Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_name 'Prof Vivian Wing-Wah Yam' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author 'Prof Vivian Wing-Wah Yam' _publ_contact_author_address ; Prof Vivian Wing-Wah Yam Department of Chemistry The University of Hong Kong Pokfulam Road Hong Kong CHINA ; _publ_contact_author_email 'ENTER EMAIL ADDRESS' loop_ _publ_author_name 'Vivian Wing-Wah Yam' 'Kai-Leung Cheung' 'Kung-Kai Cheung' ; Eddie Chung-Chin Cheng ; 'Nianyong Zhu' _publ_section_title ; Syntheses and luminescence studies of mixed-metal gold (I)-copper(I) and -silver(I) alkynyl complexes. The =A1=A7Turning-on=A1=A8 of emission upon d10 metal ion encapsulation. ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ data_mar119b _database_code_CSD 198508 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H20 Au P' _chemical_formula_sum 'C23 H20 Au P' _chemical_formula_weight 524.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.100(3) _cell_length_b 10.423(2) _cell_length_c 13.900(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.41(3) _cell_angle_gamma 90.00 _cell_volume 2025.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.719 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 7.343 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'marresearch imaging plate mar300' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9094 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0624 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 25.51 _reflns_number_total 3509 _reflns_number_gt 2713 _reflns_threshold_expression >2sigma(I) _computing_data_collection Marcontrol _computing_cell_refinement scalepack _computing_data_reduction Denzo _computing_structure_solution Shelxs-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0721P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3509 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1205 _refine_ls_wR_factor_gt 0.1150 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.23952(2) 0.05736(3) 0.386054(19) 0.04669(16) Uani 1 1 d . . . P1 P 0.25436(16) 0.20372(17) 0.50907(14) 0.0441(5) Uani 1 1 d . . . C1 C 0.2728(6) 0.3654(7) 0.4646(5) 0.050(2) Uani 1 1 d . . . C2 C 0.3483(8) 0.4423(7) 0.5048(7) 0.061(2) Uani 1 1 d . . . H2 H 0.3896 0.4133 0.5579 0.073 Uiso 1 1 calc R . . C3 C 0.3619(10) 0.5630(8) 0.4654(9) 0.083(4) Uani 1 1 d . . . H3 H 0.4123 0.6153 0.4912 0.099 Uiso 1 1 calc R . . C4 C 0.2965(11) 0.6040(10) 0.3846(8) 0.091(4) Uani 1 1 d . . . H4 H 0.3023 0.6857 0.3590 0.109 Uiso 1 1 calc R . . C5 C 0.2292(9) 0.5287(9) 0.3465(9) 0.078(3) Uani 1 1 d . . . H5 H 0.1899 0.5553 0.2911 0.093 Uiso 1 1 calc R . . C6 C 0.2135(9) 0.4085(10) 0.3861(6) 0.068(3) Uani 1 1 d . . . H6 