# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Shankar Pandey' _publ_contact_author_email DSPREWA@YAHOO.COM _publ_section_title ; First examples of homo-/heteroleptic bi-/tri-nuclear complexes containing 5-ferrocenyldipyrromethene ; loop_ _publ_author_name 'Shankar Pandey' 'Prashant Kumar' 'Joan Ribas' 'Ashish Kumar Singh' 'Mahendra Yadav' # Attachment 'CIF_FULL.cif' data_Complex1 _database_code_depnum_ccdc_archive 'CCDC 739912' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H30 Cu Fe2 N4' _chemical_formula_weight 717.90 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.485(4) _cell_length_b 8.1551(10) _cell_length_c 23.249(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.384(18) _cell_angle_gamma 90.00 _cell_volume 5727.0(14) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3320 _cell_measurement_theta_min 3.0191 _cell_measurement_theta_max 32.8505 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2936 _exptl_absorpt_coefficient_mu 1.773 _exptl_absorpt_correction_T_min 0.6859 _exptl_absorpt_correction_T_max 0.7768 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION XCALIBUR-S' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22900 _diffrn_reflns_av_R_equivalents 0.1500 _diffrn_reflns_av_sigmaI/netI 0.1249 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5054 _reflns_number_gt 3520 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.2000P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5054 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1200 _refine_ls_R_factor_gt 0.0886 _refine_ls_wR_factor_ref 0.2988 _refine_ls_wR_factor_gt 0.2311 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 0.02817(3) 0.00200(11) 0.13826(4) 0.0285(4) Uani 1 1 d . . . Fe1 Fe -0.14873(4) -0.30986(14) -0.03546(5) 0.0280(4) Uani 1 1 d . . . Fe2 Fe 0.19333(4) 0.32630(15) 0.34048(5) 0.0331(4) Uani 1 1 d . . . N1 N 0.0238(2) -0.1173(8) 0.0635(3) 0.0260(14) Uani 1 1 d . . . N2 N -0.0297(2) -0.0788(9) 0.1407(3) 0.0333(16) Uani 1 1 d . . . N3 N 0.0306(2) 0.2138(8) 0.1795(3) 0.0301(16) Uani 1 1 d . . . N4 N 0.0921(2) -0.0195(8) 0.1696(3) 0.0271(15) Uani 1 1 d . . . C1 C 0.0540(3) -0.1100(10) 0.0335(3) 0.0319(19) Uani 1 1 d . . . H1 H 0.0796 -0.0424 0.0443 0.038 Uiso 1 1 calc R . . C2 C 0.0431(3) -0.2147(10) -0.0159(3) 0.0313(18) Uani 1 1 d . . . H2 H 0.0597 -0.2311 -0.0437 0.038 Uiso 1 1 calc R . . C3 C 0.0040(3) -0.2894(10) -0.0170(4) 0.0280(17) Uani 1 1 d . . . H3 H -0.0112 -0.3694 -0.0450 0.034 Uiso 1 1 calc R . . C4 C -0.0097(2) -0.2235(10) 0.0328(3) 0.0276(17) Uani 1 1 d . . . C5 C -0.0491(2) -0.2489(9) 0.0478(3) 0.0276(18) Uani 1 1 d . . . C6 C -0.0581(3) -0.1853(9) 0.0994(4) 0.0293(19) Uani 1 1 d . . . C7 C -0.0945(3) -0.2197(10) 0.1231(4) 0.0332(19) Uani 1 1 d . . . H7 H -0.1192 -0.2871 0.1048 0.040 Uiso 1 1 calc R . . C8 C -0.0875(3) -0.1394(10) 0.1761(4) 0.0323(18) Uani 1 1 d . . . H8 H -0.1058 -0.1430 0.2022 0.039 Uiso 1 1 calc R . . C9 C -0.0481(3) -0.0504(12) 0.1850(3) 0.033(2) Uani 1 1 d . . . H9 H -0.0361 0.0204 0.2181 0.040 Uiso 1 1 calc R . . C10 C -0.0038(3) 0.3174(11) 0.1681(4) 0.035(2) Uani 1 1 d . . . H10 H -0.0338 0.2853 0.1518 0.041 Uiso 1 1 calc R . . C11 C 0.0099(3) 0.4777(11) 0.1829(4) 0.037(2) Uani 1 1 d . . . H11 H -0.0084 0.5722 0.1778 0.045 Uiso 1 1 calc R . . C12 C 0.0547(3) 0.4729(10) 0.2062(4) 0.0322(19) Uani 1 1 d . . . H12 H 0.0734 0.5640 0.2210 0.039 Uiso 1 1 calc R . . C13 C 0.0685(3) 0.3077(9) 0.2046(3) 0.0268(17) Uani 1 1 d . . . C14 C 0.1116(2) 0.2419(10) 0.2233(3) 0.0271(17) Uani 1 1 d . . . C15 C 0.1227(2) 0.0836(9) 0.2084(3) 0.0264(17) Uani 1 1 d . . . C16 C 0.1635(3) -0.0026(11) 0.2279(4) 0.034(2) Uani 1 1 d . . . H16 H 0.1902 0.0381 0.2544 0.040 Uiso 1 1 calc R . . C17 C 0.1578(3) -0.1544(10) 0.2018(4) 0.0302(18) Uani 1 1 d . . . H17 H 0.1792 -0.2392 0.2067 0.036 Uiso 1 1 calc R . . C18 C 0.1132(3) -0.1586(10) 0.1661(4) 0.035(2) Uani 1 1 d . . . H18 H 0.0999 -0.2500 0.1425 0.041 Uiso 1 1 calc R . . C19 C -0.0828(2) -0.3570(9) 0.0056(4) 0.0287(18) Uani 1 1 d . . . C20 C -0.0923(2) -0.3544(10) -0.0590(3) 0.0286(18) Uani 1 1 d . . . H20 H -0.0793 -0.2824 -0.0814 0.034 Uiso 1 1 calc R . . C21 C -0.1240(3) -0.4768(10) -0.0832(4) 0.036(2) Uani 1 1 d . . . H21 H -0.1357 -0.5027 -0.1245 0.043 Uiso 1 1 calc R . . C22 C -0.1350(3) -0.5536(11) -0.0350(4) 0.040(2) Uani 1 1 d . . . H22 H -0.1558 -0.6401 -0.0385 0.048 Uiso 1 1 calc R . . C23 C -0.1102(3) -0.4811(10) 0.0198(4) 0.0302(19) Uani 1 1 d . . . H23 H -0.1116 -0.5101 0.0588 0.036 Uiso 1 1 calc R . . C24 C -0.1630(3) -0.0768(11) -0.0148(4) 0.041(2) Uani 1 1 d . . . H24 H -0.1426 -0.0009 0.0088 0.049 Uiso 1 1 calc R . . C25 C -0.1728(3) -0.0967(10) -0.0768(4) 0.035(2) Uani 1 1 d . . . H25 H -0.1603 -0.0346 -0.1025 0.042 Uiso 1 1 calc R . . C26 C -0.2043(3) -0.2235(11) -0.0955(4) 0.038(2) Uani 1 1 d . . . H26 H -0.2163 -0.2616 -0.1354 0.046 Uiso 1 1 calc R . . C27 C -0.2148(3) -0.2845(12) -0.0432(4) 0.038(2) Uani 1 1 d . . . H27 H -0.2348 -0.3706 -0.0418 0.046 Uiso 1 1 calc R . . C28 C -0.1891(3) -0.1899(11) 0.0063(4) 0.037(2) Uani 1 1 d . . . H28 H -0.1895 -0.2014 0.0468 0.045 Uiso 1 1 calc R . . C29 C 0.1471(3) 0.3562(9) 0.2574(3) 0.0287(18) Uani 1 1 d . . . C30 C 0.1421(3) 0.4782(10) 0.2996(4) 0.038(2) Uani 1 1 d . . . H30 H 0.1164 0.4959 0.3125 0.046 Uiso 1 1 calc R . . C31 C 0.1831(3) 0.5693(10) 0.3190(4) 0.0315(19) Uani 1 1 d . . . H31 H 0.1890 0.6593 0.3460 0.038 Uiso 1 1 calc R . . C32 C 0.2130(3) 0.4991(9) 0.2902(4) 0.032(2) Uani 1 1 d . . . H32 H 0.2426 0.5337 0.2950 0.038 Uiso 1 1 calc R . . C33 C 0.1913(3) 0.3693(10) 0.2532(4) 0.0334(19) Uani 1 1 d . . . H33 H 0.2042 0.3015 0.2293 0.040 Uiso 1 1 calc R . . C34 C 0.1910(3) 0.0968(11) 0.3748(4) 0.044(2) Uani 1 1 d . . . H34 H 0.1740 0.0070 0.3546 0.053 Uiso 1 1 calc R . . C35 C 0.1765(5) 0.2150(14) 0.4096(5) 0.065(3) Uani 1 1 d . . . H35 H 0.1483 0.2175 0.4169 0.078 Uiso 1 1 calc R . . C36 C 0.2107(6) 0.3271(14) 0.4313(4) 0.083(5) Uani 1 1 d . . . H36 H 0.2098 0.4210 0.4551 0.100 Uiso 1 1 calc R . . C37 C 0.2462(5) 0.2756(15) 0.4117(6) 0.082(5) Uani 1 1 d . . . H37 H 0.2744 0.3274 0.4212 0.099 Uiso 1 1 calc R . . C38 C 0.2341(3) 0.1326(12) 0.3749(5) 0.053(3) Uani 1 1 d . . . H38 H 0.2518 0.0745 0.3548 0.064 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 Cu1 0.0127(6) 0.0340(7) 0.0308(6) -0.0045(4) -0.0067(4) -0.0023(3) Fe1 0.0127(6) 0.0327(7) 0.0304(7) -0.0022(5) -0.0075(5) 0.0006(4) Fe2 0.0251(7) 0.0328(8) 0.0288(7) 0.0008(5) -0.0128(5) -0.0039(5) N1 0.015(3) 0.030(4) 0.028(3) 0.000(3) -0.002(3) 0.000(2) N2 0.017(3) 0.038(4) 0.036(4) -0.002(3) -0.008(3) -0.006(3) N3 0.013(3) 0.035(4) 0.033(3) -0.004(3) -0.008(3) -0.003(3) N4 0.018(3) 0.035(4) 0.022(3) -0.003(3) -0.005(3) -0.004(3) C1 0.016(4) 0.036(5) 0.037(4) 0.002(4) -0.005(3) 0.000(3) C2 0.018(4) 0.038(5) 0.030(4) 0.010(4) -0.006(3) 0.001(3) C3 0.021(4) 0.025(4) 0.032(4) -0.001(3) -0.001(3) 0.003(3) C4 0.013(4) 0.030(4) 0.031(4) 0.000(3) -0.008(3) 0.003(3) C5 0.017(4) 0.022(4) 0.032(4) 0.004(3) -0.013(3) -0.003(3) C6 0.019(4) 0.026(4) 0.031(4) 0.000(3) -0.014(3) 0.002(3) C7 0.013(4) 0.042(5) 0.037(4) 0.000(4) -0.007(3) 0.003(3) C8 0.022(4) 0.036(5) 0.032(4) -0.001(4) -0.002(3) 0.001(3) C9 0.016(4) 0.064(6) 0.020(4) -0.011(4) 0.006(3) 0.003(4) C10 0.016(4) 0.052(6) 0.030(4) -0.002(4) -0.005(3) 0.001(3) C11 0.022(5) 0.054(6) 0.032(4) -0.001(4) -0.001(3) 0.011(4) C12 0.024(4) 0.040(5) 0.029(4) 0.005(4) 0.001(3) -0.001(3) C13 0.013(4) 0.035(5) 0.027(4) -0.004(3) -0.004(3) 0.000(3) C14 0.015(4) 0.031(4) 0.028(4) -0.007(3) -0.006(3) 0.000(3) C15 0.020(4) 0.023(4) 0.027(4) 0.003(3) -0.006(3) 0.000(3) C16 0.011(4) 0.056(6) 0.028(4) -0.003(4) -0.005(3) 0.002(3) C17 0.014(4) 0.035(5) 0.035(4) 0.003(3) -0.003(3) 0.005(3) C18 0.022(4) 0.033(5) 0.037(5) 0.000(4) -0.011(3) -0.002(3) C19 0.015(4) 0.016(4) 0.047(5) -0.005(3) -0.005(3) 0.005(3) C20 0.011(4) 0.041(5) 0.030(4) -0.005(3) 0.000(3) 0.004(3) C21 0.019(4) 0.041(5) 0.039(5) -0.006(4) -0.006(3) 0.002(3) C22 0.023(4) 0.026(5) 0.057(6) -0.005(4) -0.013(4) -0.001(3) C23 0.021(4) 0.036(5) 0.029(4) 0.009(3) 0.000(3) -0.002(3) C24 0.024(5) 0.027(5) 0.058(6) -0.015(4) -0.008(4) 0.007(3) C25 0.033(5) 0.025(4) 0.042(5) 0.012(4) 0.004(4) 0.008(3) C26 0.027(5) 0.043(5) 0.032(4) -0.001(4) -0.011(4) 0.009(4) C27 0.011(4) 0.060(6) 0.039(5) -0.003(4) 0.000(3) 0.002(4) C28 0.015(4) 0.054(6) 0.037(5) -0.002(4) -0.003(3) 0.006(3) C29 0.020(4) 0.026(4) 0.030(4) 0.006(3) -0.009(3) -0.003(3) C30 0.022(5) 0.041(5) 0.038(5) 0.002(4) -0.013(4) -0.006(3) C31 0.031(5) 0.019(4) 0.034(4) -0.002(3) -0.008(3) 0.002(3) C32 0.024(5) 0.034(5) 0.030(4) 0.005(3) -0.004(3) -0.006(3) C33 0.023(4) 0.029(5) 0.039(4) 0.006(4) -0.008(3) -0.003(3) C34 0.044(6) 0.027(5) 0.045(5) 0.008(4) -0.013(4) 0.003(4) C35 0.087(10) 0.054(7) 0.051(6) 0.018(5) 0.014(6) 0.010(6) C36 0.161(16) 0.047(7) 0.017(5) 0.002(4) -0.016(7) 0.002(8) C37 0.073(9) 0.048(7) 0.080(9) 0.041(7) -0.053(7) -0.032(6) C38 0.041(6) 0.032(5) 0.069(7) 0.017(5) -0.012(5) 0.017(4) _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 N4 1.946(6) . ? Cu1 N2 1.952(7) . ? Cu1 N1 1.962(6) . ? Cu1 N3 1.967(7) . ? Fe1 C25 2.027(8) . ? Fe1 C26 2.030(8) . ? Fe1 C22 2.033(9) . ? Fe1 C20 2.034(8) . ? Fe1 C24 2.041(8) . ? Fe1 C21 2.045(9) . ? Fe1 C27 2.046(8) . ? Fe1 C23 2.048(8) . ? Fe1 C28 2.053(9) . ? Fe1 C19 2.061(7) . ? Fe2 C36 2.027(10) . ? Fe2 C37 2.032(10) . ? Fe2 C32 2.036(8) . ? Fe2 C35 2.042(11) . ? Fe2 C33 2.043(9) . ? Fe2 C30 2.044(9) . ? Fe2 C34 2.044(9) . ? Fe2 C31 2.047(8) . ? Fe2 C38 2.050(9) . ? Fe2 C29 2.079(7) . ? N1 C1 1.330(10) . ? N1 C4 1.395(9) . ? N2 C9 1.339(10) . ? N2 C6 1.411(10) . ? N3 C10 1.338(10) . ? N3 C13 1.399(10) . ? N4 C18 1.328(10) . ? N4 C15 1.400(9) . ? C1 C2 