3) 0.0339(6) Uani 1 1 d . . . H26A H 1.5452 0.3702 1.0312 0.051 Uiso 1 1 calc R . . H26B H 1.5576 0.2784 0.9241 0.051 Uiso 1 1 calc R . . H26C H 1.4801 0.2238 1.0062 0.051 Uiso 1 1 calc R . . C31 C 0.8245(2) 0.1964(2) 0.21821(19) 0.0209(4) Uani 1 1 d . . . C32 C 0.9150(2) 0.1377(2) 0.2194(2) 0.0230(4) Uani 1 1 d . . . H32 H 0.9422 0.1114 0.2834 0.028 Uiso 1 1 calc R . . C33 C 0.9648(3) 0.1183(3) 0.1249(2) 0.0302(6) Uani 1 1 d . . . H33 H 1.0239 0.0773 0.1252 0.036 Uiso 1 1 calc R . . C34 C 0.9269(3) 0.1598(3) 0.0305(2) 0.0338(6) Uani 1 1 d . . . H34 H 0.9618 0.1480 -0.0318 0.041 Uiso 1 1 calc R . . C35 C 0.8371(3) 0.2186(4) 0.0283(2) 0.0390(7) Uani 1 1 d . . . H35 H 0.8121 0.2467 -0.0351 0.047 Uiso 1 1 calc R . . C36 C 0.7841(3) 0.2357(3) 0.1215(2) 0.0328(6) Uani 1 1 d . . . H36 H 0.7221 0.2732 0.1194 0.039 Uiso 1 1 calc R . . C41 C 0.5945(2) 0.1917(2) 0.2886(2) 0.0184(4) Uani 1 1 d . . . C42 C 0.5122(3) 0.0681(3) 0.2615(3) 0.0306(6) Uani 1 1 d . . . H42 H 0.5437 0.0028 0.2673 0.037 Uiso 1 1 calc R . . C43 C 0.3824(3) 0.0419(3) 0.2258(3) 0.0402(7) Uani 1 1 d . . . H43 H 0.3275 -0.0408 0.2078 0.048 Uiso 1 1 calc R . . C44 C 0.3357(2) 0.1385(3) 0.2173(3) 0.0341(6) Uani 1 1 d . . . H44 H 0.2492 0.1205 0.1924 0.041 Uiso 1 1 calc R . . C45 C 0.4159(2) 0.2613(3) 0.2452(2) 0.0295(5) Uani 1 1 d . . . H45 H 0.3838 0.3263 0.2404 0.035 Uiso 1 1 calc R . . C46 C 0.5451(2) 0.2877(2) 0.2807(2) 0.0252(5) Uani 1 1 d . . . H46 H 0.5993 0.3708 0.2994 0.030 Uiso 1 1 calc R . . C51 C 0.8230(2) 0.3932(2) 0.4021(2) 0.0178(4) Uani 1 1 d . . . C52 C 0.8788(2) 0.4909(3) 0.3512(2) 0.0276(5) Uani 1 1 d . . . H52 H 0.8934 0.4789 0.2783 0.033 Uiso 1 1 calc R . . C53 C 0.9076(2) 0.6086(3) 0.4318(3) 0.0363(7) Uani 1 1 d . . . H53 H 0.9445 0.6874 0.4208 0.044 Uiso 1 1 calc R . . C54 C 0.8709(2) 0.5869(2) 0.5320(3) 0.0324(6) Uani 1 1 d . . . H54 H 0.8796 0.6486 0.5979 0.039 Uiso 1 1 calc R . . C55 C 0.8186(2) 0.4542(2) 0.5141(2) 0.0210(4) Uani 1 1 d . . . H55 H 0.7868 0.4139 0.5664 0.025 Uiso 1 1 calc R . . N1 N 0.93666(19) 0.2817(2) 0.78175(17) 0.0219(4) Uani 1 1 d . . . N2 N 0.81000(18) 0.2502(2) 0.72663(16) 0.0197(4) Uani 1 1 d . . . N3 N 0.5863(2) 0.4062(2) 0.6924(2) 0.0384(6) Uani 1 1 d . . . N4 N 1.11057(19) 0.2184(2) 0.79913(17) 0.0208(4) Uani 1 1 d . . . P1 P 0.76225(5) 0.22482(6) 0.34325(5) 0.01539(10) Uani 1 1 d . . . Fe1 Fe 1.0000 0.5000 0.5000 0.02006(9) Uani 1 2 d S . . Se1 Se 0.90055(2) 0.03991(2) 0.625086(19) 0.01823(5) Uani 1 1 d . . . Au1 Au 