Electronic Supplementary Material for Chemical Communications This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Jose Real' _publ_contact_author_address ; Department de Quimica Inorganica Universitat de Valencia Institut de Ciencia Molecular Edificio de Institutos de Paterna, P. O. Box 22085 Valencia 46071 SPAIN ; _publ_contact_author_email JOSE.A.REAL@UV.ES _publ_section_title ; Coordination polymers undergoing spin crossover and reversible ligand exchange in the solid ; loop_ _publ_author_name 'Ana Galet' 'M. Carmen Munoz' 'Jose A. Real' # Attachment 'compound 2.CIF' ################################################################ #Supramolecular isomerism in spin crossover networks with aurophillic #interactions #Ana Galeta, M. Carmen Mu\~noza, V\'ictor Mart\'inezb and Jos\'e Antonio Realb #aDepartament de F\'isica Aplicada, Universitat Polit\'ecnica de Val\`encia, #Camino de Vera s/n, 46071, Valencia, Spain; E-mail: mcmunoz@fis.upv.es #bInstitut de Ciencia Molecular/Departament de Qu\'imica Inorg\'anica, #Universitat de Val\`encia, Doctor Moliner 50, Burjassot, Spain. #Tel: 34 963544856; #E-mail: jose.a.real@uv.es ################################################################ data_1a_at_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_at_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_Compound1 _database_code_depnum_ccdc_archive 'CCDC 297493' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H16 Au3 Fe1.50 N12 O' _chemical_formula_weight 1175.17 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.240(3) _cell_length_b 14.790(4) _cell_length_c 14.532(6) _cell_angle_alpha 112.694(11) _cell_angle_beta 95.567(13) _cell_angle_gamma 97.10(2) _cell_volume 1601.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 14.404 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 3419 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0668 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 20.53 _reflns_number_total 2334 _reflns_number_gt 1860 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement 'HKL DENZO' _computing_data_reduction 'HKL DENZO and SCALEPACK' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+369.2444P] 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 2334 _refine_ls_number_parameters 169 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1392 _refine_ls_R_factor_gt 0.0959 _refine_ls_wR_factor_ref 0.2690 _refine_ls_wR_factor_gt 0.2124 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.135 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.001 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 Fe1 Fe 0.5000 0.5000 1.0000 0.063(4) Uani 1 2 d S . . Fe2 Fe -0.5000 0.0000 1.0000 0.054(3) Uani 1 2 d S . . Fe3 Fe -1.5000 0.0000 0.5000 