Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Grepioni, Fabrizia' 'Bracaccini, Marco' 'Braga, Dario' _publ_contact_author_name 'Prof Fabrizia Grepioni' _publ_contact_author_address ; Prof Fabrizia Grepioni Department of Chemistry University of Sassari Via Vienna 2 Sassari 07100 ITALY ; _publ_contact_author_email 'GREPIONI@SSMAIN.UNISS.I' _publ_section_title ; Novel Hetero-Bimetallic Metalla-Macrocycles Based on the Bis-1-Pyridyl Ferrocene [Fe(eta5-C5H4-1-C5H4N)2] Ligand. Design, Synthesis and Structural Characterization of the Complexes [Fe(eta5-C5H4-1-C5H4N)2](Ag I)2 2+/(Cu II)2 4+/ (Zn II)2 4+. ; data_1zn _database_code_CSD 177935 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H32 Cl4 Fe2 N4 Zn2' _chemical_formula_weight 952.94 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 18.1586(8) _cell_length_b 14.4554(6) _cell_length_c 14.44580(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3791.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description red _exptl_crystal_colour prism _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 2.318 _exptl_absorpt_correction_type 'Bruker Smart' _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 1.00 _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 'Bruker Smart CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26764 _diffrn_reflns_av_R_equivalents 0.1518 _diffrn_reflns_av_sigmaI/netI 0.0821 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 23.01 _reflns_number_total 2630 _reflns_number_gt 1984 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+19.5532P] 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 2630 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1202 _refine_ls_R_factor_gt 0.0897 _refine_ls_wR_factor_ref 0.1710 _refine_ls_wR_factor_gt 0.1586 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.170 _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 Zn1 Zn 0.21531(7) 0.04279(9) -0.04589(9) 0.0471(4) Uani 1 1 d . . . Fe1 Fe 0.57060(8) 0.17163(10) 0.22232(10) 0.0379(4) Uani 1 1 d . . . Cl1 Cl 0.20450(19) 0.1083(3) -0.1829(2) 0.0894(13) Uani 1 1 d . . . Cl2 Cl 0.17732(17) -0.1027(2) -0.0306(3) 0.0786(11) Uani 1 1 d . . . N1 N 0.3179(4) 0.0628(6) 0.0070(6) 0.041(2) Uani 1 1 d . . . N2 N 0.1477(5) 0.1089(6) 0.0468(6) 0.048(2) Uani 1 1 d . . . C1 C 0.5359(3) 0.0898(5) 0.1156(5) 0.037(3) Uani 1 1 d G . . C2 C 0.5647(5) 0.0341(5) 0.1881(5) 0.066(4) Uani 1 1 d G . . H2 H 0.5393 -0.0117 0.2201 0.080 Uiso 1 1 calc R . . C3 C 0.6391(5) 0.0605(6) 0.2029(6) 0.078(5) Uani 1 1 d G . . H3 H 0.6709 0.0351 0.2464 0.093 Uiso 1 1 calc R . . C4 C 0.6563(3) 0.1326(7) 0.1397(7) 0.071(4) Uani 1 1 d G . . H4 H 0.7014 0.1626 0.1346 0.085 Uiso 1 1 calc R . . C5 C 0.5925(4) 0.1507(5) 0.0858(5) 0.050(3) Uani 1 1 d G . . H5 H 0.5885 0.1947 0.0391 0.060 Uiso 1 1 calc R . . C6 C 0.4606(6) 0.0821(7) 0.0801(7) 0.037(3) Uani 1 1 d . . . C7 C 0.4096(6) 0.0208(8) 0.1164(8) 0.056(3) Uani 1 1 d . . . H7 H 0.4228 -0.0161 0.1665 0.067 Uiso 1 1 calc R . . C8 C 0.3408(6) 0.0134(8) 0.0805(8) 0.053(3) Uani 1 1 d . . . H8 H 0.3080 -0.0277 0.1080 0.064 Uiso 1 1 calc R . . C9 C 0.3663(6) 0.1232(8) -0.0281(7) 0.049(3) Uani 1 1 d . . . H9 H 0.3515 0.1599 -0.0776 0.058 Uiso 1 1 calc R . . C10 C 0.4361(6) 0.1341(7) 0.0045(7) 0.048(3) Uani 1 1 d . . . H10 H 0.4676 0.1763 -0.0235 0.057 Uiso 1 1 calc R . . C11 C -0.0037(4) 0.2186(5) 0.2445(4) 0.044(3) Uani 1 1 d G . . C12 C 0.0114(3) 0.2880(5) 0.3114(5) 0.046(3) Uani 1 1 d G . . H12 H 0.0565 0.3171 0.3206 0.055 Uiso 1 1 calc R . . C13 C -0.0543(4) 0.3053(5) 0.3616(4) 0.062(4) Uani 1 1 d G . . H13 H -0.0599 0.3477 0.4095 0.074 Uiso 1 1 calc R . . C14 C -0.1102(3) 0.2466(6) 0.3258(5) 0.058(3) Uani 1 1 d G . . H14 H -0.1587 0.2437 0.3462 0.069 Uiso 1 1 calc R . . C15 C -0.0789(4) 0.1930(5) 0.2535(5) 0.047(3) Uani 1 1 d G . . H15 H -0.1033 0.1488 0.2181 0.057 Uiso 1 1 calc R . . C16 C 0.0484(5) 0.1814(7) 0.1759(7) 0.039(3) Uani 1 1 d . . . C17 C 0.1241(6) 0.1953(7) 0.1838(8) 0.047(3) Uani 1 1 d . . . H17 H 0.1431 0.2299 0.2326 0.056 Uiso 1 1 calc R . . C18 C 0.1700(6) 0.1578(7) 0.1195(7) 0.047(3) Uani 1 1 d . . . H18 H 0.2204 0.1670 0.1270 0.057 Uiso 1 1 calc R . . C19 C 0.0745(6) 0.0962(8) 0.0388(8) 0.058(3) Uani 1 1 d . . . H19 H 0.0571 0.0620 -0.0111 0.069 Uiso 1 1 calc R . . C20 C 0.0249(6) 0.1309(8) 0.0999(8) 0.050(3) Uani 1 1 d . . . H20 H -0.0251 0.1207 0.0906 0.059 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 Zn1 0.0359(7) 0.0581(8) 0.0472(7) -0.0107(7) 0.0039(6) -0.0010(7) Fe1 0.0353(8) 0.0410(9) 0.0375(8) -0.0055(7) -0.0025(7) 0.0082(7) Cl1 0.070(2) 0.141(4) 0.057(2) 0.026(2) 0.0021(18) 0.029(2) Cl2 0.0557(19) 0.063(2) 0.117(3) -0.024(2) 0.035(2) -0.0163(17) N1 0.032(5) 0.046(6) 0.045(5) -0.008(5) 0.003(4) -0.004(4) N2 0.038(5) 0.059(6) 0.046(6) -0.015(5) 0.009(5) 0.007(5) C1 0.048(7) 0.026(6) 0.037(6) -0.015(5) -0.002(5) 0.000(5) C2 0.074(9) 0.028(6) 0.097(10) -0.004(7) -0.029(8) 0.010(7) C3 0.060(9) 0.068(9) 0.105(12) -0.044(9) -0.040(9) 0.041(8) C4 0.027(7) 0.096(11) 0.091(10) -0.047(9) 0.013(7) 0.008(7) C5 0.043(7) 0.071(8) 0.036(6) -0.023(6) 0.019(6) -0.005(6) C6 0.044(6) 0.033(6) 0.034(6) -0.008(5) 0.000(5) 0.003(5) C7 0.051(8) 0.054(8) 0.064(8) 0.032(6) -0.016(6) -0.015(6) C8 0.045(7) 0.062(8) 0.052(7) 0.021(6) -0.002(6) 0.000(6) C9 0.049(7) 0.050(7) 0.046(7) 0.000(6) -0.004(6) -0.008(6) C10 0.047(7) 0.049(7) 0.048(7) 0.009(6) -0.010(6) -0.014(6) C11 0.056(7) 0.035(6) 0.040(6) 0.005(5) -0.011(6) 0.014(6) C12 0.046(7) 0.066(8) 0.027(6) 0.007(6) 0.000(5) 0.016(6) C13 0.058(8) 0.108(11) 0.020(6) 0.003(6) 0.004(6) 0.025(8) C14 0.050(7) 0.075(9) 0.048(7) 0.033(7) 0.024(6) 0.022(7) C15 0.047(7) 0.049(7) 0.046(7) 0.016(5) 0.011(6) -0.002(6) C16 0.044(7) 0.039(6) 0.034(6) -0.001(5) -0.002(5) 0.018(5) C17 0.045(7) 0.048(7) 0.048(7) -0.008(6) -0.004(6) 0.005(6) C18 0.039(6) 0.052(7) 0.051(7) -0.018(6) 0.002(6) 0.013(6) C19 0.040(7) 0.074(9) 0.060(8) -0.012(7) -0.005(6) 0.014(7) C20 0.038(6) 0.050(7) 0.061(8) 0.002(6) 0.001(6) 0.004(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.034(8) . ? Zn1 N2 2.052(8) . ? Zn1 Cl1 2.202(3) . ? Zn1 Cl2 2.224(3) . ? Fe1 C15 2.01(6) 2 ? Fe1 C11 2.024(7) 2 ? Fe1 C5 2.035(7) . ? Fe1 C14 2.04(6) 2 ? Fe1 C4 2.040(7) . ? Fe1 C1 2.042(7) . ? Fe1 C3 2.050(7) . ? Fe1 C2 2.052(7) . ? Fe1 C12 2.05(3) 2 ? Fe1 C13 2.06(5) 2 ? N1 C9 1.340(13) . ? N1 C8 1.346(13) . ? N2 C18 1.330(12) . ? N2 C19 1.347(13) . ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C1 C6 1.465(11) . ? C2 C3 1.4200 . ? C3 C4 1.4200 . ? C4 C5 1.4200 . ? C6 C7 1.385(14) . ? C6 C10 1.398(13) . ? C7 C8 1.357(15) . ? C9 C10 1.361(14) . ? C11 C12 1.4200 . ? C11 C15 1.4200 . ? C11 C16 1.472(10) . ? C11 Fe1 2.024(7) 2 ? C12 C13 1.4200 . ? C12 Fe1 2.053(7) 2 ? C13 C14 1.4200 . ? C13 Fe1 2.061(7) 2 ? C14 C15 1.4200 . ? C14 Fe1 2.037(7) 2 ? C15 Fe1 2.014(7) 2 ? C16 C20 1.387(14) . ? C16 C17 1.395(14) . ? C17 C18 1.361(13) . ? C19 C20 1.356(14) . ? 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 Zn1 N2 103.7(3) . . ? N1 Zn1 Cl1 111.0(3) . . ? N2 Zn1 Cl1 109.4(3) . . ? N1 Zn1 Cl2 112.4(3) . . ? N2 Zn1 Cl2 101.0(3) . . ? Cl1 Zn1 Cl2 117.89(17) . . ? C15 Fe1 C11 41.2(4) 2 2 ? C15 Fe1 C5 110.3(15) 2 . ? C11 Fe1 C5 112.8(3) 2 . ? C15 Fe1 C14 41.0(11) 2 2 ? C11 Fe1 C14 68.9(11) 2 2 ? C5 Fe1 C14 136.8(12) . 2 ? C15 Fe1 C4 110.0(9) 2 . ? C11 Fe1 C4 140.1(4) 2 . ? C5 Fe1 C4 40.79(13) . . ? C14 Fe1 C4 108.7(6) 2 . ? C15 Fe1 C1 139.0(14) 2 . ? C11 Fe1 C1 112.9(3) 2 . ? C5 Fe1 C1 40.77(12) . . ? C14 Fe1 C1 177.2(7) 2 . ? C4 Fe1 C1 68.51(15) . . ? C15 Fe1 C3 138.3(4) 2 . ? C11 Fe1 C3 178.7(3) 2 . ? C5 Fe1 C3 68.44(16) . . ? C14 Fe1 C3 109.9(11) 2 . ? C4 Fe1 C3 40.62(13) . . ? C1 Fe1 C3 68.31(16) . . ? C15 Fe1 C2 178.4(11) 2 . ? C11 Fe1 C2 140.1(3) 2 . ? C5 Fe1 C2 68.42(15) . . ? C14 Fe1 C2 139.3(16) 2 . ? C4 Fe1 C2 68.32(16) . . ? C1 Fe1 C2 40.59(12) . . ? C3 Fe1 C2 40.51(13) . . ? C15 Fe1 C12 68.8(16) 2 2 ? C11 Fe1 C12 40.8(12) 2 2 ? C5 Fe1 C12 142.3(10) . 2 ? C14 Fe1 C12 68.4(16) 2 2 ? C4 Fe1 C12 176.8(10) . 2 ? C1 Fe1 C12 114.4(11) . 2 ? C3 Fe1 C12 138.4(13) . 2 ? C2 Fe1 C12 112.8(13) . 2 ? C15 Fe1 C13 68.6(18) 2 2 ? C11 Fe1 C13 68.5(12) 2 2 ? C5 Fe1 C13 176.9(6) . 2 ? C14 Fe1 C13 40.5(12) 2 2 ? C4 Fe1 C13 136.5(5) . 2 ? C1 Fe1 C13 141.8(12) . 2 ? C3 Fe1 C13 110.3(12) . 2 ? C2 Fe1 C13 112.6(15) . 2 ? C12 Fe1 C13 40.4(7) 2 2 ? C9 N1 C8 116.2(9) . . ? C9 N1 Zn1 123.5(7) . . ? C8 N1 Zn1 120.3(7) . . ? C18 N2 C19 116.1(9) . . ? C18 N2 Zn1 125.5(7) . . ? C19 N2 Zn1 118.1(8) . . ? C2 C1 C5 108.0 . . ? C2 C1 C6 123.9(7) . . ? C5 C1 C6 128.1(7) . . ? C2 C1 Fe1 70.1(3) . . ? C5 C1 Fe1 69.3(3) . . ? C6 C1 Fe1 126.7(6) . . ? C1 C2 C3 108.0 . . ? C1 C2 Fe1 69.3(3) . . ? C3 C2 Fe1 69.7(3) . . ? C4 C3 C2 108.0 . . ? C4 C3 Fe1 69.3(3) . . ? C2 C3 Fe1 69.8(3) . . ? C3 C4 C5 108.0 . . ? C3 C4 Fe1 70.1(3) . . ? C5 C4 Fe1 69.4(3) . . ? C1 C5 C4 108.0 . . ? C1 C5 Fe1 69.9(3) . . ? C4 C5 Fe1 69.8(3) . . ? C7 C6 C10 115.3(10) . . ? C7 C6 C1 122.7(9) . . ? C10 C6 C1 121.9(9) . . ? C8 C7 C6 121.4(10) . . ? N1 C8 C7 123.0(11) . . ? N1 C9 C10 123.7(10) . . ? C9 C10 C6 120.3(10) . . ? C12 C11 C15 108.0 . . ? C12 C11 C16 126.3(7) . . ? C15 C11 C16 125.7(7) . . ? C12 C11 Fe1 70.7(3) . 2 ? C15 C11 Fe1 69.0(3) . 2 ? C16 C11 Fe1 124.4(6) . 2 ? C13 C12 C11 108.0 . . ? C13 C12 Fe1 70.1(3) . 2 ? C11 C12 Fe1 68.5(3) . 2 ? C14 C13 C12 108.0 . . ? C14 C13 Fe1 68.8(3) . 2 ? C12 C13 Fe1 69.5(3) . 2 ? C15 C14 C13 108.0 . . ? C15 C14 Fe1 68.6(3) . 2 ? C13 C14 Fe1 70.6(3) . 2 ? C14 C15 C11 108.0 . . ? C14 C15 Fe1 70.4(3) . 2 ? C11 C15 Fe1 69.8(3) . 2 ? C20 C16 C17 116.3(10) . . ? C20 C16 C11 121.9(9) . . ? C17 C16 C11 121.8(9) . . ? C18 C17 C16 119.4(10) . . ? N2 C18 C17 124.4(10) . . ? N2 C19 C20 123.4(11) . . ? C19 C20 C16 120.4(10) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.01 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.492 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.102 data_1cu _database_code_CSD 177936 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H50 Cu2 Fe2 N4 O11' _chemical_formula_weight 1097.70 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' 'Cu' 'Cu' 0.3201 1.2651 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9155(7) _cell_length_b 11.5519(7) _cell_length_c 23.424(2) _cell_angle_alpha 85.162(2) _cell_angle_beta 90.241(2) _cell_angle_gamma 75.431(2) _cell_volume 2586.7(3) _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 red _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.420 _exptl_absorpt_correction_type 'Bruker Smart' _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_T_max 1.00 _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 'Bruker Smart CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19143 _diffrn_reflns_av_R_equivalents 0.1232 _diffrn_reflns_av_sigmaI/netI 0.0882 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 34.16 _reflns_number_total 18329 _reflns_number_gt 2463 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1617P)^2^+68.2627P] 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 18329 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0996 _refine_ls_wR_factor_ref 0.2375 _refine_ls_wR_factor_gt 0.2375 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 Cu1 Cu 0.1011(3) 0.5712(3) 0.03649(17) 0.0182(11) Uani 1 1 d . . . Cu2 Cu 0.3917(3) 0.1243(3) 0.46180(17) 0.0196(11) Uani 1 1 d . . . Fe1 Fe -0.4453(4) 0.4803(4) 0.2579(2) 0.0229(12) Uani 1 1 d . . . Fe2 Fe 0.9698(4) -0.1172(4) 0.2506(2) 0.0208(12) Uani 1 1 d . . . C1 C -0.4428(18) 0.3154(15) 0.2282(9) 0.035(9) Uiso 1 1 d G . . H1 H -0.3689 0.2470 0.2312 0.042 Uiso 1 1 calc R . . C2 C -0.549(2) 0.3469(17) 0.2689(8) 0.039(9) Uiso 1 1 d G . . H2 H -0.5562 0.3027 0.3033 0.047 Uiso 1 1 calc R . . C3 C -0.6409(17) 0.4576(17) 0.2479(8) 0.028(8) Uiso 1 1 d G . . H3 H -0.7195 0.4987 0.2661 0.033 Uiso 1 1 calc R . . C4 C -0.5921(18) 0.4946(14) 0.1942(8) 0.012(6) Uiso 1 1 d G . . H4 H -0.6331 0.5642 0.1711 0.014 Uiso 1 1 calc R . . C5 C -0.4697(18) 0.4067(18) 0.1820(8) 0.019(7) Uiso 1 1 d G . . C6 C -0.2605(19) 0.4665(17) 0.2963(10) 0.028(8) Uiso 1 1 d G . . H6 H -0.1865 0.3984 0.3014 0.034 Uiso 1 1 calc R . . C7 C -0.375(2) 0.4972(19) 0.3331(8) 0.044(9) Uiso 1 1 d G . . H7 H -0.3893 0.4527 0.3665 0.053 Uiso 1 1 calc R . . C8 C -0.4642(19) 0.608(2) 0.3100(10) 0.040(9) Uiso 1 1 d G . . H8 H -0.5470 0.6484 0.3256 0.048 Uiso 1 1 calc R . . C9 C -0.405(2) 0.6454(17) 0.2590(10) 0.039(10) Uiso 1 1 d G . . H9 H -0.4417 0.7150 0.2352 0.047 Uiso 1 1 calc R . . C10 C -0.279(2) 0.558(2) 0.2505(9) 0.039(9) Uiso 1 1 d G . . C11 C -0.388(3) 0.414(2) 0.1313(13) 0.020(7) Uiso 1 1 d . . . C12 C -0.433(3) 0.504(2) 0.0846(12) 0.013(6) Uiso 1 1 d . . . H12 H -0.5175 0.5614 0.0867 0.015 Uiso 1 1 calc R . . C13 C -0.352(3) 0.508(3) 0.0350(14) 0.025(8) Uiso 1 1 d . . . H13 H -0.3821 0.5682 0.0056 0.030 Uiso 1 1 calc R . . N1 N -0.230(2) 0.424(2) 0.0301(11) 0.027(6) Uiso 1 1 d . . . C14 C -0.179(3) 0.336(3) 0.0733(14) 0.028(8) Uiso 1 1 d . . . H14 H -0.0964 0.2775 0.0697 0.034 Uiso 1 1 calc R . . C15 C -0.260(3) 0.338(3) 0.1244(15) 