1.394(12) . ? C1 H1 0.9500 . ? C2 C3 1.365(11) . ? C2 H2 0.9500 . ? C3 C4 1.448(11) . ? C3 H3 0.9500 . ? C4 C5 1.394(11) . ? C5 C6 1.409(12) . ? C5 C19 1.511(10) . ? C6 C7 1.431(12) . ? C7 C8 1.358(11) . ? C7 H7 0.9500 . ? C8 C9 1.400(12) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.389(12) . ? C10 H10 0.9500 . ? C11 C12 1.360(12) . ? C11 H11 0.9500 . ? C12 C13 1.420(11) . ? C12 H12 0.9500 . ? C13 C14 1.410(10) . ? C14 C15 1.406(11) . ? C14 C29 1.499(10) . ? C15 C16 1.422(11) . ? C16 C17 1.367(11) . ? C16 H16 0.9500 . ? C17 C18 1.415(11) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C23 1.426(11) . ? C19 C20 1.446(11) . ? C20 C21 1.411(11) . ? C20 H20 0.9500 . ? C21 C22 1.412(14) . ? C21 H21 0.9500 . ? C22 C23 1.421(11) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.394(12) . ? C24 C28 1.412(13) . ? C24 H24 0.9500 . ? C25 C26 1.412(12) . ? C25 H25 0.9500 . ? C26 C27 1.435(13) . ? C26 H26 0.9500 . ? C27 C28 1.432(12) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C33 1.427(12) . ? C29 C30 1.438(12) . ? C30 C31 1.448(11) . ? C30 H30 0.9500 . ? C31 C32 1.419(13) . ? C31 H31 0.9500 . ? C32 C33 1.412(11) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C38 1.385(15) . ? C34 C35 1.415(16) . ? C34 H34 0.9500 . ? C35 C36 1.394(19) . ? C35 H35 0.9500 . ? C36 C37 1.39(2) . ? C36 H36 0.9500 . ? C37 C38 1.433(17) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 N2 146.5(3) . . ? N4 Cu1 N1 95.4(3) . . ? N2 Cu1 N1 91.4(3) . . ? N4 Cu1 N3 90.2(3) . . ? N2 Cu1 N3 101.0(3) . . ? N1 Cu1 N3 148.3(3) . . ? C25 Fe1 C26 40.7(3) . . ? C25 Fe1 C22 153.1(4) . . ? C26 Fe1 C22 118.9(3) . . ? C25 Fe1 C20 105.3(4) . . ? C26 Fe1 C20 121.7(4) . . ? C22 Fe1 C20 68.1(4) . . ? C25 Fe1 C24 40.1(4) . . ? C26 Fe1 C24 68.5(3) . . ? C22 Fe1 C24 165.8(4) . . ? C20 Fe1 C24 119.8(4) . . ? C25 Fe1 C21 117.5(4) . . ? C26 Fe1 C21 104.1(3) . . ? C22 Fe1 C21 40.5(4) . . ? C20 Fe1 C21 40.5(3) . . ? C24 Fe1 C21 152.9(4) . . ? C25 Fe1 C27 68.7(4) . . ? C26 Fe1 C27 41.2(4) . . ? C22 Fe1 C27 107.9(4) . . ? C20 Fe1 C27 159.6(3) . . ? C24 Fe1 C27 68.9(4) . . ? C21 Fe1 C27 123.6(3) . . ? C25 Fe1 C23 163.4(3) . . ? C26 Fe1 C23 155.6(4) . . ? C22 Fe1 C23 40.7(3) . . ? C20 Fe1 C23 68.8(3) . . ? C24 Fe1 C23 128.2(3) . . ? C21 Fe1 C23 68.7(3) . . ? C27 Fe1 C23 122.1(4) . . ? C25 Fe1 C28 67.5(4) . . ? C26 Fe1 C28 68.4(3) . . ? C22 Fe1 C28 128.4(4) . . ? C20 Fe1 C28 156.5(3) . . ? C24 Fe1 C28 40.4(4) . . ? C21 Fe1 C28 162.9(4) . . ? C27 Fe1 C28 40.9(3) . . ? C23 Fe1 C28 111.4(4) . . ? C25 Fe1 C19 125.0(3) . . ? C26 Fe1 C19 160.4(4) . . ? C22 Fe1 C19 68.3(3) . . ? C20 Fe1 C19 41.3(3) . . ? C24 Fe1 C19 109.0(3) . . ? C21 Fe1 C19 68.8(3) . . ? C27 Fe1 C19 157.7(3) . . ? C23 Fe1 C19 40.6(3) . . ? C28 Fe1 C19 123.1(3) . . ? C36 Fe2 C37 40.0(6) . . ? C36 Fe2 C32 124.1(5) . . ? C37 Fe2 C32 107.3(4) . . ? C36 Fe2 C35 40.1(6) . . ? C37 Fe2 C35 66.6(6) . . ? C32 Fe2 C35 161.5(4) . . ? C36 Fe2 C33 163.4(5) . . ? C37 Fe2 C33 129.3(6) . . ? C32 Fe2 C33 40.5(3) . . ? C35 Fe2 C33 156.4(4) . . ? C36 Fe2 C30 115.3(6) . . ? C37 Fe2 C30 149.3(6) . . ? C32 Fe2 C30 69.0(4) . . ? C35 Fe2 C30 106.8(5) . . ? C33 Fe2 C30 68.6(4) . . ? C36 Fe2 C34 67.9(4) . . ? C37 Fe2 C34 66.8(4) . . ? C32 Fe2 C34 155.2(4) . . ? C35 Fe2 C34 40.5(4) . . ? C33 Fe2 C34 123.4(4) . . ? C30 Fe2 C34 128.8(4) . . ? C36 Fe2 C31 103.2(4) . . ? C37 Fe2 C31 115.6(4) . . ? C32 Fe2 C31 40.7(4) . . ? C35 Fe2 C31 124.4(4) . . ? C33 Fe2 C31 68.4(3) . . ? C30 Fe2 C31 41.5(3) . . ? C34 Fe2 C31 164.1(4) . . ? C36 Fe2 C38 68.9(5) . . ? C37 Fe2 C38 41.1(5) . . ? C32 Fe2 C38 120.0(4) . . ? C35 Fe2 C38 67.9(5) . . ? C33 Fe2 C38 111.1(4) . . ? C30 Fe2 C38 166.8(4) . . ? C34 Fe2 C38 39.5(4) . . ? C31 Fe2 C38 151.6(4) . . ? C36 Fe2 C29 151.7(6) . . ? C37 Fe2 C29 168.2(6) . . ? C32 Fe2 C29 68.4(3) . . ? C35 Fe2 C29 121.0(4) . . ? C33 Fe2 C29 40.5(3) . . ? C30 Fe2 C29 40.8(3) . . ? C34 Fe2 C29 112.2(3) . . ? C31 Fe2 C29 68.8(3) . . ? C38 Fe2 C29 130.5(4) . . ? C1 N1 C4 108.0(6) . . ? C1 N1 Cu1 124.1(5) . . ? C4 N1 Cu1 128.0(5) . . ? C9 N2 C6 107.5(7) . . ? C9 N2 Cu1 125.0(5) . . ? C6 N2 Cu1 127.3(6) . . ? C10 N3 C13 106.5(7) . . ? C10 N3 Cu1 122.6(5) . . ? C13 N3 Cu1 126.5(5) . . ? C18 N4 C15 106.7(6) . . ? C18 N4 Cu1 122.4(5) . . ? C15 N4 Cu1 129.7(5) . . ? N1 C1 C2 111.0(7) . . ? N1 C1 H1 124.5 . . ? C2 C1 H1 124.5 . . ? C3 C2 C1 107.4(8) . . ? C3 C2 H2 126.3 . . ? C1 C2 H2 126.3 . . ? C2 C3 C4 106.9(7) . . ? C2 C3 H3 126.6 . . ? C4 C3 H3 126.6 . . ? C5 C4 N1 124.1(7) . . ? C5 C4 C3 129.2(7) . . ? N1 C4 C3 106.6(7) . . ? C4 C5 C6 124.5(7) . . ? C4 C5 C19 115.9(7) . . ? C6 C5 C19 119.6(7) . . ? C5 C6 N2 124.3(8) . . ? C5 C6 C7 129.1(7) . . ? N2 C6 C7 106.4(7) . . ? C8 C7 C6 108.2(7) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? C7 C8 C9 107.1(8) . . ? C7 C8 H8 126.4 . . ? C9 C8 H8 126.4 . . ? N2 C9 C8 110.7(7) . . ? N2 C9 H9 124.6 . . ? C8 C9 H9 124.6 . . ? N3 C10 C11 111.6(7) . . ? N3 C10 H10 124.2 . . ? C11 C10 H10 124.2 . . ? C12 C11 C10 106.6(8) . . ? C12 C11 H11 126.7 . . ? C10 C11 H11 126.7 . . ? C11 C12 C13 107.8(7) . . ? C11 C12 H12 126.1 . . ? C13 C12 H12 126.1 . . ? N3 C13 C14 123.7(7) . . ? N3 C13 C12 107.4(7) . . ? C14 C13 C12 128.9(7) . . ? C15 C14 C13 124.0(7) . . ? C15 C14 C29 120.0(7) . . ? C13 C14 C29 115.9(7) . . ? N4 C15 C14 122.4(6) . . ? N4 C15 C16 107.7(7) . . ? C14 C15 C16 129.9(7) . . ? C17 C16 C15 108.1(7) . . ? C17 C16 H16 125.9 . . ? C15 C16 H16 125.9 . . ? C16 C17 C18 105.5(7) . . ? C16 C17 H17 127.2 . . ? C18 C17 H17 127.2 . . ? N4 C18 C17 111.9(7) . . ? N4 C18 H18 124.0 . . ? C17 C18 H18 124.0 . . ? C23 C19 C20 106.8(7) . . ? C23 C19 C5 128.7(8) . . ? C20 C19 C5 124.5(8) . . ? C23 C19 Fe1 69.2(4) . . ? C20 C19 Fe1 68.3(4) . . ? C5 C19 Fe1 128.6(5) . . ? C21 C20 C19 108.7(8) . . ? C21 C20 Fe1 70.2(5) . . ? C19 C20 Fe1 70.3(4) . . ? C21 C20 H20 125.7 . . ? C19 C20 H20 125.7 . . ? Fe1 C20 H20 125.4 . . ? C20 C21 C22 107.5(7) . . ? C20 C21 Fe1 69.3(5) . . ? C22 C21 Fe1 69.3(5) . . ? C20 C21 H21 126.2 . . ? C22 C21 H21 126.2 . . ? Fe1 C21 H21 126.7 . . ? C21 C22 C23 109.3(8) . . ? C21 C22 Fe1 70.2(5) . . ? C23 C22 Fe1 70.2(5) . . ? C21 C22 H22 125.4 . . ? C23 C22 H22 125.4 . . ? Fe1 C22 H22 125.9 . . ? C22 C23 C19 107.7(8) . . ? C22 C23 Fe1 69.1(5) . . ? C19 C23 Fe1 70.2(4) . . ? C22 C23 H23 126.1 . . ? C19 C23 H23 126.1 . . ? Fe1 C23 H23 126.2 . . ? C25 C24 C28 107.7(8) . . ? C25 C24 Fe1 69.4(5) . . ? C28 C24 Fe1 70.3(5) . . ? C25 C24 H24 126.2 . . ? C28 C24 H24 126.2 . . ? Fe1 C24 H24 125.7 . . ? C24 C25 C26 109.5(8) . . ? C24 C25 Fe1 70.5(5) . . ? C26 C25 Fe1 69.8(5) . . ? C24 C25 H25 125.2 . . ? C26 C25 H25 125.2 . . ? Fe1 C25 H25 126.1 . . ? C25 C26 C27 107.6(8) . . ? C25 C26 Fe1 69.5(4) . . ? C27 C26 Fe1 70.0(4) . . ? C25 C26 H26 126.2 . . ? C27 C26 H26 126.2 . . ? Fe1 C26 H26 125.9 . . ? C28 C27 C26 106.4(8) . . ? C28 C27 Fe1 69.8(5) . . ? C26 C27 Fe1 68.8(5) . . ? C28 C27 H27 126.8 . . ? C26 C27 H27 126.8 . . ? Fe1 C27 H27 126.2 . . ? C24 C28 C27 108.8(8) . . ? C24 C28 Fe1 69.4(5) . . ? C27 C28 Fe1 69.3(5) . . ? C24 C28 H28 125.6 . . ? C27 C28 H28 125.6 . . ? Fe1 C28 H28 127.3 . . ? C33 C29 C30 107.0(7) . . ? C33 C29 C14 127.4(8) . . ? C30 C29 C14 125.6(8) . . ? C33 C29 Fe2 68.4(4) . . ? C30 C29 Fe2 68.3(4) . . ? C14 C29 Fe2 129.8(5) . . ? C29 C30 C31 107.9(8) . . ? C29 C30 Fe2 70.9(5) . . ? C31 C30 Fe2 69.4(5) . . ? C29 C30 H30 126.1 . . ? C31 C30 H30 126.1 . . ? Fe2 C30 H30 125.2 . . ? C32 C31 C30 107.4(7) . . ? C32 C31 Fe2 69.3(4) . . ? C30 C31 Fe2 69.2(5) . . ? C32 C31 H31 126.3 . . ? C30 C31 H31 126.3 . . ? Fe2 C31 H31 126.8 . . ? C33 C32 C31 108.6(8) . . ? C33 C32 Fe2 70.0(5) . . ? C31 C32 Fe2 70.1(5) . . ? C33 C32 H32 125.7 . . ? C31 C32 H32 125.7 . . ? Fe2 C32 H32 125.8 . . ? C32 C33 C29 109.1(8) . . ? C32 C33 Fe2 69.5(5) . . ? C29 C33 Fe2 71.1(5) . . ? C32 C33 H33 125.4 . . ? C29 C33 H33 125.4 . . ? Fe2 C33 H33 125.5 . . ? C38 C34 C35 109.3(9) . . ? C38 C34 Fe2 70.5(5) . . ? C35 C34 Fe2 69.7(6) . . ? C38 C34 H34 125.3 . . ? C35 C34 H34 125.3 . . ? Fe2 C34 H34 126.1 . . ? C36 C35 C34 108.2(13) . . ? C36 C35 Fe2 69.4(7) . . ? C34 C35 Fe2 69.8(6) . . ? C36 C35 H35 125.9 . . ? C34 C35 H35 125.9 . . ? Fe2 C35 H35 126.4 . . ? C37 C36 C35 107.1(11) . . ? C37 C36 Fe2 70.2(7) . . ? C35 C36 Fe2 70.5(6) . . ? C37 C36 H36 126.4 . . ? C35 C36 H36 126.4 . . ? Fe2 C36 H36 124.4 . . ? C36 C37 C38 109.8(11) . . ? C36 C37 Fe2 69.8(6) . . ? C38 C37 Fe2 70.1(5) . . ? C36 C37 H37 125.1 . . ? C38 C37 H37 125.1 . . ? Fe2 C37 H37 126.6 . . ? C34 C38 C37 105.5(11) . . ? C34 C38 Fe2 70.0(5) . . ? C37 C38 Fe2 68.8(5) . . ? C34 C38 H38 127.2 . . ? C37 C38 H38 127.2 . . ? Fe2 C38 H38 125.