0.064(4) Uani 1 2 d S . . Au1 Au 0.0036(3) 0.2277(2) 0.9616(2) 0.0729(11) Uani 1 1 d . . . Au2 Au 0.1043(4) 0.7065(2) 1.2259(2) 0.0859(12) Uani 1 1 d . . . Au3 Au -1.0095(3) 0.0096(2) 0.7607(2) 0.0719(11) Uani 1 1 d . . . O1 O -1.589(6) 0.098(4) 0.624(3) 0.089(15) Uani 1 1 d . E . N1 N 0.322(7) 0.376(4) 0.985(4) 0.070(16) Uiso 1 1 d . A . N2 N 0.371(7) 0.599(4) 1.107(4) 0.082(18) Uiso 1 1 d . A . N4 N -0.144(5) 0.817(3) 1.342(3) 0.044(12) Uiso 1 1 d D A . N5 N 0.314(12) 0.360(6) 0.522(4) 0.17(4) Uiso 1 1 d D . . N6 N -0.323(8) 0.095(5) 0.971(4) 0.086(18) Uiso 1 1 d . B . N7 N -0.705(7) 0.020(4) 0.906(4) 0.074(17) Uiso 1 1 d . C . N9 N -1.003(5) 0.261(5) 1.254(5) 0.11(2) Uiso 1 1 d D . . N10 N -1.294(7) -0.025(4) 0.592(4) 0.074(17) Uiso 1 1 d . C . N12 N -1.334(13) 0.475(5) 0.623(7) 0.19(4) Uiso 1 1 d D . . C1 C 0.224(7) 0.314(4) 0.978(4) 0.047(16) Uiso 1 1 d . A . C2 C 0.245(9) 0.636(5) 1.155(6) 0.08(2) Uiso 1 1 d . . . C3 C -0.081(4) 0.760(3) 1.281(3) 0.000(9) Uiso 1 1 d D . . N3 N 0.330(5) 0.508(3) 0.870(3) 0.083(18) Uiso 1 1 d G A 1 C4 C 0.194(6) 0.554(4) 0.893(3) 0.10(3) Uiso 1 1 d G A 1 H4 H 0.1758 0.5828 0.9593 0.120 Uiso 1 1 calc R A 1 C5 C 0.084(5) 0.557(4) 0.816(4) 0.14(4) Uiso 1 1 d G A 1 H5 H -0.0078 0.5881 0.8307 0.166 Uiso 1 1 calc R A 1 C6 C 0.110(6) 0.514(4) 0.716(4) 0.10(3) Uiso 1 1 d G A 1 H6 H 0.0366 0.5160 0.6645 0.124 Uiso 1 1 calc R A 1 C7 C 0.247(7) 0.468(4) 0.694(3) 0.11(3) Uiso 1 1 d GD A 1 C8 C 0.357(5) 0.464(3) 0.771(4) 0.08(2) Uiso 1 1 d G A 1 H8 H 0.4481 0.4333 0.7556 0.090 Uiso 1 1 calc R A 1 C9 C 0.284(11) 0.409(6) 0.604(4) 0.12(3) Uiso 1 1 d D A 1 C10 C -0.206(7) 0.137(4) 0.962(4) 0.042(15) Uiso 1 1 d . B 1 C11 C -0.816(8) 0.017(5) 0.859(5) 0.059(18) Uiso 1 1 d . C 1 N8 N -0.532(5) 0.134(2) 1.134(3) 0.068(16) Uiso 1 1 d G D 2 C12 C -0.392(4) 0.200(3) 1.197(3) 0.063(19) Uiso 1 1 d G D 2 H12 H -0.2873 0.1873 1.1837 0.075 Uiso 1 1 calc R D 2 C13 C -0.410(4) 0.284(3) 1.280(3) 0.10(3) Uiso 1 1 d G D 2 H13 H -0.3167 0.3273 1.3218 0.118 Uiso 1 1 calc R D 2 C14 C -0.567(5) 0.302(3) 1.299(3) 0.08(2) Uiso 1 1 d G D 2 H14 H -0.5789 0.3581 1.3548 0.092 Uiso 1 1 calc R D 2 C15 C -0.707(4) 0.237(3) 1.237(3) 0.056(17) Uiso 1 1 d GD D 2 C16 C -0.689(4) 0.153(3) 1.154(3) 0.09(2) Uiso 1 1 d G D 2 H16 H -0.7824 0.1088 1.1118 0.105 Uiso 1 1 calc R D 2 C17 C -0.862(4) 0.256(4) 1.242(5) 0.058(18) Uiso 1 1 d D D 2 C18 C -1.189(6) -0.003(4) 0.666(4) 0.033(13) Uiso 1 1 d . C 2 N11 N -1.337(5) 0.128(3) 0.494(3) 0.079(17) Uiso 1 1 d G E 3 C19 C -1.189(5) 0.113(3) 0.457(3) 0.09(3) Uiso 1 1 d G E 3 H19 H -1.1625 0.0492 0.4332 0.114 Uiso 1 1 calc R E 3 C20 C -1.080(4) 0.192(4) 0.456(3) 0.07(2) Uiso 1 1 d G E 3 H20 H -0.9810 0.1817 0.4319 0.085 Uiso 1 1 calc R E 3 C21 C -1.120(5) 0.287(3) 