data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H41 Fe2 N2' _chemical_formula_weight 565.37 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnn2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x, -y, z' _cell_length_a 12.0653(17) _cell_length_b 15.218(2) _cell_length_c 15.969(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2932.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'blocks' _exptl_crystal_colour 'dark green brown' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1196 _exptl_absorpt_coefficient_mu 1.011 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.5821 _exptl_absorpt_correction_T_max 0.7512 _exptl_absorpt_process_details 'ABSCOR' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU RAXIS RAPID' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27158 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6715 _reflns_number_gt 4507 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RIGAKU PROCESS AUTO' _computing_cell_refinement 'RIGAKU PROCESS AUTO' _computing_data_reduction 'RIGAKU PROCESS AUTO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0746P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.33(3) _refine_ls_number_reflns 6715 _refine_ls_number_parameters 325 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1309 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.002 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.28750(4) 0.33911(3) 0.79852(10) 0.03970(14) Uani 1 1 d . . . Fe2 Fe 0.18130(4) 0.19868(3) 0.79844(9) 0.04142(14) Uani 1 1 d . . . N1 N 0.2444(3) 0.2651(3) 0.8960(3) 0.0496(9) Uani 1 1 d . . . H1 H 0.3018 0.2380 0.9224 0.060 Uiso 1 1 calc R . . N2 N 0.1823(3) 0.2935(3) 0.7368(2) 0.0521(10) Uani 1 1 d . . . C1 C 0.1622(9) 0.3062(6) 0.9526(9) 0.111(5) Uani 1 1 d . . . C2 C 0.2058(11) 0.2935(7) 1.0310(9) 0.112(5) Uani 1 1 d . . . H2 H 0.2721 0.2627 1.0365 0.134 Uiso 1 1 calc R . . C3 C 0.1562(11) 0.3237(8) 1.0987(8) 0.108(4) Uani 1 1 d . . . H3 H 0.1887 0.3156 1.1509 0.129 Uiso 1 1 calc R . . C4 C 0.0598(11) 0.3657(8) 1.0924(7) 0.099(4) Uani 1 1 d . . . H4 H 0.0248 0.3856 1.1407 0.119 Uiso 1 1 calc R . . C5 C 0.0070(9) 0.3814(7) 1.0094(8) 0.094(4) Uani 1 1 d . . . H5 H -0.0601 0.4105 1.0025 0.113 Uiso 1 1 calc R . . C6 C 0.0703(13) 0.3471(7) 0.9417(5) 0.106(4) Uani 1 1 d . . . H6 H 0.0440 0.3546 0.8875 0.127 Uiso 1 1 calc R . . C7 C 0.1557(13) 0.3075(7) 0.6484(5) 0.120(5) Uani 1 1 d . . . C8 C 0.1969(8) 0.2930(5) 0.5714(8) 0.092(4) Uani 1 1 d . . . H8 H 0.2623 0.2613 0.5652 0.110 Uiso 1 1 calc R . . C9 C 0.1424(8) 0.3251(6) 