# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name A.Eichhofer G.Buth F.Dolci K.Fink R.Mole P.Wood _publ_contact_author_name 'Andreas Eichhofer' _publ_contact_author_email Andreas.Eichhoefer@int.fzk.de # Attachment '- data_1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 737597' #TrackingRef '- data_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Fe(SeC6H5)2]2' _chemical_formula_sum 'C12 H10 Fe Se2' _chemical_formula_weight 367.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0043 0.0021 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3562 1.0571 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.5931 2.6709 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 22.092(3) _cell_length_b 22.092(3) _cell_length_c 10.887(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5313.5(15) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9182 _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 26.17 _exptl_crystal_description 'elongated plates' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.840 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816 _exptl_absorpt_coefficient_mu 8.866 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.3908 _exptl_absorpt_correction_T_max 0.6439 _exptl_absorpt_process_details XRED-32 _exptl_special_details ; The quality and intensity of the reflections with a resolution smaller than d = 0.92 decreases significantly indicated by a decrease of the mean I/s ratio below 6.04 and an increase of the R(int) value above 0.2526. Therefore data were measured only up to 2theta 52 deg. at lambda = 0.80000 Ang ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.80000 _diffrn_radiation_type synchrotron _diffrn_radiation_source SY _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8899 _diffrn_reflns_av_R_equivalents 0.0791 _diffrn_reflns_av_sigmaI/netI 0.0567 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.65 _reflns_number_total 1752 _reflns_number_gt 1314 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _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. Lattice THF molecules were identified within the structure of 1, but these were located on a fourfold axis and therefore badly disordered and could not be adequately refined. The data were therefore corrected for these using the SQEEZE option within the PLATON program package finding a total of 130 electrons (~2.5 THF) in a potential solvent accessible area of 615 cubic Angstroem. ; _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^)+(0.0280P)^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 1752 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0689 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Se1 Se 0.76091(3) 0.41212(3) 0.12688(7) 0.0374(2) Uani 1 1 d . . . Se2 Se 0.67605(3) 0.55618(3) -0.00861(6) 0.0383(2) Uani 1 1 d . . . Fe1 Fe 0.77464(4) 0.51720(4) 0.06014(9) 0.0357(3) Uani 1 1 d . . . C1 C 0.8421(3) 0.3847(3) 0.0880(6) 0.0374(16) Uani 1 1 d . . . C2 C 0.8503(3) 0.3571(3) -0.0247(6) 0.0474(18) Uani 1 1 d . . . H2 H 0.8171 0.3523 -0.0795 0.057 Uiso 1 1 calc R . . C3 C 0.9067(4) 0.3368(4) -0.0568(8) 0.064(2) Uani 1 1 d . . . H3 H 0.9123 0.3171 -0.1334 0.076 Uiso 1 1 calc R . . C4 C 0.9550(4) 0.3445(4) 0.0197(9) 0.069(2) Uani 1 1 d . . . H4 H 0.9939 0.3302 -0.0036 0.083 Uiso 1 1 calc R . . C5 C 0.9471(4) 0.3729(4) 0.1301(9) 0.071(2) Uani 1 1 d . . . H5 H 0.9810 0.3792 0.1822 0.085 Uiso 1 1 calc R . . C6 C 0.8905(3) 0.3927(4) 0.1672(7) 0.055(2) Uani 1 1 d . . . H6 H 0.8850 0.4112 0.2452 0.067 Uiso 1 1 calc R . . C7 C 0.6882(3) 0.6421(3) 0.0182(6) 0.0422(17) Uani 1 1 d . . . C8 C 0.7029(4) 0.6816(3) -0.0764(7) 0.052(2) Uani 1 1 d . . . H8 H 0.7083 0.6666 -0.1575 0.063 Uiso 1 1 calc R . . C9 C 0.7099(4) 0.7429(4) -0.0525(8) 0.059(2) Uani 1 1 d . . . H9 H 0.7205 0.7699 -0.1170 0.071 Uiso 1 1 calc R . . C10 C 0.7013(4) 0.7649(4) 0.0661(9) 0.064(2) Uani 1 1 d . . . H10 H 0.7053 0.8069 0.0825 0.076 Uiso 1 1 calc R . . C11 C 0.6869(4) 0.7255(4) 0.1587(8) 0.066(2) Uani 1 1 d . . . H11 H 0.6818 0.7404 0.2399 0.079 Uiso 1 1 calc R . . C12 C 0.6799(4) 0.6638(4) 0.1356(7) 0.057(2) Uani 1 1 d . . . H12 H 0.6694 0.6369 0.2004 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Se1 0.0446(4) 0.0402(4) 0.0275(3) -0.0013(3) 0.0002(3) -0.0005(3) Se2 0.0421(4) 0.0456(4) 0.0271(4) -0.0001(3) 0.0026(3) 0.0025(3) Fe1 0.0427(6) 0.0417(6) 0.0227(5) 0.0010(4) -0.0006(4) 0.0004(5) C1 0.045(4) 0.034(4) 0.033(4) 0.002(3) 0.010(3) 0.000(3) C2 0.053(5) 0.059(5) 0.031(4) -0.001(3) 0.008(3) 0.006(4) C3 0.075(6) 0.060(5) 0.056(5) 0.000(4) 0.018(5) 0.010(5) C4 0.056(6) 0.068(6) 0.083(7) 0.003(5) 0.019(5) 0.014(5) C5 0.052(5) 0.092(7) 0.069(6) -0.009(5) -0.004(5) 0.001(5) C6 0.048(5) 0.071(6) 0.047(5) -0.009(4) 0.002(4) -0.001(4) C7 0.044(4) 0.047(4) 0.035(4) -0.015(3) -0.004(3) 0.009(3) C8 0.071(5) 0.047(5) 0.040(4) -0.004(3) 0.008(4) 0.003(4) C9 0.073(6) 0.051(5) 0.054(5) 0.003(4) 0.010(4) -0.006(4) C10 0.075(6) 0.050(5) 0.066(6) -0.007(5) -0.006(5) 0.001(4) C11 0.092(7) 0.062(6) 0.043(5) -0.022(4) -0.011(4) 0.020(5) C12 0.077(5) 0.051(5) 0.042(5) -0.005(4) 0.001(4) 0.014(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 Se1 C1 1.939(7) . ? Se1 Fe1 2.4397(13) 8_454 ? Se1 Fe1 2.4513(12) . ? Se2 C7 1.939(7) . ? Se2 Fe1 2.4395(13) 7_544 ? Se2 Fe1 2.4586(12) . ? Fe1 Se2 2.4396(13) 8_454 ? Fe1 Se1 2.4397(13) 7_544 ? Fe1 Fe1 2.8791(15) 8_454 ? Fe1 Fe1 2.8792(15) 7_544 ? C1 C2 1.381(9) . ? C1 C6 1.386(10) . ? C2 C3 1.371(11) . ? C3 C4 1.363(12) . ? C4 C5 1.367(12) . ? C5 C6 1.385(11) . ? C7 C12 1.378(10) . ? C7 C8 1.388(10) . ? C8 C9 1.388(10) . ? C9 C10 1.392(12) . ? C10 C11 1.369(12) . ? C11 C12 1.395(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Se1 Fe1 107.8(2) . 8_454 ? C1 Se1 Fe1 96.72(19) . . ? Fe1 Se1 Fe1 72.12(3) 8_454 . ? C7 Se2 Fe1 109.3(2) . 