H 0.1626 0.3579 0.3590 0.082 Uiso 1 1 calc R . . C7 C 0.3552(6) 0.1726(7) 0.6010(5) 0.0467(18) Uani 1 1 d . . . C8 C 0.4369(8) 0.1196(13) 0.5744(8) 0.091(4) Uani 1 1 d . . . H8 H 0.4389 0.0987 0.5096 0.110 Uiso 1 1 calc R . . C9 C 0.5141(10) 0.0971(14) 0.6394(11) 0.116(5) Uani 1 1 d . . . H9 H 0.5690 0.0633 0.6187 0.139 Uiso 1 1 calc R . . C10 C 0.5132(9) 0.1238(12) 0.7374(8) 0.090(3) Uani 1 1 d . . . H10 H 0.5659 0.1056 0.7828 0.108 Uiso 1 1 calc R . . C11 C 0.4336(10) 0.1767(13) 0.7641(7) 0.104(4) Uani 1 1 d . . . H11 H 0.4314 0.1968 0.8290 0.125 Uiso 1 1 calc R . . C12 C 0.3554(8) 0.2013(11) 0.6968(7) 0.088(4) Uani 1 1 d . . . H12 H 0.3013 0.2384 0.7171 0.105 Uiso 1 1 calc R . . C13 C 0.1513(6) 0.2135(7) 0.5737(5) 0.0474(19) Uani 1 1 d . . . C14 C 0.0986(7) 0.1027(8) 0.5849(6) 0.059(2) Uani 1 1 d . . . H14 H 0.1147 0.0262 0.5565 0.071 Uiso 1 1 calc R . . C15 C 0.0225(8) 0.1065(11) 0.6381(7) 0.071(3) Uani 1 1 d . . . H15 H -0.0124 0.0323 0.6456 0.085 Uiso 1 1 calc R . . C16 C -0.0021(7) 0.2174(12) 0.6797(7) 0.079(3) Uani 1 1 d . . . H16 H -0.0539 0.2187 0.7148 0.095 Uiso 1 1 calc R . . C17 C 0.0488(8) 0.3267(11) 0.6702(8) 0.084(3) Uani 1 1 d . . . H17 H 0.0316 0.4023 0.6990 0.101 Uiso 1 1 calc R . . C18 C 0.1262(7) 0.3255(9) 0.6176(7) 0.066(2) Uani 1 1 d . . . H18 H 0.1612 0.4002 0.6119 0.080 Uiso 1 1 calc R . . C19 C 0.2282(6) -0.0690(7) 0.2741(6) 0.0469(19) Uani 1 1 d . . . C20 C 0.2214(7) -0.1409(7) 0.2091(5) 0.056(2) Uani 1 1 d . . . C21 C 0.2126(10) -0.2296(9) 0.1276(6) 0.079(3) Uani 1 1 d . . . C22 C 0.2827(11) -0.3157(10) 0.1143(8) 0.099(4) Uani 1 1 d . . . H22A H 0.2753 -0.3699 0.0607 0.119 Uiso 1 1 calc R . . H22B H 0.3378 -0.3202 0.1589 0.119 Uiso 1 1 calc R . . C23 C 0.1256(13) -0.2184(13) 0.0610(8) 0.142(7) Uani 1 1 d . . . H23A H 0.0859 -0.1528 0.0833 0.213 Uiso 1 1 calc R . . H23B H 0.0921 -0.2988 0.0576 0.213 Uiso 1 1 calc R . . H23C H 0.1410 -0.1961 -0.0022 0.213 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 0.0564(3) 0.0413(2) 0.0423(2) -0.00464(11) 0.00602(14) 0.00077(14) P1 0.0527(14) 0.0390(10) 0.0413(10) -0.0046(7) 0.0088(9) -0.0005(9) C1 0.062(6) 0.046(4) 0.045(4) 0.001(3) 0.018(4) 0.005(4) C2 0.075(7) 0.048(5) 0.059(5) -0.001(4) 0.005(5) -0.008(4) C3 0.108(11) 0.045(5) 0.094(8) 0.001(5) 0.015(7) -0.025(5) C4 0.156(13) 0.038(5) 0.082(7) 0.025(5) 0.027(7) 0.013(7) C5 0.091(9) 0.051(6) 0.087(7) 0.016(5) -0.003(6) 0.007(5) C6 0.091(8) 0.063(5) 0.048(6) 0.018(4) 0.002(5) 0.003(5) C7 0.047(5) 0.042(4) 0.052(5) 0.001(3) 0.010(3) -0.005(4) C8 0.061(8) 0.125(9) 0.084(8) -0.042(7) -0.006(6) 0.031(7) C9 0.071(9) 0.137(11) 0.131(12) -0.063(9) -0.019(8) 0.040(8) C10 0.081(10) 0.096(8) 0.085(8) 0.008(6) -0.021(7) 0.002(7) C11 