0.5002(5) 0.071(3) Uani 1 1 d . . . H9 H 0.1738 0.3170 0.4476 0.086 Uiso 1 1 calc R . . C10 C 0.0431(9) 0.3683(6) 0.5073(7) 0.075(3) Uani 1 1 d . . . H10 H 0.0046 0.3887 0.4608 0.090 Uiso 1 1 calc R . . C11 C 0.0076(10) 0.3786(7) 0.5799(7) 0.096(4) Uani 1 1 d . . . H11 H -0.0598 0.4080 0.5840 0.115 Uiso 1 1 calc R . . C12 C 0.0519(11) 0.3538(7) 0.6521(7) 0.104(4) Uani 1 1 d . . . H12 H 0.0174 0.3658 0.7029 0.125 Uiso 1 1 calc R . . C13 C 0.4599(3) 0.3639(2) 0.7993(7) 0.0464(8) Uani 1 1 d . . . C14 C 0.4130(6) 0.4040(5) 0.7292(4) 0.049(2) Uani 1 1 d . . . C15 C 0.3265(6) 0.4603(5) 0.7547(5) 0.0435(19) Uani 1 1 d . . . C16 C 0.3298(6) 0.4648(5) 0.8442(5) 0.052(2) Uani 1 1 d . . . C17 C 0.4078(6) 0.4001(5) 0.8721(5) 0.050(2) Uani 1 1 d . . . C18 C 0.5516(3) 0.2977(3) 0.7975(7) 0.0705(13) Uani 1 1 d . . . H18A H 0.5390 0.2569 0.7527 0.106 Uiso 1 1 calc R . . H18B H 0.5535 0.2666 0.8498 0.106 Uiso 1 1 calc R . . H18C H 0.6210 0.3272 0.7889 0.106 Uiso 1 1 calc R . . C19 C 0.4418(8) 0.3897(6) 0.6384(5) 0.069(2) Uani 1 1 d . . . H19A H 0.5051 0.4248 0.6240 0.104 Uiso 1 1 calc R . . H19B H 0.3800 0.4065 0.6040 0.104 Uiso 1 1 calc R . . H19C H 0.4584 0.3288 0.6293 0.104 Uiso 1 1 calc R . . C20 C 0.2573(9) 0.5191(6) 0.6994(7) 0.078(3) Uani 1 1 d . . . H20A H 0.1879 0.5311 0.7264 0.117 Uiso 1 1 calc R . . H20B H 0.2439 0.4902 0.6469 0.117 Uiso 1 1 calc R . . H20C H 0.2961 0.5732 0.6897 0.117 Uiso 1 1 calc R . . C21 C 0.2581(8) 0.5184(5) 0.8982(5) 0.058(2) Uani 1 1 d . . . H21A H 0.2474 0.4889 0.9508 0.086 Uiso 1 1 calc R . . H21B H 0.1877 0.5268 0.8714 0.086 Uiso 1 1 calc R . . H21C H 0.2924 0.5744 0.9078 0.086 Uiso 1 1 calc R . . C22 C 0.4469(7) 0.3794(5) 0.9591(5) 0.061(2) Uani 1 1 d . . . H22A H 0.5114 0.4140 0.9716 0.092 Uiso 1 1 calc R . . H22B H 0.4653 0.3181 0.9628 0.092 Uiso 1 1 calc R . . H22C H 0.3893 0.3928 0.9985 0.092 Uiso 1 1 calc R . . C23 C 0.2323(4) 0.0659(3) 0.8059(6) 0.0557(12) Uani 1 1 d . . . C24 C 0.1692(8) 0.0824(5) 0.7302(5) 0.059(2) Uani 1 1 d . . . C25 C 0.0606(6) 0.1137(5) 0.7537(5) 0.0474(18) Uani 1 1 d . . . C26 C 0.0678(8) 0.1113(5) 0.8436(6) 0.070(3) Uani 1 1 d . . . C27 C 0.1695(7) 0.0850(5) 0.8724(5) 0.053(2) Uani 1 1 d . . . C28 C 0.3491(5) 0.0302(3) 0.7940(10) 0.0954(19) Uani 1 1 d . . . H28A H 0.4012 0.0779 0.7951 0.143 Uiso 1 1 calc R . . H28B H 0.3538 0.0005 0.7410 0.143 Uiso 1 1 calc R . . H28C H 0.3660 -0.0103 0.8382 0.143 Uiso 1 1 calc R . . C29 C 0.2114(8) 0.0716(6) 0.6364(4) 0.075(3) Uani 1 1 d . . . H29A H 0.2886 0.0865 0.6333 0.112 Uiso 1 1 calc R . . H29B H 0.1698 