0.032(8) Uiso 1 1 d . . . H15 H -0.2217 0.2827 0.1552 0.039 Uiso 1 1 calc R . . C16 C -0.192(3) 0.563(3) 0.2012(14) 0.026(8) Uiso 1 1 d . . . C17 C -0.225(3) 0.642(3) 0.1527(13) 0.024(8) Uiso 1 1 d . . . H17 H -0.3127 0.6966 0.1495 0.029 Uiso 1 1 calc R . . C18 C -0.133(3) 0.643(3) 0.1087(14) 0.025(7) Uiso 1 1 d . . . H18 H -0.1562 0.7022 0.0782 0.030 Uiso 1 1 calc R . . N2 N -0.010(2) 0.5623(18) 0.1089(10) 0.010(5) Uiso 1 1 d . . . C19 C 0.020(3) 0.480(3) 0.1539(15) 0.034(9) Uiso 1 1 d . . . H19 H 0.1030 0.4207 0.1529 0.041 Uiso 1 1 calc R . . C20 C -0.060(3) 0.477(3) 0.2016(15) 0.037(9) Uiso 1 1 d . . . H20 H -0.0289 0.4210 0.2329 0.044 Uiso 1 1 calc R . . C21 C 1.095(2) -0.2815(19) 0.2424(8) 0.025(8) Uiso 1 1 d G . . H21 H 1.1072 -0.3199 0.2088 0.030 Uiso 1 1 calc R . . C22 C 1.1743(18) -0.2050(18) 0.2614(8) 0.021(7) Uiso 1 1 d G . . H22 H 1.2482 -0.1844 0.2423 0.026 Uiso 1 1 calc R . . C23 C 1.121(2) -0.1655(18) 0.3145(8) 0.029(8) Uiso 1 1 d G . . H23 H 1.1545 -0.1144 0.3364 0.035 Uiso 1 1 calc R . . C24 C 1.0090(19) -0.218(2) 0.3284(8) 0.018(7) Uiso 1 1 d G . . C25 C 0.992(2) -0.2893(19) 0.2839(10) 0.048(10) Uiso 1 1 d G . . H25 H 0.9264 -0.3335 0.2821 0.058 Uiso 1 1 calc R . . C26 C 0.911(2) 0.0649(18) 0.2400(9) 0.024(8) Uiso 1 1 d G . . H26 H 0.9435 0.1164 0.2618 0.028 Uiso 1 1 calc R . . C27 C 0.9687(19) 0.0196(19) 0.1886(9) 0.035(9) Uiso 1 1 d G . . H27 H 1.0462 0.0362 0.1707 0.042 Uiso 1 1 calc R . . C28 C 0.888(2) -0.0554(19) 0.1693(8) 0.029(8) Uiso 1 1 d G . . H28 H 0.9028 -0.0966 0.1365 0.035 Uiso 1 1 calc R . . C29 C 0.7796(19) -0.0565(19) 0.2087(10) 0.043(9) Uiso 1 1 d G . . H29 H 0.7115 -0.0986 0.2064 0.051 Uiso 1 1 calc R . . C30 C 0.794(2) 0.018(2) 0.2525(8) 0.030(8) Uiso 1 1 d G . . C31 C 0.916(3) -0.198(3) 0.3804(15) 0.033(9) Uiso 1 1 d . . . C32 C 0.949(3) -0.134(3) 0.4225(13) 0.027(8) Uiso 1 1 d . . . H32 H 1.0275 -0.1042 0.4207 0.032 Uiso 1 1 calc R . . C33 C 0.861(3) -0.116(2) 0.4676(13) 0.018(7) Uiso 1 1 d . . . H33 H 0.8833 -0.0729 0.4964 0.022 Uiso 1 1 calc R . . N3 N 0.744(2) -0.155(2) 0.4743(11) 0.020(6) Uiso 1 1 d . . . C34 C 0.724(3) -0.222(3) 0.4353(13) 0.024(7) Uiso 1 1 d . . . H34 H 0.6480 -0.2553 0.4394 0.029 Uiso 1 1 calc R . . C35 C 0.809(3) -0.251(3) 0.3859(14) 0.020(7) Uiso 1 1 d . . . H35 H 0.7915 -0.3026 0.3599 0.024 Uiso 1 1 calc R . . C36 C 0.699(3) 0.041(3) 0.3044(14) 0.027(8) Uiso 1 1 d . . . C37 C 0.723(3) 0.106(3) 0.3459(13) 0.024(7) Uiso 1 1 d . . . H37 H 0.8011 0.1372 0.3457 0.029 Uiso 1 1 calc R . . C38 C 0.632(3) 0.125(3) 0.3876(14) 0.023(7) Uiso 1 1 d . . . H38 H 0.6527 0.1690 0.4166 0.028 Uiso 1 1 calc R . . N4 N 0.519(2) 0.0907(19) 0.3927(10) 0.015(6) Uiso 1 1 d . . . C39 C 0.491(3) 0.030(2) 0.3517(12) 0.017(7) Uiso 1 1 d . . . H39 H 0.4124 0.0007 0.3538 0.020 Uiso 1 1 calc R . . C40 C 0.576(3) 0.009(3) 0.3053(16) 0.037(9) Uiso 1 1 d . . . H40 H 0.5494 -0.0275 0.2747 0.044 Uiso 1 1 calc R . . C41 C 0.204(3) 0.317(2) 0.0544(12) 0.011(6) Uiso 1 1 d . . . C42 C 0.206(3) 0.193(2) 0.0512(13) 0.023(7) Uiso 1 1 d . . . H42A H 0.2919 0.1438 0.0680 0.034 Uiso 1 1 calc R . . H42B H 0.1991 0.1780 0.0118 0.034 Uiso 1 1 calc R . . H42C H 0.1291 0.1754 0.0716 0.034 Uiso 1 1 calc R . . C43 C 0.164(3) 0.783(2) 0.0626(13) 0.017(7) Uiso 1 1 d . . . C44 C 0.154(5) 0.912(4) 0.057(2) 0.080(15) Uiso 1 1 d . . . H44A H 0.2058 0.9323 0.0874 0.120 Uiso 1 1 calc R . . H44B H 0.0582 0.9558 0.0578 0.120 Uiso 1 1 calc R . . H44C H 0.1919 0.9332 0.0206 0.120 Uiso 1 1 calc R . . C45 C 0.301(3) 0.359(3) 0.4106(15) 0.032(8) Uiso 1 1 d . . . C46 C 0.283(4) 0.489(3) 0.4022(17) 0.054(11) Uiso 1 1 d . . . H46A H 0.2916 0.5120 0.3623 0.081 Uiso 1 1 calc R . . H46B H 0.3537 0.5107 0.4240 0.081 Uiso 1 1 calc R . . H46C H 0.1928 0.5288 0.4147 0.081 Uiso 1 1 calc R . . C47 C 0.317(3) -0.091(3) 0.4516(15) 0.030(8) Uiso 1 1 d . . . C48 C 0.332(3) -0.224(3) 0.4569(14) 0.027(8) Uiso 1 1 d . . . H48A H 0.2902 -0.2465 0.4916 0.040 Uiso 1 1 calc R . . H48B H 0.4294 -0.2652 0.4580 0.040 Uiso 1 1 calc R . . H48C H 0.2870 -0.2456 0.4246 0.040 Uiso 1 1 calc R . . O1 O 0.295(2) 0.349(2) 0.0832(11) 0.044(6) Uiso 1 1 d . . . O2 O 0.107(2) 0.4024(17) 0.0279(9) 0.028(5) Uiso 1 1 d . . . O3 O 0.267(2) 0.713(2) 0.0881(11) 0.051(7) Uiso 1 1 d . . . O4 O 0.0750(18) 0.7446(16) 0.0379(9) 0.022(5) Uiso 1 1 d . . . O5 O 0.2291(19) -0.0234(16) 0.4176(9) 0.023(5) Uiso 1 1 d . . . O6 O 0.4066(17) -0.0568(15) 0.4781(8) 0.012(4) Uiso 1 1 d . . . O7 O 0.236(2) 0.316(2) 0.3827(11) 0.049(7) Uiso 1 1 d . . . O8 O 0.391(2) 0.294(2) 0.4536(11) 0.047(7) Uiso 1 1 d . . . O9 O 0.510(3) 0.159(3) 0.1244(15) 0.094(10) Uiso 1 1 d . . . O10 O -0.144(4) 0.296(3) 0.4347(16) 0.111(12) Uiso 1 1 d . . . O11 O 0.063(3) 0.181(2) 0.3550(13) 0.070(8) 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 Cu1 0.019(2) 0.020(2) 0.023(3) -0.0050(19) 0.0024(18) -0.0190(18) Cu2 0.017(2) 0.018(2) 0.029(3) -0.0044(19) 0.0006(18) -0.0125(17) Fe1 0.024(3) 0.027(3) 0.021(3) -0.002(2) 0.008(2) -0.014(2) Fe2 0.017(2) 0.027(3) 0.024(3) -0.012(2) 0.008(2) -0.012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O4 1.957(19) . ? Cu1 O2 1.96(2) . ? Cu1 N1 2.03(3) 2_565 ? Cu1 N2 2.04(2) . ? Cu2 O8 1.95(2) . ? Cu2 N3 2.01(3) 2_656 ? Cu2 N4 2.06(2) . ? Cu2 O6 2.062(17) . ? Cu2 O6 2.366(17) 2_656 ? Fe1 C7 1.94(2) . ? Fe1 C8 1.97(2) . ? Fe1 C6 2.00(2) . ? Fe1 C3 2.037(19) . ? Fe1 C9 2.05(2) . ? Fe1 C4 2.047(18) . ? Fe1 C2 2.06(2) . ? Fe1 C10 2.07(2) . ? Fe1 C5 2.071(19) . ? Fe1 C1 2.08(2) . ? Fe2 C21 2.01(2) . ? Fe2 C25 2.03(2) . ? Fe2 C26 2.03(2) . ? Fe2 C30 2.03(2) . ? Fe2 C22 2.030(19) . ? Fe2 C27 2.05(2) . ? Fe2 C29 2.05(2) . ? Fe2 C24 2.06(2) . ? Fe2 C23 2.06(2) . ? Fe2 C28 2.07(2) . ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C2 C3 1.4200 . ? C3 C4 1.4200 . ? C4 C5 1.4200 . ? C5 C11 1.45(3) . ? C6 C7 1.4200 . ? C6 C10 1.4200 . ? C7 C8 1.4200 . ? C8 C9 1.4200 . ? C9 C10 1.4200 . ? C10 C16 1.45(3) . ? C11 C15 1.37(4) . ? C11 C12 1.43(4) . ? C12 C13 1.42(4) . ? C13 N1 1.35(4) . ? N1 C14 1.37(4) . ? N1 Cu1 2.03(3) 2_565 ? C14 C15 1.44(4) . ? C16 C17 1.39(4) . ? C16 C20 1.43(4) . ? C17 C18 1.39(4) . ? C18 N2 1.33(3) . ? N2 C19 1.33(4) . ? C19 C20 1.38(4) . ? C21 C22 1.4200 . ? C21 C25 1.4200 . ? C22 C23 1.4200 . ? C23 C24 1.4200 . ? C24 C25 1.4200 . ? C24 C31 1.53(4) . ? C26 C27 1.4200 . ? C26 C30 1.4200 . ? C27 C28 1.4200 . ? C28 C29 1.4200 . ? C29 C30 1.4200 . ? C30 C36 1.54(4) . ? C31 C35 1.36(4) . ? C31 C32 1.36(4) . ? C32 C33 1.37(4) . ? C33 N3 1.35(3) . ? N3 C34 1.29(3) . ? N3 Cu2 2.01(3) 2_656 ? C34 C35 1.44(4) . ? C36 C37 1.33(4) . ? C36 C40 1.36(4) . ? C37 C38 1.33(4) . ? C38 N4 1.28(3) . ? N4 C39 1.30(3) . ? C39 C40 1.38(4) . ? C41 O1 1.27(3) . ? C41 O2 1.31(3) . ? C41 C42 1.43(3) . ? C43 O3 1.24(3) . ? C43 O4 1.24(3) . ? C43 C44 1.47(5) . ? C45 O7 1.14(3) . ? C45 O8 1.38(4) . ? C45 C46 1.46(4) . ? C47 O6 1.24(3) . ? C47 O5 1.25(3) . ? C47 C48 1.50(4) . ? O6 Cu2 2.366(17) 2_656 ? 