7_544 ? C7 Se2 Fe1 100.06(19) . . ? Fe1 Se2 Fe1 72.00(3) 7_544 . ? Se2 Fe1 Se1 121.82(5) 8_454 7_544 ? Se2 Fe1 Se1 106.39(4) 8_454 . ? Se1 Fe1 Se1 105.03(4) 7_544 . ? Se2 Fe1 Se2 108.62(4) 8_454 . ? Se1 Fe1 Se2 106.16(4) 7_544 . ? Se1 Fe1 Se2 108.20(4) . . ? Se2 Fe1 Fe1 54.31(3) 8_454 8_454 ? Se1 Fe1 Fe1 141.95(5) 7_544 8_454 ? Se1 Fe1 Fe1 53.75(4) . 8_454 ? Se2 Fe1 Fe1 110.47(4) . 8_454 ? Se2 Fe1 Fe1 145.80(5) 8_454 7_544 ? Se1 Fe1 Fe1 54.13(3) 7_544 7_544 ? Se1 Fe1 Fe1 107.13(4) . 7_544 ? Se2 Fe1 Fe1 53.69(4) . 7_544 ? Fe1 Fe1 Fe1 153.34(4) 8_454 7_544 ? C2 C1 C6 120.5(6) . . ? C2 C1 Se1 116.9(5) . . ? C6 C1 Se1 122.5(5) . . ? C3 C2 C1 119.3(7) . . ? C4 C3 C2 121.0(8) . . ? C3 C4 C5 119.6(8) . . ? C4 C5 C6 121.1(8) . . ? C5 C6 C1 118.4(7) . . ? C12 C7 C8 120.1(7) . . ? C12 C7 Se2 117.5(6) . . ? C8 C7 Se2 122.4(5) . . ? C7 C8 C9 120.0(7) . . ? C8 C9 C10 120.0(8) . . ? C11 C10 C9 119.6(8) . . ? C10 C11 C12 120.9(8) . . ? C7 C12 C11 119.5(8) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.65 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.358 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.081 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.250 -0.125 152 33 ' ' 2 0.500 0.750 0.125 152 33 ' ' 3 0.000 0.750 0.375 152 33 ' ' 4 0.000 0.250 0.625 152 33 ' ' ##END data_2 _database_code_depnum_ccdc_archive 'CCDC 737598' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Fe(SeC6H2(CH3)3)2]2' _chemical_formula_sum 'C18 H22 Fe Se2' _chemical_formula_weight 452.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/ m b c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z+1/2' 'y, -x, z+1/2' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z-1/2' '-y, x, -z-1/2' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-y-1/2, -x-1/2, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 15.710(2) _cell_length_b 15.710(2) _cell_length_c 7.0097(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1730.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used 9973 _cell_measurement_theta_min 1.30 _cell_measurement_theta_max 27.23 _exptl_crystal_description needles _exptl_crystal_colour yellow-brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 5.071 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.3428 _exptl_absorpt_correction_T_max 0.5172 _exptl_absorpt_process_details 'STOE X-RED' _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7739 _diffrn_reflns_av_R_equivalents 0.0662 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 26.72 _reflns_number_total 1001 _reflns_number_gt 926 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond2.1 _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^)+(0.0559P)^2^+1.9938P] 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 1001 _refine_ls_number_parameters 63 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0906 _refine_ls_wR_factor_gt 0.0887 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Se1 Se 0.95610(3) 0.10641(3) 0.0000 0.02822(18) Uani 1 2 d S . . Fe1 Fe 1.0000 0.0000 0.2500 0.0289(2) Uani 1 4 d S . . C1 C 1.0330(3) 0.2041(3) 0.0000 