0.1100 0.6004 0.112 Uiso 1 1 calc R . . H29C H 0.2012 0.0118 0.6187 0.112 Uiso 1 1 calc R . . C30 C -0.0283(7) 0.1321(5) 0.6989(6) 0.082(3) Uani 1 1 d . . . H30A H -0.0758 0.0817 0.6952 0.122 Uiso 1 1 calc R . . H30B H 0.0003 0.1460 0.6443 0.122 Uiso 1 1 calc R . . H30C H -0.0697 0.1813 0.7199 0.122 Uiso 1 1 calc R . . C31 C -0.0394(8) 0.1368(6) 0.8957(8) 0.129(5) Uani 1 1 d . . . H31A H -0.0885 0.0873 0.8984 0.193 Uiso 1 1 calc R . . H31B H -0.0765 0.1850 0.8689 0.193 Uiso 1 1 calc R . . H31C H -0.0181 0.1537 0.9514 0.193 Uiso 1 1 calc R . . C32 C 0.1976(10) 0.0691(7) 0.9556(5) 0.101(4) Uani 1 1 d . . . H32A H 0.1710 0.1163 0.9899 0.152 Uiso 1 1 calc R . . H32B H 0.2768 0.0651 0.9606 0.152 Uiso 1 1 calc R . . H32C H 0.1646 0.0149 0.9736 0.152 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 0.0477(2) 0.0405(2) 0.0310(2) 0.0010(7) 0.0010(7) -0.01106(18) Fe2 0.0519(3) 0.0403(2) 0.0321(2) 0.0005(7) -0.0022(7) -0.01268(19) N1 0.059(2) 0.053(2) 0.037(2) -0.0004(17) -0.0078(17) -0.0160(19) N2 0.066(2) 0.054(2) 0.0356(19) 0.0077(17) -0.0178(19) -0.027(2) C1 0.114(7) 0.057(6) 0.162(12) -0.047(6) 0.110(8) -0.045(5) C2 0.120(9) 0.100(8) 0.116(9) -0.031(7) 0.081(8) -0.043(6) C3 0.093(7) 0.112(9) 0.118(10) 0.013(7) 0.009(7) -0.032(6) C4 0.131(9) 0.104(8) 0.063(7) -0.027(6) 0.046(7) -0.048(7) C5 0.098(7) 0.073(6) 0.110(9) 0.006(6) -0.031(6) -0.013(5) C6 0.205(13) 0.089(7) 0.023(4) -0.004(4) 0.001(6) -0.068(8) C7 0.241(13) 0.076(7) 0.044(5) 0.033(5) -0.067(7) -0.098(8) C8 0.084(6) 0.040(4) 0.153(11) -0.005(6) -0.048(6) -0.004(4) C9 0.093(6) 0.084(6) 0.037(4) -0.002(4) -0.021(4) -0.018(5) C10 0.088(5) 0.075(6) 0.062(6) 0.021(5) -0.030(5) 0.015(4) C11 0.142(9) 0.073(6) 0.073(7) -0.001(5) -0.051(6) 0.000(6) C12 0.138(8) 0.088(7) 0.087(8) 0.009(6) -0.037(7) -0.043(7) C13 0.0480(17) 0.0502(18) 0.0410(18) -0.011(5) 0.000(5) -0.0098(13) C14 0.056(4) 0.059(5) 0.032(3) 0.014(3) -0.010(3) -0.023(4) C15 0.057(4) 0.033(3) 0.041(4) 0.006(3) -0.014(3) -0.004(3) C16 0.052(4) 0.051(4) 0.053(5) -0.004(4) -0.014(4) -0.025(4) C17 0.055(4) 0.040(4) 0.054(5) 0.011(3) -0.014(3) -0.009(3) C18 0.062(2) 0.071(3) 0.078(3) -0.018(6) -0.023(6) 0.0079(19) C19 0.074(5) 0.080(5) 0.054(5) -0.008(4) 0.020(4) -0.012(4) C20 0.084(6) 0.074(6) 0.076(7) 0.002(6) -0.004(6) -0.014(6) C21 0.070(5) 0.045(4) 0.057(5) -0.024(4) 0.014(5) 0.001(4) C22 0.081(5) 0.066(4) 0.036(4) -0.009(3) -0.001(4) -0.025(4) C23 0.076(2) 0.0429(18) 0.048(3) 0.004(4) -0.020(4) -0.0105(17) C24 0.089(6) 0.040(4) 0.047(5) 0.008(4) 0.014(4) -0.008(4) C25 0.042(3) 0.052(4) 