0.085(10) 0.178(13) 0.048(6) 0.010(7) 0.002(5) 0.003(9) C12 0.066(8) 0.151(11) 0.046(6) 0.005(6) 0.008(4) 0.021(7) C13 0.048(5) 0.054(5) 0.040(4) -0.003(3) 0.005(3) 0.000(4) C14 0.069(7) 0.051(5) 0.055(5) 0.003(4) 0.000(4) -0.006(5) C15 0.061(7) 0.088(7) 0.067(6) 0.019(5) 0.018(5) -0.015(6) C16 0.057(7) 0.133(10) 0.050(6) -0.008(6) 0.015(4) -0.007(7) C17 0.067(8) 0.099(8) 0.091(8) -0.043(6) 0.029(6) -0.013(6) C18 0.059(6) 0.076(6) 0.066(6) -0.031(5) 0.015(4) -0.009(5) C19 0.049(5) 0.052(5) 0.037(4) 0.003(3) -0.002(3) 0.007(4) C20 0.085(7) 0.046(4) 0.037(4) -0.005(3) 0.008(4) -0.007(4) C21 0.129(11) 0.056(6) 0.051(6) -0.008(4) 0.010(6) -0.032(6) C22 0.162(14) 0.065(7) 0.076(8) -0.031(5) 0.034(8) -0.016(7) C23 0.23(2) 0.105(10) 0.068(8) -0.003(6) -0.056(10) -0.053(11) _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 C19 2.029(8) . ? Au1 P1 2.2810(18) . ? P1 C13 1.808(8) . ? P1 C7 1.814(8) . ? P1 C1 1.825(8) . ? C1 C6 1.363(11) . ? C1 C2 1.390(12) . ? C2 C3 1.396(11) . ? C3 C4 1.424(17) . ? C4 C5 1.292(18) . ? C5 C6 1.398(13) . ? C7 C12 1.365(12) . ? C7 C8 1.370(13) . ? C8 C9 1.344(15) . ? C9 C10 1.391(17) . ? C10 C11 1.346(17) . ? C11 C12 1.375(15) . ? C13 C18 1.384(11) . ? C13 C14 1.393(12) . ? C14 C15 1.381(13) . ? C15 C16 1.356(15) . ? C16 C17 1.362(14) . ? C17 C18 1.390(13) . ? C19 C20 1.169(10) . ? C20 C21 1.455(11) . ? C21 C22 1.365(17) . ? C21 C23 1.443(17) . ? 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 C19 Au1 P1 178.3(2) . . ? C13 P1 C7 105.5(4) . . ? C13 P1 C1 106.0(4) . . ? C7 P1 C1 105.7(4) . . ? C13 P1 Au1 114.1(3) . . ? C7 P1 Au1 113.3(2) . . ? C1 P1 Au1 111.5(3) . . ? C6 C1 C2 119.4(8) . . ? C6 C1 P1 118.4(7) . . ? C2 C1 P1 122.1(7) . . ? C1 C2 C3 119.9(9) . . ? C2 C3 C4 118.2(10) . . ? C5 C4 C3 120.5(9) . . ? C4 C5 C6 121.9(11) . . ? C1 C6 C5 119.9(10) . . ? C12 C7 C8 117.1(9) . . ? C12 C7 P1 123.4(7) . . ? C8 C7 P1 119.5(7) . . ? C9 C8 C7 121.7(11) . . ? C8 C9 C10 121.0(12) . . ? C11 C10 C9 117.7(11) . . ? C10 C11 C12 120.9(11) . . ? C7 C12 C11 121.6(11) . . ? C18 C13 C14 118.7(8) . . ? C18 C13 P1 122.3(7) . . ? C14 C13 P1 118.9(6) . . ? C15 C14 C13 119.9(9) . . ? C16 C15 C14 120.8(10) . . ? C15 C16 C17 120.4(10) . . ? C16 C17 C18 120.1(9) . . ? C13 C18 C17 120.1(9) . . ? C20 C19 Au1 179.4(7) . . ? C19 C20 C21 179.6(11) . . ? C22 C21 C23 122.5(10) . . ? C22 C21 C20 122.2(11) . . ? C23 C21 C20 115.3(12) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 25.51 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 1.471 _refine_diff_density_min -2.103 _refine_diff_density_rms 0.176 data_ip588_Yam_Cheung_KL's_DAn38_08_11_98 _database_code_CSD 198509 #-------------------------------------------------------------------------- _audit_creation_date 