0.0292(8) Uani 1 2 d S . . C2 C 0.9957(3) 0.2845(3) 0.0000 0.0330(9) Uani 1 2 d S . . C3 C 1.0489(3) 0.3554(3) 0.0000 0.0392(10) Uani 1 2 d S . . H3 H 1.0239 0.4105 0.0000 0.047 Uiso 1 2 calc SR . . C4 C 1.1366(3) 0.3486(3) 0.0000 0.0379(10) Uani 1 2 d S . . C5 C 1.1714(3) 0.2674(3) 0.0000 0.0371(10) Uani 1 2 d S . . H5 H 1.2316 0.2618 0.0000 0.045 Uiso 1 2 calc SR . . C6 C 1.1222(3) 0.1939(3) 0.0000 0.0313(9) Uani 1 2 d S . . C7 C 0.9011(3) 0.2974(3) 0.0000 0.0421(11) Uani 1 2 d S . . H7A H 0.8726 0.2419 0.0000 0.063 Uiso 1 2 calc SR . . H7B H 0.8845 0.3293 -0.1142 0.063 Uiso 0.50 1 calc PR . . H7C H 0.8845 0.3293 0.1142 0.063 Uiso 0.50 1 calc PR . . C8 C 1.1933(4) 0.4263(3) 0.0000 0.0478(12) Uani 1 2 d S . . H8A H 1.2531 0.4084 0.0000 0.072 Uiso 1 2 calc SR . . H8B H 1.1818 0.4604 0.1142 0.072 Uiso 0.50 1 calc PR . . H8C H 1.1818 0.4604 -0.1142 0.072 Uiso 0.50 1 calc PR . . C9 C 1.1662(3) 0.1091(3) 0.0000 0.0332(9) Uani 1 2 d S . . H9A H 1.1236 0.0636 0.0000 0.050 Uiso 1 2 calc SR . . H9B H 1.2019 0.1042 0.1142 0.050 Uiso 0.50 1 calc PR . . H9C H 1.2019 0.1042 -0.1142 0.050 Uiso 0.50 1 calc PR . . 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 Se1 0.0293(3) 0.0288(2) 0.0266(3) 0.000 0.000 -0.00042(14) Fe1 0.0310(3) 0.0310(3) 0.0247(4) 0.000 0.000 0.000 C1 0.031(2) 0.030(2) 0.027(2) 0.000 0.000 -0.0013(15) C2 0.035(2) 0.033(2) 0.031(2) 0.000 0.000 0.0001(17) C3 0.047(3) 0.030(2) 0.041(3) 0.000 0.000 0.0003(18) C4 0.044(2) 0.035(2) 0.035(2) 0.000 0.000 -0.0085(19) C5 0.031(2) 0.047(3) 0.033(2) 0.000 0.000 -0.0040(19) C6 0.032(2) 0.038(2) 0.024(2) 0.000 0.000 0.0002(17) C7 0.037(2) 0.034(2) 0.055(3) 0.000 0.000 0.0079(19) C8 0.052(3) 0.043(3) 0.048(3) 0.000 0.000 -0.017(2) C9 0.032(2) 0.040(2) 0.027(2) 0.000 0.000 0.0013(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 Se1 C1 1.953(4) . ? Se1 Fe1 2.5181(4) . ? Se1 Fe1 2.5181(4) 9_755 ? Fe1 Se1 2.5181(4) 3_645 ? Fe1 Se1 2.5181(4) 9_755 ? Fe1 Se1 2.5181(4) 11_666 ? C1 C2 1.393(6) . ? C1 C6 1.410(6) . ? C2 C3 1.392(6) . ? C2 C7 1.500(7) . ? C3 C4 1.383(7) . ? C4 C5 1.388(7) . ? C4 C8 1.512(6) . ? C5 C6 1.390(6) . ? C6 C9 1.500(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Se1 Fe1 110.61(9) . . ? C1 Se1 Fe1 110.61(9) . 9_755 ? Fe1 Se1 Fe1 88.202(19) . 9_755 ? Se1 Fe1 Se1 118.968(11) 3_645 . ? Se1 Fe1 Se1 118.968(11) 3_645 9_755 ? Se1 Fe1 Se1 91.798(19) . 9_755 ? Se1 Fe1 Se1 91.798(19) 3_645 11_666 ? Se1 Fe1 Se1 118.967(11) . 11_666 ? Se1 Fe1 Se1 118.966(11) 9_755 11_666 ? C2 C1 C6 121.4(4) . . ? C2 C1 Se1 116.9(3) . . ? C6 C1 Se1 121.7(3) . . ? C3 C2 C1 118.3(4) . . ? C3 C2 C7 119.1(4) . . ? C1 C2 C7 122.7(4) . . ? C4 C3 C2 122.4(5) . . ? C3 C4 C5 117.7(4) . . ? C3 C4 C8 121.6(5) . . ? C5 C4 C8 120.7(5) . . ? C4 C5 C6 123.0(4) . . ? C5 C6 C1 117.3(4) . . ? C5 C6 C9 118.7(4) . . ? C1 C6 C9 124.0(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.72 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.466 _refine_diff_density_min -0.624 _refine_diff_density_rms 0.095 ##END data_3 _database_code_depnum_ccdc_archive 'CCDC 737599' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Fe(SePh)2(phen)2]*C4H8O' _chemical_formula_sum 'C40 H34 Fe N4 O Se2' _chemical_formula_weight 800.48 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.849(3) _cell_length_b 11.434(2) _cell_length_c 20.168(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.30(3) _cell_angle_gamma 90.00 _cell_volume 3414.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used 29148 _cell_measurement_theta_min 1.38 _cell_measurement_theta_max 26.15 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.193 _exptl_crystal_size_min 0.120 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 2.613 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5300 _exptl_absorpt_correction_T_max 0.6404 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22983 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.70 _reflns_number_total 6414 _reflns_number_gt 5545 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL-97 _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^)+(0.0477P)^2^+1.7683P] 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 6414 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.81115(2) 0.79243(3) 0.074917(18) 0.04009(10) Uani 1 1 d . . . Se1 Se 0.955436(19) 0.81933(2) 0.150229(14) 0.04859(9) Uani 1 1 d . . . Se2 Se 0.76921(2) 1.00942(2) 0.093829(15) 0.05129(9) Uani 1 1 d . . . N1 N 0.82586(14) 0.59711(18) 0.06127(10) 0.0414(5) Uani 1 1 d . . . N2 N 0.73043(14) 0.71265(18) 0.14868(10) 0.0409(5) Uani 1 1 d . . . N3 N 0.69319(14) 0.77383(19) -0.00056(11) 0.0445(5) Uani 1 1 d . . . N4 N 0.86664(14) 0.81558(18) -0.02118(11) 0.0424(5) Uani 1 1 d . . . C1 C 0.87651(19) 0.5394(3) 0.02093(14) 0.0486(6) Uani 1 1 d . . . H1 H 0.9127 0.5832 -0.0070 0.058 Uiso 1 1 calc R . . C2 C 0.8794(2) 0.4175(3) 0.01738(15) 0.0558(7) Uani 1 1 d . . . H2 H 0.9180 0.3801 -0.0116 0.067 Uiso 1 1 calc R . . C3 C 0.8266(2) 0.3529(3) 0.05560(15) 0.0557(7) Uani 1 1 d . . . H3 H 0.8271 0.2700 0.0530 0.067 Uiso 1 1 calc R . . C4 C 0.77126(19) 0.4098(2) 0.09911(13) 0.0479(6) Uani 1 1 d . . . C5 C 0.7145(2) 0.3479(3) 0.14169(16) 0.0575(7) Uani 1 1 d . . . H5 H 0.7093 0.2652 0.1385 0.069 Uiso 1 1 calc R . . C6 C 0.6687(2) 0.4065(3) 0.18622(15) 0.0549(7) Uani 1 1 d . . . H6 H 0.6317 0.3644 0.2144 0.066 Uiso 1 1 calc R . . C7 C 0.67443(17) 0.5311(2) 0.19201(13) 0.0442(6) Uani 1 1 d . . . C8 C 0.63296(19) 0.5941(3) 0.24120(14) 0.0510(6) Uani 1 1 d . . . H8 H 0.5989 0.5546 0.2724 0.061 Uiso 1 1 calc R . . C9 C 0.6422(2) 0.7126(3) 0.24367(14) 0.0531(7) Uani 1 1 d . . . H9 H 0.6161 0.7562 0.2775 0.064 Uiso 1 1 calc R . . C10 C 0.69022(19) 0.7696(2) 0.19613(14) 0.0478(6) Uani 1 1 d . . . H10 H 0.6944 0.8525 0.1977 0.057 Uiso 1 1 calc R . . C11 C 0.72456(16) 0.5937(2) 0.14771(12) 0.0387(5) Uani 1 1 d . . . C12 C 0.77486(16) 0.5323(2) 0.10099(12) 0.0394(5) Uani 1 1 d . . . C13 C 0.60695(19) 