0.049(5) -0.005(4) -0.003(3) -0.009(3) C26 0.100(7) 0.042(4) 0.068(6) -0.015(4) 0.039(5) -0.034(4) C27 0.070(5) 0.052(5) 0.038(4) 0.011(4) -0.004(4) -0.020(4) C28 0.092(3) 0.071(3) 0.123(5) -0.022(8) 0.006(8) 0.019(3) C29 0.113(6) 0.064(5) 0.047(5) -0.023(4) 0.023(4) -0.010(4) C30 0.090(5) 0.077(6) 0.078(5) 0.009(5) -0.003(4) -0.041(4) C31 0.116(7) 0.075(6) 0.196(11) -0.013(7) 0.132(7) -0.025(5) C32 0.185(11) 0.069(6) 0.049(5) 0.000(4) -0.027(6) -0.038(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.751(3) . ? Fe1 N1 1.990(4) . ? Fe1 C15 2.028(7) . ? Fe1 C17 2.086(7) . ? Fe1 C13 2.114(3) . ? Fe1 C16 2.110(7) . ? Fe1 C14 2.120(7) . ? Fe1 Fe2 2.4916(6) . ? Fe2 N2 1.747(4) . ? Fe2 N1 2.007(4) . ? Fe2 C26 2.041(8) . ? Fe2 C25 2.075(7) . ? Fe2 C27 2.100(7) . ? Fe2 C23 2.115(4) . ? Fe2 C24 2.083(8) . ? N1 C1 1.480(8) . ? N2 C7 1.463(8) . ? C1 C2 1.372(19) . ? C1 C6 1.283(17) . ? C2 C3 1.318(15) . ? C3 C4 1.331(16) . ? C4 C5 1.490(15) . ? C5 C6 1.422(16) . ? C7 C12 1.438(17) . ? C7 C8 1.345(15) . ? C8 C9 1.401(13) . ? C9 C10 1.372(13) . ? C10 C11 1.245(13) . ? C11 C12 1.327(14) . ? C13 C14 1.394(10) . ? C13 C17 1.433(11) . ? C13 C18 1.496(5) . ? C14 C19 1.507(11) . ? C14 C15 1.411(11) . ? C15 C16 1.432(5) . ? C15 C20 1.508(12) . ? C16 C17 1.433(11) . ? C16 C21 1.468(12) . ? C17 C22 1.500(10) . ? C23 C27 1.337(11) . ? C23 C24 1.449(11) . ? C23 C28 1.523(7) . ? C24 C25 1.444(11) . ? C24 C29 1.592(10) . ? C25 C30 1.412(11) . ? C25 C26 1.440(6) . ? C26 C27 1.371(13) . ? C26 C31 1.586(11) . ? C27 C32 1.392(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N1 91.52(18) . . ? N2 Fe1 C15 109.5(2) . . ? N1 Fe1 C15 147.7(3) . . ? N2 Fe1 C17 176.8(3) . . ? N1 Fe1 C17 89.6(2) . . ? C15 Fe1 C17 68.2(3) . . ? N2 Fe1 C13 141.9(3) . . ? N1 Fe1 C13 110.7(3) . . ? C15 Fe1 C13 67.2(3) . . ? C17 Fe1 C13 39.9(3) . . ? N2 Fe1 C16 136.9(3) . . ? N1 Fe1 C16 107.8(3) . . ? C15 Fe1 C16 40.44(14) . . ? C17 Fe1 C16 39.9(3) . . ? C13 Fe1 C16 66.3(3) . . ? N2 Fe1 C14 114.1(2) . . ? N1 Fe1 C14 149.1(2) . . ? C15 Fe1 C14 39.7(3) . . ? C17 Fe1 C14 65.77(15) . . ? C13 Fe1 C14 38.4(3) . . ? C16 Fe1 C14 65.5(3) . . ? N2 Fe1 Fe2 44.51(12) . . ? N1 Fe1 Fe2 51.74(11) . . ? C15 Fe1 Fe2 154.0(2) . . ? C17 Fe1 Fe2 137.7(2) . . ? C13 Fe1 Fe2 131.22(9) . . ? C16 Fe1 Fe2 154.4(2) . . ? C14 Fe1 Fe2 140.1(2) . . ? N2 Fe2 N1 91.08(18) . . ? N2 Fe2 C26 137.9(3) . . ? N1 Fe2 C26 108.0(3) . . ? N2 Fe2 C25 109.0(2) . . ? N1 Fe2 C25 148.0(2) . . ? C26 Fe2 C25 40.94(18) . . ? N2 Fe2 C27 176.5(3) . . ? N1 Fe2 C27 90.2(3) . . ? C26 Fe2 C27 38.6(4) . . ? C25 