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Cu1 N1 C1 -35.7(7) . . . . ? N2 Cu1 N1 C1 177.1(7) . . . . ? N3 Cu1 N1 C1 63.4(8) . . . . ? N4 Cu1 N1 C4 143.4(6) . . . . ? N2 Cu1 N1 C4 -3.7(7) . . . . ? N3 Cu1 N1 C4 -117.4(7) . . . . ? N4 Cu1 N2 C9 74.0(9) . . . . ? N1 Cu1 N2 C9 176.0(7) . . . . ? N3 Cu1 N2 C9 -33.3(8) . . . . ? N4 Cu1 N2 C6 -101.1(7) . . . . ? N1 Cu1 N2 C6 0.9(7) . . . . ? N3 Cu1 N2 C6 151.6(6) . . . . ? N4 Cu1 N3 C10 167.5(7) . . . . ? N2 Cu1 N3 C10 -44.3(7) . . . . ? N1 Cu1 N3 C10 66.9(9) . . . . ? N4 Cu1 N3 C13 14.3(7) . . . . ? N2 Cu1 N3 C13 162.5(6) . . . . ? N1 Cu1 N3 C13 -86.3(8) . . . . ? N2 Cu1 N4 C18 58.0(9) . . . . ? N1 Cu1 N4 C18 -42.8(7) . . . . ? N3 Cu1 N4 C18 168.4(7) . . . . ? N2 Cu1 N4 C15 -107.9(8) . . . . ? N1 Cu1 N4 C15 151.2(7) . . . . ? N3 Cu1 N4 C15 2.5(7) . . . . ? C4 N1 C1 C2 -2.7(9) . . . . ? Cu1 N1 C1 C2 176.6(5) . . . . ? N1 C1 C2 C3 0.6(9) . . . . ? C1 C2 C3 C4 1.7(9) . . . . ? C1 N1 C4 C5 -173.4(7) . . . . ? Cu1 N1 C4 C5 7.3(11) . . . . ? C1 N1 C4 C3 3.6(8) . . . . ? Cu1 N1 C4 C3 -175.7(5) . . . . ? C2 C3 C4 C5 173.6(8) . . . . ? C2 C3 C4 N1 -3.3(8) . . . . ? N1 C4 C5 C6 -7.3(12) . . . . ? C3 C4 C5 C6 176.3(7) . . . . ? N1 C4 C5 C19 174.7(7) . . . . ? C3 C4 C5 C19 -1.7(12) . . . . ? C4 C5 C6 N2 4.3(12) . . . . ? C19 C5 C6 N2 -177.7(7) . . . . ? C4 C5 C6 C7 -171.3(8) . . . . ? C19 C5 C6 C7 6.7(12) . . . . ? C9 N2 C6 C5 -177.2(7) . . . . ? Cu1 N2 C6 C5 -1.4(11) . . . . ? C9 N2 C6 C7 -0.8(9) . . . . ? Cu1 N2 C6 C7 175.0(5) . . . . ? C5 C6 C7 C8 175.4(8) . . . . ? N2 C6 C7 C8 -0.9(9) . . . . ? C6 C7 C8 C9 2.1(9) . . . . ? C6 N2 C9 C8 2.1(10) . . . . ? Cu1 N2 C9 C8 -173.8(5) . . . . ? C7 C8 C9 N2 -2.7(10) . . . . ? C13 N3 C10 C11 1.7(10) . . . . ? Cu1 N3 C10 C11 -156.1(6) . . . . ? N3 C10 C11 C12 -1.7(10) . . . . ? C10 C11 C12 C13 1.0(10) . . . . ? C10 N3 C13 C14 179.5(8) . . . . ? Cu1 N3 C13 C14 -23.8(11) . . . . ? C10 N3 C13 C12 -1.1(9) . . . . ? Cu1 N3 C13 C12 155.6(6) . . . . ? C11 C12 C13 N3 0.0(9) . . . . ? C11 C12 C13 C14 179.5(8) . . . . ? N3 C13 C14 C15 13.3(13) . . . . ? C12 C13 C14 C15 -166.1(8) . . . . ? N3 C13 C14 C29 -171.1(7) . . . . ? C12 C13 C14 C29 9.5(13) . . . . ? C18 N4 C15 C14 -179.1(8) . . . . ? Cu1 N4 C15 C14 -11.4(12) . . . . ? C18 N4 C15 C16 -0.1(9) . . . . ? Cu1 N4 C15 C16 167.6(6) . . . . ? C13 C14 C15 N4 4.6(13) . . . . ? C29 C14 C15 N4 -170.8(7) . . . . ? C13 C14 C15 C16 -174.2(9) . . . . ? C29 C14 C15 C16 10.4(13) . . . . ? N4 C15 C16 C17 -0.2(10) . . . . ? C14 C15 C16 C17 178.8(8) . . . . ? C15 C16 C17 C18 0.3(10) . . . . ? C15 N4 C18 C17 0.3(10) . . . . ? Cu1 N4 C18 C17 -168.5(6) . . . . ? C16 C17 C18 N4 -0.4(10) . . . . ? C4 C5 C19 C23 138.7(8) . . . . ? C6 C5 C19 C23 -39.5(11) . . . . ? C4 C5 C19 C20 -39.4(10) . . . . ? C6 C5 C19 C20 142.4(8) . . . . ? C4 C5 C19 Fe1 -128.1(7) . . . . ? C6 C5 C19 Fe1 53.8(10) . . . . ? C25 Fe1 C19 C23 168.9(5) . . . . ? C26 Fe1 C19 C23 -153.6(9) . . . . ? C22 Fe1 C19 C23 -37.9(5) . . . . ? C20 Fe1 C19 C23 -118.9(7) . . . . ? C24 Fe1 C19 C23 127.2(5) . . . . ? C21 Fe1 C19 C23 -81.6(5) . . . . ? C27 Fe1 C19 C23 46.6(11) . . . . ? C28 Fe1 C19 C23 84.7(6) . . . . ? C25 Fe1 C19 C20 -72.2(6) . . . . ? C26 Fe1 C19 C20 -34.7(12) . . . . ? C22 Fe1 C19 C20 81.0(5) . . . . ? C24 Fe1 C19 C20 -113.9(5) . . . . ? C21 Fe1 C19 C20 37.4(5) . . . . ? C27 Fe1 C19 C20 165.5(8) . . . . ? C23 Fe1 C19 C20 118.9(7) . . . . ? C28 Fe1 C19 C20 -156.3(5) . . . . ? C25 Fe1 C19 C5 45.4(9) . . . . ? C26 Fe1 C19 C5 82.9(13) . . . . ? C22 Fe1 C19 C5 -161.4(9) . . . . ? C20 Fe1 C19 C5 117.6(10) . . . . ? C24 Fe1 C19 C5 3.7(9) . . . . ? C21 Fe1 C19 C5 154.9(9) . . . . ? C27 Fe1 C19 C5 -76.9(12) . . . . ? C23 Fe1 C19 C5 -123.5(10) . . . . ? C28 Fe1 C19 C5 -38.8(9) . . . . ? C23 C19 C20 C21 -1.2(9) . . . . ? C5 C19 C20 C21 177.2(7) . . . . ? Fe1 C19 C20 C21 -59.9(6) . . . . ? C23 C19 C20 Fe1 58.7(5) . . . . ? C5 C19 C20 Fe1 -122.8(7) . . . . ? C25 Fe1 C20 C21 -114.7(5) . . . . ? C26 Fe1 C20 C21 -73.6(6) . . . . ? C22 Fe1 C20 C21 37.7(5) . . . . ? C24 Fe1 C20 C21 -155.5(5) . . . . ? C27 Fe1 C20 C21 -44.8(13) . . . . ? C23 Fe1 C20 C21 81.7(5) . . . . ? C28 Fe1 C20 C21 176.8(8) . . . . ? C19 Fe1 C20 C21 119.3(7) . . . . ? C25 Fe1 C20 C19 126.0(5) . . . . ? C26 Fe1 C20 C19 167.0(5) . . . . ? C22 Fe1 C20 C19 -81.6(5) . . . . ? C24 Fe1 C20 C19 85.2(5) . . . . ? C21 Fe1 C20 C19 -119.3(7) . . . . ? C27 Fe1 C20 C19 -164.2(9) . . . . ? C23 Fe1 C20 C19 -37.7(5) . . . . ? C28 Fe1 C20 C19 57.4(10) . . . . ? C19 C20 C21 C22 1.0(9) . . . . ? Fe1 C20 C21 C22 -59.0(6) . . . . ? C19 C20 C21 Fe1 60.0(5) . . . . ? C25 Fe1 C21 C20 81.3(6) . . . . ? C26 Fe1 C21 C20 122.7(5) . . . . ? C22 Fe1 C21 C20 -119.1(7) . . . . ? C24 Fe1 C21 C20 52.4(9) . . . . ? C27 Fe1 C21 C20 162.9(5) . . . . ? C23 Fe1 C21 C20 -81.9(5) . . . . ? C28 Fe1 C21 C20 -175.6(10) . . . . ? C19 Fe1 C21 C20 -38.1(5) . . . . ? C25 Fe1 C21 C22 -159.6(5) . . . . ? C26 Fe1 C21 C22 -118.2(5) . . . . ? C20 Fe1 C21 C22 119.1(7) . . . . ? C24 Fe1 C21 C22 171.5(6) . . . . ? C27 Fe1 C21 C22 -78.0(6) . . . . ? C23 Fe1 C21 C22 37.2(5) . . . . ? C28 Fe1 C21 C22 -56.5(13) . . . . ? C19 Fe1 C21 C22 81.0(5) . . . . ? C20 C21 C22 C23 -0.5(10) . . . . ? Fe1 C21 C22 C23 -59.5(6) . . . . ? C20 C21 C22 Fe1 59.0(6) . . . . ? C25 Fe1 C22 C21 43.0(10) . . . . ? C26 Fe1 C22 C21 77.5(6) . . . . ? C20 Fe1 C22 C21 -37.7(5) . . . . ? C24 Fe1 C22 C21 -164.1(12) . . . . ? C27 Fe1 C22 C21 121.0(5) . . . . ? C23 Fe1 C22 C21 -120.2(7) . . . . ? C28 Fe1 C22 C21 161.8(5) . . . . ? C19 Fe1 C22 C21 -82.4(5) . . . . ? C25 Fe1 C22 C23 163.2(7) . . . . ? C26 Fe1 C22 C23 -162.3(5) . . . . ? C20 Fe1 C22 C23 82.5(5) . . . . ? C24 Fe1 C22 C23 -43.9(16) . . . . ? C21 Fe1 C22 C23 120.2(7) . . . . ? C27 Fe1 C22 C23 -118.8(5) . . . . ? C28 Fe1 C22 C23 -78.0(6) . . . . ? C19 Fe1 C22 C23 37.8(5) . . . . ? C21 C22 C23 C19 -0.3(10) . . . . ? Fe1 C22 C23 C19 -59.8(6) . . . . ? C21 C22 C23 Fe1 59.5(6) . . . . ? C20 C19 C23 C22 0.9(9) . . . . ? C5 C19 C23 C22 -177.4(7) . . . . ? Fe1 C19 C23 C22 59.1(6) . . . . ? C20 C19 C23 Fe1 -58.2(5) . . . . ? C5 C19 C23 Fe1 123.5(8) . . . . ? C25 Fe1 C23 C22 -152.6(12) . . . . ? C26 Fe1 C23 C22 40.0(12) . . . . ? C20 Fe1 C23 C22 -80.6(6) . . . . ? C24 Fe1 C23 C22 167.5(6) . . . . ? C21 Fe1 C23 C22 -37.0(6) . . . . ? C27 Fe1 C23 C22 80.1(6) . . . . ? C28 Fe1 C23 C22 124.6(6) . . . . ? C19 Fe1 C23 C22 -118.9(8) . . . . ? C25 Fe1 C23 C19 -33.7(15) . . . . ? C26 Fe1 C23 C19 158.9(8) . . . . ? C22 Fe1 C23 C19 118.9(8) . . . . ? C20 Fe1 C23 C19 38.3(5) . . . . ? C24 Fe1 C23 C19 -73.6(6) . . . . ? C21 Fe1 C23 C19 81.9(5) . . . . ? C27 Fe1 C23 C19 -161.0(5) . . . . ? C28 Fe1 C23 C19 -116.4(5) . . . . ? C26 Fe1 C24 C25 -37.1(5) . . . . ? C22 Fe1 C24 C25 -161.3(12) . . . . ? C20 Fe1 C24 C25 78.0(6) . . . . ? C21 Fe1 C24 C25 41.7(9) . . . . ? C27 Fe1 C24 C25 -81.5(5) . . . . ? C23 Fe1 C24 C25 163.5(5) . . . . ? C28 Fe1 C24 C25 -118.6(7) . . . . ? C19 Fe1 C24 C25 122.2(5) . . . . ? C25 Fe1 C24 C28 118.6(7) . . . . ? C26 Fe1 C24 C28 81.5(5) . . . . ? C22 Fe1 C24 C28 -42.7(15) . . . . ? C20 Fe1 C24 C28 -163.3(5) . . . . ? C21 Fe1 C24 C28 160.3(6) . . . . ? C27 Fe1 C24 C28 37.1(5) . . . . ? C23 Fe1 C24 C28 -77.9(6) . . . . ? C19 Fe1 C24 C28 -119.2(5) . . . . ? C28 C24 C25 C26 -1.1(10) . . . . ? Fe1 C24 C25 C26 59.0(6) . . . . ? C28 C24 C25 Fe1 -60.1(6) . . . . ? C26 Fe1 C25 C24 120.6(8) . . . . ? C22 Fe1 C25 C24 170.0(7) . . . . ? C20 Fe1 C25 C24 -118.3(5) . . . . ? C21 Fe1 C25 C24 -160.0(5) . . . . ? C27 Fe1 C25 C24 82.2(6) . . . . ? C23 Fe1 C25 C24 -51.5(15) . . . . ? C28 Fe1 C25 C24 38.0(5) . . . . ? C19 Fe1 C25 C24 -77.6(6) . . . . ? C22 Fe1 C25 C26 49.4(10) . . . . ? C20 Fe1 C25 C26 121.1(6) . . . . ? C24 Fe1 C25 C26 -120.6(8) . . . . ? C21 Fe1 C25 C26 79.4(6) . . . . ? C27 Fe1 C25 C26 -38.4(5) . . . . ? C23 Fe1 C25 C26 -172.1(12) . . . . ? C28 Fe1 C25 C26 -82.6(6) . . . . ? C19 Fe1 C25 C26 161.8(5) . . . . ? C24 C25 C26 C27 0.4(10) . . . . ? Fe1 C25 C26 C27 59.9(6) . . . . ? C24 C25 C26 Fe1 -59.5(6) . . . . ? C22 Fe1 C26 C25 -156.8(5) . . . . ? C20 Fe1 C26 C25 -76.1(6) . . . . ? C24 Fe1 C26 C25 36.6(6) . . . . ? C21 Fe1 C26 C25 -116.0(6) . . . . ? C27 Fe1 C26 C25 118.7(8) . . . . ? C23 Fe1 C26 C25 174.5(8) . . . . ? C28 Fe1 C26 C25 80.1(6) . . . . ? C19 Fe1 C26 C25 -49.8(12) . . . . ? C25 Fe1 C26 C27 -118.7(8) . . . . ? C22 Fe1 C26 C27 84.5(6) . . . . ? C20 Fe1 C26 C27 165.3(5) . . . . ? C24 Fe1 C26 C27 -82.1(6) . . . . ? C21 Fe1 C26 C27 125.3(6) . . . . ? C23 Fe1 C26 C27 55.9(11) . . . . ? C28 Fe1 C26 C27 -38.6(5) . . . . ? C19 Fe1 C26 C27 -168.5(9) . . . . ? C25 C26 C27 C28 0.4(10) . . . . ? Fe1 C26 C27 C28 60.0(6) . . . . ? C25 C26 C27 Fe1 -59.6(6) . . . . ? C25 Fe1 C27 C28 -79.8(6) . . . . ? C26 Fe1 C27 C28 -117.7(8) . . . . ? C22 Fe1 C27 C28 128.6(5) . . . . ? C20 Fe1 C27 C28 -156.1(9) . . . . ? C24 Fe1 C27 C28 -36.6(5) . . . . ? C21 Fe1 C27 C28 170.5(5) . . . . ? C23 Fe1 C27 C28 86.1(6) . . . . ? C19 Fe1 C27 C28 52.2(11) . . . . ? C25 Fe1 C27 C26 37.9(5) . . . . ? C22 Fe1 C27 C26 -113.6(6) . . . . ? C20 Fe1 C27 C26 -38.4(13) . . . . ? C24 Fe1 C27 C26 81.1(6) . . . . ? C21 Fe1 C27 C26 -71.8(7) . . . . ? C23 Fe1 C27 C26 -156.2(5) . . . . ? C28 Fe1 C27 C26 117.7(8) . . . . ? C19 Fe1 C27 C26 169.9(8) . . . . ? C25 C24 C28 C27 1.4(10) . . . . ? Fe1 C24 C28 C27 -58.2(6) . . . . ? C25 C24 C28 Fe1 59.6(6) . . . . ? C26 C27 C28 C24 -1.1(10) . . . . ? Fe1 C27 C28 C24 58.2(6) . . . . ? C26 C27 C28 Fe1 -59.3(6) . . . . ? C25 Fe1 C28 C24 -37.7(5) . . . . ? C26 Fe1 C28 C24 -81.8(5) . . . . ? C22 Fe1 C28 C24 167.7(5) . . . . ? C20 Fe1 C28 C24 38.6(11) . . . . ? C21 Fe1 C28 C24 -148.5(11) . . . . ? C27 Fe1 C28 C24 -120.7(7) . . . . ? C23 Fe1 C28 C24 124.4(5) . . . . ? C19 Fe1 C28 C24 80.3(6) . . . . ? C25 Fe1 C28 C27 83.0(6) . . . . ? C26 Fe1 C28 C27 38.9(5) . . . . ? C22 Fe1 C28 C27 -71.6(6) . . . . ? C20 Fe1 C28 C27 159.3(8) . . . . ? C24 Fe1 C28 C27 120.7(7) . . . . ? C21 Fe1 C28 C27 -27.8(14) . . . . ? C23 Fe1 C28 C27 -114.9(5) . . . . ? C19 Fe1 C28 C27 -159.0(5) . . . . ? C15 C14 C29 C33 34.3(12) . . . . ? C13 C14 C29 C33 -141.5(8) . . . . ? C15 C14 C29 C30 -147.8(8) . . . . ? C13 C14 C29 C30 36.4(11) . . . . ? C15 C14 C29 Fe2 -57.5(11) . . . . ? C13 C14 C29 Fe2 126.7(7) . . . . ? C36 Fe2 C29 C33 159.6(9) . . . . ? C37 Fe2 C29 C33 -33.2(19) . . . . ? C32 Fe2 C29 C33 37.3(5) . . . . ? C35 Fe2 C29 C33 -160.5(6) . . . . ? C30 Fe2 C29 C33 119.8(7) . . . . ? C34 Fe2 C29 C33 -116.0(5) . . . . ? C31 Fe2 C29 C33 81.2(5) . . . . ? C38 Fe2 C29 C33 -74.3(7) . . . . ? C36 Fe2 C29 C30 39.9(10) . . . . ? C37 Fe2 C29 C30 -152.9(17) . . . . ? C32 Fe2 C29 C30 -82.5(5) . . . . ? C35 Fe2 C29 C30 79.7(7) . . . . ? C33 Fe2 C29 C30 -119.8(7) . . . . ? C34 Fe2 C29 C30 124.3(6) . . . . ? C31 Fe2 C29 C30 -38.6(5) . . . . ? C38 Fe2 C29 C30 165.9(6) . . . . ? C36 Fe2 C29 C14 -79.1(12) . . . . ? C37 Fe2 C29 C14 88.1(19) . . . . ? C32 Fe2 C29 C14 158.6(9) . . . . ? C35 Fe2 C29 C14 -39.2(9) . . . . ? C33 Fe2 C29 C14 121.3(10) . . . . ? C30 Fe2 C29 C14 -118.9(10) . . . . ? C34 Fe2 C29 C14 5.3(9) . . . . ? C31 Fe2 C29 C14 -157.5(9) . . . . ? C38 Fe2 C29 C14 47.0(10) . . . . ? C33 C29 C30 C31 2.3(9) . . . . ? C14 C29 C30 C31 -176.0(7) . . . . ? Fe2 C29 C30 C31 59.8(5) . . . . ? C33 C29 C30 Fe2 -57.5(5) . . . . ? C14 C29 C30 Fe2 124.2(8) . . . . ? C36 Fe2 C30 C29 -160.3(6) . . . . ? C37 Fe2 C30 C29 169.5(9) . . . . ? C32 Fe2 C30 C29 80.9(5) . . . . ? C35 Fe2 C30 C29 -118.2(6) . . . . ? C33 Fe2 C30 C29 37.3(5) . . . . ? C34 Fe2 C30 C29 -79.1(7) . . . . ? C31 Fe2 C30 C29 118.5(8) . . . . ? C38 Fe2 C30 C29 -54(2) . . . . ? C36 Fe2 C30 C31 81.2(7) . . . . ? C37 Fe2 C30 C31 51.0(12) . . . . ? C32 Fe2 C30 C31 -37.6(5) . . . . ? C35 Fe2 C30 C31 123.3(6) . . . . ? C33 Fe2 C30 C31 -81.2(6) . . . . ? C34 Fe2 C30 C31 162.4(5) . . . . ? C38 Fe2 C30 C31 -172.6(19) . . . . ? C29 Fe2 C30 C31 -118.5(8) . . . . ? C29 C30 C31 C32 -1.9(9) . . . . ? Fe2 C30 C31 C32 58.9(5) . . . . ? C29 C30 C31 Fe2 -60.8(5) . . . . ? C36 Fe2 C31 C32 127.5(7) . . . . ? C37 Fe2 C31 C32 87.0(8) . . . . ? C35 Fe2 C31 C32 165.2(6) . . . . ? C33 Fe2 C31 C32 -37.4(5) . . . . ? C30 Fe2 C31 C32 -119.1(7) . . . . ? C34 Fe2 C31 C32 -178.0(11) . . . . ? C38 Fe2 C31 C32 57.4(10) . . . . ? C29 Fe2 C31 C32 -81.0(5) . . . . ? C36 Fe2 C31 C30 -113.4(8) . . . . ? C37 Fe2 C31 C30 -153.9(8) . . . . ? C32 Fe2 C31 C30 119.1(7) . . . . ? C35 Fe2 C31 C30 -75.8(7) . . . . ? C33 Fe2 C31 C30 81.6(6) . . . . ? C34 Fe2 C31 C30 -58.9(13) . . . . ? C38 Fe2 C31 C30 176.5(9) . . . . ? C29 Fe2 C31 C30 38.0(5) . . . . ? C30 C31 C32 C33 0.7(9) . . . . ? Fe2 C31 C32 C33 59.6(5) . . . . ? C30 C31 C32 Fe2 -58.9(6) . . . . ? C36 Fe2 C32 C33 171.7(7) . . . . ? C37 Fe2 C32 C33 131.0(7) . . . . ? C35 Fe2 C32 C33 -161.3(13) . . . . ? C30 Fe2 C32 C33 -81.2(5) . . . . ? C34 Fe2 C32 C33 59.1(10) . . . . ? C31 Fe2 C32 C33 -119.6(7) . . . . ? C38 Fe2 C32 C33 88.0(6) . . . . ? C29 Fe2 C32 C33 -37.3(5) . . . . ? C36 Fe2 C32 C31 -68.8(8) . . . . ? C37 Fe2 C32 C31 -109.4(7) . . . . ? C35 Fe2 C32 C31 -41.8(15) . . . . ? C33 Fe2 C32 C31 119.6(7) . . . . ? C30 Fe2 C32 C31 38.3(5) . . . . ? C34 Fe2 C32 C31 178.7(7) . . . . ? C38 Fe2 C32 C31 -152.4(5) . . . . ? C29 Fe2 C32 C31 82.3(5) . . . . ? C31 C32 C33 C29 0.7(9) . . . . ? Fe2 C32 C33 C29 60.3(6) . . . . ? C31 C32 C33 Fe2 -59.6(6) . . . . ? C30 C29 C33 C32 -1.8(9) . . . . ? C14 C29 C33 C32 176.4(7) . . . . ? Fe2 C29 C33 C32 -59.3(6) . . . . ? C30 C29 C33 Fe2 57.5(5) . . . . ? C14 C29 C33 Fe2 -124.3(8) . . . . ? C36 Fe2 C33 C32 -24.8(19) . . . . ? C37 Fe2 C33 C32 -68.5(7) . . . . ? C35 Fe2 C33 C32 165.3(10) . . . . ? C30 Fe2 C33 C32 82.3(5) . . . . ? C34 Fe2 C33 C32 -154.5(5) . . . . ? C31 Fe2 C33 C32 37.6(5) . . . . ? C38 Fe2 C33 C32 -111.8(6) . . . . ? C29 Fe2 C33 C32 119.8(7) . . . . ? C36 Fe2 C33 C29 -144.7(17) . . . . ? C37 Fe2 C33 C29 171.7(6) . . . . ? C32 Fe2 C33 C29 -119.8(7) . . . . ? C35 Fe2 C33 C29 45.5(13) . . . . ? C30 Fe2 C33 C29 -37.5(5) . . . . ? C34 Fe2 C33 C29 85.7(6) . . . . ? C31 Fe2 C33 C29 -82.3(5) . . . . ? C38 Fe2 C33 C29 128.3(5) . . . . ? C36 Fe2 C34 C38 -83.2(8) . . . . ? C37 Fe2 C34 C38 -39.8(8) . . . . ? C32 Fe2 C34 C38 41.2(11) . . . . ? C35 Fe2 C34 C38 -120.4(9) . . . . ? C33 Fe2 C34 C38 83.1(7) . . . . ? C30 Fe2 C34 C38 171.3(6) . . . . ? C31 Fe2 C34 C38 -142.0(11) . . . . ? C29 Fe2 C34 C38 127.4(6) . . . . ? C36 Fe2 C34 C35 37.2(9) . . . . ? C37 Fe2 C34 C35 80.6(9) . . . . ? C32 Fe2 C34 C35 161.5(8) . . . . ? C33 Fe2 C34 C35 -156.6(7) . . . . ? C30 Fe2 C34 C35 -68.3(8) . . . . ? C31 Fe2 C34 C35 -21.6(15) . . . . ? C38 Fe2 C34 C35 120.4(9) . . . . ? C29 Fe2 C34 C35 -112.2(7) . . . . ? C38 C34 C35 C36 0.5(11) . . . . ? Fe2 C34 C35 C36 -59.0(7) . . . . ? C38 C34 C35 Fe2 59.5(7) . . . . ? C37 Fe2 C35 C36 38.4(8) . . . . ? C32 Fe2 C35 C36 -35.7(18) . . . . ? C33 Fe2 C35 C36 175.5(10) . . . . ? C30 Fe2 C35 C36 -109.6(9) . . . . ? C34 Fe2 C35 C36 119.5(11) . . . . ? C31 Fe2 C35 C36 -67.5(10) . . . . ? C38 Fe2 C35 C36 83.2(9) . . . . ? C29 Fe2 C35 C36 -151.8(8) . . . . ? C36 Fe2 C35 C34 -119.5(11) . . . . ? C37 Fe2 C35 C34 -81.1(8) . . . . ? C32 Fe2 C35 C34 -155.3(11) . . . . ? C33 Fe2 C35 C34 56.0(14) . . . . ? C30 Fe2 C35 C34 130.8(6) . . . . ? C31 Fe2 C35 C34 173.0(5) . . . . ? C38 Fe2 C35 C34 -36.4(6) . . . . ? C29 Fe2 C35 C34 88.7(7) . . . . ? C34 C35 C36 C37 -1.8(12) . . . . ? Fe2 C35 C36 C37 -61.0(8) . . . . ? C34 C35 C36 Fe2 59.2(7) . . . . ? C32 Fe2 C36 C37 -75.6(8) . . . . ? C35 Fe2 C36 C37 117.3(11) . . . . ? C33 Fe2 C36 C37 -56.4(19) . . . . ? C30 Fe2 C36 C37 -156.4(6) . . . . ? C34 Fe2 C36 C37 79.8(7) . . . . ? C31 Fe2 C36 C37 -114.2(7) . . . . ? C38 Fe2 C36 C37 37.1(7) . . . . ? C29 Fe2 C36 C37 175.9(7) . . . . ? C37 Fe2 C36 C35 -117.3(11) . . . . ? C32 Fe2 C36 C35 167.1(7) . . . . ? C33 Fe2 C36 C35 -173.7(14) . . . . ? C30 Fe2 C36 C35 86.2(8) . . . . ? C34 Fe2 C36 C35 -37.6(7) . . . . ? C31 Fe2 C36 C35 128.5(8) . . . . ? C38 Fe2 C36 C35 -80.2(8) . . . . ? C29 Fe2 C36 C35 58.6(12) . . . . ? C35 C36 C37 C38 2.4(12) . . . . ? Fe2 C36 C37 C38 -58.8(7) . . . . ? C35 C36 C37 Fe2 61.2(7) . . . . ? C32 Fe2 C37 C36 122.8(7) . . . . ? C35 Fe2 C37 C36 -38.5(7) . . . . ? C33 Fe2 C37 C36 162.1(7) . . . . ? C30 Fe2 C37 C36 45.1(12) . . . . ? C34 Fe2 C37 C36 -82.8(8) . . . . ? C31 Fe2 C37 C36 79.9(8) . . . . ? C38 Fe2 C37 C36 -121.1(11) . . . . ? C29 Fe2 C37 C36 -170.6(16) . . . . ? C36 Fe2 C37 C38 121.1(11) . . . . ? C32 Fe2 C37 C38 -116.1(7) . . . . ? C35 Fe2 C37 C38 82.6(8) . . . . ? C33 Fe2 C37 C38 -76.8(8) . . . . ? C30 Fe2 C37 C38 166.2(8) . . . . ? C34 Fe2 C37 C38 38.3(7) . . . . ? C31 Fe2 C37 C38 -159.0(7) . . . . ? C29 Fe2 C37 C38 -49(2) . . . . ? C35 C34 C38 C37 0.9(10) . . . . ? Fe2 C34 C38 C37 59.9(6) . . . . ? C35 C34 C38 Fe2 -59.0(7) . . . . ? C36 C37 C38 C34 -2.1(11) . . . . ? Fe2 C37 C38 C34 -60.7(6) . . . . ? C36 C37 C38 Fe2 58.7(8) . . . . ? C36 Fe2 C38 C34 80.5(8) . . . . ? C37 Fe2 C38 C34 116.6(11) . . . . ? C32 Fe2 C38 C34 -161.5(5) . . . . ? C35 Fe2 C38 C34 37.2(6) . . . . ? C33 Fe2 C38 C34 -117.3(6) . . . . ? C30 Fe2 C38 C34 -31(2) . . . . ? C31 Fe2 C38 C34 159.2(7) . . . . ? C29 Fe2 C38 C34 -75.3(8) . . . . ? C36 Fe2 C38 C37 -36.1(8) . . . . ? C32 Fe2 C38 C37 82.0(9) . . . . ? C35 Fe2 C38 C37 -79.3(9) . . . . ? C33 Fe2 C38 C37 126.1(9) . . . . ? C30 Fe2 C38 C37 -147.7(19) . . . . ? C34 Fe2 C38 C37 -116.6(11) . . . . ? C31 Fe2 C38 C37 42.6(13) . . . . ? C29 Fe2 C38 C37 168.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.489 _refine_diff_density_min -2.329 _refine_diff_density_rms 0.258 #end data_complex2 _database_code_depnum_ccdc_archive 'CCDC 739913' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H44 Cu2 Fe2 N4 O4' _chemical_formula_weight 979.65 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.903(5) _cell_length_b 15.047(5) _cell_length_c 13.607(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 123.984(5) _cell_angle_gamma 90.000(5) _cell_volume 3888(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2296 _cell_measurement_theta_min 2.9847 _cell_measurement_theta_max 33.1309 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 1.865 _exptl_absorpt_correction_T_min 0.6631 _exptl_absorpt_correction_T_max 0.7546 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION XCALIBUR-S' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13538 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3426 _reflns_number_gt 2521 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0837P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3426 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1177 _refine_ls_wR_factor_gt 0.1142 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.926 _refine_ls_shift/su_max 0.054 _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 Cu1 Cu 0.93015(3) 0.48811(4) 0.56526(4) 0.03492(19) Uani 1 1 d . . . Fe1 Fe 0.62759(3) 0.58364(4) 0.11799(5) 0.02388(18) Uani 1 1 d . . . O1 O 1.02204(16) 0.5435(2) 0.6503(3) 0.0605(10) Uani 1 1 d . . . O2 O 0.97199(15) 0.3713(2) 0.5943(3) 0.0434(8) Uani 1 1 d . . . N1 N 0.88880(17) 0.6057(2) 0.5300(3) 0.0294(8) Uani 1 1 d . . . N2 N 0.83635(17) 0.4350(2) 0.4822(3) 0.0267(7) Uani 1 1 d . . . C1 C 1.1441(2) 0.5674(3) 0.7634(4) 0.0401(11) Uani 1 1 d . . . H1A H 1.1604 0.5782 0.7114 0.060 Uiso 1 1 calc R . . H1B H 1.1822 0.5401 0.8373 0.060 Uiso 1 1 calc R . . H1C H 1.1306 0.6239 0.7811 0.060 Uiso 1 1 calc R . . C2 C 1.0814(2) 0.5057(3) 0.7023(3) 0.0346(11) Uani 1 1 d . . . C3 C 1.0912(2) 0.4162(3) 0.7041(4) 0.0407(11) Uani 1 1 d . . . H3 H 1.1383 0.3950 0.7447 0.049 Uiso 1 1 calc R . . C4 C 1.0378(2) 0.3539(3) 0.6513(4) 0.0401(11) Uani 1 1 d . . . C5 C 1.0547(3) 0.2573(3) 0.6575(5) 0.0542(13) Uani 1 1 d . . . H5A H 1.0472 0.2277 0.7138 0.081 Uiso 1 1 calc R . . H5B H 1.1040 0.2504 0.6839 0.081 Uiso 1 1 calc R . . H5C H 1.0240 0.2305 0.5789 0.081 Uiso 1 1 calc R . . C6 C 0.9235(2) 0.6796(3) 0.5845(3) 0.0311(9) Uani 1 1 d . . . H6 H 0.9730 0.6826 0.6404 0.037 Uiso 1 1 calc R . . C7 C 0.8783(2) 0.7524(3) 0.5495(3) 0.0321(10) Uani 1 1 d . . . H7 H 0.8909 0.8117 0.5776 0.038 Uiso 1 1 calc R . . C8 C 0.8122(2) 0.7216(3) 0.4666(3) 0.0275(9) Uani 1 1 d . . . H8 H 0.7702 0.7559 0.4255 0.033 Uiso 1 1 calc R . . C9 C 0.8176(2) 0.6292(3) 0.4531(3) 0.0249(9) Uani 1 1 d . . . C10 C 0.7635(2) 0.5680(3) 0.3842(3) 0.0226(8) Uani 1 1 d . . . C11 C 0.7718(2) 0.4753(3) 0.3982(3) 0.0247(9) Uani 1 1 d . . . C12 C 0.7206(2) 0.4078(3) 0.3423(3) 0.0254(8) Uani 1 1 d . . . H12 H 0.6725 0.4160 0.2802 0.031 Uiso 1 1 calc R . . C13 C 0.7525(2) 0.3286(3) 0.3935(3) 0.0296(9) Uani 1 1 d . . . H13 