0.492(4) 0.09(2) Uiso 1 1 d G E 3 H21 H -1.0472 0.3401 0.4917 0.105 Uiso 1 1 calc R E 3 C22 C -1.268(6) 0.303(3) 0.529(4) 0.11(3) Uiso 1 1 d GD E 3 C23 C -1.377(4) 0.223(3) 0.530(3) 0.062(19) Uiso 1 1 d G E 3 H23 H -1.4763 0.2337 0.5542 0.074 Uiso 1 1 calc R E 3 C24 C -1.298(16) 0.397(4) 0.572(9) 0.17(5) Uiso 1 1 d D E 3 C25 C -1.511(10) 0.120(6) 0.730(6) 0.10(3) Uiso 1 1 d . E 3 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 Fe1 0.044(8) 0.055(9) 0.076(10) 0.012(8) 0.010(7) 0.001(6) Fe2 0.044(8) 0.054(9) 0.054(8) 0.017(7) -0.001(6) 0.000(6) Fe3 0.049(8) 0.080(10) 0.059(9) 0.023(8) 0.001(7) 0.022(7) Au1 0.0527(18) 0.068(2) 0.094(2) 0.0331(17) 0.0105(15) -0.0034(14) Au2 0.078(2) 0.089(3) 0.083(2) 0.0227(19) 0.0184(17) 0.0264(18) Au3 0.0542(19) 0.089(2) 0.070(2) 0.0294(17) -0.0011(14) 0.0191(16) O1 0.11(4) 0.08(4) 0.06(3) 0.01(3) 0.01(3) 0.02(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 Fe1 N1 2.13(6) . ? Fe1 N1 2.13(6) 2_667 ? Fe1 N2 2.16(6) . ? Fe1 N2 2.16(6) 2_667 ? Fe1 N3 2.28(4) . ? Fe1 N3 2.28(4) 2_667 ? Fe2 N6 2.09(7) 2_457 ? Fe2 N6 2.09(7) . ? Fe2 N7 2.19(6) . ? Fe2 N7 2.19(6) 2_457 ? Fe2 N8 2.25(3) . ? Fe2 N8 2.25(3) 2_457 ? Fe3 O1 2.10(4) 2_256 ? Fe3 O1 2.10(5) . ? Fe3 N10 2.21(6) . ? Fe3 N10 2.21(6) 2_256 ? Fe3 N11 2.22(3) 2_256 ? Fe3 N11 2.22(3) . ? Au1 C1 2.02(6) . ? Au1 C10 2.05(6) . ? Au1 Au2 3.309(5) 2_567 ? Au2 C2 1.78(8) . ? Au2 C3 1.91(3) . ? Au2 Au1 3.309(5) 2_567 ? Au3 C18 1.86(5) . ? Au3 C11 2.00(7) . ? O1 C25 1.51(9) . ? N1 C1 1.11(7) . ? N2 C2 1.36(8) . ? N4 C3 1.183(10) . ? N5 C9 1.199(10) . ? N6 C10 1.13(7) . ? N7 C11 1.07(7) . ? N9 C17 1.199(10) . ? N10 C18 1.22(6) . ? N12 C24 1.201(10) . ? N3 C4 1.3900 . ? N3 C8 1.3900 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 C6 1.3900 . ? C5 H5 0.9300 . ? C6 C7 1.3900 . ? C6 H6 0.9300 . ? C7 C9 1.350(10) . ? C7 C8 1.3900 . ? C8 H8 0.9300 . ? N8 C12 1.3900 . ? N8 C16 1.3900 . ? C12 C13 1.3900 . ? C12 H12 0.9300 . ? C13 C14 1.3900 . ? C13 H13 0.9300 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 C17 1.350(10) . ? C15 C16 1.3900 . ? C16 H16 0.9300 . ? N11 C19 1.3900 . ? N11 C23 1.3900 . ? C19 C20 1.3900 . ? C19 H19 0.9300 . ? C20 C21 1.3900 . ? C20 H20 0.9300 . ? C21 C22 1.3900 . ? C21 H21 0.9300 . ? C22 C24 1.352(10) . ? C22 C23 1.3900 . ? C23 H23 0.9300 . ? 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 Fe1 N1 180.000(7) . 2_667 ? N1 Fe1 N2 90(2) . . ? N1 Fe1 N2 90(2) 2_667 . ? N1 Fe1 N2 90(2) . 2_667 ? N1 Fe1 N2 90(2) 2_667 2_667 ? N2 Fe1 N2 180(3) . 2_667 ? N1 Fe1 N3 86.2(18) . . ? N1 Fe1 N3 93.8(18) 2_667 . ? N2 Fe1 N3 90(2) . . ? N2 Fe1 N3 90(2) 2_667 . ? N1 Fe1 N3 93.8(18) . 2_667 ? N1 Fe1 N3 86.2(18) 2_667 2_667 ? N2 Fe1 N3 90(2) . 2_667 ? N2 Fe1 N3 90(2) 2_667 2_667 ? N3 Fe1 N3 180.0 . 