Fe2 C27 68.5(3) . . ? N2 Fe2 C23 145.0(3) . . ? N1 Fe2 C23 109.1(3) . . ? C26 Fe2 C23 63.4(3) . . ? C25 Fe2 C23 68.2(3) . . ? C27 Fe2 C23 37.0(3) . . ? N2 Fe2 C24 114.1(3) . . ? N1 Fe2 C24 149.3(3) . . ? C26 Fe2 C24 65.4(3) . . ? C25 Fe2 C24 40.6(3) . . ? C27 Fe2 C24 65.75(16) . . ? C23 Fe2 C24 40.4(3) . . ? N2 Fe2 Fe1 44.63(11) . . ? N1 Fe2 Fe1 51.14(11) . . ? C26 Fe2 Fe1 154.7(2) . . ? C25 Fe2 Fe1 153.6(2) . . ? C27 Fe2 Fe1 137.8(2) . . ? C23 Fe2 Fe1 132.03(12) . . ? C24 Fe2 Fe1 139.9(2) . . ? C1 N1 Fe1 114.4(6) . . ? C1 N1 Fe2 115.6(6) . . ? Fe1 N1 Fe2 77.12(15) . . ? C7 N2 Fe2 131.5(4) . . ? C7 N2 Fe1 130.1(5) . . ? Fe2 N2 Fe1 90.86(17) . . ? C2 C1 C6 121.6(9) . . ? C2 C1 N1 103.9(11) . . ? C6 C1 N1 134.6(14) . . ? C1 C2 C3 121.6(14) . . ? C4 C3 C2 120.2(14) . . ? C3 C4 C5 121.1(11) . . ? C6 C5 C4 112.8(10) . . ? C1 C6 C5 122.6(10) . . ? N2 C7 C12 102.8(11) . . ? N2 C7 C8 141.0(14) . . ? C12 C7 C8 116.1(9) . . ? C9 C8 C7 120.7(11) . . ? C8 C9 C10 120.7(9) . . ? C11 C10 C9 116.0(9) . . ? C10 C11 C12 129.4(13) . . ? C11 C12 C7 117.1(12) . . ? C14 C13 C17 107.8(3) . . ? C14 C13 C18 125.4(9) . . ? C17 C13 C18 126.8(8) . . ? C14 C13 Fe1 71.0(3) . . ? C17 C13 Fe1 69.0(3) . . ? C18 C13 Fe1 127.4(2) . . ? C13 C14 C19 128.0(8) . . ? C13 C14 C15 109.6(6) . . ? C19 C14 C15 122.3(7) . . ? C13 C14 Fe1 70.6(3) . . ? C19 C14 Fe1 126.8(6) . . ? C15 C14 Fe1 66.6(4) . . ? C16 C15 C14 107.2(8) . . ? C16 C15 C20 124.9(9) . . ? C14 C15 C20 127.0(8) . . ? C16 C15 Fe1 72.9(5) . . ? C14 C15 Fe1 73.7(4) . . ? C20 C15 Fe1 127.8(6) . . ? C17 C16 C15 107.2(9) . . ? C17 C16 C21 125.9(8) . . ? C15 C16 C21 126.6(9) . . ? C17 C16 Fe1 69.1(4) . . ? C15 C16 Fe1 66.7(5) . . ? C21 C16 Fe1 124.3(6) . . ? C16 C17 C13 107.5(7) . . ? C16 C17 C22 129.7(8) . . ? C13 C17 C22 122.2(7) . . ? C16 C17 Fe1 71.0(4) . . ? C13 C17 Fe1 71.1(3) . . ? C22 C17 Fe1 130.4(5) . . ? C27 C23 C24 109.1(4) . . ? C27 C23 C28 134.5(10) . . ? C24 C23 C28 116.3(10) . . ? C27 C23 Fe2 70.9(4) . . ? C24 C23 Fe2 68.6(4) . . ? C28 C23 Fe2 127.1(4) . . ? C23 C24 C25 108.5(7) . . ? C23 C24 C29 126.9(8) . . ? C25 C24 C29 124.6(8) . . ? C23 C24 Fe2 71.0(4) . . ? C25 C24 Fe2 69.4(5) . . ? C29 C24 Fe2 123.9(6) . . ? C30 C25 C26 132.0(9) . . ? C30 C25 C24 126.5(8) . . ? C26 C25 C24 101.3(9) . . ? C30 C25 Fe2 128.5(6) . . ? C26 C25 Fe2 68.3(5) . . ? C24 C25 Fe2 70.0(5) . . ? C27 C26 C25 113.3(9) . . ? C27 C26 C31 128.7(9) . . ? C25 C26 C31 117.9(11) . . ? C27 C26 Fe2 73.0(5) . . ? C25 C26 Fe2 70.8(5) . . ? C31 C26 Fe2 124.9(6) . . ? C26 C27 C23 107.7(7) . . ? C26 C27 C32 