0.7606(3) 0.01017(16) 0.0555(7) Uani 1 1 d . . . H13 H 0.5912 0.7530 0.0548 0.067 Uiso 1 1 calc R . . C14 C 0.5382(2) 0.7572(3) -0.04069(18) 0.0682(9) Uani 1 1 d . . . H14 H 0.4772 0.7469 -0.0308 0.082 Uiso 1 1 calc R . . C15 C 0.5595(2) 0.7689(4) -0.10465(19) 0.0736(10) Uani 1 1 d . . . H15 H 0.5132 0.7669 -0.1398 0.088 Uiso 1 1 calc R . . C16 C 0.6490(2) 0.7838(3) -0.11884(16) 0.0632(8) Uani 1 1 d . . . C17 C 0.6783(3) 0.7960(4) -0.18467(18) 0.0823(12) Uani 1 1 d . . . H17 H 0.6350 0.7923 -0.2217 0.099 Uiso 1 1 calc R . . C18 C 0.7654(3) 0.8126(4) -0.19492(17) 0.0773(11) Uani 1 1 d . . . H18 H 0.7828 0.8177 -0.2392 0.093 Uiso 1 1 calc R . . C19 C 0.8328(2) 0.8226(3) -0.14068(15) 0.0560(7) Uani 1 1 d . . . C20 C 0.9227(2) 0.8517(3) -0.14861(15) 0.0601(8) Uani 1 1 d . . . H20 H 0.9428 0.8630 -0.1918 0.072 Uiso 1 1 calc R . . C21 C 0.9814(2) 0.8636(3) -0.09374(15) 0.0560(7) Uani 1 1 d . . . H21 H 1.0424 0.8851 -0.0983 0.067 Uiso 1 1 calc R . . C22 C 0.95117(18) 0.8439(2) -0.03069(14) 0.0480(6) Uani 1 1 d . . . H22 H 0.9932 0.8511 0.0070 0.058 Uiso 1 1 calc R . . C23 C 0.80717(18) 0.8075(2) -0.07555(13) 0.0444(6) Uani 1 1 d . . . C24 C 0.71424(19) 0.7862(2) -0.06440(14) 0.0464(6) Uani 1 1 d . . . C25 C 0.97971(18) 0.6652(3) 0.18426(13) 0.0472(6) Uani 1 1 d . . . C26 C 1.0469(2) 0.5973(3) 0.16045(16) 0.0635(8) Uani 1 1 d . . . H26 H 1.0816 0.6272 0.1265 0.076 Uiso 1 1 calc R . . C27 C 1.0647(3) 0.4857(4) 0.1854(2) 0.0830(12) Uani 1 1 d . . . H27 H 1.1107 0.4396 0.1680 0.100 Uiso 1 1 calc R . . C28 C 1.0167(3) 0.4419(3) 0.2347(2) 0.0865(13) Uani 1 1 d . . . H28 H 1.0285 0.3652 0.2512 0.104 Uiso 1 1 calc R . . C29 C 0.9509(3) 0.5096(3) 0.2604(2) 0.0731(10) Uani 1 1 d . . . H29 H 0.9187 0.4803 0.2959 0.088 Uiso 1 1 calc R . . C30 C 0.9315(2) 0.6199(3) 0.23502(15) 0.0540(7) Uani 1 1 d . . . H30 H 0.8849 0.6651 0.2523 0.065 Uiso 1 1 calc R . . C31 C 0.7316(2) 1.0552(2) 0.00450(15) 0.0516(6) Uani 1 1 d . . . C32 C 0.7950(2) 1.0868(2) -0.03984(15) 0.0549(7) Uani 1 1 d . . . H32 H 0.8571 1.0878 -0.0248 0.066 Uiso 1 1 calc R . . C33 C 0.7703(3) 1.1166(3) -0.10477(18) 0.0722(9) Uani 1 1 d . . . H33 H 0.8151 1.1383 -0.1337 0.087 Uiso 1 1 calc R . . C34 C 0.6815(3) 1.1148(4) -0.1274(2) 0.0945(13) Uani 1 1 d . . . H34 H 0.6642 1.1346 -0.1723 0.113 Uiso 1 1 calc R . . C35 C 0.6171(3) 1.0844(4) -0.0851(3) 0.0981(14) Uani 1 1 d . . . H35 H 0.5554 1.0826 -0.1013 0.118 Uiso 1 1 calc R . . C36 C 0.6410(2) 1.0560(3) -0.0187(2) 0.0716(9) Uani 1 1 d . . . H36 H 0.5957 1.0373 0.0104 0.086 Uiso 1 1 calc R . . O1 O 0.4204(2) 0.5969(3) 0.18795(17) 0.1085(10) Uani 1 1 d . . . C38 C 0.3587(5) 0.5037(5) 0.1811(4) 0.143(3) Uani 1 1 d . . . H38A H 0.3209 0.5007 0.2195 0.172 Uiso 1 1 calc R . . H38B H 0.3909 0.4282 0.1781 0.172 Uiso 1 1 calc R . . C39 C 0.3006(4) 0.5287(5) 0.1165(3) 0.1192(19) Uani 1 1 d . . . H39A H 0.2719 0.4564 0.0982 0.143 Uiso 1 1 calc R . . H39B H 0.2531 0.5871 0.1239 0.143 Uiso 1 1 calc R . . C40 C 0.3668(4) 