# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Jose Antonio Real' _publ_contact_author_address ; Institut de Ciencia Molecular/Quimica Inorganica Universitat de Valencia Doctor Moliner 50 Burjassot Valencia 46100 SPAIN ; _publ_contact_author_email JOSE.A.REAL@UV.ES _publ_section_title ; Supramolecular isomerism in spin crossover networks with aurophillic interactions ; loop_ _publ_author_name 'Jose Antonio Real' 'Ana Galet' 'Victor Martinez' 'M. Carmen Munoz' data_1a_293K _database_code_depnum_ccdc_archive 'CCDC 243010' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H28 Au6 Fe3 N24 O2' _chemical_formula_weight 2322.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 15.7900(7) _cell_length_b 15.7900(7) _cell_length_c 7.0130(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1514.25(11) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 20 _exptl_crystal_description needles _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 15.227 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.642 _exptl_absorpt_correction_T_max 0.833 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3820 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0659 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2306 _reflns_number_gt 1623 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ;Refinement in the higher symmetry space group was attempted but was not posible. All non-hydrogen atoms were refined isotropically except for iron and gold atoms that were refined anisotropically. The hydrogen atoms were not localised. 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^)+(0.1447P)^2^+15.2647P] 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 2306 _refine_ls_number_parameters 54 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1093 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.2513 _refine_ls_wR_factor_gt 0.2094 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.004 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 0.26114(5) -0.26108(5) -0.00008(9) 0.0546(4) Uani 1 1 d . . . Fe1 Fe 0.5000 0.0000 -0.5000 0.0207(6) Uani 1 2 d S . . N1 N 0.4026(10) -0.1126(10) -0.305(2) 0.039(3) Uiso 1 1 d . . . C1 C 0.3511(14) -0.1673(15) -0.196(3) 0.051(4) Uiso 1 1 d . . . N2 N 0.5153(10) 0.1122(10) -0.3073(19) 0.038(3) Uiso 1 1 d . . . C2 C 0.1680(15) -0.3497(15) 0.193(3) 0.054(5) Uiso 1 1 d . . . N3 N 0.3728(9) -0.0005(9) -0.6269(19) 0.043(3) Uiso 1 1 d G . . C7 C 0.2810(11) -0.0803(8) -0.664(3) 0.085(8) Uiso 1 1 d G . . C6 C 0.2063(9) -0.0658(14) -0.730(3) 0.106(10) Uiso 1 1 d GD . . C5 C 0.2234(13) 0.0285(17) -0.760(3) 0.102(10) Uiso 1 1 d G . . C4 C 0.3153(16) 0.1084(12) -0.723(4) 0.162(18) Uiso 1 1 d G . . C3 C 0.3900(11) 0.0938(8) -0.656(3) 0.076(7) Uiso 1 1 d G . . C8 C 0.1142(18) -0.140(3) -0.759(8) 0.166(19) Uiso 1 1 d D . . N4 N 0.0258(17) -0.205(3) -0.772(8) 0.194(18) Uiso 1 1 d D . . O1 O 1.0000 0.0000 0.5000 0.061(9) Uiso 1 6 d S . . O2 O 0.0000 0.0000 -1.0000 0.188(8) Uiso 1 6 d S . . 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 0.0493(5) 0.0491(5) 0.0287(4) 0.0108(3) 0.0107(3) -0.0029(3) Fe1 0.0231(13) 0.0199(13) 0.0178(12) 0.0011(9) 0.0024(10) 0.0098(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 C2 1.98(2) . ? Au1 C1 2.00(2) . ? Fe1 N2 2.144(14) . ? Fe1 N2 2.144(14) 4_654 ? Fe1 N1 2.158(14) 4_654 ? Fe1 N1 2.158(14) . ? Fe1 N3 2.193(11) 4_654 ? Fe1 N3 2.193(11) . ? N1 C1 1.13(2) . ? N2 C2 1.18(2) 6 ? C2 N2 1.18(2) 5 ? N3 C7 1.3900 . ? N3 C3 1.3900 . ? C7 C6 1.3900 . ? C6 C8 1.352(10) . ? C6 C5 1.3900 . ? C5 C4 1.3900 . ? C4 C3 1.3900 . ? C8 N4 1.256(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Au1 C1 176.7(8) . . ? N2 Fe1 N2 180.0(7) . 4_654 ? N2 Fe1 N1 88.8(5) . 4_654 ? N2 Fe1 N1 91.2(5) 4_654 4_654 ? N2 Fe1 N1 91.2(5) . . ? N2 Fe1 N1 88.8(5) 4_654 . ? N1 Fe1 N1 180.0(8) 4_654 . ? N2 Fe1 N3 90.9(5) . 4_654 ? N2 Fe1 N3 89.1(5) 4_654 4_654 ? N1 Fe1 N3 88.8(5) 4_654 4_654 ? N1 Fe1 N3 91.2(5) . 4_654 ? N2 Fe1 N3 89.1(5) . . ? N2 Fe1 N3 90.9(5) 4_654 . ? N1 Fe1 N3 91.2(5) 4_654 . ? N1 Fe1 N3 88.8(5) . . ? N3 Fe1 N3 180.0 4_654 . ? C1 N1 Fe1 175.7(15) . . ? N1 C1 Au1 178.6(17) . . ? C2 N2 Fe1 174.7(15) 6 . ? N2 C2 Au1 179(2) 5 . ? C7 N3 C3 120.0 . . ? C7 N3 Fe1 128.2(8) . . ? C3 N3 Fe1 111.6(8) . . ? C6 C7 N3 120.0 . . ? C8 C6 C7 123(3) . . ? C8 C6 C5 117(3) . . ? C7 C6 C5 120.0 . . ? C4 C5 C6 120.0 . . ? C3 C4 C5 120.0 . . ? C4 C3 N3 120.0 . . ? N4 C8 C6 174(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.575 _refine_diff_density_min -1.262 _refine_diff_density_rms 0.600 #END data_1,_120K _database_code_depnum_ccdc_archive 'CCDC 243011' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H28 Au6 Fe3 N24 O2' _chemical_formula_weight 2322.2 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 15.6730(9) _cell_length_b 15.6730(9) _cell_length_c 6.9500(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1478.49(19) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 20 _exptl_crystal_description needles _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 15.595 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4008 _diffrn_reflns_av_R_equivalents 0.1197 _diffrn_reflns_av_sigmaI/netI 0.1796 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2252 _reflns_number_gt 1083 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; All non-hydrogen atoms were refined isotropically except for iron and gold atoms that were refined anisotropically. The hydrogen atoms were not localised. 