126.1(9) . . ? C23 C27 C32 125.6(9) . . ? C26 C27 Fe2 68.4(5) . . ? C23 C27 Fe2 72.1(4) . . ? C32 C27 Fe2 131.6(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.544 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.074 #===END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H40 Fe2 N2' _chemical_formula_weight 564.36 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C2/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 17.918(6) _cell_length_b 11.820(3) _cell_length_c 13.751(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.07(2) _cell_angle_gamma 90.00 _cell_volume 2908.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plates' _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 1.020 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.6297 _exptl_absorpt_correction_T_max 0.9049 _exptl_absorpt_process_details 'ABSCOR' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU RAXIS RAPID' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13725 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3308 _reflns_number_gt 2389 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RIGAKU PROCESS AUTO' _computing_cell_refinement 'RIGAKU PROCESS AUTO' _computing_data_reduction 'RIGAKU PROCESS AUTO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^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 3308 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0943 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.815123(15) 0.22353(3) 0.01980(2) 0.03974(11) Uani 1 1 d . . . N1 N 0.76441(10) 0.35393(16) 0.03245(15) 0.0533(5) Uani 1 1 d . . . C1 C 0.78045(12) 0.46083(19) 0.07247(18) 0.0531(6) Uani 1 1 d . . . C2 C 0.80167(14) 0.5500(2) 0.0138(2) 0.0668(7) Uani 1 1 d . . . H2 H 0.8044 0.5395 -0.0529 0.080 Uiso 1 1 calc R . . C3 C 0.81893(17) 0.6558(3) 0.0555(3) 0.0834(9) Uani 1 1 d . . . H3 H 0.8329 0.7152 0.0160 0.100 Uiso 1 1 calc R . . C4 C 0.81536(18) 0.6723(3) 0.1534(3) 0.0847(9) Uani 1 1 d . . . H4 H 0.8270 0.7428 0.1803 0.102 Uiso 1 1 calc R . . C5 C 0.79479(16) 0.5859(3) 0.2119(2) 0.0777(8) Uani 1 1 d . . . H5 H 0.7926 0.5975 0.2786 0.093 Uiso 1 1 calc R . . C6 C 0.77711(14) 0.4804(2) 0.1722(2) 0.0640(6) Uani 1 1 d . . . H6 H 0.7629 0.4222 0.2127 0.077 Uiso 1 1 calc R . . C7 C 0.92802(11) 0.27987(19) 0.06861(16) 0.0454(5) Uani 1 1 d . . . C8 C 0.93321(12) 0.2255(2) -0.02259(17) 0.0531(5) Uani 1 1 d . . . C9 C 0.90977(12) 0.1129(2) -0.01136(17) 0.0528(6) Uani 1 1 d . . . C10 C 0.89243(12) 0.09576(19) 0.08814(16) 0.0471(5) Uani 1 1 d . . . C11 C 0.90402(11) 0.19803(18) 