0.5754(6) 0.0720(4) 0.139(2) Uani 1 1 d . . . H40A H 0.3431 0.6455 0.0477 0.167 Uiso 1 1 calc R . . H40B H 0.3837 0.5157 0.0396 0.167 Uiso 1 1 calc R . . C41 C 0.4460(3) 0.6058(7) 0.1209(3) 0.128(2) Uani 1 1 d . . . H41A H 0.4968 0.5518 0.1146 0.153 Uiso 1 1 calc R . . H41B H 0.4665 0.6864 0.1124 0.153 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 0.04253(19) 0.03547(19) 0.0429(2) 0.00005(15) 0.00763(15) -0.00153(14) Se1 0.05079(16) 0.04512(16) 0.04956(16) -0.00091(12) 0.00180(12) -0.00589(11) Se2 0.06291(18) 0.03625(15) 0.05522(17) -0.00216(11) 0.00773(13) -0.00001(12) N1 0.0435(11) 0.0387(11) 0.0421(11) -0.0019(9) 0.0040(9) 0.0009(9) N2 0.0423(11) 0.0367(11) 0.0438(11) -0.0007(9) 0.0044(9) 0.0003(9) N3 0.0429(11) 0.0407(11) 0.0502(12) 0.0032(10) 0.0050(9) 0.0018(9) N4 0.0447(11) 0.0366(11) 0.0464(12) 0.0035(9) 0.0072(9) -0.0003(9) C1 0.0514(15) 0.0459(15) 0.0493(15) -0.0036(12) 0.0089(12) 0.0015(12) C2 0.0637(17) 0.0472(16) 0.0574(16) -0.0102(13) 0.0109(14) 0.0081(14) C3 0.0692(18) 0.0367(14) 0.0608(17) -0.0066(13) 0.0029(14) 0.0037(13) C4 0.0569(15) 0.0384(14) 0.0475(14) -0.0010(11) -0.0023(12) 0.0005(12) C5 0.0726(19) 0.0365(14) 0.0635(18) 0.0064(13) 0.0056(15) -0.0027(13) C6 0.0644(17) 0.0436(15) 0.0573(16) 0.0134(13) 0.0089(14) -0.0039(13) C7 0.0460(14) 0.0436(14) 0.0428(13) 0.0076(11) 0.0009(11) 0.0004(11) C8 0.0523(15) 0.0560(17) 0.0455(14) 0.0109(13) 0.0098(12) 0.0017(13) C9 0.0571(16) 0.0578(18) 0.0458(14) -0.0003(13) 0.0124(12) 0.0056(13) C10 0.0519(15) 0.0423(14) 0.0502(15) -0.0030(12) 0.0105(12) 0.0022(12) C11 0.0382(12) 0.0367(12) 0.0406(12) 0.0027(10) -0.0019(10) 0.0010(10) C12 0.0424(13) 0.0365(12) 0.0385(12) 0.0018(10) -0.0018(10) 0.0001(10) C13 0.0432(15) 0.0595(18) 0.0641(18) 0.0057(15) 0.0067(13) 0.0017(13) C14 0.0435(16) 0.085(2) 0.076(2) 0.0082(19) 0.0039(15) 0.0010(16) C15 0.0507(17) 0.093(3) 0.074(2) 0.012(2) -0.0131(16) 0.0042(17) C16 0.0570(18) 0.075(2) 0.0556(17) 0.0092(16) -0.0063(14) -0.0011(16) C17 0.068(2) 0.123(4) 0.0539(19) 0.019(2) -0.0103(16) -0.004(2) C18 0.079(2) 0.106(3) 0.0459(17) 0.0156(18) -0.0011(16) -0.005(2) C19 0.0602(17) 0.0617(18) 0.0469(15) 0.0087(14) 0.0083(13) 0.0025(14) C20 0.0643(18) 0.0675(19) 0.0503(16) 0.0104(14) 0.0160(14) -0.0014(15) C21 0.0530(16) 0.0553(17) 0.0615(17) 0.0084(14) 0.0163(14) -0.0018(13) C22 0.0464(14) 0.0435(14) 0.0547(15) 0.0047(12) 0.0069(12) -0.0028(11) C23 0.0491(14) 0.0398(13) 0.0447(14) 0.0050(11) 0.0061(11) 0.0015(11) C24 0.0495(14) 0.0432(14) 0.0461(14) 0.0034(11) 0.0015(11) 0.0028(11) C25 0.0477(14) 0.0493(15) 0.0434(14) -0.0057(12) -0.0053(11) -0.0026(12) C26 0.0630(18) 0.068(2) 0.0590(18) -0.0131(16) -0.0013(14) 0.0099(16) C27 0.076(2) 0.064(2) 0.105(3) -0.020(2) -0.015(2) 0.0205(19) C28 0.082(3) 0.050(2) 0.120(3) 0.008(2) -0.036(2) -0.0015(19) C29 0.070(2) 0.066(2) 0.079(2) 0.0209(18) -0.0184(18) -0.0204(18) C30 0.0525(15) 0.0523(16) 0.0560(16) 0.0012(13) -0.0042(13) -0.0090(13) C31 0.0567(16) 0.0319(13) 