H 0.7309 0.2717 0.3755 0.036 Uiso 1 1 calc R . . C14 C 0.8233(2) 0.3486(3) 0.4775(3) 0.0317(10) Uani 1 1 d . . . H14 H 0.8581 0.3053 0.5256 0.038 Uiso 1 1 calc R . . C15 C 0.69314(19) 0.6070(3) 0.2967(3) 0.0231(8) Uani 1 1 d . . . C16 C 0.6819(2) 0.6855(3) 0.2305(3) 0.0281(9) Uani 1 1 d . . . H16 H 0.7175 0.7194 0.2323 0.034 Uiso 1 1 calc R . . C17 C 0.6092(2) 0.7050(3) 0.1614(3) 0.0310(9) Uani 1 1 d . . . H17 H 0.5876 0.7541 0.1093 0.037 Uiso 1 1 calc R . . C18 C 0.5743(2) 0.6392(3) 0.1833(3) 0.0300(9) Uani 1 1 d . . . H18 H 0.5251 0.6363 0.1489 0.036 Uiso 1 1 calc R . . C19 C 0.6252(2) 0.5779(2) 0.2656(3) 0.0234(8) Uani 1 1 d . . . H19 H 0.6160 0.5263 0.2950 0.028 Uiso 1 1 calc R . . C20 C 0.6732(2) 0.5622(3) 0.0279(3) 0.0337(10) Uani 1 1 d . . . H20 H 0.7155 0.5888 0.0448 0.040 Uiso 1 1 calc R . . C21 C 0.6050(2) 0.5966(3) -0.0484(3) 0.0337(10) Uani 1 1 d . . . H21 H 0.5933 0.6505 -0.0917 0.040 Uiso 1 1 calc R . . C22 C 0.5567(2) 0.5373(3) -0.0498(3) 0.0318(9) Uani 1 1 d . . . H22 H 0.5070 0.5442 -0.0940 0.038 Uiso 1 1 calc R . . C23 C 0.5955(2) 0.4663(3) 0.0261(3) 0.0297(9) Uani 1 1 d . . . H23 H 0.5767 0.4164 0.0421 0.036 Uiso 1 1 calc R . . C24 C 0.6679(2) 0.4820(3) 0.0747(3) 0.0304(9) Uani 1 1 d . . . H24 H 0.7061 0.4448 0.1293 0.036 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 Cu1 0.0153(3) 0.0449(4) 0.0334(3) -0.0098(2) 0.0068(2) 0.0044(2) Fe1 0.0166(3) 0.0287(3) 0.0223(3) -0.0019(2) 0.0084(2) -0.0017(2) O1 0.0187(18) 0.058(2) 0.079(3) -0.025(2) 0.0117(18) 0.0019(16) O2 0.0191(16) 0.0483(19) 0.0464(19) -0.0077(15) 0.0083(14) 0.0085(14) N1 0.0156(17) 0.040(2) 0.0264(17) -0.0030(15) 0.0081(15) 0.0006(15) N2 0.0193(18) 0.032(2) 0.0252(17) 0.0020(14) 0.0098(15) 0.0059(14) C1 0.020(2) 0.065(3) 0.032(2) 0.002(2) 0.012(2) 0.002(2) C2 0.016(2) 0.060(3) 0.022(2) -0.002(2) 0.0073(18) 0.0050(19) C3 0.013(2) 0.062(3) 0.035(2) 0.007(2) 0.0067(19) 0.010(2) C4 0.026(3) 0.060(3) 0.027(2) 0.003(2) 0.010(2) 0.012(2) C5 0.030(3) 0.056(3) 0.056(3) 0.006(3) 0.012(2) 0.013(2) C6 0.018(2) 0.042(2) 0.025(2) -0.0056(18) 0.0072(18) -0.0073(18) C7 0.030(2) 0.034(2) 0.028(2) -0.0066(18) 0.0139(19) -0.0084(18) C8 0.022(2) 0.036(2) 0.0228(19) -0.0014(17) 0.0112(17) -0.0026(17) C9 0.017(2) 0.037(2) 0.0194(19) -0.0018(17) 0.0092(17) 0.0005(16) C10 0.018(2) 0.032(2) 0.0190(18) 0.0010(16) 0.0112(17) 0.0023(16) C11 0.018(2) 0.037(2) 0.0197(19) -0.0001(17) 0.0107(17) 0.0019(17) C12 0.019(2) 0.032(2) 0.025(2) 0.0005(17) 0.0125(17) 0.0016(16) C13 0.032(2) 0.026(2) 0.034(2) -0.0022(17) 0.020(2) -0.0012(17) C14 0.024(2) 0.036(2) 0.030(2) 0.0044(18) 0.0119(19) 0.0119(18) C15 0.017(2) 0.028(2) 0.0222(19) -0.0019(16) 0.0092(17) -0.0001(16) C16 0.026(2) 0.027(2) 0.026(2) -0.0024(17) 0.0115(18) -0.0032(17) C17 0.027(2) 0.030(2) 0.024(2) -0.0022(17) 0.0065(18) 0.0026(17) C18 0.021(2) 0.036(2) 0.029(2) -0.0073(18) 0.0111(18) 0.0005(17) C19 0.021(2) 0.028(2) 0.0227(19) -0.0036(16) 0.0125(17) -0.0004(16) C20 0.028(2) 0.050(3) 0.027(2) -0.0108(19) 0.019(2) -0.011(2) C21 0.039(3) 0.038(2) 0.022(2) -0.0026(18) 0.015(2) -0.003(2) C22 0.020(2) 0.041(3) 0.025(2) -0.0041(18) 0.0072(18) -0.0005(18) C23 0.029(2) 0.031(2) 0.031(2) -0.0094(18) 0.0175(19) -0.0056(18) C24 0.021(2) 0.041(2) 0.027(2) -0.0047(18) 0.0125(19) 0.0032(18) _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 O2 1.934(3) . ? Cu1 O1 1.934(3) . ? Cu1 N1 1.937(3) . ? Cu1 N2 1.954(3) . ? Fe1 C21 2.030(4) . ? Fe1 C16 2.027(4) . ? Fe1 C20 2.031(4) . ? Fe1 C24 2.037(4) . ? Fe1 C17 2.035(4) . ? Fe1 C19 2.041(4) . ? Fe1 C18 2.047(4) . ? Fe1 C22 2.047(4) . ? Fe1 C23 2.048(4) . ? Fe1 C15 2.052(4) . ? O1 C2 1.264(5) . ? O2 C4 1.278(5) . ? N1 C6 1.326(5) . ? N1 C9 1.405(5) . ? N2 C14 1.328(5) . ? N2 C11 1.404(5) . ? C1 C2 1.510(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.364(6) . ? C3 C4 1.382(7) . ? C3 H3 0.9500 . ? C4 C5 1.493(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.396(6) . ? C6 H6 0.9500 . ? C7 C8 1.368(5) . ? C7 H7 0.9500 . ? C8 C9 1.417(5) . ? C8 H8 0.9500 . ? C9 C10 1.400(5) . ? C10 C11 1.406(5) . ? C10 C15 1.488(5) . ? C11 C12 1.410(5) . ? C12 C13 1.368(5) . ? C12 H12 0.9500 . ? C13 C14 1.399(6) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.419(5) . ? C15 C19 1.433(5) . ? C16 C17 1.413(6) . ? C16 H16 0.9500 . ? C17 C18 1.404(6) . ? C17 H17 0.9500 . ? C18 C19 1.416(5) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.404(6) . ? C20 C24 1.400(6) . ? C20 H20 0.9500 . ? C21 C22 1.413(6) . ? C21 H21 0.9500 . ? C22 C23 1.404(6) . ? C22 H22 0.9500 . ? C23 C24 1.420(6) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O1 91.15(14) . . ? O2 Cu1 N1 177.29(14) . . ? O1 Cu1 N1 88.41(14) . . ? O2 Cu1 N2 90.34(13) . . ? O1 Cu1 N2 177.95(14) . . ? N1 Cu1 N2 90.17(14) . . ? C21 Fe1 C16 115.86(16) . . ? C21 Fe1 C20 40.44(17) . . ? C16 Fe1 C20 105.68(16) . . ? C21 Fe1 C24 67.88(17) . . ? C16 Fe1 C24 126.84(16) . . ? C20 Fe1 C24 40.27(17) . . ? C21 Fe1 C17 105.86(17) . . ? C16 Fe1 C17 40.70(16) . . ? C20 Fe1 C17 125.30(17) . . ? C24 Fe1 C17 163.57(17) . . ? C21 Fe1 C19 166.17(17) . . ? C16 Fe1 C19 68.39(15) . . ? C20 Fe1 C19 153.15(17) . . ? C24 Fe1 C19 121.22(16) . . ? C17 Fe1 C19 68.18(16) . . ? C21 Fe1 C18 127.08(17) . . ? C16 Fe1 C18 68.07(16) . . ? C20 Fe1 C18 163.52(17) . . ? C24 Fe1 C18 155.39(17) . . ? C17 Fe1 C18 40.23(16) . . ? C19 Fe1 C18 40.54(15) . . ? C21 Fe1 C22 40.55(17) . . ? C16 Fe1 C22 150.37(16) . . ? C20 Fe1 C22 68.15(17) . . ? C24 Fe1 C22 68.10(17) . . ? C17 Fe1 C22 117.77(16) . . ? C19 Fe1 C22 129.94(16) . . ? C18 Fe1 C22 109.25(17) . . ? C21 Fe1 C23 67.70(17) . . ? C16 Fe1 C23 166.39(17) . . ? C20 Fe1 C23 67.94(16) . . ? C24 Fe1 C23 40.69(16) . . ? C17 Fe1 C23 152.78(17) . . ? C19 Fe1 C23 111.50(16) . . ? C18 Fe1 C23 121.34(16) . . ? C22 Fe1 C23 40.10(17) . . ? C21 Fe1 C15 150.11(16) . . ? C16 Fe1 C15 40.70(15) . . ? C20 Fe1 C15 117.39(16) . . ? C24 Fe1 C15 108.76(16) . . ? C17 Fe1 C15 68.60(15) . . ? C19 Fe1 C15 40.99(15) . . ? C18 Fe1 C15 68.54(15) . . ? C22 Fe1 C15 168.19(16) . . ? C23 Fe1 C15 130.27(16) . . ? C2 O1 Cu1 127.7(3) . . ? C4 O2 Cu1 126.3(3) . . ? C6 N1 C9 106.9(3) . . ? C6 N1 Cu1 124.8(3) . . ? C9 N1 Cu1 128.1(3) . . ? C14 N2 C11 106.1(3) . . ? C14 N2 Cu1 124.9(3) . . ? C11 N2 Cu1 127.7(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 124.7(4) . . ? O1 C2 C1 115.3(4) . . ? C3 C2 C1 120.0(4) . . ? C2 C3 C4 124.9(4) . . ? C2 C3 H3 117.6 . . ? C4 C3 H3 117.6 . . ? O2 C4 C3 125.2(4) . . ? O2 C4 C5 114.5(4) . . ? C3 C4 C5 120.2(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C7 111.6(4) . . ? N1 C6 H6 124.2 . . ? C7 C6 H6 124.2 . . ? C8 C7 C6 106.5(4) . . ? C8 C7 H7 126.8 . . ? C6 C7 H7 126.8 . . ? C7 C8 C9 107.6(4) . . ? C7 C8 H8 126.2 . . ? C9 C8 H8 126.2 . . ? C10 C9 N1 123.9(4) . . ? C10 C9 C8 128.6(4) . . ? N1 C9 C8 107.4(3) . . ? C9 C10 C11 124.0(4) . . ? C9 C10 C15 115.7(3) . . ? C11 C10 C15 120.2(3) . . ? N2 C11 C10 122.6(3) . . ? N2 C11 C12 108.0(3) . . ? C10 C11 C12 129.3(4) . . ? C13 C12 C11 107.9(4) . . ? C13 C12 H12 126.1 . . ? C11 C12 H12 126.1 . . ? C12 C13 C14 105.9(4) . . ? C12 C13 H13 127.0 . . ? C14 C13 H13 127.0 . . ? N2 C14 C13 112.1(4) . . ? N2 C14 H14 124.0 . . ? C13 C14 H14 124.0 . . ? C16 C15 C19 106.6(3) . . ? C16 C15 C10 124.5(3) . . ? C19 C15 C10 128.8(3) . . ? C16 C15 Fe1 68.7(2) . . ? C19 C15 Fe1 69.1(2) . . ? C10 C15 Fe1 128.9(3) . . ? C17 C16 C15 108.8(3) . . ? C17 C16 Fe1 69.9(2) . . ? C15 C16 Fe1 70.6(2) . . ? C17 C16 H16 125.6 . . ? C15 C16 H16 125.6 . . ? Fe1 C16 H16 125.5 . . ? C18 C17 C16 108.1(4) . . ? C18 C17 Fe1 70.4(2) . . ? C16 C17 Fe1 69.4(2) . . ? C18 C17 H17 125.9 . . ? C16 C17 H17 125.9 . . ? Fe1 C17 H17 125.9 . . ? C17 C18 C19 108.2(4) . . ? C17 C18 Fe1 69.4(2) . . ? C19 C18 Fe1 69.5(2) . . ? C17 C18 H18 125.9 . . ? C19 C18 H18 125.9 . . ? Fe1 C18 H18 126.8 . . ? C18 C19 C15 108.2(3) . . ? C18 C19 Fe1 70.0(2) . . ? C15 C19 Fe1 69.9(2) . . ? C18 C19 H19 125.9 . . ? C15 C19 H19 125.9 . . ? Fe1 C19 H19 125.8 . . ? C21 C20 C24 108.1(4) . . ? C21 C20 Fe1 69.7(2) . . ? C24 C20 Fe1 70.1(2) . . ? C21 C20 H20 125.9 . . ? C24 C20 H20 125.9 . . ? Fe1 C20 H20 125.9 . . ? C20 C21 C22 108.5(4) . . ? C20 C21 Fe1 69.8(2) . . ? C22 C21 Fe1 70.4(2) . . ? C20 C21 H21 125.8 . . ? C22 C21 H21 125.8 . . ? Fe1 C21 H21 125.6 . . ? C23 C22 C21 107.5(4) . . ? C23 C22 Fe1 70.0(2) . . ? C21 C22 Fe1 69.1(2) . . ? C23 C22 H22 126.3 . . ? C21 C22 H22 126.3 . . ? Fe1 C22 H22 126.3 . . ? C22 C23 C24 108.1(4) . . ? C22 C23 Fe1 69.9(2) . . ? C24 C23 Fe1 69.2(2) . . ? C22 C23 H23 125.9 . . ? C24 C23 H23 125.9 . . ? Fe1 C23 H23 126.5 . . ? C20 C24 C23 107.8(4) . . ? C20 C24 Fe1 69.7(2) . . ? C23 C24 Fe1 70.1(2) . . ? C20 C24 H24 126.1 . . ? C23 C24 H24 126.1 . . ? Fe1 C24 H24 125.