0.13814(15) 0.0440(5) Uani 1 1 d . . . C12 C 0.95496(14) 0.3974(2) 0.0941(2) 0.0663(7) Uani 1 1 d . . . H12A H 1.0080 0.3961 0.1078 0.099 Uiso 1 1 calc R . . H12B H 0.9307 0.4237 0.1504 0.099 Uiso 1 1 calc R . . H12C H 0.9433 0.4473 0.0403 0.099 Uiso 1 1 calc R . . C13 C 0.96105(16) 0.2801(3) -0.1135(2) 0.0853(10) Uani 1 1 d . . . H13A H 0.9392 0.3538 -0.1217 0.128 Uiso 1 1 calc R . . H13B H 0.9471 0.2341 -0.1691 0.128 Uiso 1 1 calc R . . H13C H 1.0145 0.2868 -0.1074 0.128 Uiso 1 1 calc R . . C14 C 0.90944(16) 0.0205(3) -0.08684(19) 0.0797(9) Uani 1 1 d . . . H14A H 0.9089 0.0536 -0.1506 0.120 Uiso 1 1 calc R . . H14B H 0.8658 -0.0257 -0.0815 0.120 Uiso 1 1 calc R . . H14C H 0.9534 -0.0252 -0.0765 0.120 Uiso 1 1 calc R . . C15 C 0.87014(15) -0.0156(2) 0.13136(19) 0.0648(7) Uani 1 1 d . . . H15A H 0.9142 -0.0576 0.1514 0.097 Uiso 1 1 calc R . . H15B H 0.8411 -0.0582 0.0835 0.097 Uiso 1 1 calc R . . H15C H 0.8410 -0.0020 0.1867 0.097 Uiso 1 1 calc R . . C16 C 0.89499(15) 0.2201(2) 0.24474(16) 0.0598(6) Uani 1 1 d . . . H16A H 0.8520 0.1801 0.2655 0.090 Uiso 1 1 calc R . . H16B H 0.8885 0.2997 0.2550 0.090 Uiso 1 1 calc R . . H16C H 0.9387 0.1945 0.2817 0.090 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 0.02785(16) 0.03943(18) 0.05139(19) -0.00028(13) -0.00298(11) -0.00082(13) N1 0.0336(10) 0.0423(10) 0.0824(12) -0.0100(9) -0.0105(8) -0.0006(8) C1 0.0301(11) 0.0427(13) 0.0853(16) -0.0082(11) -0.0093(10) 0.0003(9) C2 0.0528(16) 0.0549(16) 0.0909(18) 0.0026(12) -0.0129(14) -0.0036(12) C3 0.0639(19) 0.0464(16) 0.137(3) 0.0095(17) -0.0226(17) -0.0095(13) C4 0.073(2) 0.0513(18) 0.127(3) -0.0259(18) -0.0196(18) -0.0038(15) C5 0.0629(18) 0.072(2) 0.097(2) -0.0286(16) -0.0091(15) -0.0001(15) C6 0.0483(14) 0.0552(15) 0.0882(17) -0.0111(13) 0.0003(12) -0.0013(12) C7 0.0287(10) 0.0469(12) 0.0598(12) 0.0090(10) -0.0061(8) -0.0047(9) C8 0.0299(10) 0.0732(16) 0.0562(13) 0.0110(11) 0.0026(9) 0.0036(11) C9 0.0314(11) 0.0632(15) 0.0627(14) -0.0110(11) -0.0064(10) 0.0097(10) C10 0.0333(11) 0.0466(13) 0.0604(13) 0.0037(9) -0.0073(9) 0.0029(9) C11 0.0337(10) 0.0476(13) 0.0498(11) 0.0030(8) -0.0063(8) -0.0026(9) C12 0.0423(14) 0.0543(15) 0.1006(19) 0.0139(13) -0.0106(13) -0.0132(11) C13 0.0543(17) 0.131(3) 0.0712(18) 0.0303(17) 0.0134(13) 0.0020(17) C14 0.0541(17) 0.103(2) 0.0811(18) -0.0359(16) -0.0074(13) 0.0214(16) C15 0.0580(16) 0.0446(14) 0.0903(18) 0.0093(12) -0.0107(13) -0.0016(11) C16 0.0562(15) 0.0695(16) 0.0526(14) 0.0020(11) -0.0070(10) -0.0074(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.8022(19) . ? Fe1 