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 O4 Cu1 O2 172.5(8) . . ? O4 Cu1 N1 88.5(9) . 2_565 ? O2 Cu1 N1 91.4(9) . 2_565 ? O4 Cu1 N2 91.8(8) . . ? O2 Cu1 N2 89.1(9) . . ? N1 Cu1 N2 174.0(9) 2_565 . ? O8 Cu2 N3 90.0(10) . 2_656 ? O8 Cu2 N4 91.3(10) . . ? N3 Cu2 N4 175.9(9) 2_656 . ? O8 Cu2 O6 173.8(9) . . ? N3 Cu2 O6 88.8(8) 2_656 . ? N4 Cu2 O6 90.3(8) . . ? O8 Cu2 O6 97.2(8) . 2_656 ? N3 Cu2 O6 95.8(8) 2_656 2_656 ? N4 Cu2 O6 88.0(7) . 2_656 ? O6 Cu2 O6 76.9(6) . 2_656 ? C7 Fe1 C8 42.7(4) . . ? C7 Fe1 C6 42.2(4) . . ? C8 Fe1 C6 70.8(5) . . ? C7 Fe1 C3 120.2(8) . . ? C8 Fe1 C3 105.4(8) . . ? C6 Fe1 C3 157.7(9) . . ? C7 Fe1 C9 70.4(5) . . ? C8 Fe1 C9 41.4(4) . . ? C6 Fe1 C9 69.1(5) . . ? C3 Fe1 C9 123.2(8) . . ? C7 Fe1 C4 156.6(9) . . ? C8 Fe1 C4 120.1(8) . . ? C6 Fe1 C4 160.1(9) . . ? C3 Fe1 C4 40.7(3) . . ? C9 Fe1 C4 107.0(7) . . ? C7 Fe1 C2 106.0(8) . . ? C8 Fe1 C2 122.8(9) . . ? C6 Fe1 C2 122.1(8) . . ? C3 Fe1 C2 40.6(3) . . ? C9 Fe1 C2 160.0(9) . . ? C4 Fe1 C2 68.1(4) . . ? C7 Fe1 C10 69.9(5) . . ? C8 Fe1 C10 69.4(5) . . ? C6 Fe1 C10 40.8(4) . . ? C3 Fe1 C10 159.9(9) . . ? C9 Fe1 C10 40.3(4) . . ? C4 Fe1 C10 123.9(8) . . ? C2 Fe1 C10 158.4(9) . . ? C7 Fe1 C5 160.3(9) . . ? C8 Fe1 C5 156.5(9) . . ? C6 Fe1 C5 124.0(8) . . ? C3 Fe1 C5 68.0(4) . . ? C9 Fe1 C5 122.0(9) . . ? C4 Fe1 C5 40.3(3) . . ? C2 Fe1 C5 67.7(4) . . ? C10 Fe1 C5 108.7(8) . . ? C7 Fe1 C1 123.3(8) . . ? C8 Fe1 C1 160.3(10) . . ? C6 Fe1 C1 108.0(7) . . ? C3 Fe1 C1 67.9(4) . . ? C9 Fe1 C1 157.8(10) . . ? C4 Fe1 C1 67.7(4) . . ? C2 Fe1 C1 40.2(4) . . ? C10 Fe1 C1 123.3(8) . . ? C5 Fe1 C1 40.0(3) . . ? C21 Fe2 C25 41.1(4) . . ? C21 Fe2 C26 155.9(9) . . ? C25 Fe2 C26 161.6(9) . . ? C21 Fe2 C30 160.2(8) . . ? C25 Fe2 C30 125.6(8) . . ? C26 Fe2 C30 40.9(4) . . ? C21 Fe2 C22 41.1(4) . . ? C25 Fe2 C22 68.9(5) . . ? C26 Fe2 C22 120.5(7) . . ? C30 Fe2 C22 158.5(8) . . ? C21 Fe2 C27 119.4(8) . . ? C25 Fe2 C27 157.0(9) . . ? C26 Fe2 C27 40.7(4) . . ? C30 Fe2 C27 68.5(5) . . ? C22 Fe2 C27 104.1(7) . . ? C21 Fe2 C29 122.3(8) . . ? C25 Fe2 C29 109.4(7) . . ? C26 Fe2 C29 68.5(5) . . ? C30 Fe2 C29 40.7(4) . . ? C22 Fe2 C29 157.0(9) . . ? C27 Fe2 C29 68.1(5) . . ? C21 Fe2 C24 68.7(5) . . ? C25 Fe2 C24 40.7(4) . . ? C26 Fe2 C24 124.8(8) . . ? C30 Fe2 C24 111.0(8) . . ? C22 Fe2 C24 68.4(4) . . ? C27 Fe2 C24 158.9(8) . . ? C29 Fe2 C24 126.2(8) . . ? C21 Fe2 C23 68.7(4) . . ? C25 Fe2 C23 68.4(5) . . ? C26 Fe2 C23 107.6(7) . . ? C30 Fe2 C23 124.8(8) . . ? C22 Fe2 C23 40.7(4) . . ? C27 Fe2 C23 121.3(7) . . ? C29 Fe2 C23 161.8(9) . . ? C24 Fe2 C23 40.4(4) . . ? C21 Fe2 C28 105.1(7) . . ? C25 Fe2 C28 122.8(8) . . ? C26 Fe2 C28 68.2(5) . . ? C30 Fe2 C28 68.2(5) . . ? C22 Fe2 C28 119.9(8) . . ? C27 Fe2 C28 40.3(4) . . ? C29 Fe2 C28 40.3(4) . . ? C24 Fe2 C28 160.5(8) . . ? C23 Fe2 C28 156.4(8) . . ? C2 C1 C5 108.0 . . ? C2 C1 Fe1 69.1(7) . . ? C5 C1 Fe1 69.8(7) . . ? C3 C2 C1 108.0 . . ? C3 C2 Fe1 69.0(7) . . ? C1 C2 Fe1 70.7(8) . . ? C2 C3 C4 108.0 . . ? C2 C3 Fe1 70.4(8) . . ? C4 C3 Fe1 70.0(7) . . ? C5 C4 C3 108.0 . . ? C5 C4 Fe1 70.8(8) . . ? C3 C4 Fe1 69.3(8) . . ? C4 C5 C1 108.0 . . ? C4 C5 C11 124.4(17) . . ? C1 C5 C11 127.6(17) . . ? C4 C5 Fe1 68.9(7) . . ? C1 C5 Fe1 70.2(7) . . ? C11 C5 Fe1 125.5(16) . . ? C7 C6 C10 108.0 . . ? C7 C6 Fe1 66.4(9) . . ? C10 C6 Fe1 72.2(9) . . ? C8 C7 C6 108.0 . . ? C8 C7 Fe1 69.8(9) . . ? C6 C7 Fe1 71.4(9) . . ? C7 C8 C9 108.0 . . ? C7 C8 Fe1 67.5(8) . . ? C9 C8 Fe1 72.4(9) . . ? C10 C9 C8 108.0 . . ? C10 C9 Fe1 70.7(8) . . ? C8 C9 Fe1 66.2(9) . . ? C9 C10 C6 108.0 . . ? C9 C10 C16 124.2(19) . . ? C6 C10 C16 127.7(19) . . ? C9 C10 Fe1 69.0(8) . . ? C6 C10 Fe1 67.0(8) . . ? C16 C10 Fe1 127.1(19) . . ? C15 C11 C12 114(3) . . ? C15 C11 C5 123(3) . . ? C12 C11 C5 122(2) . . ? C13 C12 C11 121(3) . . ? N1 C13 C12 121(3) . . ? C13 N1 C14 121(3) . . ? C13 N1 Cu1 123(2) . 2_565 ? C14 N1 Cu1 115(2) . 2_565 ? N1 C14 C15 117(3) . . ? C11 C15 C14 125(3) . . ? C17 C16 C20 116(3) . . ? C17 C16 C10 126(3) . . ? C20 C16 C10 118(3) . . ? C16 C17 C18 122(3) . . ? N2 C18 C17 122(3) . . ? C18 N2 C19 117(3) . . ? C18 N2 Cu1 115.0(19) . . ? C19 N2 Cu1 128(2) . . ? N2 C19 C20 126(3) . . ? C19 C20 C16 117(3) . . ? C22 C21 C25 108.0 . . ? C22 C21 Fe2 70.1(8) . . ? C25 C21 Fe2 70.1(8) . . ? C23 C22 C21 108.0 . . ? C23 C22 Fe2 70.7(8) . . ? C21 C22 Fe2 68.8(8) . . ? C22 C23 C24 108.0 . . ? C22 C23 Fe2 68.7(8) . . ? C24 C23 Fe2 69.8(8) . . ? C23 C24 C25 108.0 . . ? C23 C24 C31 127.3(18) . . ? C25 C24 C31 124.7(18) . . ? C23 C24 Fe2 69.8(8) . . ? C25 C24 Fe2 68.6(8) . . ? C31 C24 Fe2 125.2(17) . . ? C21 C25 C24 108.0 . . ? C21 C25 Fe2 68.8(8) . . ? C24 C25 Fe2 70.7(8) . . ? C27 C26 C30 108.0 . . ? C27 C26 Fe2 70.5(8) . . ? C30 C26 Fe2 69.5(8) . . ? C28 C27 C26 108.0 . . ? C28 C27 Fe2 70.3(8) . . ? C26 C27 Fe2 68.8(8) . . ? C27 C28 C29 108.0 . . ? C27 C28 Fe2 69.3(8) . . ? C29 C28 Fe2 69.3(8) . . ? C30 C29 C28 108.0 . . ? C30 C29 Fe2 68.8(8) . . ? C28 C29 Fe2 70.3(8) . . ? C29 C30 C26 108.0 . . ? C29 C30 C36 125.4(18) . . ? C26 C30 C36 126.6(18) . . ? C29 C30 Fe2 70.5(8) . . ? C26 C30 Fe2 69.5(8) . . ? C36 C30 Fe2 125.0(17) . . ? C35 C31 C32 121(3) . . ? C35 C31 C24 120(3) . . ? C32 C31 C24 119(3) . . ? C31 C32 C33 117(3) . . ? N3 C33 C32 126(3) . . ? C34 N3 C33 114(3) . . ? C34 N3 Cu2 119(2) . 2_656 ? C33 N3 Cu2 127(2) . 2_656 ? N3 C34 C35 126(3) . . ? C31 C35 C34 115(3) . . ? C37 C36 C40 117(3) . . ? C37 C36 C30 123(3) . . ? C40 C36 C30 120(3) . . ? C38 C37 C36 118(3) . . ? N4 C38 C37 128(3) . . ? C38 N4 C39 116(3) . . ? C38 N4 Cu2 123(2) . . ? C39 N4 Cu2 121.8(18) . . ? N4 C39 C40 122(3) . . ? C36 C40 C39 120(3) . . ? O1 C41 O2 116(2) . . ? O1 C41 C42 122(2) . . ? O2 C41 C42 121(2) . . ? O3 C43 O4 121(3) . . ? O3 C43 C44 120(3) . . ? O4 C43 C44 119(3) . . ? O7 C45 O8 123(3) . . ? O7 C45 C46 118(3) . . ? O8 C45 C46 119(3) . . ? O6 C47 O5 123(3) . . ? O6 C47 C48 116(3) . . ? O5 C47 C48 121(3) . . ? C41 O2 Cu1 120.3(17) . . ? C43 O4 Cu1 119.3(18) . . ? C47 O6 Cu2 113.4(18) . . ? C47 O6 Cu2 143.4(19) . 2_656 ? Cu2 O6 Cu2 103.1(6) . 2_656 ? C45 O8 Cu2 112.9(19) . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 34.16 _diffrn_measured_fraction_theta_full 0.903 _refine_diff_density_max 1.063 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.167 data_1ag _database_code_CSD 177937 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H35 Ag2 Fe2 N6 O7.50' _chemical_formula_weight 1047.18 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' 'Ag' 'Ag' -0.8971 1.1015 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/a 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' _cell_length_a 11.620(3) _cell_length_b 16.597(8) _cell_length_c 20.762(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.67(2) _cell_angle_gamma 90.00 _cell_volume 3855(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.804 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2092 _exptl_absorpt_coefficient_mu 1.800 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.58 _exptl_absorpt_correction_T_max 1.00 _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 'Nonius CAD4 - point detector' _diffrn_measurement_method 'w/2 theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6935 _diffrn_reflns_av_R_equivalents 0.1237 _diffrn_reflns_av_sigmaI/netI 0.2257 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 24.98 _reflns_number_total 6741 _reflns_number_gt 3258 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0649P)^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 6741 _refine_ls_number_parameters 477 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1424 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1635 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.001 _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 Ag1 Ag 0.27292(9) 0.74790(7) 0.00533(4) 0.0541(3) Uani 1 1 d . . . Ag2 Ag 0.13564(9) 0.56277(7) 0.01685(5) 0.0499(3) Uani 1 1 d . . . Fe1 Fe 0.52522(14) 0.65504(10) 0.38004(7) 0.0329(5) Uani 1 1 d . . . C1 C 0.5617(7) 0.7366(5) 0.3147(3) 0.035(3) Uani 1 1 d G . . C2 C 0.6641(7) 0.6889(5) 0.3437(4) 0.036(3) Uani 1 1 d G . . H2 H 0.7045 0.6562 0.3207 0.043 Uiso 1 1 calc R . . C3 C 0.6941(6) 0.7001(5) 0.4141(4) 0.044(3) Uani 1 1 d G . . H3 H 0.7575 0.6759 0.4453 0.053 Uiso 1 1 calc R . . C4 C 0.6102(8) 0.7546(5) 0.4286(3) 0.044(3) Uani 1 1 d G . . H4 H 0.6090 0.7724 0.4709 0.053 Uiso 1 1 calc R . . C5 C 0.5284(6) 0.7772(5) 0.3671(4) 0.044(3) Uani 1 1 d G . . H5 H 0.4643 0.8123 0.3621 0.053 Uiso 1 1 calc R . . C6 C 0.3949(7) 0.5758(5) 0.3303(3) 0.030(3) Uani 1 1 d G . . C7 C 0.5002(7) 0.5331(4) 0.3633(4) 0.040(3) Uani 1 1 d G . . H7 H 0.5442 0.4996 0.3431 0.048 Uiso 1 1 calc R . . C8 C 0.5263(6) 0.5506(5) 0.4327(3) 0.037(3) Uani 1 1 d G . . H8 H 0.5906 0.5306 0.4659 0.045 Uiso 1 1 calc R . . C9 C 0.4372(8) 0.6041(5) 0.4426(3) 0.041(3) Uani 1 1 d G . . H9 H 0.4329 0.6252 0.4833 0.049 Uiso 1 1 calc R . . C10 C 0.3560(6) 0.6197(5) 0.3792(4) 0.039(3) Uani 1 1 d G . . H10 H 0.2890 0.6528 0.3712 0.047 Uiso 1 1 calc R . . C11 C 0.5013(10) 0.7390(7) 0.2423(5) 0.029(3) Uani 1 1 d . . . C12 C 0.5302(11) 0.6900(7) 0.1968(6) 0.042(3) Uani 1 1 d . . . H12 H 0.5927 0.6534 0.2100 0.050 Uiso 1 1 calc R . . C13 C 0.4661(12) 0.6954(8) 0.1314(7) 0.051(4) Uani 1 1 d . . . H13 H 0.4868 0.6605 0.1013 0.062 Uiso 1 1 calc R . . N1 N 0.3760(9) 0.7465(7) 0.1068(4) 0.042(3) Uani 1 1 d . . . C14 C 0.3501(12) 0.7962(8) 0.1507(6) 0.043(3) Uani 1 1 d . . . H14 H 0.2892 0.8336 0.1357 0.052 Uiso 1 1 calc R . . C15 C 0.4090(10) 0.7948(8) 0.2172(5) 0.038(3) Uani 1 1 d . . . H15 H 0.3878 0.8311 0.2462 0.046 Uiso 1 1 calc R . . C16 C 0.3360(10) 0.5752(7) 0.2596(5) 0.031(3) Uani 1 1 d . . . C17 C 0.3733(11) 0.5249(7) 0.2157(6) 0.040(3) Uani 1 1 d . . . H17 H 0.4382 0.4908 0.2318 0.048 Uiso 1 1 calc R . . C18 C 0.3155(12) 0.5251(8) 0.1487(6) 0.045(4) Uani 1 1 d . . . H18 H 0.3433 0.4910 0.1207 0.055 Uiso 1 1 calc R . . N2 N 0.2221(9) 0.5715(6) 0.1219(4) 0.036(2) Uani 1 1 d . . . C19 C 0.1836(11) 0.6206(8) 0.1631(6) 0.046(4) Uani 1 1 d . . . H19 H 0.1174 0.6532 0.1454 0.056 Uiso 1 1 calc R . . C20 C 0.2391(10) 0.6245(7) 0.2307(6) 0.037(3) Uani 1 1 d . . . H20 H 0.2113 0.6606 0.2574 0.044 Uiso 1 1 calc R . . Fe2 Fe -0.12753(14) 0.66391(10) -0.35645(8) 0.0341(4) Uiso 1 1 d . . . C21 C 0.0077(7) 0.7394(5) -0.3074(3) 0.037(3) Uani 1 1 d G . . C22 C 0.0414(7) 0.6953(5) -0.3581(4) 0.048(4) Uani 1 1 d G . . H22 H 0.1065 0.6607 -0.3516 0.058 Uiso 1 1 calc R . . C23 C -0.0418(9) 0.7132(6) -0.4203(3) 0.061(4) Uani 1 1 d G . . H23 H -0.0408 0.6924 -0.4617 0.073 Uiso 1 1 calc R . . C24 C -0.1269(7) 0.7684(6) -0.4081(4) 0.060(4) Uani 1 1 d G . . H24 H -0.1913 0.7901 -0.4401 0.072 Uiso 1 1 calc R . . C25 C -0.0963(7) 0.7846(5) -0.3384(4) 0.051(4) Uani 1 1 d G . . H25 H -0.1372 0.8188 -0.3167 0.062 Uiso 1 1 calc R . . C26 C -0.1613(7) 0.5804(5) -0.2918(3) 0.031(3) Uani 1 1 d G . . C27 C -0.1294(6) 0.5420(5) -0.3456(4) 0.039(3) Uani 1 1 d G . . H27 H -0.0646 0.5077 -0.3419 0.046 Uiso 1 1 calc R . . C28 C -0.2139(7) 0.5650(6) -0.4060(3) 0.045(3) Uani 1 1 d G . . H28 H -0.2141 0.5485 -0.4488 0.054 Uiso 1 1 calc R . . C29 C -0.2979(6) 0.6177(5) -0.3895(4) 0.045(4) Uani 1 1 d G . . H29 H -0.3629 0.6417 -0.4196 0.054 Uiso 1 1 calc R . . C30 C -0.2654(7) 0.6272(5) -0.3189(4) 0.038(3) Uani 1 1 d G . . H30 H -0.3054 0.6586 -0.2947 0.046 Uiso 1 1 calc R . . C31 C 0.0684(10) 0.7407(7) -0.2354(5) 0.033(3) Uani 1 1 d . . . C32 C 0.1630(11) 0.6879(7) -0.2072(6) 0.043(4) Uani 1 1 d . . . H32 H 0.1885 0.6511 -0.2342 0.052 Uiso 1 1 calc R . . C33 C 0.2170(11) 0.6907(7) -0.1409(6) 0.041(3) Uani 1 1 d . . . H33 H 0.2798 0.6551 -0.1240 0.049 Uiso 1 1 calc R . . N3 N 0.1869(9) 0.7400(6) -0.0987(5) 0.042(3) Uani 1 1 d . . . C34 C 0.0957(11) 0.7917(8) -0.1248(6) 0.041(3) Uani 1 1 d . . . H34 H 0.0717 0.8272 -0.0963 0.049 Uiso 1 1 calc R . . C35 C 0.0370(11) 0.7936(7) -0.1925(6) 0.039(3) Uani 1 1 d . . . H35 H -0.0238 0.8307 -0.2087 0.047 Uiso 1 1 calc R . . C36 C -0.0946(10) 0.5745(7) -0.2203(5) 0.026(3) Uani 1 1 d . . . C37 C -0.0009(11) 0.5217(7) -0.1980(6) 0.043(3) Uani 1 1 d . . . H37 H 0.0220 0.4875 -0.2278 0.052 Uiso 1 1 calc R . . C38 C 0.0586(11) 0.5202(7) -0.1306(6) 0.045(4) Uani 1 1 d . . . H38 H 0.1222 0.4845 -0.1165 0.053 Uiso 1 1 calc R . . N4 N 0.0308(9) 0.5666(7) -0.0845(4) 0.043(3) Uani 1 1 d . . . C39 C -0.0632(11) 0.6167(8) -0.1070(6) 0.044(3) Uani 1 1 d . . . H39 H -0.0863 0.6485 -0.0758 0.053 Uiso 1 1 calc R . . C40 C -0.1251(10) 0.6235(7) -0.1709(5) 0.037(3) Uani 1 1 d . . . H40 H -0.1879 0.6601 -0.1833 0.044 Uiso 1 1 calc R . . N5 N 0.1874(12) 0.9317(9) 0.0145(5) 0.054(3) Uani 1 1 d . . . O1 O 0.1626(9) 1.0040(7) 0.0163(5) 0.070(3) Uani 1 1 d . . . O2 O 0.2781(9) 0.9115(5) -0.0033(5) 0.067(3) Uani 1 1 d . . . O3 O 0.1256(9) 0.8771(7) 0.0300(5) 0.072(3) Uani 1 1 d . . . N6 N 0.2364(14) 0.4910(9) -0.2793(9) 0.070(4) Uani 1 1 d . . . O4 O 0.1503(11) 0.4580(7) -0.3227(6) 0.094(4) Uani 1 1 d . . . O5 O 0.2847(11) 0.5512(7) -0.2923(7) 0.099(4) Uani 1 1 d . . . O6 O 0.2639(10) 0.4579(7) -0.2251(7) 0.092(4) Uani 1 1 d . . . O7 O 0.0629(8) 1.0483(6) 0.1226(5) 0.079(3) Uani 1 1 d . . . O8 O 0.835(2) 0.4486(16) 0.4605(13) 0.123(9) Uiso 0.50 1 d P . . 