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^)+(0.1274P)^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 2252 _refine_ls_number_parameters 54 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1841 _refine_ls_R_factor_gt 0.0828 _refine_ls_wR_factor_ref 0.2544 _refine_ls_wR_factor_gt 0.2033 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.008 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.26100(7) -0.26125(7) -0.00019(12) 0.0486(4) Uani 1 1 d . . . Fe1 Fe 0.5000 0.0000 -0.5000 0.0237(9) Uani 1 2 d S . . N1 N 0.4059(12) -0.1086(12) -0.306(2) 0.031(4) Uiso 1 1 d . . . C1 C 0.3500(16) -0.1693(16) -0.201(3) 0.040(5) Uiso 1 1 d . . . N2 N 0.5150(12) 0.1098(12) -0.307(2) 0.034(4) Uiso 1 1 d . . . C2 C 0.1665(17) -0.3532(17) 0.198(3) 0.046(6) Uiso 1 1 d . . . N3 N 0.3736(9) 0.0005(10) -0.621(2) 0.039(4) Uiso 1 1 d G . . C7 C 0.2857(12) -0.0853(8) -0.661(3) 0.055(7) Uiso 1 1 d G . . C6 C 0.2060(10) -0.0798(15) -0.734(4) 0.106(11) Uiso 1 1 d GD . . C5 C 0.2142(14) 0.0115(19) -0.767(4) 0.141(16) Uiso 1 1 d G . . C4 C 0.3021(18) 0.0973(14) -0.727(4) 0.140(17) Uiso 1 1 d G . . C3 C 0.3819(12) 0.0918(8) -0.654(3) 0.059(7) Uiso 1 1 d G . . C8 C 0.1094(19) -0.148(4) -0.753(10) 0.24(3) Uiso 1 1 d D . . N4 N 0.0207(16) -0.213(3) -0.773(7) 0.166(16) Uiso 1 1 d D . . O1 O 1.0000 0.0000 0.5000 0.21(5) Uiso 1 6 d S . . O2 O 0.0000 0.0000 -1.0000 0.15(3) Uiso 1 6 d S . . 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 0.0452(7) 0.0449(7) 0.0325(6) 0.0007(4) 0.0004(4) 0.0052(5) Fe1 0.020(2) 0.023(2) 0.029(2) 0.0008(16) 0.0006(15) 0.0113(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 C1 1.99(2) . ? Au1 C2 2.01(2) . ? Fe1 N1 2.091(16) 4_654 ? Fe1 N1 2.091(16) . ? Fe1 N2 2.099(17) . ? Fe1 N2 2.099(17) 4_654 ? Fe1 N3 2.157(12) 4_654 ? Fe1 N3 2.157(12) . ? N1 C1 1.17(2) . ? N2 C2 1.14(3) 6 ? C2 N2 1.14(3) 5 ? N3 C7 1.3900 . ? N3 C3 1.3900 . ? C7 C6 1.3900 . ? C6 C8 1.352(10) . ? C6 C5 1.3900 . ? C5 C4 1.3900 . ? C4 C3 1.3900 . ? C8 N4 1.256(10) . ? 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 Au1 C2 177.5(9) . . ? N1 Fe1 N1 180.0(9) 4_654 . ? N1 Fe1 N2 90.0(6) 4_654 . ? N1 Fe1 N2 90.0(6) . . ? N1 Fe1 N2 90.0(6) 4_654 4_654 ? N1 Fe1 N2 90.0(6) . 4_654 ? N2 Fe1 N2 180.0(10) . 4_654 ? N1 Fe1 N3 88.8(6) 4_654 4_654 ? N1 Fe1 N3 91.2(6) . 4_654 ? N2 Fe1 N3 91.5(6) . 4_654 ? N2 Fe1 N3 88.5(6) 4_654 4_654 ? N1 Fe1 N3 91.2(6) 4_654 . ? N1 Fe1 N3 88.8(6) . . ? N2 Fe1 N3 88.5(6) . . ? N2 Fe1 N3 91.5(6) 4_654 . ? N3 Fe1 N3 180.0 4_654 . ? C1 N1 Fe1 177.3(17) . . ? N1 C1 Au1 173.9(19) . . ? C2 N2 Fe1 177.0(18) 6 . ? N2 C2 Au1 177(2) 5 . ? C7 N3 C3 120.0 . . ? C7 N3 Fe1 122.9(9) . . ? C3 N3 Fe1 117.1(9) . . ? C6 C7 N3 120.0 . . ? C8 C6 C7 132(4) . . ? C8 C6 C5 106(4) . . ? C7 C6 C5 120.0 . . ? C4 C5 C6 120.0 . . ? C5 C4 C3 120.0 . . ? C4 C3 N3 120.0 . . ? N4 C8 C6 178(8) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.001 _refine_diff_density_min -1.212 _refine_diff_density_rms 0.408 #END data_1b,_293K _database_code_depnum_ccdc_archive 'CCDC 243012' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H16 Au4 Fe2 N16' _chemical_formula_weight 1524.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 15.8890(5) _cell_length_b 13.1450(4) _cell_length_c 24.6820(7) _cell_angle_alpha 90.00 _cell_angle_beta 127.4320(10) _cell_angle_gamma 90.00 _cell_volume 4093.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 20 _exptl_crystal_description square _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 15.016 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.604 _exptl_absorpt_correction_T_max 0.776 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16327 _diffrn_reflns_av_R_equivalents 0.0864 _diffrn_reflns_av_sigmaI/netI 0.1299 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.46 _reflns_number_total 9308 _reflns_number_gt 4892 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ;All non hydrogen atoms were refined anisotropically. The hydrogen atoms are refined as riding atoms with a common fixed isotropic thermal parameter. 