N1 1.8100(18) 7_655 ? Fe1 C9 2.202(2) . ? Fe1 C7 2.200(2) . ? Fe1 C10 2.223(2) . ? Fe1 C8 2.225(2) . ? Fe1 C11 2.236(2) . ? Fe1 Fe1 2.4492(9) 7_655 ? N1 C1 1.402(3) . ? N1 Fe1 1.8100(18) 7_655 ? C1 C2 1.393(3) . ? C1 C6 1.395(4) . ? C2 C3 1.403(4) . ? C3 C4 1.366(4) . ? C4 C5 1.363(4) . ? C5 C6 1.391(4) . ? C7 C8 1.417(3) . ? C7 C11 1.442(3) . ? C7 C12 1.506(3) . ? C8 C9 1.406(3) . ? C8 C13 1.515(3) . ? C9 C10 1.434(3) . ? C9 C14 1.507(3) . ? C10 C11 1.401(3) . ? C10 C15 1.507(3) . ? C11 C16 1.506(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N1 94.62(8) . 7_655 ? N1 Fe1 C9 157.55(9) . . ? N1 Fe1 C9 102.75(9) 7_655 . ? N1 Fe1 C7 99.89(9) . . ? N1 Fe1 C7 164.96(8) 7_655 . ? C9 Fe1 C7 62.22(9) . . ? N1 Fe1 C10 147.78(9) . . ? N1 Fe1 C10 106.48(9) 7_655 . ? C9 Fe1 C10 37.80(8) . . ? C7 Fe1 C10 62.27(8) . . ? N1 Fe1 C8 120.52(9) . . ? N1 Fe1 C8 129.87(9) 7_655 . ? C9 Fe1 C8 37.05(8) . . ? C7 Fe1 C8 37.34(9) . . ? C10 Fe1 C8 62.49(8) . . ? N1 Fe1 C11 112.85(8) . . ? N1 Fe1 C11 137.38(8) 7_655 . ? C9 Fe1 C11 62.31(8) . . ? C7 Fe1 C11 37.92(7) . . ? C10 Fe1 C11 36.61(8) . . ? C8 Fe1 C11 62.71(8) . . ? N1 Fe1 Fe1 47.44(6) . 7_655 ? N1 Fe1 Fe1 47.18(6) 7_655 7_655 ? C9 Fe1 Fe1 147.48(6) . 7_655 ? C7 Fe1 Fe1 147.15(7) . 7_655 ? C10 Fe1 Fe1 146.32(6) . 7_655 ? C8 Fe1 Fe1 147.93(6) . 7_655 ? C11 Fe1 Fe1 146.05(6) . 7_655 ? C1 N1 Fe1 135.63(15) . . ? C1 N1 Fe1 138.79(15) . 7_655 ? Fe1 N1 Fe1 85.38(8) . 7_655 ? C2 C1 N1 120.8(2) . . ? C2 C1 C6 118.1(2) . . ? N1 C1 C6 121.1(2) . . ? C1 C2 C3 120.0(3) . . ? C4 C3 C2 120.6(3) . . ? C3 C4 C5 120.2(3) . . ? C6 C5 C4 120.2(3) . . ? C5 C6 C1 120.9(3) . . ? C8 C7 C11 108.6(2) . . ? C8 C7 C12 126.1(2) . . ? C11 C7 C12 124.6(2) . . ? C8 C7 Fe1 72.27(13) . . ? C11 C7 Fe1 72.38(11) . . ? C12 C7 Fe1 128.92(16) . . ? C7 C8 C9 107.33(19) . . ? C7 C8 C13 125.3(2) . . ? C9 C8 C13 127.4(2) . . ? C7 C8 Fe1 70.39(11) . . ? C9 C8 Fe1 70.58(12) . . ? C13 C8 Fe1 125.48(17) . . ? C8 C9 C10 108.65(19) . . ? C8 C9 C14 126.9(2) . . ? C10 C9 C14 124.2(2) . . ? C8 C9 Fe1 72.37(12) . . ? C10 C9 Fe1 71.92(12) . . ? C14 C9 Fe1 126.15(17) . . ? C11 C10 C9 108.21(19) . . ? C11 C10 C15 126.6(2) . . ? C9 C10 C15 125.1(2) . . ? C11 C10 Fe1 72.18(12) . . ? C9 C10 Fe1 70.27(12) . . ? C15 C10 Fe1 126.00(16) . . ? C10 C11 C7 107.16(18) . . ? C10 C11 C16 127.32(19) . . ? C7 C11 C16 125.5(2) . . ? C10 C11 Fe1 71.21(12) . . ? C7 C11 Fe1 69.70(11) . . ? C16 C11 Fe1 125.14(15) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.407 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.058 #===END