'Tue Jan 19 10:32:35 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #-------------------------------------------------------------------------- _computing_data_collection 'MAR Data Collection Software & DENZO' _computing_cell_refinement 'MAR Data Collection Software & DENZO' _computing_data_reduction teXsan _computing_structure_solution SIR92 _computing_structure_refinement teXsan _computing_publication_material teXsan #-------------------------------------------------------------------------- _cell_length_a 10.464(2) _cell_length_b 9.378(2) _cell_length_c 19.868(3) _cell_angle_alpha 90 _cell_angle_beta 104.14(2) _cell_angle_gamma 90 _cell_volume 1890.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #-------------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #-------------------------------------------------------------------------- _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.450 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.894 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 1078.51 _chemical_formula_analytical ? _chemical_formula_sum 'C44 H38 Au2 Fe P2 ' _chemical_formula_moiety 'C44 H38 Au2 Fe P2 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1032.00 _exptl_absorpt_coefficient_mu 8.261 _exptl_absorpt_correction_type none #-------------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 301.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'MAR IPDS' _diffrn_measurement_method oscillation _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 3483 _reflns_number_total 3483 _reflns_number_observed 2782 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.43 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #-------------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 88 0.003 0.002 'International Tables' H 0 76 0.000 0.000 'International Tables' P 0 4 0.102 0.094 'International Tables' Fe 0 2 0.346 0.844 'International Tables' Au 0 4 -2.013 8.802 'International Tables' #-------------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Au(1) 0.33965(3) 0.59070(3) 0.41520(2) 0.0508(1) Uij ? ? Fe(1) 0.0000 0.5000 0.5000 0.0458(5) Uij ? ? P(1) 0.1977(2) 0.7470(2) 0.4465(1) 0.0469(6) Uij ? ? C(1) 0.4484(10) 0.454(1) 0.3749(5) 0.057(3) Uij ? ? C(2) 0.491(1) 0.372(1) 0.3391(6) 0.067(3) Uij ? ? C(3) 0.529(1) 0.275(1) 0.2921(6) 0.081(4) Uij ? ? C(4) 0.444(3) 0.155(2) 0.270(1) 0.164(10) Uij ? ? C(5) 0.639(2) 0.290(2) 0.2675(7) 0.104(5) Uij ? ? C(6) 0.1152(9) 0.6772(8) 0.5090(4) 0.047(2) Uij ? ? C(7) -0.013(1) 0.713(1) 0.5168(6) 0.063(3) Uij ? ? C(8) -0.030(1) 0.634(1) 0.5752(6) 0.070(3) Uij ? ? C(9) 0.079(1) 0.551(1) 0.6008(5) 0.083(4) Uij ? ? C(10) 0.175(1) 0.5757(10) 