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^)+(0.0652P)^2^+1.1153P] 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 9308 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1382 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1376 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 0.884 _refine_ls_restrained_S_all 0.884 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.64320(4) 0.27275(4) 0.11413(3) 0.03916(17) Uani 1 1 d . . . Au2 Au 0.11978(4) 0.24694(4) 0.09854(3) 0.03816(16) Uani 1 1 d . . . Au3 Au 0.55069(4) 0.77115(4) 0.03559(3) 0.03773(17) Uani 1 1 d . . . Au4 Au 0.06582(4) 0.74082(4) 0.05657(3) 0.03945(16) Uani 1 1 d . . . Fe2 Fe -0.17156(13) 1.00791(11) 0.06109(10) 0.0263(4) Uani 1 1 d . . . Fe1 Fe 0.35878(13) 0.50841(11) 0.08822(10) 0.0276(5) Uani 1 1 d . . . N1 N 0.4873(8) 0.4098(7) 0.1185(6) 0.046(3) Uani 1 1 d . . . C3 C 0.4778(9) 0.6783(8) 0.0597(6) 0.031(3) Uani 1 1 d . . . N14 N -0.1049(8) 0.9364(7) 0.1631(6) 0.036(3) Uani 1 1 d . . . C1 C 0.5491(10) 0.3604(9) 0.1224(7) 0.038(3) Uani 1 1 d . . . C4 C 0.1708(10) 0.6548(9) 0.0590(7) 0.038(3) Uani 1 1 d . . . N15 N -0.2140(10) 1.0268(12) -0.2212(7) 0.090(5) Uani 1 1 d . . . N12 N -0.3119(8) 0.9151(7) 0.0187(6) 0.041(3) Uani 1 1 d . . . N6 N 0.4455(8) 0.5598(7) 0.1967(6) 0.036(3) Uani 1 1 d . . . C17 C -0.0375(9) 0.8320(8) 0.0529(7) 0.037(3) Uani 1 1 d . . . C20 C -0.3676(10) 0.8622(9) 0.0204(8) 0.044(4) Uani 1 1 d . . . N5 N 0.2667(9) 0.4663(7) -0.0222(6) 0.046(3) Uani 1 1 d . . . C28 C 0.0232(13) 0.8303(13) 0.2556(9) 0.073(5) Uani 1 1 d . . . H28 H 0.0918 0.8044 0.2829 0.063(11) Uiso 1 1 calc R . . N4 N 0.2343(8) 0.6086(7) 0.0637(6) 0.042(3) Uani 1 1 d . . . C30 C -0.1488(11) 0.8470(10) 0.2261(7) 0.047(4) Uani 1 1 d . . . N13 N -0.2521(8) 1.0659(7) -0.0450(6) 0.036(3) Uani 1 1 d . . . N2 N 0.2769(8) 0.3913(7) 0.0991(6) 0.046(3) Uani 1 1 d . . . C18 C 0.0237(10) 1.1535(9) 0.1000(7) 0.041(4) Uani 1 1 d . . . C19 C -0.2704(9) 1.1811(9) 0.1016(7) 0.036(3) Uani 1 1 d . . . C15 C 0.4102(10) 0.5405(8) 0.2323(8) 0.041(4) Uani 1 1 d . . . H15 H 0.3490 0.5017 0.2121 0.063(11) Uiso 1 1 calc R . . C29 C -0.0502(13) 0.8040(11) 0.2674(9) 0.073(5) Uani 1 1 d . . . H29 H -0.0324 0.7589 0.3019 0.063(11) Uiso 1 1 calc R . . C14 C 0.4594(11) 0.5749(9) 0.2972(8) 0.042(4) Uani 1 1 d . . . C31 C -0.1730(10) 0.9130(9) 0.1766(7) 0.037(3) Uani 1 1 d . . . H31 H -0.2395 0.9435 0.1506 0.063(11) Uiso 1 1 calc R . . C25 C -0.2221(11) 1.0439(9) -0.0850(8) 0.043(4) Uani 1 1 d . . . H25 H -0.1614 1.0051 -0.0668 0.063(11) Uiso 1 1 calc R . . C24 C -0.2783(10) 1.0772(9) -0.1513(7) 0.036(3) Uani 1 1 d . . . C9 C 0.1608(13) 0.4491(10) -0.0607(9) 0.061(4) Uani 1 1 d . . . H9 H 0.1272 0.4518 -0.0403 0.063(11) Uiso 1 1 calc R . . C12 C 0.5867(12) 0.6544(10) 0.2908(9) 0.059(5) Uani 1 1 d . . . H12 H 0.6458 0.6955 0.3086 0.063(11) Uiso 1 1 calc R . . N9 N -0.0960(8) 0.8880(7) 0.0475(5) 0.036(3) Uani 1 1 d . . . N3 N 0.4360(8) 0.6233(7) 0.0711(6) 0.043(3) Uani 1 1 d . . . N11 N -0.2312(8) 1.1277(7) 0.0879(6) 0.043(3) Uani 1 1 d . . . C13 C 0.5524(11) 0.6351(9) 0.3286(8) 0.048(4) Uani 1 1 d . . . H13 H 0.5879 0.6601 0.3727 0.063(11) Uiso 1 1 calc R . . C11 C 0.5353(9) 0.6141(9) 0.2273(8) 0.037(3) Uani 1 1 d . . . H11 H 0.5636 0.6246 0.2040 0.063(11) Uiso 1 1 calc R . . C22 C -0.4034(12) 1.1507(9) -0.1425(8) 0.048(4) Uani 1 1 d . . . H22 H -0.4667 1.1853 -0.1616 0.063(11) Uiso 1 1 calc R . . N10 N -0.0356(8) 1.0991(7) 0.0967(6) 0.046(3) Uani 1 1 d . . . C23 C -0.3695(12) 1.1302(10) -0.1793(8) 0.053(4) Uani 1 1 d . . . H23 H -0.4084 1.1524 -0.2243 0.063(11) Uiso 1 1 calc R . . C21 C -0.3428(11) 1.1195(9) -0.0761(8) 0.046(4) Uani 1 1 d . . . H21 H -0.3657 1.1365 -0.0504 0.063(11) Uiso 1 1 calc R . . C5 C 0.3116(13) 0.4656(10) -0.0544(9) 0.061(5) Uani 1 1 d . . . H5 H 0.3838 0.4786 -0.0292 0.063(11) Uiso 1 1 calc R . . C26 C -0.2414(12) 1.0497(12) -0.1900(9) 0.062(5) Uani 1 1 d . . . C8 C 0.1027(15) 0.4278(11) -0.1286(10) 0.064(4) Uani 1 1 d . . . N16 N -0.2993(12) 0.7988(12) 0.2339(8) 0.107(6) Uani 1 1 d . . . C2 C 0.2224(11) 0.3393(9) 0.1009(8) 0.047(4) Uani 1 1 d . . . C27 C -0.0089(11) 0.8954(10) 0.2027(9) 0.054(4) Uani 1 1 d . . . H27 H 0.0391 0.9116 0.1942 0.063(11) Uiso 1 1 calc R . . C16 C 0.4239(11) 0.5448(10) 0.3374(8) 0.049(4) Uani 1 1 d . . . N8 N 0.3983(11) 0.5164(10) 0.3692(7) 0.079(5) Uani 1 1 d . . . C32 C -0.2313(12) 0.8210(13) 0.2324(8) 0.075(5) Uani 1 1 d . . . C6 C 0.2552(18) 0.4467(12) -0.1221(11) 0.082(6) Uani 1 1 d . . . H6 H 0.2895 0.4452 -0.1420 0.063(11) Uiso 1 1 calc R . . C7 C 0.1498(18) 0.4300(12) -0.1609(11) 0.087(6) Uani 1 1 d . . . H7 H 0.1101 0.4202 -0.2078 0.063(11) Uiso 1 1 calc R . . N7 N -0.1001(15) 0.4041(19) -0.1971(12) 0.166(10) Uani 1 1 d . . . C10 C -0.0144(19) 0.4130(17) -0.1686(13) 0.103(7) 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 Au1 0.0356(3) 0.0403(3) 0.0455(4) -0.0060(3) 0.0267(3) 0.0094(2) Au2 0.0330(3) 0.0430(3) 0.0396(4) -0.0018(3) 0.0227(3) -0.0137(2) Au3 0.0373(3) 0.0416(3) 0.0416(4) -0.0011(3) 0.0278(3) -0.0128(2) Au4 0.0355(3) 0.0394(3) 0.0453(4) -0.0002(3) 0.0255(3) 0.0121(2) Fe2 0.0280(10) 