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Cu1 O1 C2 -1.6(4) . . . . ? N1 Cu1 O1 C2 -179.0(4) . . . . ? N2 Cu1 O1 C2 135(4) . . . . ? O1 Cu1 O2 C4 0.0(4) . . . . ? N1 Cu1 O2 C4 81(3) . . . . ? N2 Cu1 O2 C4 -178.6(4) . . . . ? O2 Cu1 N1 C6 -96(3) . . . . ? O1 Cu1 N1 C6 -15.4(3) . . . . ? N2 Cu1 N1 C6 163.1(3) . . . . ? O2 Cu1 N1 C9 90(3) . . . . ? O1 Cu1 N1 C9 171.3(3) . . . . ? N2 Cu1 N1 C9 -10.2(3) . . . . ? O2 Cu1 N2 C14 8.1(3) . . . . ? O1 Cu1 N2 C14 -128(4) . . . . ? N1 Cu1 N2 C14 -174.6(3) . . . . ? O2 Cu1 N2 C11 -157.6(3) . . . . ? O1 Cu1 N2 C11 66(5) . . . . ? N1 Cu1 N2 C11 19.8(3) . . . . ? Cu1 O1 C2 C3 2.5(7) . . . . ? Cu1 O1 C2 C1 -178.8(3) . . . . ? O1 C2 C3 C4 -1.3(8) . . . . ? C1 C2 C3 C4 -180.0(4) . . . . ? Cu1 O2 C4 C3 1.0(7) . . . . ? Cu1 O2 C4 C5 -178.7(3) . . . . ? C2 C3 C4 O2 -0.5(8) . . . . ? C2 C3 C4 C5 179.2(4) . . . . ? C9 N1 C6 C7 1.3(4) . . . . ? Cu1 N1 C6 C7 -173.3(3) . . . . ? N1 C6 C7 C8 -1.4(5) . . . . ? C6 C7 C8 C9 0.9(4) . . . . ? C6 N1 C9 C10 -176.7(3) . . . . ? Cu1 N1 C9 C10 -2.3(5) . . . . ? C6 N1 C9 C8 -0.7(4) . . . . ? Cu1 N1 C9 C8 173.6(3) . . . . ? C7 C8 C9 C10 175.6(4) . . . . ? C7 C8 C9 N1 -0.2(4) . . . . ? N1 C9 C10 C11 11.4(6) . . . . ? C8 C9 C10 C11 -163.7(4) . . . . ? N1 C9 C10 C15 -172.1(3) . . . . ? C8 C9 C10 C15 12.8(5) . . . . ? C14 N2 C11 C10 174.8(3) . . . . ? Cu1 N2 C11 C10 -17.4(5) . . . . ? C14 N2 C11 C12 -1.2(4) . . . . ? Cu1 N2 C11 C12 166.6(2) . . . . ? C9 C10 C11 N2 -1.3(6) . . . . ? C15 C10 C11 N2 -177.7(3) . . . . ? C9 C10 C11 C12 173.7(4) . . . . ? C15 C10 C11 C12 -2.6(6) . . . . ? N2 C11 C12 C13 1.8(4) . . . . ? C10 C11 C12 C13 -173.8(4) . . . . ? C11 C12 C13 C14 -1.8(4) . . . . ? C11 N2 C14 C13 0.1(4) . . . . ? Cu1 N2 C14 C13 -168.2(3) . . . . ? C12 C13 C14 N2 1.1(5) . . . . ? C9 C10 C15 C16 37.5(5) . . . . ? C11 C10 C15 C16 -145.9(4) . . . . ? C9 C10 C15 C19 -139.5(4) . . . . ? C11 C10 C15 C19 37.1(6) . . . . ? C9 C10 C15 Fe1 126.9(3) . . . . ? C11 C10 C15 Fe1 -56.4(5) . . . . ? C21 Fe1 C15 C16 47.1(4) . . . . ? C20 Fe1 C15 C16 82.2(3) . . . . ? C24 Fe1 C15 C16 125.2(2) . . . . ? C17 Fe1 C15 C16 -37.5(2) . . . . ? C19 Fe1 C15 C16 -118.5(3) . . . . ? C18 Fe1 C15 C16 -80.9(2) . . . . ? C22 Fe1 C15 C16 -162.3(7) . . . . ? C23 Fe1 C15 C16 165.6(2) . . . . ? C21 Fe1 C15 C19 165.6(3) . . . . ? C16 Fe1 C15 C19 118.5(3) . . . . ? C20 Fe1 C15 C19 -159.3(2) . . . . ? C24 Fe1 C15 C19 -116.3(2) . . . . ? C17 Fe1 C15 C19 80.9(2) . . . . ? C18 Fe1 C15 C19 37.6(2) . . . . ? C22 Fe1 C15 C19 -43.8(8) . . . . ? C23 Fe1 C15 C19 -76.0(3) . . . . ? C21 Fe1 C15 C10 -70.7(5) . . . . ? C16 Fe1 C15 C10 -117.9(4) . . . . ? C20 Fe1 C15 C10 -35.7(4) . . . . ? C24 Fe1 C15 C10 7.3(4) . . . . ? C17 Fe1 C15 C10 -155.4(4) . . . . ? C19 Fe1 C15 C10 123.7(4) . . . . ? C18 Fe1 C15 C10 161.3(4) . . . . ? C22 Fe1 C15 C10 79.8(9) . . . . ? C23 Fe1 C15 C10 47.7(4) . . . . ? C19 C15 C16 C17 0.7(4) . . . . ? C10 C15 C16 C17 -176.9(3) . . . . ? Fe1 C15 C16 C17 59.7(3) . . . . ? C19 C15 C16 Fe1 -59.0(2) . . . . ? C10 C15 C16 Fe1 123.4(4) . . . . ? C21 Fe1 C16 C17 84.4(3) . . . . ? C20 Fe1 C16 C17 126.5(3) . . . . ? C24 Fe1 C16 C17 165.2(2) . . . . ? C19 Fe1 C16 C17 -81.2(3) . . . . ? C18 Fe1 C16 C17 -37.4(2) . . . . ? C22 Fe1 C16 C17 53.2(4) . . . . ? C23 Fe1 C16 C17 -173.5(6) . . . . ? C15 Fe1 C16 C17 -119.6(3) . . . . ? C21 Fe1 C16 C15 -156.0(2) . . . . ? C20 Fe1 C16 C15 -114.0(2) . . . . ? C24 Fe1 C16 C15 -75.2(3) . . . . ? C17 Fe1 C16 C15 119.6(3) . . . . ? C19 Fe1 C16 C15 38.3(2) . . . . ? C18 Fe1 C16 C15 82.1(2) . . . . ? C22 Fe1 C16 C15 172.8(3) . . . . ? C23 Fe1 C16 C15 -53.9(7) . . . . ? C15 C16 C17 C18 -0.2(4) . . . . ? Fe1 C16 C17 C18 59.9(3) . . . . ? C15 C16 C17 Fe1 -60.1(3) . . . . ? C21 Fe1 C17 C18 129.4(2) . . . . ? C16 Fe1 C17 C18 -119.2(3) . . . . ? C20 Fe1 C17 C18 169.2(2) . . . . ? C24 Fe1 C17 C18 -165.5(5) . . . . ? C19 Fe1 C17 C18 -37.4(2) . . . . ? C22 Fe1 C17 C18 87.4(3) . . . . ? C23 Fe1 C17 C18 57.4(4) . . . . ? C15 Fe1 C17 C18 -81.7(2) . . . . ? C21 Fe1 C17 C16 -111.4(2) . . . . ? C20 Fe1 C17 C16 -71.6(3) . . . . ? C24 Fe1 C17 C16 -46.3(6) . . . . ? C19 Fe1 C17 C16 81.8(2) . . . . ? C18 Fe1 C17 C16 119.2(3) . . . . ? C22 Fe1 C17 C16 -153.4(2) . . . . ? C23 Fe1 C17 C16 176.6(3) . . . . ? C15 Fe1 C17 C16 37.5(2) . . . . ? C16 C17 C18 C19 -0.4(4) . . . . ? Fe1 C17 C18 C19 58.8(3) . . . . ? C16 C17 C18 Fe1 -59.3(3) . . . . ? C21 Fe1 C18 C17 -68.7(3) . . . . ? C16 Fe1 C18 C17 37.9(2) . . . . ? C20 Fe1 C18 C17 -32.6(7) . . . . ? C24 Fe1 C18 C17 170.2(3) . . . . ? C19 Fe1 C18 C17 119.8(3) . . . . ? C22 Fe1 C18 C17 -110.6(2) . . . . ? C23 Fe1 C18 C17 -153.2(2) . . . . ? C15 Fe1 C18 C17 81.8(2) . . . . ? C21 Fe1 C18 C19 171.5(2) . . . . ? C16 Fe1 C18 C19 -81.9(2) . . . . ? C20 Fe1 C18 C19 -152.4(5) . . . . ? C24 Fe1 C18 C19 50.4(5) . . . . ? C17 Fe1 C18 C19 -119.8(3) . . . . ? C22 Fe1 C18 C19 129.6(2) . . . . ? C23 Fe1 C18 C19 87.0(3) . . . . ? C15 Fe1 C18 C19 -38.0(2) . . . . ? C17 C18 C19 C15 0.9(4) . . . . ? Fe1 C18 C19 C15 59.7(3) . . . . ? C17 C18 C19 Fe1 -58.8(3) . . . . ? C16 C15 C19 C18 -1.0(4) . . . . ? C10 C15 C19 C18 176.5(3) . . . . ? Fe1 C15 C19 C18 -59.7(3) . . . . ? C16 C15 C19 Fe1 58.7(2) . . . . ? C10 C15 C19 Fe1 -123.8(4) . . . . ? C21 Fe1 C19 C18 -29.6(8) . . . . ? C16 Fe1 C19 C18 81.1(3) . . . . ? C20 Fe1 C19 C18 163.1(3) . . . . ? C24 Fe1 C19 C18 -158.0(2) . . . . ? C17 Fe1 C19 C18 37.1(2) . . . . ? C22 Fe1 C19 C18 -71.5(3) . . . . ? C23 Fe1 C19 C18 -113.5(2) . . . . ? C15 Fe1 C19 C18 119.2(3) . . . . ? C21 Fe1 C19 C15 -148.8(6) . . . . ? C16 Fe1 C19 C15 -38.1(2) . . . . ? C20 Fe1 C19 C15 43.9(5) . . . . ? C24 Fe1 C19 C15 82.9(3) . . . . ? C17 Fe1 C19 C15 -82.0(2) . . . . ? C18 Fe1 C19 C15 -119.2(3) . . . . ? C22 Fe1 C19 C15 169.3(2) . . . . ? C23 Fe1 C19 C15 127.3(2) . . . . ? C16 Fe1 C20 C21 -111.7(3) . . . . ? C24 Fe1 C20 C21 119.1(4) . . . . ? C17 Fe1 C20 C21 -71.7(3) . . . . ? C19 Fe1 C20 C21 175.3(3) . . . . ? C18 Fe1 C20 C21 -46.4(7) . . . . ? C22 Fe1 C20 C21 37.7(2) . . . . ? C23 Fe1 C20 C21 81.1(3) . . . . ? C15 Fe1 C20 C21 -153.8(2) . . . . ? C21 Fe1 C20 C24 -119.1(4) . . . . ? C16 Fe1 C20 C24 129.2(2) . . . . ? C17 Fe1 C20 C24 169.2(2) . . . . ? C19 Fe1 C20 C24 56.2(4) . . . . ? C18 Fe1 C20 C24 -165.5(5) . . . . ? C22 Fe1 C20 C24 -81.5(3) . . . . ? C23 Fe1 C20 C24 -38.1(2) . . . . ? C15 Fe1 C20 C24 87.1(3) . . . . ? C24 C20 C21 C22 -0.3(4) . . . . ? Fe1 C20 C21 C22 -60.0(3) . . . . ? C24 C20 C21 Fe1 59.8(3) . . . . ? C16 Fe1 C21 C20 83.9(3) . . . . ? C24 Fe1 C21 C20 -37.6(2) . . . . ? C17 Fe1 C21 C20 126.4(3) . . . . ? C19 Fe1 C21 C20 -171.2(6) . . . . ? C18 Fe1 C21 C20 165.1(2) . . . . ? C22 Fe1 C21 C20 -119.3(4) . . . . ? C23 Fe1 C21 C20 -81.7(3) . . . . ? C15 Fe1 C21 C20 51.8(4) . . . . ? C16 Fe1 C21 C22 -156.8(2) . . . . ? C20 Fe1 C21 C22 119.3(4) . . . . ? C24 Fe1 C21 C22 81.7(3) . . . . ? C17 Fe1 C21 C22 -114.4(3) . . . . ? C19 Fe1 C21 C22 -51.9(8) . . . . ? C18 Fe1 C21 C22 -75.7(3) . . . . ? C23 Fe1 C21 C22 37.6(2) . . . . ? C15 Fe1 C21 C22 171.1(3) . . . . ? C20 C21 C22 C23 0.0(4) . . . . ? Fe1 C21 C22 C23 -59.7(3) . . . . ? C20 C21 C22 Fe1 59.7(3) . . . . ? C21 Fe1 C22 C23 118.8(4) . . . . ? C16 Fe1 C22 C23 164.6(3) . . . . ? C20 Fe1 C22 C23 81.2(3) . . . . ? C24 Fe1 C22 C23 37.7(2) . . . . ? C17 Fe1 C22 C23 -159.2(2) . . . . ? C19 Fe1 C22 C23 -75.4(3) . . . . ? C18 Fe1 C22 C23 -116.1(2) . . . . ? C15 Fe1 C22 C23 -39.0(9) . . . . ? C16 Fe1 C22 C21 45.8(4) . . . . ? C20 Fe1 C22 C21 -37.6(3) . . . . ? C24 Fe1 C22 C21 -81.1(3) . . . . ? C17 Fe1 C22 C21 81.9(3) . . . . ? C19 Fe1 C22 C21 165.8(2) . . . . ? C18 Fe1 C22 C21 125.0(3) . . . . ? C23 Fe1 C22 C21 -118.8(4) . . . . ? C15 Fe1 C22 C21 -157.9(7) . . . . ? C21 C22 C23 C24 0.2(4) . . . . ? Fe1 C22 C23 C24 -58.9(3) . . . . ? C21 C22 C23 Fe1 59.1(3) . . . . ? C21 Fe1 C23 C22 -38.0(2) . . . . ? C16 Fe1 C23 C22 -146.1(6) . . . . ? C20 Fe1 C23 C22 -81.8(3) . . . . ? C24 Fe1 C23 C22 -119.5(3) . . . . ? C17 Fe1 C23 C22 43.3(4) . . . . ? C19 Fe1 C23 C22 127.1(2) . . . . ? C18 Fe1 C23 C22 82.9(3) . . . . ? C15 Fe1 C23 C22 170.3(2) . . . . ? C21 Fe1 C23 C24 81.5(3) . . . . ? C16 Fe1 C23 C24 -26.5(8) . . . . ? C20 Fe1 C23 C24 37.7(2) . . . . ? C17 Fe1 C23 C24 162.8(3) . . . . ? C19 Fe1 C23 C24 -113.4(2) . . . . ? C18 Fe1 C23 C24 -157.6(2) . . . . ? C22 Fe1 C23 C24 119.5(3) . . . . ? C15 Fe1 C23 C24 -70.2(3) . . . . ? C21 C20 C24 C23 0.4(4) . . . . ? Fe1 C20 C24 C23 60.0(3) . . . . ? C21 C20 C24 Fe1 -59.5(3) . . . . ? C22 C23 C24 C20 -0.4(4) . . . . ? Fe1 C23 C24 C20 -59.7(3) . . . . ? C22 C23 C24 Fe1 59.3(3) . . . . ? C21 Fe1 C24 C20 37.7(2) . . . . ? C16 Fe1 C24 C20 -68.8(3) . . . . ? C17 Fe1 C24 C20 -32.7(7) . . . . ? C19 Fe1 C24 C20 -154.0(2) . . . . ? C18 Fe1 C24 C20 170.2(3) . . . . ? C22 Fe1 C24 C20 81.6(3) . . . . ? C23 Fe1 C24 C20 118.8(3) . . . . ? C15 Fe1 C24 C20 -110.5(2) . . . . ? C21 Fe1 C24 C23 -81.1(3) . . . . ? C16 Fe1 C24 C23 172.5(2) . . . . ? C20 Fe1 C24 C23 -118.8(3) . . . . ? C17 Fe1 C24 C23 -151.5(5) . . . . ? C19 Fe1 C24 C23 87.3(3) . . . . ? C18 Fe1 C24 C23 51.4(5) . . . . ? C22 Fe1 C24 C23 -37.2(2) . . . . ? C15 Fe1 C24 C23 130.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.142 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.153 #end data_Complex3 _database_code_depnum_ccdc_archive 'CCDC 739914' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H22 Fe N2 Ni O2' _chemical_formula_weight 485.00 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' O O 0.0106 0.0060 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.3441(9) _cell_length_b 11.8082(8) _cell_length_c 10.6964(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.557(6) _cell_angle_gamma 90.00 _cell_volume 2022.