2_667 ? N6 Fe2 N6 180.000(8) 2_457 . ? N6 Fe2 N7 86(2) 2_457 . ? N6 Fe2 N7 94(2) . . ? N6 Fe2 N7 94(2) 2_457 2_457 ? N6 Fe2 N7 86(2) . 2_457 ? N7 Fe2 N7 180.000(15) . 2_457 ? N6 Fe2 N8 93.0(19) 2_457 . ? N6 Fe2 N8 87.0(19) . . ? N7 Fe2 N8 91.2(17) . . ? N7 Fe2 N8 88.8(17) 2_457 . ? N6 Fe2 N8 87.0(19) 2_457 2_457 ? N6 Fe2 N8 93.0(19) . 2_457 ? N7 Fe2 N8 88.8(17) . 2_457 ? N7 Fe2 N8 91.2(17) 2_457 2_457 ? N8 Fe2 N8 180.0 . 2_457 ? O1 Fe3 O1 180.000(11) 2_256 . ? O1 Fe3 N10 85.1(19) 2_256 . ? O1 Fe3 N10 94.9(19) . . ? O1 Fe3 N10 94.9(19) 2_256 2_256 ? O1 Fe3 N10 85.1(19) . 2_256 ? N10 Fe3 N10 180.000(6) . 2_256 ? O1 Fe3 N11 89.7(18) 2_256 2_256 ? O1 Fe3 N11 90.3(18) . 2_256 ? N10 Fe3 N11 89.7(18) . 2_256 ? N10 Fe3 N11 90.3(18) 2_256 2_256 ? O1 Fe3 N11 90.3(18) 2_256 . ? O1 Fe3 N11 89.7(18) . . ? N10 Fe3 N11 90.3(18) . . ? N10 Fe3 N11 89.7(18) 2_256 . ? N11 Fe3 N11 180.0(13) 2_256 . ? C1 Au1 C10 172(2) . . ? C1 Au1 Au2 84.4(16) . 2_567 ? C10 Au1 Au2 103.7(15) . 2_567 ? C2 Au2 C3 168(3) . . ? C2 Au2 Au1 90(2) . 2_567 ? C3 Au2 Au1 86.2(11) . 2_567 ? C18 Au3 C11 177(2) . . ? C25 O1 Fe3 121(4) . . ? C1 N1 Fe1 176(5) . . ? C2 N2 Fe1 160(5) . . ? C10 N6 Fe2 166(6) . . ? C11 N7 Fe2 169(6) . . ? C18 N10 Fe3 156(5) . . ? N1 C1 Au1 164(6) . . ? N2 C2 Au2 169(6) . . ? N4 C3 Au2 154(4) . . ? C4 N3 C8 120.0 . . ? C4 N3 Fe1 118(3) . . ? C8 N3 Fe1 122(3) . . ? C5 C4 N3 120.0 . . ? C5 C4 H4 120.0 . . ? N3 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C7 120.0 . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C9 C7 C6 130(6) . . ? C9 C7 C8 109(6) . . ? C6 C7 C8 120.0 . . ? C7 C8 N3 120.0 . . ? C7 C8 H8 120.0 . . ? N3 C8 H8 120.0 . . ? N5 C9 C7 178(10) . . ? N6 C10 Au1 173(6) . . ? N7 C11 Au3 174(6) . . ? C12 N8 C16 120.0 . . ? C12 N8 Fe2 119(2) . . ? C16 N8 Fe2 121(2) . . ? C13 C12 N8 120.0 . . ? C13 C12 H12 120.0 . . ? N8 C12 H12 120.0 . . ? C12 C13 C14 120.00(8) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C17 C15 C14 124(4) . . ? C17 C15 C16 116(4) . . ? C14 C15 C16 120.0 . . ? C15 C16 N8 120.00(7) . . ? C15 C16 H16 120.0 . . ? N8 C16 H16 120.0 . . ? N9 C17 C15 168(7) . . ? N10 C18 Au3 168(5) . . ? C19 N11 C23 120.0 . . ? C19 N11 Fe3 118(2) . . ? C23 N11 Fe3 122(2) . . ? C20 C19 N11 120.0 . . ? C20 C19 H19 120.0 . . ? N11 C19 H19 120.0 . . ? C21 C20 C19 120.0 . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C24 C22 C23 121(7) . . ? C24 C22 C21 119(7) . . ? C23 C22 C21 120.0 . . ? C22 C23 N11 120.0 . . ? C22 C23 H23 120.0 . . ? N11 C23 H23 120.0 . . ? N12 C24 C22 168(10) . . ? _diffrn_measured_fraction_theta_max 0.724 _diffrn_reflns_theta_full 20.53 _diffrn_measured_fraction_theta_full 0.724 _refine_diff_density_max 1.594 _refine_diff_density_min -1.620 _refine_diff_density_rms 0.340