0.0244(8) 0.0375(13) 0.0001(8) 0.0256(11) 0.0004(7) Fe1 0.0265(10) 0.0233(8) 0.0429(14) 0.0007(8) 0.0262(11) -0.0001(7) N1 0.044(7) 0.037(6) 0.069(10) 0.002(6) 0.040(8) 0.008(5) C3 0.037(8) 0.040(7) 0.029(9) 0.003(6) 0.027(8) -0.007(6) N14 0.042(7) 0.044(6) 0.039(8) 0.002(5) 0.033(7) 0.001(5) C1 0.034(8) 0.044(7) 0.045(10) -0.003(7) 0.029(8) 0.005(6) C4 0.030(8) 0.034(7) 0.051(11) -0.002(7) 0.025(9) 0.003(6) N15 0.051(9) 0.165(15) 0.058(12) 0.006(10) 0.034(10) 0.011(9) N12 0.028(6) 0.050(6) 0.041(9) -0.004(6) 0.020(7) -0.014(5) N6 0.032(6) 0.041(6) 0.044(8) 0.006(5) 0.028(7) 0.003(5) C17 0.029(7) 0.036(7) 0.039(10) -0.013(6) 0.017(8) 0.009(6) C20 0.036(8) 0.047(8) 0.045(11) -0.011(7) 0.023(9) -0.016(7) N5 0.042(8) 0.036(6) 0.036(9) -0.001(6) 0.011(8) -0.005(6) C28 0.046(11) 0.098(14) 0.065(15) 0.015(11) 0.030(12) 0.015(10) N4 0.040(7) 0.039(6) 0.048(9) 0.000(6) 0.028(8) 0.003(5) C30 0.042(9) 0.070(10) 0.025(10) 0.007(8) 0.019(9) -0.011(8) N13 0.041(7) 0.030(5) 0.050(9) 0.002(5) 0.034(7) -0.001(5) N2 0.046(8) 0.038(6) 0.068(10) 0.001(6) 0.042(8) -0.009(5) C18 0.042(9) 0.045(8) 0.043(11) -0.015(7) 0.029(9) -0.022(7) C19 0.027(7) 0.043(7) 0.042(10) -0.007(7) 0.023(8) 0.006(6) C15 0.043(9) 0.031(7) 0.059(12) -0.008(7) 0.036(10) -0.002(6) C29 0.076(13) 0.062(10) 0.060(14) 0.018(10) 0.030(13) 0.003(10) C14 0.051(10) 0.040(7) 0.055(12) 0.006(7) 0.042(10) 0.005(7) C31 0.027(8) 0.054(8) 0.034(10) 0.005(7) 0.020(8) 0.007(6) C25 0.047(9) 0.047(8) 0.049(11) 0.008(7) 0.035(10) 0.006(7) C24 0.032(8) 0.050(8) 0.023(9) 0.010(7) 0.016(8) -0.001(6) C9 0.064(13) 0.060(10) 0.050(14) 0.012(9) 0.031(12) 0.003(9) C12 0.062(11) 0.059(10) 0.077(15) -0.001(9) 0.053(12) -0.016(8) N9 0.035(7) 0.044(6) 0.025(8) 0.012(5) 0.016(7) 0.026(5) N3 0.043(7) 0.036(6) 0.062(10) -0.001(6) 0.038(8) -0.008(5) N11 0.047(7) 0.039(6) 0.055(9) 0.001(6) 0.036(8) 0.005(5) C13 0.054(10) 0.040(8) 0.051(12) -0.016(7) 0.032(10) -0.008(7) C11 0.018(7) 0.047(8) 0.040(11) 0.002(7) 0.015(8) -0.007(6) C22 0.061(11) 0.044(8) 0.036(11) -0.004(7) 0.028(10) 0.009(7) N10 0.049(8) 0.043(6) 0.056(10) 0.003(6) 0.037(8) -0.002(6) C23 0.063(11) 0.053(9) 0.030(11) 0.016(8) 0.022(10) 0.013(8) C21 0.051(10) 0.033(7) 0.059(13) 0.002(8) 0.036(11) 0.006(7) C5 0.063(12) 0.061(10) 0.064(15) -0.003(9) 0.041(13) -0.001(9) C26 0.045(10) 0.100(12) 0.048(12) 0.003(10) 0.031(10) -0.004(9) C8 0.069(13) 0.062(10) 0.034(12) -0.007(9) 0.018(12) -0.001(9) N16 0.093(13) 0.154(14) 0.083(14) 0.020(11) 0.059(12) -0.048(11) C2 0.047(9) 0.036(7) 0.067(13) -0.004(7) 0.038(10) -0.008(7) C27 0.039(9) 0.066(10) 0.065(13) 0.005(9) 0.037(10) 0.015(8) C16 0.059(10) 0.053(8) 0.045(11) -0.018(7) 0.037(10) -0.007(7) N8 0.081(11) 0.125(12) 0.064(12) -0.019(9) 0.061(11) -0.024(9) C32 0.055(11) 0.127(15) 0.033(12) 0.026(10) 0.022(10) -0.016(10) C6 0.13(2) 0.062(11) 0.069(18) -0.010(11) 0.070(18) -0.014(12) C7 0.127(19) 0.068(12) 0.051(16) -0.018(10) 0.046(17) -0.019(13) N7 0.089(16) 0.22(2) 0.12(2) 0.035(18) 0.025(18) -0.029(18) C10 0.082(17) 0.107(16) 0.08(2) 0.015(14) 0.033(18) -0.009(15) _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 1.987(10) 1_645 ? Au1 C1 1.995(10) . ? Au1 Au3 3.1048(8) 3_665 ? Au2 C18 1.976(11) 1_545 ? Au2 C2 2.005(12) . ? Au2 Au4 3.1072(8) 3_565 ? Au3 C20 1.962(11) 1_655 ? Au3 C3 2.005(10) . ? Au3 Au1 3.1048(8) 3_665 ? Au4 C17 1.990(10) . ? Au4 C4 1.985(11) . ? Au4 Au2 3.1072(8) 3_565 ? Fe2 N9 2.128(8) . ? Fe2 N11 2.140(9) . ? Fe2 N10 2.137(10) . ? Fe2 N12 2.172(9) . ? Fe2 N13 2.237(11) . ? Fe2 N14 2.258(10) . ? Fe1 N1 2.134(9) . ? Fe1 N4 2.135(9) . ? Fe1 N3 2.143(9) . ? Fe1 N2 2.136(9) . ? Fe1 N6 2.245(11) . ? Fe1 N5 2.243(12) . ? N1 C1 1.131(12) . ? C3 N3 1.128(12) . ? N14 C27 1.327(16) . ? N14 C31 1.346(12) . ? C4 N4 1.122(12) . ? N15 C26 1.132(15) . ? N12 C20 1.146(12) . ? N6 C15 1.321(13) . ? N6 C11 1.345(14) . ? C17 N9 1.128(12) . ? C20 Au3 1.962(11) 1_455 ? N5 C9 1.358(17) . ? N5 C5 1.351(16) . ? C28 C27 1.37(2) . ? C28 C29 1.407(18) . ? C28 H28 0.9300 . ? C30 C29 1.368(18) . ? C30 C31 1.351(16) . ? C30 C32 1.451(16) . ? N13 C25 1.364(14) . ? N13 C21 1.348(14) . ? N2 C2 1.124(13) . ? C18 N10 1.147(12) . ? C18 Au2 1.976(11) 1_565 ? C19 N11 1.118(12) . ? C19 Au1 1.987(10) 1_465 ? C15 C14 1.363(18) . ? C15 H15 0.9300 . ? C29 H29 0.9300 . ? C14 C13 1.420(16) . ? C14 C16 1.465(16) . ? C31 H31 0.9300 . ? C25 C24 1.374(18) . ? C25 H25 0.9300 . ? C24 C23 1.358(16) . ? C24 C26 1.437(17) . ? C9 C8 1.36(2) . ? C9 H9 0.9300 . ? C12 C11 1.359(19) . ? C12 C13 1.360(17) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C11 H11 0.9300 . ? C22 C23 1.335(16) . ? C22 C21 1.365(19) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C21 H21 0.9300 . ? C5 C6 1.36(2) . ? C5 H5 0.9300 . ? C8 C10 1.50(2) . ? C8 C7 1.39(2) . ? N16 C32 1.142(15) . ? C27 H27 0.9300 . ? C16 N8 1.142(15) . ? C6 C7 1.35(2) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? N7 C10 1.09(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 C19 Au1 C1 176.7(5) 1_645 . ? C19 Au1 Au3 88.9(4) 1_645 3_665 ? C1 Au1 Au3 88.1(4) . 