0.817145(7) 0.128266(7) 0.478198(6) 0.01476(3) Uani 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 C1 0.0172(9) 0.0290(11) 0.0125(9) 0.0065(8) 0.0034(7) 0.0109(9) C2 0.0181(10) 0.0308(12) 0.0175(10) -0.0003(9) 0.0047(8) 0.0125(9) C3 0.0269(13) 0.0439(17) 0.0373(16) -0.0186(13) -0.0061(12) 0.0184(13) C11 0.0168(9) 0.0272(11) 0.0205(10) 0.0049(9) 0.0080(8) 0.0115(9) C12 0.0167(10) 0.0207(10) 0.0280(12) 0.0071(9) 0.0059(9) 0.0070(8) C13 0.0169(10) 0.0280(12) 0.0301(13) 0.0058(10) 0.0049(9) 0.0054(9) C14 0.0197(11) 0.0373(15) 0.0344(14) 0.0115(12) 0.0023(10) 0.0136(11) C15 0.0299(15) 0.0352(16) 0.063(2) 0.0004(15) -0.0005(14) 0.0236(13) C21 0.0190(10) 0.0298(12) 0.0203(10) 0.0040(9) 0.0034(8) 0.0144(9) C22 0.0193(10) 0.0315(13) 0.0255(12) 0.0072(10) 0.0054(9) 0.0147(10) C23 0.0170(10) 0.0339(13) 0.0271(12) 0.0071(10) 0.0008(9) 0.0112(10) C24 0.0212(11) 0.0426(15) 0.0224(12) 0.0014(11) 0.0001(9) 0.0147(11) C25 0.0218(11) 0.0374(14) 0.0213(11) -0.0016(10) 0.0000(9) 0.0169(11) C26 0.0200(11) 0.0487(17) 0.0317(14) 0.0077(13) -0.0006(10) 0.0163(12) C31 0.0197(10) 0.0314(12) 0.0154(9) 0.0072(9) 0.0038(8) 0.0143(9) C32 0.0200(10) 0.0283(12) 0.0222(11) 0.0061(9) 0.0044(9) 0.0118(9) C33 0.0254(12) 0.0398(15) 0.0306(13) 0.0063(11) 0.0107(10) 0.0186(11) C34 0.0347(14) 0.0480(17) 0.0210(12) 0.0050(11) 0.0122(11) 0.0171(13) C35 0.0482(18) 0.063(2) 0.0172(12) 0.0157(13) 0.0106(12) 0.0309(17) C36 0.0379(15) 0.0550(18) 0.0193(11) 0.0153(12) 0.0094(11) 0.0310(14) C41 0.0138(9) 0.0193(10) 0.0207(10) 0.0063(8) 0.0018(8) 0.0047(8) C42 0.0231(12) 0.0216(12) 0.0424(16) 0.0089(11) -0.0006(11) 0.0060(10) C43 0.0232(13) 0.0320(15) 0.0531(19) 0.0149(14) -0.0046(13) -0.0018(11) C44 0.0142(10) 0.0447(17) 0.0411(16) 0.0189(13) -0.0005(10) 0.0062(11) C45 0.0200(11) 0.0382(15) 0.0336(14) 0.0118(12) 0.0034(10) 0.0153(11) C46 0.0199(11) 0.0227(11) 0.0306(13) 0.0051(10) 0.0002(9) 0.0089(9) C51 0.0126(8) 0.0193(10) 0.0224(10) 0.0102(8) 0.0027(8) 0.0048(7) C52 0.0160(10) 0.0335(13) 0.0371(14) 0.0244(12) 0.0022(9) 0.0066(9) C53 0.0145(10) 0.0243(12) 0.070(2) 0.0260(14) -0.0027(12) 0.0053(9) C54 0.0192(11) 0.0192(11) 0.0499(17) 0.0006(11) -0.0054(11) 0.0079(9) C55 0.0141(9) 0.0203(10) 0.0266(11) 0.0024(9) 0.0025(8) 0.0071(8) N1 0.0166(8) 0.0344(11) 0.0155(8) 0.0015(8) 0.0016(7) 0.0146(8) N2 0.0154(8) 0.0297(10) 0.0165(8) 0.0067(8) 0.0035(7) 0.0114(8) N3 0.0266(12) 0.0316(13) 0.0497(16) -0.0071(11) -0.0012(11) 0.0180(10) N4 0.0169(8) 0.0278(10) 0.0169(9) 0.0006(7) 