0.5604(6) 0.064(3) Uij ? ? C(11) 0.270(1) 0.9162(8) 0.4835(6) 0.059(3) Uij ? ? C(12) 0.309(1) 1.013(1) 0.4411(7) 0.082(4) Uij ? ? C(13) 0.363(1) 1.145(1) 0.470(1) 0.106(6) Uij ? ? C(14) 0.376(1) 1.176(1) 0.536(1) 0.110(6) Uij ? ? C(15) 0.344(2) 1.074(1) 0.580(1) 0.111(6) Uij ? ? C(16) 0.286(1) 0.946(1) 0.5530(7) 0.078(4) Uij ? ? C(17) 0.0701(10) 0.801(1) 0.3718(5) 0.056(3) Uij ? ? C(18) 0.049(1) 0.722(1) 0.3116(5) 0.068(3) Uij ? ? C(19) -0.055(1) 0.755(1) 0.2543(6) 0.085(4) Uij ? ? C(20) -0.129(1) 0.873(2) 0.2551(7) 0.099(5) Uij ? ? C(21) -0.109(1) 0.954(2) 0.3164(8) 0.095(5) Uij ? ? C(22) -0.011(1) 0.914(1) 0.3735(7) 0.081(5) Uij ? ? H(1) 0.3729 0.1590 0.2912 0.1603 Uij ? ? H(2) 0.4127 0.1588 0.2209 0.1603 Uij ? ? H(3) 0.4932 0.0702 0.2829 0.1603 Uij ? ? H(4) 0.6967 0.3694 0.2817 0.1252 Uij ? ? H(5) 0.6589 0.2223 0.2360 0.1252 Uij ? ? H(6) -0.0742 0.7759 0.4884 0.0753 Uij ? ? H(7) -0.1055 0.6387 0.5938 0.0849 Uij ? ? H(8) 0.0910 0.4868 0.6391 0.0989 Uij ? ? H(9) 0.2595 0.5337 0.5668 0.0775 Uij ? ? H(10) 0.3005 0.9927 0.3931 0.0977 Uij ? ? H(11) 0.3908 1.2129 0.4413 0.1288 Uij ? ? H(12) 0.4076 1.2667 0.5529 0.1323 Uij ? ? H(13) 0.3606 1.0929 0.6288 0.1314 Uij ? ? H(14) 0.2578 0.8793 0.5824 0.0941 Uij ? ? H(15) 0.1063 0.6441 0.3089 0.0817 Uij ? ? H(16) -0.0737 0.6942 0.2149 0.1026 Uij ? ? H(17) -0.1932 0.9005 0.2149 0.1187 Uij ? ? H(18) -0.1613 1.0357 0.3183 0.1135 Uij ? ? H(19) 0.0003 0.9670 0.4154 0.0978 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au(1) 0.0444(3) 0.0477(3) 0.0632(3) -0.0042(1) 0.0189(2) -0.0042(1) Fe(1) 0.0458(10) 0.050(1) 0.0423(9) -0.0161(7) 0.0129(7) -0.0037(6) P(1) 0.044(1) 0.044(1) 0.057(1) -0.0047(8) 0.0195(10) -0.0018(9) C(1) 0.056(6) 0.054(5) 0.065(6) -0.005(4) 0.019(5) -0.003(4) C(2) 0.064(7) 0.077(6) 0.062(6) 0.003(5) 0.023(5) -0.005(5) C(3) 0.079(8) 0.085(8) 0.080(8) 0.025(6) 0.024(6) -0.010(6) C(4) 0.21(2) 0.10(1) 0.21(2) -0.03(1) 0.12(2) -0.08(1) C(5) 0.11(1) 0.11(1) 0.095(10) 0.012(8) 0.031(8) -0.031(8) C(6) 0.049(5) 0.049(4) 0.045(4) -0.012(3) 0.014(4) -0.009(3) C(7) 0.056(6) 0.063(6) 0.077(7) -0.016(4) 0.032(5) -0.012(5) C(8) 0.076(8) 0.083(7) 0.064(6) -0.034(6) 0.039(6) -0.025(5) C(9) 0.11(1) 0.099(8) 0.039(5) -0.060(8) 0.020(6) -0.012(5) C(10) 0.063(7) 0.067(7) 0.056(6) -0.025(4) 0.003(5) 0.001(4) C(11) 0.046(6) 0.052(6) 0.084(7) -0.009(3) 0.028(5) -0.006(4) C(12) 0.078(8) 0.055(6) 0.13(1) -0.019(5) 0.056(8) -0.002(6) C(13) 0.071(8) 0.049(8) 0.21(2) -0.011(6) 0.05(1) 0.010(9) C(14) 0.065(8) 0.050(8) 0.23(2) -0.015(5) 0.06(1) -0.033(10) C(15) 0.09(1) 0.10(1) 0.15(2) -0.033(8) 0.04(1) -0.059(9) C(16) 0.076(8) 0.063(6) 0.103(9) -0.031(6) 0.034(7) -0.019(6) C(17) 0.055(6) 0.058(5) 0.059(5) 0.002(4) 0.024(4) 