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 Ag1 0.0611(7) 0.0649(8) 0.0290(5) 0.0020(6) -0.0007(5) -0.0081(7) Ag2 0.0584(7) 0.0567(7) 0.0277(5) -0.0002(5) -0.0005(5) 0.0003(6) Fe1 0.0328(10) 0.0394(11) 0.0225(8) 0.0006(8) 0.0010(8) -0.0031(9) C1 0.027(7) 0.046(9) 0.033(6) 0.006(6) 0.009(5) -0.004(6) C2 0.028(7) 0.042(9) 0.035(7) 0.007(6) 0.006(6) 0.004(6) C3 0.029(8) 0.047(9) 0.044(8) 0.003(7) -0.010(6) -0.001(7) C4 0.054(9) 0.045(8) 0.028(6) -0.003(7) 0.003(6) -0.012(8) C5 0.050(9) 0.031(8) 0.049(8) -0.010(6) 0.008(7) -0.005(7) C6 0.036(7) 0.032(7) 0.021(6) 0.005(5) 0.007(5) 0.000(6) C7 0.049(9) 0.032(8) 0.034(7) -0.002(6) 0.002(6) 0.000(7) C8 0.053(8) 0.035(8) 0.018(6) 0.018(6) 0.000(6) -0.011(7) C9 0.050(9) 0.051(9) 0.023(6) -0.013(6) 0.014(6) -0.007(7) C10 0.029(7) 0.063(9) 0.025(7) 0.001(6) 0.006(6) -0.010(7) C11 0.035(7) 0.019(7) 0.033(6) 0.011(6) 0.009(6) -0.012(6) C12 0.054(9) 0.038(8) 0.033(7) 0.000(6) 0.013(7) 0.009(7) C13 0.059(10) 0.050(10) 0.048(9) -0.016(7) 0.021(8) 0.000(8) N1 0.044(7) 0.054(7) 0.026(5) 0.006(6) 0.006(5) 0.007(6) C14 0.059(9) 0.041(8) 0.027(7) 0.002(6) 0.005(7) 0.002(7) C15 0.046(8) 0.054(9) 0.020(6) 0.010(6) 0.015(6) -0.005(7) C16 0.029(7) 0.038(8) 0.029(6) -0.013(6) 0.010(5) -0.012(6) C17 0.037(8) 0.037(8) 0.042(8) -0.002(6) 0.004(6) 0.004(6) C18 0.055(9) 0.051(9) 0.029(7) -0.010(6) 0.008(7) -0.002(8) N2 0.044(7) 0.042(7) 0.018(5) -0.001(5) 0.001(5) 0.003(6) C19 0.042(8) 0.066(10) 0.026(7) 0.005(7) 0.001(6) 0.017(7) C20 0.030(7) 0.039(8) 0.038(7) -0.009(6) 0.003(6) 0.009(6) C21 0.046(8) 0.029(8) 0.033(7) -0.002(6) 0.006(6) -0.006(6) C22 0.040(8) 0.064(10) 0.041(8) -0.003(7) 0.012(7) -0.016(7) C23 0.054(10) 0.105(13) 0.021(7) 0.007(8) 0.006(7) -0.021(9) C24 0.048(9) 0.064(11) 0.061(10) 0.026(8) 0.004(8) -0.006(8) C25 0.053(9) 0.050(9) 0.043(8) 0.009(7) 0.000(7) -0.007(8) C26 0.034(7) 0.033(8) 0.028(6) -0.005(5) 0.012(6) -0.014(6) C27 0.036(8) 0.039(8) 0.036(7) -0.001(6) 0.002(6) 0.006(6) C28 0.040(8) 0.053(9) 0.033(7) -0.012(7) -0.007(6) -0.005(7) C29 0.039(8) 0.055(9) 0.028(7) -0.007(7) -0.014(6) -0.001(7) C30 0.017(7) 0.039(8) 0.057(8) -0.004(7) 0.008(6) 0.005(6) C31 0.033(7) 0.040(8) 0.027(6) -0.011(6) 0.009(5) -0.017(7) C32 0.039(8) 0.054(10) 0.030(7) -0.008(6) -0.004(6) -0.002(7) C33 0.040(8) 0.039(9) 0.046(8) -0.002(7) 0.016(7) -0.008(6) N3 0.050(7) 0.036(7) 0.035(6) 0.003(5) 0.002(5) 0.003(6) C34 0.052(9) 0.043(8) 0.031(7) -0.003(6) 0.017(7) -0.006(7) C35 0.039(8) 0.047(8) 0.030(7) -0.009(6) 0.007(6) 0.001(7) C36 0.033(7) 0.022(7) 0.024(6) 0.001(5) 0.008(5) -0.006(6) C37 0.046(9) 0.044(9) 0.037(7) -0.001(6) 0.008(7) 0.020(7) C38 0.043(9) 0.040(9) 0.045(8) -0.010(7) 0.002(7) 0.002(7) N4 0.042(7) 0.052(7) 0.028(6) -0.001(6) 0.000(5) -0.015(6) C39 0.050(9) 0.058(9) 0.028(7) 0.002(7) 0.017(6) 0.006(8) C40 0.033(8) 0.046(8) 0.027(7) 0.005(6) 0.003(6) 0.012(6) N5 0.065(10) 0.054(9) 0.033(6) 0.002(7) -0.005(6) 0.004(9) O1 0.070(8) 0.066(8) 0.082(8) 0.000(6) 0.033(6) 0.010(6) O2 0.063(8) 0.058(7) 0.085(8) -0.006(6) 0.027(6) 0.008(6) O3 0.066(7) 0.079(8) 0.074(7) 0.012(6) 0.022(6) -0.011(6) N6 0.064(11) 0.043(10) 0.116(14) 0.003(10) 0.044(11) 0.016(8) O4 0.083(9) 0.093(10) 0.107(10) 0.005(8) 0.027(8) 0.022(8) O5 0.121(10) 0.048(8) 0.164(12) -0.005(8) 0.100(10) -0.003(7) O6 0.094(9) 0.073(9) 0.103(9) 0.024(8) 0.017(8) -0.002(7) O7 0.062(7) 0.083(8) 0.097(8) -0.007(7) 0.028(6) 0.001(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.124(9) . ? Ag1 N3 2.126(9) . ? Ag2 N4 2.128(9) . ? Ag2 N2 2.146(8) . ? Fe1 C2 2.036(8) . ? Fe1 C1 2.040(8) . ? Fe1 C3 2.039(8) . ? Fe1 C9 2.040(8) . ? Fe1 C5 2.046(8) . ? Fe1 C10 2.048(8) . ? Fe1 C4 2.046(8) . ? Fe1 C8 2.048(7) . ? Fe1 C6 2.061(8) . ? Fe1 C7 2.060(8) . ? C1 C5 1.4200 . ? C1 C2 1.4200 . ? C1 C11 1.477(11) . ? C2 C3 1.4200 . ? C3 C4 1.4200 . ? C4 C5 1.4200 . ? C6 C10 1.4200 . ? C6 C7 1.4200 . ? C6 C16 1.441(11) . ? C7 C8 1.4200 . ? C8 C9 1.4200 . ? C9 C10 1.4200 . ? C11 C12 1.355(14) . ? C11 C15 1.406(15) . ? C12 C13 1.365(16) . ? C13 N1 1.337(15) . ? N1 C14 1.323(14) . ? C14 C15 1.366(14) . ? C16 C20 1.391(14) . ? C16 C17 1.389(15) . ? C17 C18 1.371(15) . ? C18 N2 1.324(14) . ? N2 C19 1.342(14) . ? C19 C20 1.380(14) . ? Fe2 C23 2.032(8) . ? Fe2 C27 2.037(8) . ? Fe2 C22 2.040(8) . ? Fe2 C24 2.040(8) . ? Fe2 C26 2.041(7) . ? Fe2 C28 2.050(8) . ? Fe2 C21 2.052(8) . ? Fe2 C25 2.052(8) . ? Fe2 C30 2.055(8) . ? Fe2 C29 2.061(8) . ? C21 C22 1.4200 . ? C21 C25 1.4200 . ? C21 C31 1.472(11) . ? C22 C23 1.4200 . ? C23 C24 1.4200 . ? C24 C25 1.4200 . ? C26 C27 1.4200 . ? C26 C30 1.4200 . ? C26 C36 1.480(11) . ? C27 C28 1.4200 . ? C28 C29 1.4200 . ? C29 C30 1.4200 . ? C31 C35 1.368(15) . ? C31 C32 1.403(15) . ? C32 C33 1.350(15) . ? C33 N3 1.314(13) . ? N3 C34 1.358(14) . ? C34 C35 1.386(15) . ? C36 C37 1.377(14) . ? C36 C40 1.426(14) . ? C37 C38 1.384(15) . ? C38 N4 1.335(14) . ? N4 C39 1.352(14) . ? C39 C40 1.332(14) . ? N5 O1 1.237(13) . ? N5 O3 1.251(13) . ? N5 O2 1.253(14) . ? N6 O5 1.211(15) . ? N6 O6 1.216(16) . ? N6 O4 1.275(16) . ? 