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3874 _cell_measurement_theta_min 3.0421 _cell_measurement_theta_max 32.6153 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 1.672 _exptl_absorpt_correction_T_min 0.6997 _exptl_absorpt_correction_T_max 0.7876 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION XCALIBUR-S' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9379 _diffrn_reflns_av_R_equivalents 0.0841 _diffrn_reflns_av_sigmaI/netI 0.0739 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3538 _reflns_number_gt 2631 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.1715P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3538 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0901 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.2507 _refine_ls_wR_factor_gt 0.1830 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.149 _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 Fe1 Fe 0.64604(5) -0.40928(8) 0.44210(8) 0.0200(4) Uani 1 1 d . . . Ni1 Ni 0.81822(5) 0.02950(7) 0.32021(8) 0.0231(3) Uani 1 1 d . . . N1 N 0.8467(4) -0.0950(5) 0.4304(5) 0.0249(13) Uani 1 1 d . . . N2 N 0.7096(3) 0.0349(5) 0.3570(5) 0.0237(13) Uani 1 1 d . . . O1 O 0.9211(3) 0.0117(4) 0.2692(5) 0.0299(12) Uani 1 1 d . . . O2 O 0.7943(3) 0.1636(4) 0.2300(4) 0.0294(12) Uani 1 1 d . . . C1 C 1.0383(5) 0.0442(8) 0.1806(9) 0.045(2) Uani 1 1 d . . . H1A H 1.0784 0.0399 0.2619 0.068 Uiso 1 1 calc R . . H1B H 1.0580 0.0992 0.1246 0.068 Uiso 1 1 calc R . . H1C H 1.0330 -0.0304 0.1397 0.068 Uiso 1 1 calc R . . C2 C 0.9535(4) 0.0815(7) 0.2046(7) 0.0304(17) Uani 1 1 d . . . C3 C 0.9195(5) 0.1837(7) 0.1579(7) 0.0357(19) Uani 1 1 d . . . H3 H 0.9508 0.2308 0.1128 0.043 Uiso 1 1 calc R . . C4 C 0.8418(5) 0.2208(7) 0.1736(7) 0.0325(18) Uani 1 1 d . . . C5 C 0.8073(5) 0.3327(7) 0.1226(8) 0.043(2) Uani 1 1 d . . . H5A H 0.7562 0.3206 0.0585 0.065 Uiso 1 1 calc R . . H5B H 0.8486 0.3720 0.0834 0.065 Uiso 1 1 calc R . . H5C H 0.7946 0.3787 0.1926 0.065 Uiso 1 1 calc R . . C6 C 0.9253(4) -0.1315(6) 0.4738(6) 0.0280(16) Uani 1 1 d . . . H6 H 0.9738 -0.0969 0.4546 0.034 Uiso 1 1 calc R . . C7 C 0.9258(4) -0.2279(6) 0.5516(6) 0.0277(16) Uani 1 1 d . . . H7 H 0.9736 -0.2670 0.5966 0.033 Uiso 1 1 calc R . . C8 C 0.8448(4) -0.2536(6) 0.5495(6) 0.0255(15) Uani 1 1 d . . . H8 H 0.8253 -0.3172 0.5895 0.031 Uiso 1 1 calc R . . C9 C 0.7939(4) -0.1694(6) 0.4775(6) 0.0200(14) Uani 1 1 d . . . C10 C 0.7075(4) -0.1527(6) 0.4566(6) 0.0214(14) Uani 1 1 d . . . C11 C 0.6698(4) -0.0511(5) 0.4071(6) 0.0188(14) Uani 1 1 d . . . C12 C 0.5875(5) -0.0123(6) 0.4123(7) 0.0300(17) Uani 1 1 d . . . H12 H 0.5457 -0.0538 0.4427 0.036 Uiso 1 1 calc R . . C13 C 0.5805(5) 0.0954(6) 0.3654(7) 0.0305(17) Uani 1 1 d . . . H13 H 0.5329 0.1432 0.3575 0.037 Uiso 1 1 calc R . . C14 C 0.6565(4) 0.1226(6) 0.3311(6) 0.0285(17) Uani 1 1 d . . . H14 H 0.6687 0.1926 0.2950 0.034 Uiso 1 1 calc R . . C15 C 0.6519(4) -0.2402(5) 0.4930(6) 0.0197(14) Uani 1 1 d . . . C16 C 0.5712(4) -0.2695(5) 0.4160(6) 0.0211(14) Uani 1 1 d . . . H16 H 0.5469 -0.2370 0.3359 0.025 Uiso 1 1 calc R . . C17 C 0.5350(4) -0.3542(6) 0.4802(7) 0.0241(15) Uani 1 1 d . . . H17 H 0.4819 -0.3880 0.4513 0.029 Uiso 1 1 calc R . . C18 C 0.5918(4) -0.3804(6) 0.5957(7) 0.0295(16) Uani 1 1 d . . . H18 H 0.5830 -0.4347 0.6572 0.035 Uiso 1 1 calc R . . C19 C 0.6635(4) -0.3122(6) 0.6033(6) 0.0236(15) Uani 1 1 d . . . H19 H 0.7114 -0.3136 0.6703 0.028 Uiso 1 1 calc R . . C20 C 0.7345(4) -0.4396(7) 0.3341(7) 0.0306(17) Uani 1 1 d . . . H20 H 0.7720 -0.3856 0.3111 0.037 Uiso 1 1 calc R . . C21 C 0.6534(5) -0.4665(6) 0.2625(7) 0.0301(17) Uani 1 1 d . . . H21 H 0.6272 -0.4338 0.1834 0.036 Uiso 1 1 calc R . . C22 C 0.6191(4) -0.5507(6) 0.3308(7) 0.0258(15) Uani 1 1 d . . . H22 H 0.5655 -0.5843 0.3050 0.031 Uiso 1 1 calc R . . C23 C 0.6777(5) -0.5770(6) 0.4441(7) 0.0286(16) Uani 1 1 d . . . H23 H 0.6704 -0.6308 0.5071 0.034 Uiso 1 1 calc R . . C24 C 0.7494(4) -0.5080(6) 0.4460(7) 0.0294(17) Uani 1 1 d . . . H24 H 0.7986 -0.5077 0.5107 0.035 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 Fe1 0.0160(5) 0.0172(6) 0.0245(6) 0.0000(4) -0.0016(4) 0.0005(4) Ni1 0.0179(5) 0.0179(5) 0.0312(6) 0.0020(3) -0.0005(4) -0.0023(3) N1 0.023(3) 0.018(3) 0.030(3) -0.003(2) -0.004(2) -0.001(2) N2 0.015(3) 0.020(3) 0.031(3) -0.002(2) -0.007(2) 0.000(2) O1 0.020(2) 0.032(3) 0.041(3) -0.002(2) 0.015(2) 0.003(2) O2 0.028(3) 0.025(3) 0.034(3) 0.006(2) 0.004(2) -0.004(2) C1 0.034(4) 0.046(5) 0.053(5) 0.004(4) 0.002(4) -0.008(4) C2 0.023(4) 0.036(4) 0.033(4) 0.009(3) 0.009(3) -0.013(3) C3 0.028(4) 0.039(5) 0.038(4) 0.011(4) 0.001(3) -0.016(3) C4 0.027(4) 0.029(4) 0.038(4) 0.009(3) -0.005(3) -0.014(3) C5 0.037(4) 0.037(5) 0.050(5) 0.012(4) -0.004(4) -0.007(4) C6 0.019(3) 0.029(4) 0.033(4) -0.003(3) -0.001(3) -0.004(3) C7 0.020(3) 0.024(4) 0.035(4) 0.003(3) -0.003(3) 0.006(3) C8 0.024(4) 0.025(4) 0.025(3) 0.001(3) -0.002(3) -0.002(3) C9 0.022(3) 0.019(3) 0.019(3) 0.000(3) 0.006(3) -0.009(3) C10 0.018(3) 0.020(3) 0.022(3) -0.002(3) -0.005(3) 0.000(3) C11 0.023(3) 0.016(3) 0.015(3) 0.003(3) 0.000(3) -0.009(3) C12 0.025(4) 0.026(4) 0.033(4) 0.001(3) -0.010(3) 0.000(3) C13 0.026(4) 0.023(4) 0.038(4) -0.003(3) -0.006(3) 0.005(3) C14 0.032(4) 0.016(3) 0.031(4) 0.004(3) -0.009(3) 0.000(3) C15 0.017(3) 0.016(3) 0.025(3) -0.003(3) 0.003(3) 0.001(3) C16 0.014(3) 0.018(3) 0.030(3) 0.002(3) 0.000(3) 0.001(3) C17 0.016(3) 0.021(3) 0.037(4) -0.010(3) 0.010(3) -0.002(3) C18 0.025(4) 0.022(4) 0.040(4) 0.003(3) 0.003(3) -0.002(3) C19 0.018(3) 0.024(4) 0.027(3) -0.002(3) 0.000(3) 0.000(3) C20 0.025(4) 0.029(4) 0.038(4) 0.012(3) 0.006(3) -0.004(3) C21 0.031(4) 0.029(4) 0.026(4) -0.004(3) -0.004(3) 0.003(3) C22 0.022(3) 0.020(3) 0.035(4) -0.007(3) 0.005(3) -0.004(3) C23 0.030(4) 0.019(4) 0.036(4) 0.001(3) 0.007(3) 0.004(3) C24 0.019(3) 0.027(4) 0.040(4) -0.006(3) -0.001(3) 0.007(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 C16 2.040(6) . ? Fe1 C17 2.044(7) . ? Fe1 C19 2.043(7) . ? Fe1 C23 2.047(7) . ? Fe1 C18 2.046(8) . ? Fe1 C24 2.047(7) . ? Fe1 C22 2.047(7) . ? Fe1 C20 2.055(8) . ? Fe1 C21 2.063(7) . ? Fe1 C15 2.066(6) . ? Ni1 O2 1.855(5) . ? Ni1 O1 1.881(5) . ? Ni1 N1 1.884(6) . ? Ni1 N2 1.895(6) . ? N1 C6 1.345(9) . ? N1 C9 1.394(9) . ? N2 C14 1.344(9) . ? N2 C11 1.371(9) . ? O1 C2 1.258(9) . ? O2 C4 1.269(9) . ? C1 C2 1.524(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.380(11) . ? C3 C4 1.385(11) . ? C3 H3 0.9500 . ? C4 C5 1.496(11) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.409(10) . ? C6 H6 0.9500 . ? C7 C8 1.355(10) . ? C7 H7 0.9500 . ? C8 C9 1.421(9) . ? C8 H8 0.9500 . ? C9 C10 1.399(9) . ? C10 C11 1.404(9) . ? C10 C15 1.478(10) . ? C11 C12 1.432(10) . ? C12 C13 1.364(10) . ? C12 H12 0.9500 . ? C13 C14 1.402(11) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C19 1.435(9) . ? C15 C16 1.450(8) . ? C16 C17 1.409(10) . ? C16 H16 0.9500 . ? C17 C18 1.423(10) . ? C17 H17 0.9500 . ? C18 C19 1.410(10) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C24 1.424(10) . ? C20 C21 1.427(10) . ? C20 H20 0.9500 . ? C21 C22 1.415(11) . ? C21 H21 0.9500 . ? C22 C23 1.421(10) . ? C22 H22 0.9500 . ? C23 C24 1.424(10) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Fe1 C17 40.4(3) . . ? C16 Fe1 C19 68.9(3) . . ? C17 Fe1 C19 68.4(3) . . ? C16 Fe1 C23 158.2(3) . . ? C17 Fe1 C23 122.6(3) . . ? C19 Fe1 C23 122.8(3) . . ? C16 Fe1 C18 68.4(3) . . ? C17 Fe1 C18 40.7(3) . . ? C19 Fe1 C18 40.4(3) . . ? C23 Fe1 C18 107.6(3) . . ? C16 Fe1 C24 159.0(3) . . ? C17 Fe1 C24 160.0(3) . . ? C19 Fe1 C24 109.1(3) . . ? C23 Fe1 C24 40.7(3) . . ? C18 Fe1 C24 124.6(3) . . ? C16 Fe1 C22 121.8(3) . . ? C17 Fe1 C22 106.2(3) . . ? C19 Fe1 C22 157.9(3) . . ? C23 Fe1 C22 40.6(3) . . ? C18 Fe1 C22 121.7(3) . . ? C24 Fe1 C22 68.1(3) . . ? C16 Fe1 C20 122.3(3) . . ? C17 Fe1 C20 157.0(3) . . ? C19 Fe1 C20 125.3(3) . . ? C23 Fe1 C20 68.4(3) . . ? C18 Fe1 C20 161.3(3) . . ? C24 Fe1 C20 40.6(3) . . ? C22 Fe1 C20 67.9(3) . . ? C16 Fe1 C21 106.4(3) . . ? C17 Fe1 C21 120.6(3) . . ? C19 Fe1 C21 161.1(3) . . ? C23 Fe1 C21 68.3(3) . . ? C18 Fe1 C21 156.7(3) . . ? C24 Fe1 C21 68.3(3) . . ? C22 Fe1 C21 40.3(3) . . ? C20 Fe1 C21 40.6(3) . . ? C16 Fe1 C15 41.3(2) . . ? C17 Fe1 C15 68.7(3) . . ? C19 Fe1 C15 40.9(3) . . ? C23 Fe1 C15 159.1(3) . . ? C18 Fe1 C15 68.4(3) . . ? C24 Fe1 C15 123.4(3) . . ? C22 Fe1 C15 159.2(3) . . ? C20 Fe1 C15 108.4(3) . . ? C21 Fe1 C15 123.6(3) . . ? O2 Ni1 O1 93.0(2) . . ? O2 Ni1 N1 172.7(2) . . ? O1 Ni1 N1 88.3(3) . . ? O2 Ni1 N2 88.3(2) . . ? O1 Ni1 N2 173.4(2) . . ? N1 Ni1 N2 91.2(3) . . ? C6 N1 C9 106.9(6) . . ? C6 N1 Ni1 124.4(5) . . ? C9 N1 Ni1 128.6(5) . . ? C14 N2 C11 108.3(6) . . ? C14 N2 Ni1 125.2(5) . . ? C11 N2 Ni1 126.4(5) . . ? C2 O1 Ni1 125.8(5) . . ? C4 O2 Ni1 128.0(5) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 126.0(7) . . ? O1 C2 C1 113.6(7) . . ? C3 C2 C1 120.3(7) . . ? C2 C3 C4 123.0(7) . . ? C2 C3 H3 118.5 . . ? C4 C3 H3 118.5 . . ? O2 C4 C3 123.6(7) . . ? O2 C4 C5 114.9(7) . . ? C3 C4 C5 121.5(7) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C7 110.8(6) . . ? N1 C6 H6 124.6 . . ? C7 C6 H6 124.6 . . ? C8 C7 C6 106.3(6) . . ? C8 C7 H7 126.8 . . ? C6 C7 H7 126.8 . . ? C7 C8 C9 108.4(6) . . ? C7 C8 H8 125.8 . . ? C9 C8 H8 125.8 . . ? N1 C9 C10 122.2(6) . . ? N1 C9 C8 107.4(6) . . ? C10 C9 C8 130.3(6) . . ? C9 C10 C11 122.2(6) . . ? C9 C10 C15 120.9(6) . . ? C11 C10 C15 116.8(6) . . ? N2 C11 C10 125.0(6) . . ? N2 C11 C12 107.5(6) . . ? C10 C11 C12 127.1(6) . . ? C13 C12 C11 107.1(7) . . ? C13 C12 H12 126.4 . . ? C11 C12 H12 126.4 . . ? C12 C13 C14 107.2(7) . . ? C12 C13 H13 126.4 . . ? C14 C13 H13 126.4 . . ? N2 C14 C13 109.8(6) . . ? N2 C14 H14 125.1 . . ? C13 C14 H14 125.1 . . ? C19 C15 C16 106.4(5) . . ? C19 C15 C10 130.0(6) . . ? C16 C15 C10 123.6(6) . . ? C19 C15 Fe1 68.7(4) . . ? C16 C15 Fe1 68.4(3) . . ? C10 C15 Fe1 127.2(5) . . ? C17 C16 C15 108.4(6) . . ? C17 C16 Fe1 70.0(4) . . ? C15 C16 Fe1 70.3(3) . . ? C17 C16 H16 125.8 . . ? C15 C16 H16 125.8 . . ? Fe1 C16 H16 125.5 . . ? C16 C17 C18 108.2(6) . . ? C16 C17 Fe1 69.7(4) . . ? C18 C17 Fe1 69.7(4) . . ? C16 C17 H17 125.9 . . ? C18 C17 H17 125.9 . . ? Fe1 C17 H17 126.3 . . ? C19 C18 C17 108.4(6) . . ? C19 C18 Fe1 69.7(4) . . ? C17 C18 Fe1 69.6(4) . . ? C19 C18 H18 125.8 . . ? C17 C18 H18 125.8 . . ? Fe1 C18 H18 126.5 . . ? C18 C19 C15 108.6(6) . . ? C18 C19 Fe1 69.9(4) . . ? C15 C19 Fe1 70.4(4) . . ? C18 C19 H19 125.7 . . ? C15 C19 H19 125.7 . . ? Fe1 C19 H19 125.5 . . ? C24 C20 C21 108.0(6) . . ? C24 C20 Fe1 69.4(4) . . ? C21 C20 Fe1 70.0(4) . . ? C24 C20 H20 126.0 . . ? C21 C20 H20 126.0 . . ? Fe1 C20 H20 126.2 . . ? C22 C21 C20 107.5(6) . . ? C22 C21 Fe1 69.3(4) . . ? C20 C21 Fe1 69.4(4) . . ? C22 C21 H21 126.2 . . ? C20 C21 H21 126.2 . . ? Fe1 C21 H21 126.6 . . ? C21 C22 C23 109.0(6) . . ? C21 C22 Fe1 70.4(4) . . ? C23 C22 Fe1 69.7(4) . . ? C21 C22 H22 125.5 . . ? C23 C22 H22 125.5 . . ? Fe1 C22 H22 125.9 . . ? C22 C23 C24 107.4(6) . . ? C22 C23 Fe1 69.7(4) . . ? C24 C23 Fe1 69.6(4) . . ? C22 C23 H23 126.3 . . ? C24 C23 H23 126.3 . . ? Fe1 C23 H23 125.9 . . ? C20 C24 C23 108.1(6) . . ? C20 C24 Fe1 70.0(4) . . ? C23 C24 Fe1 69.6(4) . . ? C20 C24 H24 125.9 . . ? C23 C24 H24 125.9 . . ? Fe1 C24 H24 126.