0.0020(7) 0.0117(8) P1 0.0150(2) 0.0182(2) 0.0144(2) 0.0055(2) 0.00276(19) 0.0076(2) Fe1 0.01150(18) 0.0162(2) 0.0327(3) 0.01248(19) 0.00122(17) 0.00376(16) Se1 0.01932(10) 0.01818(10) 0.01853(10) 0.00788(8) 0.00178(8) 0.00825(8) Au1 0.01522(4) 0.01413(4) 0.01415(4) 0.00423(3) 0.00103(3) 0.00523(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 C1 N1 1.306(3) . Y C1 N4 1.386(3) . Y C1 Se1 1.941(2) . Y C2 N2 1.291(3) . Y C2 C11 1.491(3) . Y C2 C3 1.502(4) . Y C3 H3A 0.9600 . N C3 H3B 0.9600 . N C3 H3C 0.9600 . N C11 N3 1.341(3) . Y C11 C12 1.396(3) . Y C12 C13 1.384(3) . Y C12 H12 0.9300 . N C13 C14 1.372(4) . Y C13 H13 0.9300 . N C14 C15 1.369(4) . Y C14 H14 0.9300 . N C15 N3 1.351(4) . Y C15 H15 0.9300 . N C21 N4 1.480(3) . Y C21 C22 1.521(3) . Y C21 H21A 0.9700 . N C21 H21B 0.9700 . N C22 C23 1.523(4) . Y C22 H22A 0.9700 . N C22 H22B 0.9700 . N C23 C26 1.523(4) . Y C23 C24 1.528(4) . Y C23 H23 0.9800 . N C24 C25 1.525(4) . Y C24 H24A 0.9700 . N C24 H24B 0.9700 . N C25 N4 1.475(3) . Y C25 H25A 0.9700 . N C25 H25B 0.9700 . N C26 H26A 0.9600 . N C26 H26B 0.9600 . N C26 H26C 0.9600 . N C31 C32 1.391(3) . Y C31 C36 1.400(3) . Y C31 P1 1.818(2) . Y C32 C33 1.390(3) . Y C32 H32 0.9300 . N C33 C34 1.384(4) . Y C33 H33 0.9300 . N C34 C35 1.384(4) . Y C34 H34 0.9300 . N C35 C36 1.396(4) . Y C35 H35 0.9300 . N C36 H36 0.9300 . N C41 C46 1.389(3) . Y C41 C42 1.391(3) . Y C41 P1 1.815(2) . Y C42 C43 1.395(4) . Y C42 H42 0.9300 . N C43 C44 1.377(5) . Y C43 H43 0.9300 . N C44 C45 1.375(4) . Y C44 H44 0.9300 . N C45 C46 1.388(4) . Y C45 H45 0.9300 . N C46 H46 0.9300 . N C51 C55 1.430(3) . Y C51 C52 1.439(3) . Y C51 P1 1.793(2) . Y C51 Fe1 2.035(2) . Y C52 C53 1.414(4) . Y C52 Fe1 2.046(2) . Y C52 H52 0.9300 . N C53 C54 1.415(5) . Y C53 Fe1 2.058(3) . Y C53 H53 0.9300 . N C54 C55 1.420(4) . Y C54 Fe1 2.061(3) . Y C54 H54 0.9300 . N C55 Fe1 2.042(2) . Y C55 H55 0.9300 . N N1 N2 1.391(3) . Y P1 Au1 2.2633(6) . Y Fe1 C51 2.035(2) 2_766 ? Fe1 C55 2.042(2) 2_766 ? Fe1 C52 2.046(3) 2_766 ? Fe1 C53 2.058(3) 2_766 ? Fe1 C54 2.061(3) 2_766 ? Se1 Au1 2.4194(2) . Y 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 N1 C1 N4 117.5(2) . . Y N1 C1 Se1 126.26(18) . . Y N4 C1 Se1 116.19(17) . . Y N2 C2 C11 114.6(2) . . Y N2 C2 C3 125.5(2) . . Y C11 C2 C3 119.6(2) . . Y C2 C3 H3A 109.5 . . N C2 C3 H3B 109.5 . . N H3A C3 H3B 109.5 . . N C2 C3 H3C 109.5 . . N H3A C3 H3C 109.5 . . N H3B C3 H3C 109.5 . . N N3 C11 C12 122.0(2) . . Y N3 C11 C2 116.7(2) . . Y