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 Ag1 N3 172.8(4) . . ? N4 Ag2 N2 171.3(4) . . ? C2 Fe1 C1 40.77(14) . . ? C2 Fe1 C3 40.78(14) . . ? C1 Fe1 C3 68.55(17) . . ? C2 Fe1 C9 159.0(3) . . ? C1 Fe1 C9 158.1(3) . . ? C3 Fe1 C9 122.1(3) . . ? C2 Fe1 C5 68.50(17) . . ? C1 Fe1 C5 40.67(14) . . ? C3 Fe1 C5 68.44(17) . . ? C9 Fe1 C5 121.6(3) . . ? C2 Fe1 C10 158.7(3) . . ? C1 Fe1 C10 123.8(3) . . ? C3 Fe1 C10 160.0(3) . . ? C9 Fe1 C10 40.65(14) . . ? C5 Fe1 C10 109.5(3) . . ? C2 Fe1 C4 68.51(17) . . ? C1 Fe1 C4 68.43(18) . . ? C3 Fe1 C4 40.68(14) . . ? C9 Fe1 C4 106.2(3) . . ? C5 Fe1 C4 40.61(14) . . ? C10 Fe1 C4 124.8(3) . . ? C2 Fe1 C8 122.7(3) . . ? C1 Fe1 C8 160.8(3) . . ? C3 Fe1 C8 105.0(3) . . ? C9 Fe1 C8 40.65(13) . . ? C5 Fe1 C8 155.6(3) . . ? C10 Fe1 C8 68.24(17) . . ? C4 Fe1 C8 119.2(3) . . ? C2 Fe1 C6 122.7(3) . . ? C1 Fe1 C6 110.3(3) . . ? C3 Fe1 C6 156.3(4) . . ? C9 Fe1 C6 68.15(17) . . ? C5 Fe1 C6 127.1(3) . . ? C10 Fe1 C6 40.44(14) . . ? C4 Fe1 C6 162.6(4) . . ? C8 Fe1 C6 68.01(17) . . ? C2 Fe1 C7 107.4(3) . . ? C1 Fe1 C7 125.8(3) . . ? C3 Fe1 C7 119.8(3) . . ? C9 Fe1 C7 68.15(17) . . ? C5 Fe1 C7 163.2(3) . . ? C10 Fe1 C7 68.01(17) . . ? C4 Fe1 C7 154.7(3) . . ? C8 Fe1 C7 40.44(14) . . ? C6 Fe1 C7 40.31(14) . . ? C5 C1 C2 108.0 . . ? C5 C1 C11 127.8(7) . . ? C2 C1 C11 124.1(7) . . ? C5 C1 Fe1 69.9(3) . . ? C2 C1 Fe1 69.5(3) . . ? C11 C1 Fe1 124.5(6) . . ? C3 C2 C1 108.0 . . ? C3 C2 Fe1 69.7(3) . . ? C1 C2 Fe1 69.8(3) . . ? C2 C3 C4 108.0 . . ? C2 C3 Fe1 69.5(3) . . ? C4 C3 Fe1 69.9(3) . . ? C5 C4 C3 108.0 . . ? C5 C4 Fe1 69.7(3) . . ? C3 C4 Fe1 69.4(3) . . ? C1 C5 C4 108.0 . . ? C1 C5 Fe1 69.4(3) . . ? C4 C5 Fe1 69.7(3) . . ? C10 C6 C7 108.0 . . ? C10 C6 C16 125.3(7) . . ? C7 C6 C16 126.7(7) . . ? C10 C6 Fe1 69.3(3) . . ? C7 C6 Fe1 69.8(3) . . ? C16 C6 Fe1 126.7(7) . . ? C8 C7 C6 108.0 . . ? C8 C7 Fe1 69.3(3) . . ? C6 C7 Fe1 69.8(3) . . ? C7 C8 C9 108.0 . . ? C7 C8 Fe1 70.3(3) . . ? C9 C8 Fe1 69.4(3) . . ? C8 C9 C10 108.0 . . ? C8 C9 Fe1 70.0(3) . . ? C10 C9 Fe1 70.0(3) . . ? C6 C10 C9 108.0 . . ? C6 C10 Fe1 70.3(3) . . ? C9 C10 Fe1 69.4(3) . . ? C12 C11 C15 116.4(10) . . ? C12 C11 C1 123.6(10) . . ? C15 C11 C1 120.0(10) . . ? C11 C12 C13 118.9(12) . . ? N1 C13 C12 125.6(12) . . ? C14 N1 C13 115.6(10) . . ? C14 N1 Ag1 120.3(8) . . ? C13 N1 Ag1 124.0(9) . . ? N1 C14 C15 122.8(12) . . ? C14 C15 C11 120.6(12) . . ? C20 C16 C17 115.5(10) . . ? C20 C16 C6 122.7(10) . . ? C17 C16 C6 121.8(10) . . ? C18 C17 C16 120.7(12) . . ? N2 C18 C17 123.3(12) . . ? C18 N2 C19 117.5(10) . . ? C18 N2 Ag2 119.5(8) . . ? C19 N2 Ag2 122.9(8) . . ? N2 C19 C20 122.1(11) . . ? C19 C20 C16 120.8(11) . . ? C23 Fe2 C27 119.6(4) . . ? C23 Fe2 C22 40.82(15) . . ? C27 Fe2 C22 107.1(3) . . ? C23 Fe2 C24 40.82(15) . . ? C27 Fe2 C24 154.8(4) . . ? C22 Fe2 C24 68.55(18) . . ? C23 Fe2 C26 156.6(4) . . ? C27 Fe2 C26 40.76(14) . . ? C22 Fe2 C26 122.8(3) . . ? C24 Fe2 C26 162.2(4) . . ? C23 Fe2 C28 104.8(3) . . ? C27 Fe2 C28 40.66(15) . . ? C22 Fe2 C28 122.6(3) . . ? C24 Fe2 C28 119.2(3) . . ? C26 Fe2 C28 68.35(18) . . ? C23 Fe2 C21 68.46(18) . . ? C27 Fe2 C21 125.5(3) . . ? C22 Fe2 C21 40.61(14) . . ? C24 Fe2 C21 68.31(18) . . ? C26 Fe2 C21 110.2(3) . . ? C28 Fe2 C21 160.6(4) . . ? C23 Fe2 C25 68.46(18) . . ? C27 Fe2 C25 163.0(3) . . ? C22 Fe2 C25 68.32(18) . . ? C24 Fe2 C25 40.61(15) . . ? C26 Fe2 C25 126.8(3) . . ? C28 Fe2 C25 155.8(3) . . ? C21 Fe2 C25 40.48(14) . . ? C23 Fe2 C30 159.5(4) . . ? C27 Fe2 C30 68.31(17) . . ? C22 Fe2 C30 159.1(3) . . ? C24 Fe2 C30 124.4(4) . . ? C26 Fe2 C30 40.57(14) . . ? C28 Fe2 C30 68.08(18) . . ? C21 Fe2 C30 124.3(3) . . ? C25 Fe2 C30 109.7(3) . . ? C23 Fe2 C29 122.0(3) . . ? C27 Fe2 C29 68.20(18) . . ? C22 Fe2 C29 158.8(4) . . ? C24 Fe2 C29 106.3(3) . . ? C26 Fe2 C29 68.14(17) . . ? C28 Fe2 C29 40.42(14) . . ? C21 Fe2 C29 158.5(4) . . ? C25 Fe2 C29 122.1(3) . . ? C30 Fe2 C29 40.37(14) . . ? C22 C21 C25 108.0 . . ? C22 C21 C31 127.4(8) . . ? C25 C21 C31 124.6(8) . . ? C22 C21 Fe2 69.2(3) . . ? C25 C21 Fe2 69.8(3) . . ? C31 C21 Fe2 127.3(7) . . ? C21 C22 C23 108.0 . . ? C21 C22 Fe2 70.2(3) . . ? C23 C22 Fe2 69.3(3) . . ? C24 C23 C22 108.0 . . ? C24 C23 Fe2 69.9(3) . . ? C22 C23 Fe2 69.9(3) . . ? C25 C24 C23 108.0 . . ? C25 C24 Fe2 70.2(3) . . ? C23 C24 Fe2 69.3(3) . . ? C24 C25 C21 108.0 . . ? C24 C25 Fe2 69.2(3) . . ? C21 C25 Fe2 69.8(3) . . ? C27 C26 C30 108.0 . . ? C27 C26 C36 125.6(7) . . ? C30 C26 C36 126.4(7) . . ? C27 C26 Fe2 69.5(3) . . ? C30 C26 Fe2 70.3(3) . . ? C36 C26 Fe2 124.3(6) . . ? C26 C27 C28 108.0 . . ? C26 C27 Fe2 69.7(3) . . ? C28 C27 Fe2 70.1(3) . . ? C29 C28 C27 108.0 . . ? C29 C28 Fe2 70.2(3) . . ? C27 C28 Fe2 69.2(3) . . ? C28 C29 C30 108.0 . . ? C28 C29 Fe2 69.4(3) . . ? C30 C29 Fe2 69.6(3) . . ? C29 C30 C26 108.0 . . ? C29 C30 Fe2 70.0(3) . . ? C26 C30 Fe2 69.2(3) . . ? C35 C31 C32 116.5(10) . . ? C35 C31 C21 122.2(11) . . ? C32 C31 C21 121.4(10) . . ? C33 C32 C31 120.0(12) . . ? N3 C33 C32 124.5(12) . . ? C33 N3 C34 116.6(10) . . ? C33 N3 Ag1 125.4(8) . . ? C34 N3 Ag1 117.9(8) . . ? N3 C34 C35 122.4(12) . . ? C31 C35 C34 120.1(12) . . ? C37 C36 C40 116.7(10) . . ? C37 C36 C26 122.1(10) . . ? C40 C36 C26 121.2(9) . . ? C36 C37 C38 119.0(12) . . ? N4 C38 C37 124.3(12) . . ? C38 N4 C39 115.9(10) . . ? C38 N4 Ag2 120.4(9) . . ? C39 N4 Ag2 123.6(8) . . ? C40 C39 N4 124.4(12) . . ? C39 C40 C36 119.7(11) . . ? O1 N5 O3 122.7(14) . . ? O1 N5 O2 119.3(14) . . ? O3 N5 O2 118.0(13) . . ? O5 N6 O6 123.9(18) . . ? O5 N6 O4 121.3(18) . . ? O6 N6 O4 114.8(15) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.948 _refine_diff_density_min -0.825 _refine_diff_density_rms 0.137 data_mb003 _database_code_CSD 177938 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H16 Fe N2' _chemical_formula_weight 340.20 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' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 7.746(6) _cell_length_b 10.462(9) _cell_length_c 19.738(9) _cell_angle_alpha 90.00 _cell_angle_beta 106.60(6) _cell_angle_gamma 90.00 _cell_volume 1532.9(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 0.984 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 1.00 _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 'Nonius CAD4 - point detector' _diffrn_measurement_method 'w/2 theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2778 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.1027 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2694 _reflns_number_gt 1316 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0987P)^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 2694 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1507 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1786 _refine_ls_wR_factor_gt 0.1375 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _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 Fe Fe 0.20735(11) -0.18480(8) -0.33103(4) 0.0461(3) Uani 1 1 d . . . C1 C 0.0816(6) -0.0748(4) -0.27413(19) 0.0470(15) Uani 1 1 d G . . C2 C -0.0432(5) -0.1598(4) -0.3189(3) 0.0633(19) Uani 1 1 d G . . H2 H -0.1115 -0.2214 -0.3043 0.076 Uiso 1 1 calc R . . C3 C -0.0454(7) -0.1342(5) -0.3898(2) 0.086(3) Uani 1 1 d G . . H3 H -0.1154 -0.1760 -0.4298 0.103 Uiso 1 1 calc R . . C4 C 0.0780(8) -0.0334(5) -0.3888(2) 0.078(2) Uani 1 1 d G . . H4 H 0.1030 0.0024 -0.4281 0.094 Uiso 1 1 calc R . . C5 C 0.1565(6) 0.0033(4) -0.3174(3) 0.0571(17) Uani 1 1 d G . . H5 H 0.2419 0.0673 -0.3016 0.069 Uiso 1 1 calc R . . C6 