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Ni1 N1 C6 -79(2) . . . . ? O1 Ni1 N1 C6 21.8(6) . . . . ? N2 Ni1 N1 C6 -164.8(6) . . . . ? O2 Ni1 N1 C9 104.6(19) . . . . ? O1 Ni1 N1 C9 -154.9(6) . . . . ? N2 Ni1 N1 C9 18.5(6) . . . . ? O2 Ni1 N2 C14 -8.3(5) . . . . ? O1 Ni1 N2 C14 -110(2) . . . . ? N1 Ni1 N2 C14 164.4(5) . . . . ? O2 Ni1 N2 C11 167.6(5) . . . . ? O1 Ni1 N2 C11 66(2) . . . . ? N1 Ni1 N2 C11 -19.7(5) . . . . ? O2 Ni1 O1 C2 4.7(6) . . . . ? N1 Ni1 O1 C2 -168.1(6) . . . . ? N2 Ni1 O1 C2 106(2) . . . . ? O1 Ni1 O2 C4 -8.3(6) . . . . ? N1 Ni1 O2 C4 92(2) . . . . ? N2 Ni1 O2 C4 178.2(6) . . . . ? Ni1 O1 C2 C3 -0.7(11) . . . . ? Ni1 O1 C2 C1 178.9(5) . . . . ? O1 C2 C3 C4 -2.3(12) . . . . ? C1 C2 C3 C4 178.2(7) . . . . ? Ni1 O2 C4 C3 7.9(10) . . . . ? Ni1 O2 C4 C5 -172.9(5) . . . . ? C2 C3 C4 O2 -1.5(12) . . . . ? C2 C3 C4 C5 179.4(7) . . . . ? C9 N1 C6 C7 -1.2(8) . . . . ? Ni1 N1 C6 C7 -178.5(5) . . . . ? N1 C6 C7 C8 3.2(8) . . . . ? C6 C7 C8 C9 -3.7(8) . . . . ? C6 N1 C9 C10 176.3(6) . . . . ? Ni1 N1 C9 C10 -6.6(9) . . . . ? C6 N1 C9 C8 -1.1(7) . . . . ? Ni1 N1 C9 C8 176.0(4) . . . . ? C7 C8 C9 N1 3.1(8) . . . . ? C7 C8 C9 C10 -174.0(7) . . . . ? N1 C9 C10 C11 -11.5(10) . . . . ? C8 C9 C10 C11 165.2(6) . . . . ? N1 C9 C10 C15 172.0(6) . . . . ? C8 C9 C10 C15 -11.3(11) . . . . ? C14 N2 C11 C10 -173.9(6) . . . . ? Ni1 N2 C11 C10 9.6(9) . . . . ? C14 N2 C11 C12 -0.3(7) . . . . ? Ni1 N2 C11 C12 -176.8(4) . . . . ? C9 C10 C11 N2 10.0(10) . . . . ? C15 C10 C11 N2 -173.4(6) . . . . ? C9 C10 C11 C12 -162.3(6) . . . . ? C15 C10 C11 C12 14.3(9) . . . . ? N2 C11 C12 C13 0.0(8) . . . . ? C10 C11 C12 C13 173.4(6) . . . . ? C11 C12 C13 C14 0.4(8) . . . . ? C11 N2 C14 C13 0.6(7) . . . . ? Ni1 N2 C14 C13 177.1(5) . . . . ? C12 C13 C14 N2 -0.6(8) . . . . ? C9 C10 C15 C19 39.4(10) . . . . ? C11 C10 C15 C19 -137.3(7) . . . . ? C9 C10 C15 C16 -140.0(6) . . . . ? C11 C10 C15 C16 43.3(9) . . . . ? C9 C10 C15 Fe1 -53.0(8) . . . . ? C11 C10 C15 Fe1 130.3(5) . . . . ? C16 Fe1 C15 C19 118.7(5) . . . . ? C17 Fe1 C15 C19 81.3(4) . . . . ? C23 Fe1 C15 C19 -45.4(9) . . . . ? C18 Fe1 C15 C19 37.4(4) . . . . ? C24 Fe1 C15 C19 -80.7(5) . . . . ? C22 Fe1 C15 C19 160.7(7) . . . . ? C20 Fe1 C15 C19 -123.1(4) . . . . ? C21 Fe1 C15 C19 -165.3(4) . . . . ? C17 Fe1 C15 C16 -37.4(4) . . . . ? C19 Fe1 C15 C16 -118.7(5) . . . . ? C23 Fe1 C15 C16 -164.1(7) . . . . ? C18 Fe1 C15 C16 -81.3(4) . . . . ? C24 Fe1 C15 C16 160.7(4) . . . . ? C22 Fe1 C15 C16 42.0(9) . . . . ? C20 Fe1 C15 C16 118.3(4) . . . . ? C21 Fe1 C15 C16 76.0(5) . . . . ? C16 Fe1 C15 C10 -116.5(7) . . . . ? C17 Fe1 C15 C10 -153.9(6) . . . . ? C19 Fe1 C15 C10 124.8(7) . . . . ? C23 Fe1 C15 C10 79.4(10) . . . . ? C18 Fe1 C15 C10 162.2(6) . . . . ? C24 Fe1 C15 C10 44.1(6) . . . . ? C22 Fe1 C15 C10 -74.5(10) . . . . ? C20 Fe1 C15 C10 1.8(6) . . . . ? C21 Fe1 C15 C10 -40.5(7) . . . . ? C19 C15 C16 C17 1.4(7) . . . . ? C10 C15 C16 C17 -179.0(6) . . . . ? Fe1 C15 C16 C17 59.8(5) . . . . ? C19 C15 C16 Fe1 -58.4(4) . . . . ? C10 C15 C16 Fe1 121.1(6) . . . . ? C19 Fe1 C16 C17 -81.1(4) . . . . ? C23 Fe1 C16 C17 45.6(9) . . . . ? C18 Fe1 C16 C17 -37.7(4) . . . . ? C24 Fe1 C16 C17 -169.6(7) . . . . ? C22 Fe1 C16 C17 77.1(5) . . . . ? C20 Fe1 C16 C17 159.6(4) . . . . ? C21 Fe1 C16 C17 118.3(4) . . . . ? C15 Fe1 C16 C17 -119.1(6) . . . . ? C17 Fe1 C16 C15 119.1(6) . . . . ? C19 Fe1 C16 C15 38.0(4) . . . . ? C23 Fe1 C16 C15 164.8(7) . . . . ? C18 Fe1 C16 C15 81.5(4) . . . . ? C24 Fe1 C16 C15 -50.5(9) . . . . ? C22 Fe1 C16 C15 -163.7(4) . . . . ? C20 Fe1 C16 C15 -81.3(5) . . . . ? C21 Fe1 C16 C15 -122.6(4) . . . . ? C15 C16 C17 C18 -0.8(8) . . . . ? Fe1 C16 C17 C18 59.2(5) . . . . ? C15 C16 C17 Fe1 -60.1(4) . . . . ? C19 Fe1 C17 C16 82.3(4) . . . . ? C23 Fe1 C17 C16 -161.6(4) . . . . ? C18 Fe1 C17 C16 119.5(6) . . . . ? C24 Fe1 C17 C16 169.2(7) . . . . ? C22 Fe1 C17 C16 -120.4(4) . . . . ? C20 Fe1 C17 C16 -48.8(8) . . . . ? C21 Fe1 C17 C16 -79.1(5) . . . . ? C15 Fe1 C17 C16 38.3(4) . . . . ? C16 Fe1 C17 C18 -119.5(6) . . . . ? C19 Fe1 C17 C18 -37.2(4) . . . . ? C23 Fe1 C17 C18 78.9(5) . . . . ? C24 Fe1 C17 C18 49.6(9) . . . . ? C22 Fe1 C17 C18 120.1(4) . . . . ? C20 Fe1 C17 C18 -168.3(7) . . . . ? C21 Fe1 C17 C18 161.4(4) . . . . ? C15 Fe1 C17 C18 -81.3(4) . . . . ? C16 C17 C18 C19 -0.1(8) . . . . ? Fe1 C17 C18 C19 59.1(5) . . . . ? C16 C17 C18 Fe1 -59.2(5) . . . . ? C16 Fe1 C18 C19 -82.4(4) . . . . ? C17 Fe1 C18 C19 -119.8(6) . . . . ? C23 Fe1 C18 C19 120.4(4) . . . . ? C24 Fe1 C18 C19 78.7(5) . . . . ? C22 Fe1 C18 C19 162.6(4) . . . . ? C20 Fe1 C18 C19 45.9(11) . . . . ? C21 Fe1 C18 C19 -163.7(6) . . . . ? C15 Fe1 C18 C19 -37.8(4) . . . . ? C16 Fe1 C18 C17 37.3(4) . . . . ? C19 Fe1 C18 C17 119.8(6) . . . . ? C23 Fe1 C18 C17 -119.9(4) . . . . ? C24 Fe1 C18 C17 -161.5(4) . . . . ? C22 Fe1 C18 C17 -77.6(5) . . . . ? C20 Fe1 C18 C17 165.7(8) . . . . ? C21 Fe1 C18 C17 -43.9(9) . . . . ? C15 Fe1 C18 C17 81.9(4) . . . . ? C17 C18 C19 C15 1.0(8) . . . . ? Fe1 C18 C19 C15 60.0(5) . . . . ? C17 C18 C19 Fe1 -59.0(5) . . . . ? C16 C15 C19 C18 -1.5(7) . . . . ? C10 C15 C19 C18 179.0(7) . . . . ? Fe1 C15 C19 C18 -59.7(5) . . . . ? C16 C15 C19 Fe1 58.2(4) . . . . ? C10 C15 C19 Fe1 -121.3(7) . . . . ? C16 Fe1 C19 C18 81.0(4) . . . . ? C17 Fe1 C19 C18 37.5(4) . . . . ? C23 Fe1 C19 C18 -78.2(5) . . . . ? C24 Fe1 C19 C18 -121.3(4) . . . . ? C22 Fe1 C19 C18 -42.4(9) . . . . ? C20 Fe1 C19 C18 -163.6(4) . . . . ? C21 Fe1 C19 C18 160.0(8) . . . . ? C15 Fe1 C19 C18 119.4(6) . . . . ? C16 Fe1 C19 C15 -38.4(4) . . . . ? C17 Fe1 C19 C15 -81.9(4) . . . . ? C23 Fe1 C19 C15 162.4(4) . . . . ? C18 Fe1 C19 C15 -119.4(6) . . . . ? C24 Fe1 C19 C15 119.3(4) . . . . ? C22 Fe1 C19 C15 -161.8(7) . . . . ? C20 Fe1 C19 C15 76.9(5) . . . . ? C21 Fe1 C19 C15 40.6(10) . . . . ? C16 Fe1 C20 C24 163.7(4) . . . . ? C17 Fe1 C20 C24 -161.1(6) . . . . ? C19 Fe1 C20 C24 78.0(5) . . . . ? C23 Fe1 C20 C24 -37.8(4) . . . . ? C18 Fe1 C20 C24 43.2(11) . . . . ? C22 Fe1 C20 C24 -81.7(4) . . . . ? C21 Fe1 C20 C24 -119.3(6) . . . . ? C15 Fe1 C20 C24 120.2(4) . . . . ? C16 Fe1 C20 C21 -77.1(5) . . . . ? C17 Fe1 C20 C21 -41.9(9) . . . . ? C19 Fe1 C20 C21 -162.8(4) . . . . ? C23 Fe1 C20 C21 81.5(5) . . . . ? C18 Fe1 C20 C21 162.5(8) . . . . ? C24 Fe1 C20 C21 119.3(6) . . . . ? C22 Fe1 C20 C21 37.6(4) . . . . ? C15 Fe1 C20 C21 -120.6(4) . . . . ? C24 C20 C21 C22 0.1(9) . . . . ? Fe1 C20 C21 C22 -59.0(5) . . . . ? C24 C20 C21 Fe1 59.1(5) . . . . ? C16 Fe1 C21 C22 -120.2(4) . . . . ? C17 Fe1 C21 C22 -78.6(5) . . . . ? C19 Fe1 C21 C22 167.2(7) . . . . ? C23 Fe1 C21 C22 37.4(4) . . . . ? C18 Fe1 C21 C22 -46.9(9) . . . . ? C24 Fe1 C21 C22 81.4(4) . . . . ? C20 Fe1 C21 C22 119.0(6) . . . . ? C15 Fe1 C21 C22 -162.1(4) . . . . ? C16 Fe1 C21 C20 120.8(4) . . . . ? C17 Fe1 C21 C20 162.3(4) . . . . ? C19 Fe1 C21 C20 48.1(10) . . . . ? C23 Fe1 C21 C20 -81.7(5) . . . . ? C18 Fe1 C21 C20 -165.9(7) . . . . ? C24 Fe1 C21 C20 -37.7(4) . . . . ? C22 Fe1 C21 C20 -119.0(6) . . . . ? C15 Fe1 C21 C20 78.9(5) . . . . ? C20 C21 C22 C23 -0.1(8) . . . . ? Fe1 C21 C22 C23 -59.2(5) . . . . ? C20 C21 C22 Fe1 59.1(5) . . . . ? C16 Fe1 C22 C21 77.4(5) . . . . ? C17 Fe1 C22 C21 118.5(4) . . . . ? C19 Fe1 C22 C21 -169.0(6) . . . . ? C23 Fe1 C22 C21 -119.9(6) . . . . ? C18 Fe1 C22 C21 160.1(4) . . . . ? C24 Fe1 C22 C21 -81.8(5) . . . . ? C20 Fe1 C22 C21 -37.8(4) . . . . ? C15 Fe1 C22 C21 46.1(9) . . . . ? C16 Fe1 C22 C23 -162.6(4) . . . . ? C17 Fe1 C22 C23 -121.5(4) . . . . ? C19 Fe1 C22 C23 -49.0(9) . . . . ? C18 Fe1 C22 C23 -79.9(5) . . . . ? C24 Fe1 C22 C23 38.1(4) . . . . ? C20 Fe1 C22 C23 82.1(5) . . . . ? C21 Fe1 C22 C23 119.9(6) . . . . ? C15 Fe1 C22 C23 166.0(7) . . . . ? C21 C22 C23 C24 0.0(8) . . . . ? Fe1 C22 C23 C24 -59.7(5) . . . . ? C21 C22 C23 Fe1 59.7(5) . . . . ? C16 Fe1 C23 C22 43.0(10) . . . . ? C17 Fe1 C23 C22 76.3(5) . . . . ? C19 Fe1 C23 C22 160.2(4) . . . . ? C18 Fe1 C23 C22 118.5(4) . . . . ? C24 Fe1 C23 C22 -118.5(6) . . . . ? C20 Fe1 C23 C22 -80.8(5) . . . . ? C21 Fe1 C23 C22 -37.1(4) . . . . ? C15 Fe1 C23 C22 -166.1(7) . . . . ? C16 Fe1 C23 C24 161.5(7) . . . . ? C17 Fe1 C23 C24 -165.1(4) . . . . ? C19 Fe1 C23 C24 -81.3(5) . . . . ? C18 Fe1 C23 C24 -123.0(4) . . . . ? C22 Fe1 C23 C24 118.5(6) . . . . ? C20 Fe1 C23 C24 37.7(4) . . . . ? C21 Fe1 C23 C24 81.5(5) . . . . ? C15 Fe1 C23 C24 -47.6(10) . . . . ? C21 C20 C24 C23 -0.1(9) . . . . ? Fe1 C20 C24 C23 59.4(5) . . . . ? C21 C20 C24 Fe1 -59.5(5) . . . . ? C22 C23 C24 C20 0.1(8) . . . . ? Fe1 C23 C24 C20 -59.7(5) . . . . ? C22 C23 C24 Fe1 59.7(5) . . . . ? C16 Fe1 C24 C20 -41.6(9) . . . . ? C17 Fe1 C24 C20 158.3(7) . . . . ? C19 Fe1 C24 C20 -122.3(4) . . . . ? C23 Fe1 C24 C20 119.2(6) . . . . ? C18 Fe1 C24 C20 -164.6(4) . . . . ? C22 Fe1 C24 C20 81.1(4) . . . . ? C21 Fe1 C24 C20 37.6(4) . . . . ? C15 Fe1 C24 C20 -79.2(5) . . . . ? C16 Fe1 C24 C23 -160.8(7) . . . . ? C17 Fe1 C24 C23 39.1(10) . . . . ? C19 Fe1 C24 C23 118.5(4) . . . . ? C18 Fe1 C24 C23 76.2(5) . . . . ? C22 Fe1 C24 C23 -38.0(4) . . . . ? C20 Fe1 C24 C23 -119.2(6) . . . . ? C21 Fe1 C24 C23 -81.6(5) . . . . ? C15 Fe1 C24 C23 161.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.701 _refine_diff_density_min -1.766 _refine_diff_density_rms 0.204