3_665 ? C18 Au2 C2 177.6(6) 1_545 . ? C18 Au2 Au4 83.6(4) 1_545 3_565 ? C2 Au2 Au4 98.7(4) . 3_565 ? C20 Au3 C3 175.0(6) 1_655 . ? C20 Au3 Au1 100.3(4) 1_655 3_665 ? C3 Au3 Au1 84.6(4) . 3_665 ? C17 Au4 C4 177.6(5) . . ? C17 Au4 Au2 76.9(4) . 3_565 ? C4 Au4 Au2 102.6(4) . 3_565 ? N9 Fe2 N11 172.9(4) . . ? N9 Fe2 N10 87.4(4) . . ? N11 Fe2 N10 89.3(4) . . ? N9 Fe2 N12 91.2(4) . . ? N11 Fe2 N12 92.5(4) . . ? N10 Fe2 N12 176.5(4) . . ? N9 Fe2 N13 92.5(4) . . ? N11 Fe2 N13 93.8(4) . . ? N10 Fe2 N13 90.4(4) . . ? N12 Fe2 N13 86.5(4) . . ? N9 Fe2 N14 86.6(4) . . ? N11 Fe2 N14 87.5(4) . . ? N10 Fe2 N14 95.9(4) . . ? N12 Fe2 N14 87.2(4) . . ? N13 Fe2 N14 173.6(3) . . ? N1 Fe1 N4 176.8(4) . . ? N1 Fe1 N3 87.5(4) . . ? N4 Fe1 N3 93.0(4) . . ? N1 Fe1 N2 92.5(4) . . ? N4 Fe1 N2 87.1(4) . . ? N3 Fe1 N2 176.6(5) . . ? N1 Fe1 N6 90.1(4) . . ? N4 Fe1 N6 86.8(4) . . ? N3 Fe1 N6 90.8(4) . . ? N2 Fe1 N6 92.6(4) . . ? N1 Fe1 N5 93.1(4) . . ? N4 Fe1 N5 90.0(4) . . ? N3 Fe1 N5 87.9(4) . . ? N2 Fe1 N5 88.7(4) . . ? N6 Fe1 N5 176.5(4) . . ? C1 N1 Fe1 167.1(12) . . ? N3 C3 Au3 177.0(11) . . ? C27 N14 C31 117.5(11) . . ? C27 N14 Fe2 122.7(8) . . ? C31 N14 Fe2 117.9(8) . . ? N1 C1 Au1 171.4(13) . . ? N4 C4 Au4 176.2(13) . . ? C20 N12 Fe2 155.8(12) . . ? C15 N6 C11 117.6(12) . . ? C15 N6 Fe1 122.3(9) . . ? C11 N6 Fe1 120.1(8) . . ? N9 C17 Au4 174.9(11) . . ? N12 C20 Au3 172.9(13) . 1_455 ? C9 N5 C5 117.4(14) . . ? C9 N5 Fe1 120.4(10) . . ? C5 N5 Fe1 121.9(11) . . ? C27 C28 C29 118.3(14) . . ? C27 C28 H28 120.9 . . ? C29 C28 H28 120.9 . . ? C4 N4 Fe1 169.5(11) . . ? C29 C30 C31 120.4(12) . . ? C29 C30 C32 121.6(13) . . ? C31 C30 C32 118.0(13) . . ? C25 N13 C21 115.0(12) . . ? C25 N13 Fe2 124.9(9) . . ? C21 N13 Fe2 119.8(8) . . ? C2 N2 Fe1 170.2(10) . . ? N10 C18 Au2 176.0(13) . 1_565 ? N11 C19 Au1 172.8(13) . 1_465 ? N6 C15 C14 123.0(12) . . ? N6 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? C30 C29 C28 117.6(14) . . ? C30 C29 H29 121.2 . . ? C28 C29 H29 121.2 . . ? C15 C14 C13 119.3(11) . . ? C15 C14 C16 121.7(12) . . ? C13 C14 C16 118.8(13) . . ? C30 C31 N14 122.8(12) . . ? C30 C31 H31 118.6 . . ? N14 C31 H31 118.6 . . ? N13 C25 C24 122.3(12) . . ? N13 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? C23 C24 C25 119.3(12) . . ? C23 C24 C26 122.1(13) . . ? C25 C24 C26 118.5(12) . . ? N5 C9 C8 121.3(15) . . ? N5 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C11 C12 C13 120.5(13) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C17 N9 Fe2 165.5(11) . . ? C3 N3 Fe1 174.8(10) . . ? C19 N11 Fe2 171.2(9) . . ? C12 C13 C14 116.5(14) . . ? C12 C13 H13 121.7 . . ? C14 C13 H13 121.7 . . ? N6 C11 C12 122.9(12) . . ? N6 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C23 C22 C21 118.4(14) . . ? C23 C22 H22 120.8 . . ? C21 C22 H22 120.8 . . ? C18 N10 Fe2 163.9(12) . . ? C22 C23 C24 120.3(14) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? N13 C21 C22 124.7(13) . . ? N13 C21 H21 117.7 . . ? C22 C21 H21 117.7 . . ? N5 C5 C6 122.5(16) . . ? N5 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? N15 C26 C24 178.6(18) . . ? C10 C8 C9 118.7(17) . . ? C10 C8 C7 120.8(19) . . ? C9 C8 C7 120.2(17) . . ? N2 C2 Au2 176.9(14) . . ? N14 C27 C28 123.4(12) . . ? N14 C27 H27 118.3 . . ? C28 C27 H27 118.3 . . ? N8 C16 C14 176.4(15) . . ? N16 C32 C30 176.4(19) . . ? C5 C6 C7 120.6(19) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C6 118(2) . . ? C8 C7 H7 121.1 . . ? C6 C7 H7 121.1 . . ? N7 C10 C8 178(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.791 _refine_diff_density_min -1.018 _refine_diff_density_rms 0.271 #END data_1b,_105K _database_code_depnum_ccdc_archive 'CCDC 243013' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H16 Au4 Fe2 N16' _chemical_formula_weight 1524.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 15.7190(7) _cell_length_b 12.7610(5) _cell_length_c 24.2380(8) _cell_angle_alpha 90.00 _cell_angle_beta 127.152(2) _cell_angle_gamma 90.00 _cell_volume 3875.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 20 _exptl_crystal_description square _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 15.862 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13370 _diffrn_reflns_av_R_equivalents 0.0785 _diffrn_reflns_av_sigmaI/netI 0.1082 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.53 _reflns_number_total 8258 _reflns_number_gt 5528 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; All non-hydrogen atoms were refined isotropically except for iron and gold atoms that were refined anisotropically. The hydrogen atoms were not localised. 