C 0.1266(8) -0.0690(6) -0.1970(3) 0.0467(15) Uani 1 1 d . . . C7 C 0.2523(9) 0.0169(6) -0.1584(3) 0.0554(17) Uani 1 1 d . . . H7 H 0.3138 0.0697 -0.1815 0.066 Uiso 1 1 calc R . . C8 C 0.2872(11) 0.0249(8) -0.0864(4) 0.079(2) Uani 1 1 d . . . H8 H 0.3716 0.0848 -0.0626 0.095 Uiso 1 1 calc R . . N1 N 0.2091(11) -0.0468(8) -0.0487(4) 0.093(2) Uani 1 1 d . . . C9 C 0.0927(13) -0.1310(9) -0.0864(5) 0.088(3) Uani 1 1 d . . . H9 H 0.0373 -0.1846 -0.0613 0.106 Uiso 1 1 calc R . . C10 C 0.0447(10) -0.1479(7) -0.1587(4) 0.072(2) Uani 1 1 d . . . H10 H -0.0390 -0.2095 -0.1808 0.086 Uiso 1 1 calc R . . C11 C 0.4020(6) -0.2901(4) -0.26246(16) 0.0424(14) Uani 1 1 d G . . C12 C 0.2782(6) -0.3715(4) -0.3102(3) 0.0604(19) Uani 1 1 d G . . H12 H 0.2082 -0.4347 -0.2980 0.072 Uiso 1 1 calc R . . C13 C 0.2801(7) -0.3393(5) -0.37990(19) 0.077(2) Uani 1 1 d G . . H13 H 0.2116 -0.3778 -0.4213 0.092 Uiso 1 1 calc R . . C14 C 0.4051(7) -0.2381(5) -0.3752(2) 0.073(2) Uani 1 1 d G . . H14 H 0.4328 -0.1986 -0.4130 0.087 Uiso 1 1 calc R . . C15 C 0.4804(5) -0.2077(4) -0.3026(2) 0.0572(18) Uani 1 1 d G . . H15 H 0.5661 -0.1448 -0.2846 0.069 Uiso 1 1 calc R . . C16 C 0.4488(7) -0.2943(5) -0.1850(3) 0.0405(14) Uani 1 1 d . . . C17 C 0.5715(9) -0.2128(6) -0.1428(3) 0.0552(17) Uani 1 1 d . . . H17 H 0.6234 -0.1488 -0.1632 0.066 Uiso 1 1 calc R . . C18 C 0.6189(10) -0.2254(8) -0.0698(4) 0.072(2) Uani 1 1 d . . . H18 H 0.7059 -0.1702 -0.0428 0.086 Uiso 1 1 calc R . . N2 N 0.5475(9) -0.3114(8) -0.0360(3) 0.084(2) Uani 1 1 d . . . C19 C 0.4302(11) -0.3861(9) -0.0771(4) 0.077(2) Uani 1 1 d . . . H19 H 0.3792 -0.4483 -0.0552 0.093 Uiso 1 1 calc R . . C20 C 0.3724(9) -0.3835(6) -0.1502(3) 0.0565(17) Uani 1 1 d . . . H20 H 0.2848 -0.4401 -0.1753 0.068 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 Fe 0.0443(5) 0.0462(5) 0.0456(5) -0.0036(5) 0.0096(3) 0.0043(5) C1 0.032(3) 0.037(3) 0.070(4) -0.008(3) 0.011(3) 0.009(3) C2 0.040(4) 0.064(5) 0.081(5) -0.009(4) 0.009(3) 0.000(3) C3 0.054(5) 0.094(6) 0.085(6) -0.014(5) -0.019(4) 0.021(4) C4 0.094(6) 0.079(6) 0.055(5) 0.007(4) 0.011(4) 0.025(5) C5 0.063(4) 0.046(4) 0.058(4) 0.008(3) 0.011(4) 0.007(3) C6 0.038(3) 0.037(3) 0.068(4) -0.001(3) 0.020(3) 0.008(3) C7 0.067(5) 0.050(4) 0.056(4) -0.013(3) 0.028(3) -0.007(3) C8 0.086(6) 0.080(6) 0.075(6) -0.019(4) 0.031(5) -0.007(5) N1 0.108(6) 0.105(6) 0.078(5) -0.001(5) 0.046(4) -0.004(5) C9 0.102(7) 0.090(6) 0.092(7) 0.021(5) 0.057(6) -0.007(5) C10 0.073(5) 0.070(5) 0.081(6) 0.007(4) 0.036(4) -0.008(4) C11 0.042(3) 0.040(4) 0.046(3) -0.004(3) 0.015(3) 0.006(3) C12 0.073(5) 0.039(3) 0.062(5) -0.005(3) 0.008(4) 0.009(3) C13 0.103(6) 0.071(5) 0.053(4) -0.015(4) 0.018(4) 0.030(5) C14 0.080(5) 0.091(6) 0.058(5) 0.011(4) 0.037(4) 0.029(5) C15 0.049(4) 0.070(5) 0.065(4) 0.012(4) 0.036(3) 0.006(3) C16 0.034(3) 0.036(3) 0.049(3) -0.001(3) 0.010(3) 0.011(3) C17 0.059(4) 0.054(4) 0.052(4) -0.003(3) 0.014(3) -0.004(3) C18 0.069(5) 0.080(6) 0.061(5) -0.009(4) 0.009(4) 0.000(4) N2 0.086(5) 0.107(6) 0.053(4) 0.010(4) 0.009(4) 0.015(5) C19 0.073(5) 0.097(6) 0.061(5) 0.028(5) 0.019(4) 0.010(5) C20 0.053(4) 0.059(4) 0.060(4) 0.011(3) 0.019(3) -0.001(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 Fe C1 2.040(4) . ? Fe C2 2.039(5) . ? Fe C11 2.038(4) . ? Fe C12 2.039(5) . ? Fe C5 2.040(5) . ? Fe C3 2.040(5) . ? Fe C15 2.042(5) . ? Fe C4 2.040(5) . ? Fe C13 2.043(5) . ? Fe C14 2.045(5) . ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C1 C6 1.462(7) . ? C2 C3 1.4200 . ? C3 C4 1.4200 . ? C4 C5 1.4200 . ? C6 C7 1.382(8) . ? C6 C10 1.390(9) . ? C7 C8 1.372(9) . ? C8 N1 1.319(9) . ? N1 C9 1.327(11) . ? C9 C10 1.378(11) . ? C11 C12 1.4200 . ? C11 C15 1.4200 . ? C11 C16 1.468(6) . ? C12 C13 1.4200 . ? C13 C14 1.4200 . ? C14 C15 1.4200 . ? C16 C17 1.367(8) . ? C16 C20 1.388(8) . ? C17 C18 1.388(9) . ? C18 N2 1.331(9) . ? N2 C19 1.294(10) . ? C19 C20 1.382(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 C1 Fe C2 40.75(8) . . ? C1 Fe C11 108.57(16) . . ? C2 Fe C11 122.66(19) . . ? C1 Fe C12 124.96(18) . . ? C2 Fe C12 108.05(17) . . ? C11 Fe C12 40.77(8) . . ? C1 Fe C5 40.74(8) . . ? C2 Fe C5 68.56(9) . . ? C11 Fe C5 124.61(17) . . ? C12 Fe C5 161.56(19) . . ? C1 Fe C3 68.56(11) . . ? C2 Fe C3 40.74(9) . . ? C11 Fe C3 157.8(2) . . ? C12 Fe C3 121.52(19) . . ? C5 Fe C3 68.55(11) . . ? C1 Fe C15 122.37(18) . . ? C2 Fe C15 158.3(2) . . ? C11 Fe C15 40.74(8) . . ? C12 Fe C15 68.54(9) . . ? C5 Fe C15 107.51(17) . . ? C3 Fe C15 159.6(2) . . ? C1 Fe C4 68.55(11) . . ? C2 Fe C4 68.55(11) . . ? C11 Fe C4 160.6(2) . . ? C12 Fe C4 156.6(2) . . ? C5 Fe C4 40.73(9) . . ? C3 Fe C4 40.73(8) . . ? C15 Fe C4 123.3(2) . . ? C1 Fe C13 161.1(2) . . ? C2 Fe C13 123.9(2) . . ? C11 Fe C13 68.53(11) . . ? C12 Fe C13 40.72(9) . . ? C5 Fe C13 156.3(2) . . ? C3 Fe C13 106.67(17) . . ? C15 Fe C13 68.46(11) . . ? C4 Fe C13 120.55(19) . . ? C1 Fe C14 157.3(2) . . ? C2 Fe C14 159.9(2) . . ? C11 Fe C14 68.49(10) . . ? C12 Fe C14 68.49(10) . . ? C5 Fe C14 121.1(2) . . ? C3 Fe C14 122.9(2) . . ? C15 Fe C14 40.67(9) . . ? C4 Fe C14 106.34(18) . . ? C13 Fe C14 40.66(8) . . ? C2 C1 C5 108.0 . . ? C2 C1 C6 126.2(4) . . ? C5 C1 C6 125.8(4) . . ? C2 C1 Fe 69.62(17) . . ? C5 C1 Fe 69.65(19) . . ? C6 C1 Fe 126.0(3) . . ? C1 C2 C3 108.0 . . ? C1 C2 Fe 69.63(17) . . ? C3 C2 Fe 69.64(18) . . ? C4 C3 C2 108.0 . . ? C4 C3 Fe 69.65(18) . . ? C2 C3 Fe 69.61(18) . . ? C5 C4 C3 108.0 . . ? C5 C4 Fe 69.63(17) . . ? C3 C4 Fe 69.62(18) . . ? C4 C5 C1 108.0 . . ? C4 C5 Fe 69.64(17) . . ? C1 C5 Fe 69.61(18) . . ? C7 C6 C10 116.4(6) . . ? C7 C6 C1 121.5(6) . . ? C10 C6 C1 122.1(6) . . ? C8 C7 C6 120.7(7) . . ? N1 C8 C7 124.3(8) . . ? C8 N1 C9 114.1(7) . . ? N1 C9 C10 127.3(8) . . ? C9 C10 C6 117.2(7) . . ? C12 C11 C15 108.0 . . ? C12 C11 C16 126.4(4) . . ? C15 C11 C16 125.6(4) . . ? C12 C11 Fe 69.63(18) . . ? C15 C11 Fe 69.77(18) . . ? C16 C11 Fe 128.6(3) . . ? C13 C12 C11 108.0 . . ? C13 C12 Fe 69.79(16) . . ? C11 C12 Fe 69.60(17) . . ? C12 C13 C14 108.0 . . ? C12 C13 Fe 69.49(16) . . ? C14 C13 Fe 69.74(18) . . ? C13 C14 C15 108.0 . . ? C13 C14 Fe 69.60(18) . . ? C15 C14 Fe 69.56(17) . . ? C11 C15 C14 108.0 . . ? C11 C15 Fe 69.49(17) . . ? C14 C15 Fe 69.77(17) . . ? C17 C16 C20 116.0(6) . . ? C17 C16 C11 122.5(5) . . ? C20 C16 C11 121.5(5) . . ? C16 C17 C18 120.3(6) . . ? N2 C18 C17 124.1(7) . . ? C19 N2 C18 114.3(6) . . ? N2 C19 C20 127.1(8) . . ? C19 C20 C16 118.2(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.807 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.084