0.009(4) C(18) 0.068(7) 0.077(7) 0.059(6) 0.000(5) 0.016(5) 0.017(5) C(19) 0.093(9) 0.095(9) 0.062(7) 0.000(7) 0.006(6) 0.018(5) C(20) 0.085(10) 0.119(10) 0.074(8) 0.024(8) -0.019(7) 0.023(8) C(21) 0.071(8) 0.116(10) 0.100(10) 0.042(8) 0.027(7) 0.046(8) C(22) 0.077(9) 0.10(1) 0.077(8) 0.023(6) 0.033(7) 0.020(6) #-------------------------------------------------------------------------- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 3.09434 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2782 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0583 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0746 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.781 _refine_ls_shift/esd_max 0.0240 _refine_ls_shift/esd_mean 0.01 _refine_diff_density_min -3.90 _refine_diff_density_max 2.20 #-------------------------------------------------------------------------- _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au(1) P(1) 2.279(2) ? ? yes Au(1) C(1) 2.005(10) ? ? yes Fe(1) C(6) 2.035(8) ? ? yes Fe(1) C(6) 2.035(8) ? ? yes Fe(1) C(7) 2.032(9) ? ? yes Fe(1) C(7) 2.032(9) ? ? yes Fe(1) C(8) 2.04(1) ? ? yes Fe(1) C(8) 2.04(1) ? ? yes Fe(1) C(9) 2.029(10) ? ? yes Fe(1) C(9) 2.029(10) ? ? yes Fe(1) C(10) 2.054(10) ? ? yes Fe(1) C(10) 2.054(10) ? ? yes P(1) C(6) 1.800(8) ? ? yes P(1) C(11) 1.831(9) ? ? yes P(1) C(17) 1.81(1) ? ? yes C(1) C(2) 1.21(1) ? ? yes C(2) C(3) 1.43(1) ? ? yes C(3) C(4) 1.43(2) ? ? yes C(3) C(5) 1.37(2) ? ? yes C(6) C(7) 1.42(1) ? ? yes C(6) C(10) 1.42(1) ? ? yes C(7) C(8) 1.42(1) ? ? yes C(8) C(9) 1.38(2) ? ? yes C(9) C(10) 1.45(2) ? ? yes C(11) C(12) 1.37(1) ? ? yes C(11) C(16) 1.38(2) ? ? yes C(12) C(13) 1.42(2) ? ? yes C(13) C(14) 1.31(2) ? ? yes C(14) C(15) 1.40(2) ? ? yes C(15) C(16) 1.39(1) ? ? yes C(17) C(18) 1.38(1) ? ? yes C(17) C(22) 1.36(1) ? ? yes C(18) C(19) 1.41(2) ? ? yes C(19) C(20) 1.35(2) ? ? yes C(20) C(21) 1.41(2) ? ? yes C(21) C(22) 1.38(2) ? ? yes #--------------------------------------------------------------------------= #--- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(1) Au(1) C(1) 172.3(3) ? ? ? yes C(6) Fe(1) C(6) 180.0 ? ? 3_565 yes C(6) Fe(1) C(7) 41.0(4) ? ? ? yes C(6) Fe(1) C(7) 139.0(4) ? ? 3_565 yes C(6) Fe(1) C(8) 68.0(4) ? ? ? yes C(6) Fe(1) C(8) 112.0(4) ? ? 3_565 yes C(6) Fe(1) C(9) 68.3(4) ? ? ? yes C(6) Fe(1) C(9) 111.7(4) ? ? 3_565 yes C(6) Fe(1) C(10) 40.7(3) ? ? ? yes C(6) Fe(1) C(10) 139.3(3) ? ? 3_565 yes C(6) Fe(1) C(7) 139.0(4) ? ? ? yes C(6) Fe(1) C(7) 41.0(4) ? ? 3_565 yes C(6) Fe(1) C(8) 112.0(4) ? ? ? yes C(6) Fe(1) C(8) 68.0(4) ? ? 3_565 yes C(6) Fe(1) C(9) 111.7(4) ? ? ? yes C(6) Fe(1) C(9) 68.3(4) ? ? 3_565 yes C(6) Fe(1) C(10) 139.3(3) ? ? ? yes C(6) Fe(1) C(10) 40.7(3) ? ? 