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^)+(0.1114P)^2^+133.6224P] 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 8258 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1251 _refine_ls_R_factor_gt 0.0762 _refine_ls_wR_factor_ref 0.2200 _refine_ls_wR_factor_gt 0.1896 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Au3 Au 1.04419(6) 0.22851(5) 0.03616(4) 0.0142(2) Uani 1 1 d . . . Au2 Au 0.62882(5) -0.24870(5) 0.09913(4) 0.0145(2) Uani 1 1 d . . . Au1 Au 1.13943(6) 0.72014(5) 0.11455(4) 0.0152(2) Uani 1 1 d . . . Au4 Au 0.56917(6) 0.26364(5) 0.05662(4) 0.0149(2) Uani 1 1 d . . . Fe2 Fe 0.3275(2) -0.00958(19) 0.05991(15) 0.0116(6) Uani 1 1 d . . . Fe1 Fe 0.8589(2) 0.48888(19) 0.08872(15) 0.0127(6) Uani 1 1 d . . . N3 N 0.9258(12) 0.3801(12) 0.0717(9) 0.016(3) Uiso 1 1 d . . . C25 C 0.2817(14) -0.0476(13) -0.0854(10) 0.011(4) Uiso 1 1 d . . . C14 C 0.9551(14) 0.4255(13) 0.2904(10) 0.011(4) Uiso 1 1 d . . . N5 N 0.7712(12) 0.5268(12) -0.0150(9) 0.015(3) Uiso 1 1 d . . . N11 N 0.2706(13) -0.1347(13) 0.0879(10) 0.022(4) Uiso 1 1 d . . . N4 N 0.7469(12) 0.3944(12) 0.0685(9) 0.018(4) Uiso 1 1 d . . . N1 N 0.9745(12) 0.5816(12) 0.1120(9) 0.017(4) Uiso 1 1 d . . . N13 N 0.2462(12) -0.0679(12) -0.0480(9) 0.016(3) Uiso 1 1 d . . . C15 C 0.9016(14) 0.4583(13) 0.2243(10) 0.012(4) Uiso 1 1 d . . . C13 C 1.0530(16) 0.3705(15) 0.3251(12) 0.021(4) Uiso 1 1 d . . . C19 C 0.2292(15) -0.1889(14) 0.1014(11) 0.016(4) Uiso 1 1 d . . . C22 C 0.0926(14) -0.1537(14) -0.1461(11) 0.015(4) Uiso 1 1 d . . . N10 N 0.4669(12) -0.0977(12) 0.0949(9) 0.016(3) Uiso 1 1 d . . . N12 N 0.1845(12) 0.0828(12) 0.0180(9) 0.019(4) Uiso 1 1 d . . . N7 N 0.4028(17) 0.5807(16) -0.1922(12) 0.043(5) Uiso 1 1 d . . . C6 C 0.7657(16) 0.5547(15) -0.1129(12) 0.020(4) Uiso 1 1 d . . . C12 C 1.0927(15) 0.3549(15) 0.2884(12) 0.020(4) Uiso 1 1 d . . . N6 N 0.9418(11) 0.4451(11) 0.1887(8) 0.010(3) Uiso 1 1 d . . . C24 C 0.2206(15) -0.0803(15) -0.1553(11) 0.019(4) Uiso 1 1 d . . . C5 C 0.8241(15) 0.5341(15) -0.0450(11) 0.017(4) Uiso 1 1 d . . . C29 C 0.451(2) 0.2067(19) 0.2683(15) 0.038(6) Uiso 1 1 d . . . C4 C 0.6771(14) 0.3466(13) 0.0612(10) 0.011(4) Uiso 1 1 d . . . C7 C 0.6537(17) 0.5656(17) -0.1564(13) 0.028(5) Uiso 1 1 d . . . C31 C 0.3261(16) 0.0872(15) 0.1781(12) 0.021(4) Uiso 1 1 d . . . N2 N 0.7860(12) 0.5997(11) 0.0988(9) 0.013(3) Uiso 1 1 d . . . C17 C 0.4615(14) 0.1749(13) 0.0518(10) 0.013(4) Uiso 1 1 d . . . C21 C 0.1530(15) -0.1186(14) -0.0784(11) 0.017(4) Uiso 1 1 d . . . C16 C 0.9163(15) 0.4526(14) 0.3321(11) 0.015(4) Uiso 1 1 d . . . C11 C 1.0379(15) 0.3970(14) 0.2238(11) 0.016(4) Uiso 1 1 d . . . C18 C 0.5281(14) -0.1527(14) 0.1002(11) 0.014(4) Uiso 1 1 d . . . N14 N 0.3963(12) 0.0649(12) 0.1625(9) 0.015(3) Uiso 1 1 d . . . C8 C 0.6049(17) 0.5614(17) -0.1223(13) 0.029(5) Uiso 1 1 d . . . N9 N 0.3988(13) 0.1168(12) 0.0453(9) 0.020(4) Uiso 1 1 d . . . C1 C 1.0396(14) 0.6313(13) 0.1194(10) 0.010(4) Uiso 1 1 d . . . C27 C 0.4944(16) 0.1081(15) 0.2029(12) 0.021(4) Uiso 1 1 d . . . C28 C 0.5240(19) 0.1792(19) 0.2545(14) 0.036(6) Uiso 1 1 d . . . N8 N 0.8918(14) 0.4779(13) 0.3656(10) 0.025(4) Uiso 1 1 d . . . C3 C 0.9669(15) 0.3232(14) 0.0583(11) 0.016(4) Uiso 1 1 d . . . N16 N 0.1968(17) 0.2083(16) 0.2312(12) 0.043(5) Uiso 1 1 d . . . C26 C 0.2577(15) -0.0511(15) -0.1974(12) 0.019(4) Uiso 1 1 d . . . C32 C 0.2674(18) 0.1859(17) 0.2314(14) 0.031(5) Uiso 1 1 d . . . C23 C 0.1244(15) -0.1336(14) -0.1860(11) 0.017(4) Uiso 1 1 d . . . N15 N 0.2832(15) -0.0280(15) -0.2307(11) 0.034(5) Uiso 1 1 d . . . C30 C 0.3527(15) 0.1601(15) 0.2258(11) 0.019(4) Uiso 1 1 d . . . C10 C 0.4930(19) 0.5722(18) -0.1613(14) 0.034(6) Uiso 1 1 d . . . C9 C 0.6665(17) 0.5413(16) -0.0499(12) 0.024(5) Uiso 1 1 d . . . C20 C 0.1297(14) 0.1359(13) 0.0225(10) 0.011(4) Uiso 1 1 d . . . C2 C 0.7283(15) 0.6571(15) 0.0999(11) 0.019(4) 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 Au3 0.0140(4) 0.0142(3) 0.0160(5) 0.0001(3) 0.0099(3) 0.0034(3) Au2 0.0126(3) 0.0141(4) 0.0168(5) 0.0004(3) 0.0089(3) 0.0042(3) Au1 0.0131(3) 0.0148(4) 0.0189(5) 0.0017(3) 0.0103(3) -0.0031(3) Au4 0.0133(3) 0.0141(4) 0.0181(5) -0.0005(3) 0.0100(3) -0.0038(3) Fe2 0.0102(12) 0.0120(12) 0.0142(16) 0.0010(11) 0.0083(12) 0.0003(10) Fe1 0.0118(13) 0.0096(12) 0.0192(18) 0.0000(11) 0.0106(13) 0.0003(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au3 C20 1.961(17) 1_655 ? Au3 C3 2.002(19) . ? Au3 Au1 3.0609(11) 3_765 ? Au2 C2 1.964(19) 1_545 ? Au2 C18 2.014(18) . ? Au2 Au4 3.1277(11) 3_655 ? Au1 C19 1.995(18) 1_665 ? Au1 C1 1.995(17) . ? Au1 Au3 3.0609(11) 3_765 ? Au4 C4 1.945(17) . ? Au4 C17 1.979(17) . ? Au4 Au2 3.1277(11) 3_655 ? Fe2 N9 2.112(16) . ? Fe2 N11 2.132(17) . ? Fe2 N10 2.131(15) . ? Fe2 N12 2.173(16) . ? Fe2 N14 2.238(17) . ? Fe2 N13 2.234(18) . ? Fe1 N2 1.927(15) . ? Fe1 N3 1.930(15) . ? Fe1 N4 1.938(15) . ? Fe1 N1 1.945(15) . ? Fe1 N6 2.017(16) . ? Fe1 N5 2.066(17) . ? N3 C3 1.14(2) . ? C25 N13 1.35(2) . ? C25 C24 1.41(3) . ? C14 C15 1.35(3) . ? C14 C13 1.42(2) . ? C14 