C12 C11 C2 121.1(2) . . Y C13 C12 C11 119.2(2) . . Y C13 C12 H12 120.4 . . N C11 C12 H12 120.4 . . N C14 C13 C12 119.2(3) . . Y C14 C13 H13 120.4 . . N C12 C13 H13 120.4 . . N C15 C14 C13 118.2(3) . . Y C15 C14 H14 120.9 . . N C13 C14 H14 120.9 . . N N3 C15 C14 124.5(3) . . Y N3 C15 H15 117.8 . . N C14 C15 H15 117.8 . . N N4 C21 C22 111.5(2) . . Y N4 C21 H21A 109.3 . . N C22 C21 H21A 109.3 . . N N4 C21 H21B 109.3 . . N C22 C21 H21B 109.3 . . N H21A C21 H21B 108.0 . . N C21 C22 C23 111.9(2) . . Y C21 C22 H22A 109.2 . . N C23 C22 H22A 109.2 . . N C21 C22 H22B 109.2 . . N C23 C22 H22B 109.2 . . N H22A C22 H22B 107.9 . . N C26 C23 C22 111.6(2) . . Y C26 C23 C24 113.1(2) . . Y C22 C23 C24 107.7(2) . . Y C26 C23 H23 108.1 . . N C22 C23 H23 108.1 . . N C24 C23 H23 108.1 . . N C25 C24 C23 112.2(2) . . Y C25 C24 H24A 109.2 . . N C23 C24 H24A 109.2 . . N C25 C24 H24B 109.2 . . N C23 C24 H24B 109.2 . . N H24A C24 H24B 107.9 . . N N4 C25 C24 110.8(2) . . Y N4 C25 H25A 109.5 . . N C24 C25 H25A 109.5 . . N N4 C25 H25B 109.5 . . N C24 C25 H25B 109.5 . . N H25A C25 H25B 108.1 . . N C23 C26 H26A 109.5 . . N C23 C26 H26B 109.5 . . N H26A C26 H26B 109.5 . . N C23 C26 H26C 109.5 . . N H26A C26 H26C 109.5 . . N H26B C26 H26C 109.5 . . N C32 C31 C36 119.6(2) . . Y C32 C31 P1 119.87(17) . . Y C36 C31 P1 120.50(19) . . Y C33 C32 C31 120.0(2) . . Y C33 C32 H32 120.0 . . N C31 C32 H32 120.0 . . N C34 C33 C32 120.3(2) . . Y C34 C33 H33 119.9 . . N C32 C33 H33 119.9 . . N C35 C34 C33 120.3(2) . . Y C35 C34 H34 119.9 . . N C33 C34 H34 119.9 . . N C34 C35 C36 119.9(3) . . Y C34 C35 H35 120.0 . . N C36 C35 H35 120.0 . . N C35 C36 C31 119.9(3) . . Y C35 C36 H36 120.1 . . N C31 C36 H36 120.1 . . N C46 C41 C42 118.9(2) . . Y C46 C41 P1 121.64(18) . . Y C42 C41 P1 119.27(19) . . Y C41 C42 C43 120.0(3) . . Y C41 C42 H42 120.0 . . N C43 C42 H42 120.0 . . N C44 C43 C42 120.0(3) . . Y C44 C43 H43 120.0 . . N C42 C43 H43 120.0 . . N C45 C44 C43 120.5(3) . . Y C45 C44 H44 119.7 . . N C43 C44 H44 119.7 . . N C44 C45 C46 119.6(3) . . Y C44 C45 H45 120.2 . . N C46 C45 H45 120.2 . . N C45 C46 C41 120.8(2) . . Y C45 C46 H46 119.6 . . N C41 C46 H46 119.6 . . N C55 C51 C52 107.1(2) . . Y C55 C51 P1 122.98(17) . . Y C52 C51 P1 129.8(2) . . Y C55 C51 Fe1 69.73(13) . . Y C52 C51 Fe1 69.76(13) . . Y P1 C51 Fe1 127.14(12) . . Y C53 C52 C51 107.7(2) . . Y C53 C52 Fe1 70.30(16) . . Y C51 C52 Fe1 68.96(13) . . Y C53 C52 H52 126.1 . . N C51 C52 H52 126.1 . . N Fe1 C52 H52 126.2 . . N C52 C53 C54 108.9(2) . . Y C52 C53 Fe1 69.40(14) . . Y C54 C53 Fe1 70.06(15) . . Y C52 C53 H53 125.5 . . N C54 C53 H53 125.5 . . N Fe1 C53 H53 126.6 . . N C53 C54 C55 107.8(3) . . Y C53 C54 Fe1 69.77(16) . . Y C55 C54 Fe1 69.02(14) . . Y C53 C54 H54 126.1 . . N C55 C54 H54 126.1 . . N Fe1 C54 H54 126.7 . . N C54 C55 C51 108.4(2) . . Y C54 C55 Fe1 70.49(15) . . Y C51 C55 Fe1 69.21(13) . . Y C54 C55 H55 125.8 . . N C51 C55 H55 125.8 . . N Fe1 C55 H55 126.1 . . N C1 N1 N2 113.8(2) . . Y C2 N2 N1 114.7(2) . . Y C11 N3 C15 116.9(3) . . Y C1 N4 C25 116.7(2) . . Y C1 N4 C21 118.87(19) . . Y C25 N4 C21 112.7(2) . . Y C51 P1 C41 103.36(11) . . Y C51 P1 C31 104.77(11) . . Y C41 P1 C31 106.48(11) . . Y C51 P1 Au1 110.34(8) . . Y C41 P1 Au1 116.12(7) . . Y C31 P1 Au1 114.62(8) . . Y C51 Fe1 C51 180.0 2_766 . N C51 Fe1 C55 138.95(9) 2_766 . Y C51 Fe1 C55 41.06(9) . . Y C51 Fe1 C55 41.06(9) 2_766 2_766 ? C51 Fe1 C55 138.94(9) . 2_766 ? C55 Fe1 C55 180.0 . 2_766 N C51 Fe1 C52 41.29(9) 2_766 2_766 ? C51 Fe1 C52 138.71(9) . 2_766 ? C55 Fe1 C52 111.25(10) . 2_766 ? C55 Fe1 C52 68.75(10) 2_766 2_766 ? C51 Fe1 C52 138.71(9) 2_766 . Y C51 Fe1 C52 41.29(9) . . Y C55 Fe1 C52 68.75(10) . . Y C55 Fe1 C52 111.25(10) 2_766 . Y C52 Fe1 C52 179.998(1) 2_766 . Y C51 Fe1 C53 111.49(10) 2_766 . Y C51 Fe1 C53 68.51(10) . . Y C55 Fe1 C53 67.94(11) . . Y C55 Fe1 C53 112.06(11) 2_766 . Y C52 Fe1 C53 139.70(13) 2_766 . Y C52 Fe1 C53 40.30(13) . . Y C51 Fe1 C53 68.51(10) 2_766 2_766 ? C51 Fe1 C53 111.49(10) . 2_766 ? C55 Fe1 C53 112.06(11) . 2_766 ? C55 Fe1 C53 67.94(11) 2_766 2_766 ? C52 Fe1 C53 40.30(13) 2_766 2_766 ? C52 Fe1 C53 139.70(13) . 2_766 ? C53 Fe1 C53 179.999(1) . 2_766 ? C51 Fe1 C54 111.33(10) 2_766 . Y C51 Fe1 C54 68.67(10) . . Y C55 Fe1 C54 40.48(10) . . Y C55 Fe1 C54 139.52(10) 2_766 . Y C52 Fe1 C54 111.85(12) 2_766 . Y C52 Fe1 C54 68.16(12) . . Y C53 Fe1 C54 40.17(13) . . Y C53 Fe1 C54 139.83(13) 2_766 . Y C51 Fe1 C54 68.67(10) 2_766 2_766 ? C51 Fe1 C54 111.33(10) . 2_766 ? C55 Fe1 C54 139.52(10) . 2_766 ? C55 Fe1 C54 40.48(10) 2_766 2_766 ? C52 Fe1 C54 68.15(12) 2_766 2_766 ? C52 Fe1 C54 111.84(12) . 2_766 ? C53 Fe1 C54 139.83(13) . 2_766 ? C53 Fe1 C54 40.17(13) 2_766 2_766 ? C54 Fe1 C54 179.999(1) . 2_766 ? C1 Se1 Au1 97.36(7) . . Y P1 Au1 Se1 173.429(15) . . Y _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 33.20 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.072 _refine_diff_density_min -1.940 _refine_diff_density_rms 0.137