3_565 yes C(7) Fe(1) C(7) 180.0 ? ? 3_565 yes C(7) Fe(1) C(8) 41.0(4) ? ? ? yes C(7) Fe(1) C(8) 139.0(4) ? ? 3_565 yes C(7) Fe(1) C(9) 68.6(5) ? ? ? yes C(7) Fe(1) C(9) 111.4(5) ? ? 3_565 yes C(7) Fe(1) C(10) 69.5(4) ? ? ? yes C(7) Fe(1) C(10) 110.5(4) ? ? 3_565 yes C(7) Fe(1) C(8) 139.0(4) ? ? ? yes C(7) Fe(1) C(8) 41.0(4) ? ? 3_565 yes C(7) Fe(1) C(9) 111.4(5) ? ? ? yes C(7) Fe(1) C(9) 68.6(5) ? ? 3_565 yes C(7) Fe(1) C(10) 110.5(4) ? ? ? yes C(7) Fe(1) C(10) 69.5(4) ? ? 3_565 yes C(8) Fe(1) C(8) 180.0 ? ? 3_565 yes C(8) Fe(1) C(9) 39.6(6) ? ? ? yes C(8) Fe(1) C(9) 140.4(6) ? ? 3_565 yes C(8) Fe(1) C(10) 68.5(5) ? ? ? yes C(8) Fe(1) C(10) 111.5(5) ? ? 3_565 yes C(8) Fe(1) C(9) 140.4(6) ? ? ? yes C(8) Fe(1) C(9) 39.6(6) ? ? 3_565 yes C(8) Fe(1) C(10) 111.5(5) ? ? ? yes C(8) Fe(1) C(10) 68.5(5) ? ? 3_565 yes C(9) Fe(1) C(9) 180.0 ? ? 3_565 yes C(9) Fe(1) C(10) 41.5(5) ? ? ? yes C(9) Fe(1) C(10) 138.5(5) ? ? 3_565 yes C(9) Fe(1) C(10) 138.5(5) 3 ? ? yes C(9) Fe(1) C(10) 41.5(5) 3 ? ? yes C(10) Fe(1) C(10) 180.0 ? ? 3_565 yes Au(1) P(1) C(6) 114.1(3) ? ? ? yes Au(1) P(1) C(11) 115.8(3) ? ? ? yes Au(1) P(1) C(17) 110.8(3) ? ? ? yes C(6) P(1) C(11) 104.9(4) ? ? ? yes C(6) P(1) C(17) 106.5(4) ? ? ? yes C(11) P(1) C(17) 103.7(5) ? ? ? yes Au(1) C(1) C(2) 166.3(9) ? ? ? yes C(1) C(2) C(3) 174(1) ? ? ? yes C(2) C(3) C(4) 116(1) ? ? ? yes C(2) C(3) C(5) 123(1) ? ? ? yes C(4) C(3) C(5) 119(1) ? ? ? yes Fe(1) C(6) P(1) 127.6(4) ? ? ? yes Fe(1) C(6) C(7) 69.4(5) ? ? ? yes Fe(1) C(6) C(10) 70.4(5) ? ? ? yes P(1) C(6) C(7) 127.7(7) ? ? ? yes P(1) C(6) C(10) 122.5(8) ? ? ? yes C(7) C(6) C(10) 109.8(9) ? ? ? yes Fe(1) C(7) C(6) 69.6(5) ? ? ? yes Fe(1) C(7) C(8) 69.7(6) ? ? ? yes C(6) C(7) C(8) 106.2(10) ? ? ? yes Fe(1) C(8) C(7) 69.3(5) ? ? ? yes Fe(1) C(8) C(9) 69.9(6) ? ? ? yes C(7) C(8) C(9) 109.5(9) ? ? ? yes Fe(1) C(9) C(8) 70.5(6) ? ? ? yes Fe(1) C(9) C(10) 70.2(6) ? ? ? yes C(8) C(9) C(10) 109(1) ? ? ? yes Fe(1) C(10) C(6) 68.9(5) ? ? ? yes Fe(1) C(10) C(9) 68.3(6) ? ? ? yes C(6) C(10) C(9) 105(1) ? ? ? yes P(1) C(11) C(12) 119.0(9) ? ? ? yes P(1) C(11) C(16) 121.1(7) ? ? ? yes C(12) C(11) C(16) 119.9(9) ? ? ? yes C(11) C(12) C(13) 118(1) ? ? ? yes C(12) C(13) C(14) 122(1) ? ? ? yes C(13) C(14) C(15) 119(1) ? ? ? yes C(14) C(15) C(16) 119(1) ? ? ? yes C(11) C(16) C(15) 120(1) ? ? ? yes P(1) C(17) C(18) 119.4(8) ? ? ? yes P(1) C(17) C(22) 122.4(9) ? ? ? yes C(18) C(17) C(22) 118(1) ? ? ? yes C(17) C(18) C(19) 120(1) ? ? ? yes C(18) C(19) C(20) 120(1) ? ? ? yes C(19) C(20) C(21) 119(1) ? ? ? yes C(20) C(21) C(22) 118(1) ? ? ? yes C(17) C(22) C(21) 122(1) ? ? ? yes #--------------------------------------------------------------------------= #---