C16 1.50(3) . ? N5 C9 1.33(2) . ? N5 C5 1.40(2) . ? N11 C19 1.13(2) . ? N4 C4 1.17(2) . ? N1 C1 1.12(2) . ? N13 C21 1.34(2) . ? C15 N6 1.35(2) . ? C13 C12 1.38(3) . ? C19 Au1 1.995(18) 1_445 ? C22 C23 1.35(3) . ? C22 C21 1.38(3) . ? N10 C18 1.13(2) . ? N12 C20 1.15(2) . ? N7 C10 1.14(3) . ? C6 C5 1.34(3) . ? C6 C7 1.41(3) . ? C12 C11 1.36(3) . ? N6 C11 1.35(2) . ? C24 C23 1.40(3) . ? C24 C26 1.49(3) . ? C29 C30 1.37(3) . ? C29 C28 1.42(3) . ? C7 C8 1.43(3) . ? C31 C30 1.34(3) . ? C31 N14 1.40(2) . ? N2 C2 1.18(2) . ? C17 N9 1.17(2) . ? C16 N8 1.14(3) . ? N14 C27 1.35(2) . ? C8 C10 1.41(3) . ? C8 C9 1.43(3) . ? C27 C28 1.38(3) . ? N16 C32 1.14(3) . ? C26 N15 1.13(3) . ? C32 C30 1.46(3) . ? C20 Au3 1.961(17) 1_455 ? C2 Au2 1.964(19) 1_565 ? 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 C20 Au3 C3 175.4(8) 1_655 . ? C20 Au3 Au1 100.1(6) 1_655 3_765 ? C3 Au3 Au1 84.4(6) . 3_765 ? C2 Au2 C18 178.9(9) 1_545 . ? C2 Au2 Au4 100.4(6) 1_545 3_655 ? C18 Au2 Au4 80.6(6) . 3_655 ? C19 Au1 C1 175.2(8) 1_665 . ? C19 Au1 Au3 86.2(6) 1_665 3_765 ? C1 Au1 Au3 89.1(5) . 3_765 ? C4 Au4 C17 178.1(7) . . ? C4 Au4 Au2 107.5(6) . 3_655 ? C17 Au4 Au2 72.6(6) . 3_655 ? N9 Fe2 N11 173.0(7) . . ? N9 Fe2 N10 87.0(6) . . ? N11 Fe2 N10 90.3(6) . . ? N9 Fe2 N12 90.6(6) . . ? N11 Fe2 N12 92.3(6) . . ? N10 Fe2 N12 176.2(7) . . ? N9 Fe2 N14 85.0(6) . . ? N11 Fe2 N14 88.8(6) . . ? N10 Fe2 N14 95.2(6) . . ? N12 Fe2 N14 87.6(6) . . ? N9 Fe2 N13 92.6(6) . . ? N11 Fe2 N13 94.0(6) . . ? N10 Fe2 N13 90.8(6) . . ? N12 Fe2 N13 86.2(6) . . ? N14 Fe2 N13 173.4(6) . . ? N2 Fe1 N3 175.9(7) . . ? N2 Fe1 N4 88.3(6) . . ? N3 Fe1 N4 91.6(6) . . ? N2 Fe1 N1 92.3(6) . . ? N3 Fe1 N1 88.0(6) . . ? N4 Fe1 N1 178.1(8) . . ? N2 Fe1 N6 93.0(7) . . ? N3 Fe1 N6 91.0(7) . . ? N4 Fe1 N6 87.7(7) . . ? N1 Fe1 N6 90.4(7) . . ? N2 Fe1 N5 88.4(7) . . ? N3 Fe1 N5 87.6(7) . . ? N4 Fe1 N5 90.1(7) . . ? N1 Fe1 N5 91.7(7) . . ? N6 Fe1 N5 177.4(6) . . ? C3 N3 Fe1 173.1(16) . . ? N13 C25 C24 119.5(16) . . ? C15 C14 C13 122.3(18) . . ? C15 C14 C16 120.7(16) . . ? C13 C14 C16 116.9(18) . . ? C9 N5 C5 123.7(19) . . ? C9 N5 Fe1 117.7(15) . . ? C5 N5 Fe1 118.6(12) . . ? C19 N11 Fe2 168.7(16) . . ? C4 N4 Fe1 170.9(16) . . ? C1 N1 Fe1 172.8(17) . . ? C21 N13 C25 118.8(18) . . ? C21 N13 Fe2 117.8(13) . . ? C25 N13 Fe2 123.2(12) . . ? N6 C15 C14 121.4(16) . . ? C12 C13 C14 116(2) . . ? N11 C19 Au1 173.1(19) . 1_445 ? C23 C22 C21 120.1(18) . . ? C18 N10 Fe2 166.0(17) . . ? C20 N12 Fe2 153.8(17) . . ? C5 C6 C7 124(2) . . ? C11 C12 C13 117.9(18) . . ? C15 N6 C11 115.4(17) . . ? C15 N6 Fe1 121.3(12) . . ? C11 N6 Fe1 123.2(13) . . ? C23 C24 C25 121.0(19) . . ? C23 C24 C26 120.1(19) . . ? C25 C24 C26 118.8(17) . . ? C6 C5 N5 118.0(17) . . ? C30 C29 C28 115(2) . . ? N4 C4 Au4 175.5(18) . . ? C6 C7 C8 115(2) . . ? C30 C31 N14 119.4(17) . . ? C2 N2 Fe1 169.8(15) . . ? N9 C17 Au4 174.1(17) . . ? N13 C21 C22 123.0(19) . . ? N8 C16 C14 176(2) . . ? N6 C11 C12 126.4(19) . . ? N10 C18 Au2 174.1(19) . . ? C27 N14 C31 117.6(17) . . ? C27 N14 Fe2 123.7(13) . . ? C31 N14 Fe2 117.2(12) . . ? C10 C8 C7 120(2) . . ? C10 C8 C9 119(2) . . ? C7 C8 C9 121(2) . . ? C17 N9 Fe2 162.5(16) . . ? N1 C1 Au1 170.0(18) . . ? N14 C27 C28 122.7(19) . . ? C27 C28 C29 120(2) . . ? N3 C3 Au3 177.4(16) . . ? N15 C26 C24 178(2) . . ? N16 C32 C30 175(3) . . ? C22 C23 C24 117(2) . . ? C31 C30 C29 125(2) . . ? C31 C30 C32 114.2(18) . . ? C29 C30 C32 121(2) . . ? N7 C10 C8 179(3) . . ? N5 C9 C8 118(2) . . ? N12 C20 Au3 176.4(18) . 1_455 ? N2 C2 Au2 178(2) . 1_565 ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 0.856 _refine_diff_density_min -1.414 _refine_diff_density_rms 0.756 #END data_1c,_293K _database_code_depnum_ccdc_archive 'CCDC 243014' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H8 Au2 Fe N8' _chemical_formula_weight 762.09 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' Au Au -2.0133 8.8022 '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' N N 0.0061 0.0033 '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 C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 9.8900(8) _cell_length_b 10.5820(11) _cell_length_c 10.3080(9) _cell_angle_alpha 90.00 _cell_angle_beta 117.910(5) _cell_angle_gamma 90.00 _cell_volume 953.31(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 20 _exptl_crystal_description parallelogram _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.655 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 16.120 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.698 _exptl_absorpt_correction_T_max 0.843 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1867 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.49 _reflns_number_total 1867 _reflns_number_gt 1619 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ;The 3-cyanopyridine ligand is disordered and it has been modelled in two different positions with 0.5 occupancy factor. Refinement in the higher symmetry space group was attempted but was not posible. All non-hydrogen atoms were refined isotropically except for iron and gold atoms that were refined anisotropically. The hydrogen atoms were not localised. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+12.0692P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.15(9) _refine_ls_number_reflns 1867 _refine_ls_number_parameters 72 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0718 _refine_ls_wR_factor_gt 0.0662 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.920 _refine_ls_shift/su_max 0.118 _refine_ls_shift/su_mean 0.091 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 0.0000 0.2117(3) 0.0000 0.03821(12) Uani 1 2 d S . . Au2 Au 0.5000 -0.28809(16) 0.5000 0.03647(12) Uani 1 2 d S . . Fe3 Fe 0.5000 0.2131(10) 0.5000 0.0265(3) Uani 1 2 d S . . N2 N 0.2703(6) 0.2033(18) 0.3197(6) 0.0372(16) Uiso 1 1 d . A . N1 N 0.5000 0.007(4) 0.5000 0.055(12) Uiso 1 2 d SD A . C2 C 0.1691(7) 0.205(2) 0.2062(7) 0.0374(18) Uiso 1 1 d . . . N3 N 0.5000 0.416(3) 0.5000 0.048(9) Uiso 1 2 d S A . C3 C 0.5000 0.527(3) 0.5000 0.042(8) Uiso 1 2 d S . . C1 C 0.5000 -0.097(4) 0.5000 0.058(12) Uiso 1 2 d SD . . N4 N 0.572(2) 0.2326(16) 0.3269(17) 0.027(5) Uiso 0.50 1 d PG A 2 C4 C 0.627(2) 0.1289(13) 0.283(2) 0.030(6) Uiso 0.50 1 d PG A 2 C5 C 0.6740(19) 0.1431(15) 0.1762(19) 0.028(5) Uiso 0.50 1 d PGD A 2 C6 C 0.666(2) 0.2609(18) 0.1134(17) 0.041(6) Uiso 0.50 1 d PG A 2 C7 C 0.611(2) 0.3645(14) 0.157(2) 0.056(8) Uiso 0.50 1 d PG A 2 C8 C 0.564(2) 0.3503(14) 0.264(2) 0.048(8) Uiso 0.50 1 d PG A 2 C9 C 0.730(4) 0.045(3) 0.130(5) 0.073(13) Uiso 0.50 1 d PD A 2 N5 N 0.772(3) -0.0423(19) 0.084(3) 0.054(6) Uiso 0.50 1 d PD A 2 N4A N 0.589(2) 0.1901(17) 0.3301(18) 0.033(6) Uiso 0.50 1 d PG A 1 C5A C 0.588(2) 0.0713(14) 0.272(2) 0.035(6) Uiso 0.50 1 d PG A 1 C4A C 0.641(2) 0.0561(13) 0.1697(19) 0.038(5) Uiso 0.50 1 d PG A 1 C6A C 0.6963(19) 0.1597(17) 0.1260(18) 0.035(5) Uiso 0.50 1 d PG A 1 C7A C 0.698(2) 0.2785(14) 0.184(2) 0.037(7) Uiso 0.50 1 d PGD A 1 C8A C 0.645(2) 0.2937(13) 0.286(2) 0.042(8) Uiso 0.50 1 d PG A 1 C9A C 0.752(3) 0.3808(18) 0.143(3) 0.031(5) Uiso 0.50 1 d PD A 1 N5A N 0.818(3) 0.4613(19) 0.114(3) 0.053(6) Uiso 0.50 1 d PD A 1 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 0.03019(18) 0.0398(2) 0.03195(19) 0.000 0.00393(13) 0.000 Au2 0.04004(19) 0.02066(19) 0.0421(2) 0.000 0.01374(15) 0.000 Fe3 0.0290(5) 0.0207(6) 0.0248(5) 0.000 0.0084(4) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C2 1.997(6) . ? Au1 C2 1.997(6) 2 ? Au2 C3 1.96(4) 1_545 ? Au2 C1 2.02(5) . ? Fe3 N1 2.18(4) . ? Fe3 N2 2.162(5) 2_656 ? Fe3 N2 2.162(5) . ? Fe3 N3 2.14(3) . ? Fe3 N4 2.219(12) 2_656 ? Fe3 N4 2.219(12) . ? Fe3 N4A 2.315(12) . ? Fe3 N4A 2.315(12) 2_656 ? N2 C2 1.129(8) . ? N1 C1 1.103(10) . ? N3 C3 1.18(2) . ? C3 Au2 1.96(4) 1_565 ? N4 C4 1.3900 . ? N4 C8 1.3900 . ? C4 C5 1.3900 . ? C5 C9 1.358(9) . ? C5 C6 1.3900 . ? C6 C7 1.3900 . ? C7 C8 1.3900 . ? C9 N5 1.201(9) . ? N4A C5A 1.3900 . ? N4A C8A 1.3900 . ? C5A C4A 1.3900 . ? C4A C6A 1.3900 . ? C6A C7A 1.3900 . ? C7A C9A 1.361(9) . ? C7A C8A 1.3900 . ? C9A N5A 1.195(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Au1 C2 176.1(15) . 2 ? C3 Au2 C1 180.000(4) 1_545 . ? N1 Fe3 N2 87.2(5) . 2_656 ? N1 Fe3 N2 87.2(5) . . ? N2 Fe3 N2 174.5(10) 2_656 . ? N1 Fe3 N3 180.000(7) . . ? N2 Fe3 N3 92.8(5) 2_656 . ? N2 Fe3 N3 92.8(5) . . ? N1 Fe3 N4 95.3(5) . 2_656 ? N2 Fe3 N4 85.2(5) 2_656 2_656 ? N2 Fe3 N4 95.3(5) . 2_656 ? N3 Fe3 N4 84.7(5) . 2_656 ? N1 Fe3 N4 95.3(5) . . ? N2 Fe3 N4 95.3(5) 2_656 . ? N2 Fe3 N4 85.2(5) . . ? N3 Fe3 N4 84.7(5) . . ? N4 Fe3 N4 169.4(9) 2_656 . ? N1 Fe3 N4A 84.0(4) . . ? N2 Fe3 N4A 91.5(5) 2_656 . ? N2 Fe3 N4A 88.0(5) . . ? N3 Fe3 N4A 96.0(4) . . ? N4 Fe3 N4A 176.6(9) 2_656 . ? N4 Fe3 N4A 11.8(4) . . ? N1 Fe3 N4A 84.0(4) . 2_656 ? N2 Fe3 N4A 88.0(5) 2_656 2_656 ? N2 Fe3 N4A 91.5(5) . 2_656 ? N3 Fe3 N4A 96.0(4) . 2_656 ? N4 Fe3 N4A 11.8(4) 2_656 2_656 ? N4 Fe3 N4A 176.6(9) . 2_656 ? N4A Fe3 N4A 167.9(9) . 2_656 ? C2 N2 Fe3 162.7(7) . . ? C1 N1 Fe3 180.000(4) . . ? N2 C2 Au1 176.1(8) . . ? C3 N3 Fe3 180.000(7) . . ? N3 C3 Au2 180.000(5) . 1_565 ? N1 C1 Au2 180.000(4) . . ? C4 N4 C8 120.0 . . ? C4 N4 Fe3 120.7(9) . . ? C8 N4 Fe3 119.3(9) . . ? C5 C4 N4 120.0 . . ? C9 C5 C4 122(2) . . ? C9 C5 C6 118(2) . . ? C4 C5 C6 120.0 . . ? C7 C6 C5 120.0 . . ? C8 C7 C6 120.0 . . ? C7 C8 N4 120.0 . . ? N5 C9 C5 177(4) . . ? C5A N4A C8A 120.0 . . ? C5A N4A Fe3 119.4(9) . . ? C8A N4A Fe3 120.6(9) . . ? N4A C5A C4A 120.0 . . ? C6A C4A C5A 120.0 . . ? C4A C6A C7A 120.0 . . ? C9A C7A C8A 119.2(15) . . ? C9A C7A C6A 120.8(15) . . ? C8A C7A C6A 120.0 . . ? C7A C8A N4A 120.0 . . ? N5A C9A C7A 171(3) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.158 _refine_diff_density_min -1.224 _refine_diff_density_rms 0.160 #END