0.0655(17) 0.0012(12) 0.0009(13) 0.0027(12) C32 0.0644(17) 0.0404(14) 0.0594(17) 0.0006(13) 0.0022(14) -0.0030(13) C33 0.097(3) 0.0526(19) 0.066(2) 0.0075(16) 0.0009(19) -0.0086(18) C34 0.111(3) 0.083(3) 0.085(3) 0.033(2) -0.021(2) -0.014(3) C35 0.079(3) 0.086(3) 0.123(4) 0.032(3) -0.040(3) -0.006(2) C36 0.0591(18) 0.0557(19) 0.099(3) 0.0173(18) -0.0037(18) 0.0020(15) O1 0.101(2) 0.130(3) 0.096(2) 0.017(2) 0.0166(17) -0.018(2) C38 0.153(6) 0.109(4) 0.172(6) -0.050(4) 0.046(5) -0.036(4) C39 0.090(3) 0.093(4) 0.168(5) -0.032(4) -0.033(4) -0.006(3) C40 0.079(3) 0.121(5) 0.211(7) -0.012(5) -0.023(4) 0.016(3) C41 0.076(3) 0.187(7) 0.117(4) 0.030(4) -0.011(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N4 2.178(2) . ? Fe1 N2 2.179(2) . ? Fe1 N3 2.243(2) . ? Fe1 N1 2.263(2) . ? Fe1 Se1 2.5504(9) . ? Fe1 Se2 2.5932(7) . ? Se1 C25 1.916(3) . ? Se2 C31 1.919(3) . ? N1 C1 1.325(3) . ? N1 C12 1.362(3) . ? N2 C10 1.335(3) . ? N2 C11 1.363(3) . ? N3 C13 1.323(3) . ? N3 C24 1.355(3) . ? N4 C22 1.324(3) . ? N4 C23 1.359(4) . ? C1 C2 1.396(4) . ? C2 C3 1.358(4) . ? C3 C4 1.406(4) . ? C4 C12 1.402(4) . ? C4 C5 1.434(4) . ? C5 C6 1.346(4) . ? C6 C7 1.431(4) . ? C7 C11 1.402(3) . ? C7 C8 1.405(4) . ? C8 C9 1.362(4) . ? C9 C10 1.399(4) . ? C11 C12 1.430(3) . ? C13 C14 1.392(4) . ? C14 C15 1.357(5) . ? C15 C16 1.391(5) . ? C16 C24 1.409(4) . ? C16 C17 1.435(5) . ? C17 C18 1.337(5) . ? C18 C19 1.431(5) . ? C19 C20 1.397(4) . ? C19 C23 1.405(4) . ? C20 C21 1.363(4) . ? C21 C22 1.398(4) . ? C23 C24 1.435(4) . ? C25 C26 1.379(4) . ? C25 C30 1.392(4) . ? C26 C27 1.390(5) . ? C27 C28 1.360(6) . ? C28 C29 1.379(6) . ? C29 C30 1.384(5) . ? C31 C36 1.390(5) . ? C31 C32 1.394(4) . ? C32 C33 1.376(5) . ? C33 C34 1.363(6) . ? C34 C35 1.372(7) . ? C35 C36 1.398(6) . ? O1 C38 1.405(6) . ? O1 C41 1.436(6) . ? C38 C39 1.534(9) . ? C39 C40 1.479(8) . ? C40 C41 1.517(7) . ? 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 Fe1 N2 157.27(8) . . ? N4 Fe1 N3 74.69(8) . . ? N2 Fe1 N3 88.97(8) . . ? N4 Fe1 N1 88.01(8) . . ? N2 Fe1 N1 74.52(8) . . ? N3 Fe1 N1 84.34(8) . . ? N4 Fe1 Se1 99.11(6) . . ? N2 Fe1 Se1 97.15(6) . . ? N3 Fe1 Se1 173.77(6) . . ? N1 Fe1 Se1 96.15(5) . . ? N4 Fe1 Se2 97.22(6) . . ? N2 Fe1 Se2 98.60(6) . . ? N3 Fe1 Se2 90.38(6) . . ? N1 Fe1 Se2 171.35(5) . . ? Se1 Fe1 Se2 89.846(16) . . ? C25 Se1 Fe1 103.26(8) . . ? C31 Se2 Fe1 100.34(8) . . ? C1 N1 C12 117.2(2) . . ? C1 N1 Fe1 129.10(18) . . ? C12 N1 Fe1 113.72(16) . . ? C10 N2 C11 117.8(2) . . ? C10 N2 Fe1 125.69(18) . . ? C11 N2 Fe1 116.47(16) . . ? C13 N3 C24 117.5(3) . . ? C13 N3 Fe1 128.0(2) . . ? C24 N3 Fe1 114.27(17) . . ? C22 N4 C23 117.8(2) . . ? C22 N4 Fe1 125.77(19) . . ? C23 N4 Fe1 116.32(17) . . ? N1 C1 C2 123.3(3) . . ? C3 C2 C1 119.5(3) . . ? C2 C3 C4 119.5(3) . . ? C12 C4 C3 117.1(3) . . ? C12 C4 C5 120.0(3) . . ? C3 C4 C5 122.9(3) . . ? C6 C5 C4 120.2(3) . . ? C5 C6 C7 121.3(3) . . ? C11 C7 C8 118.0(3) . . ? C11 C7 C6 119.2(2) . . ? C8 C7 C6 122.8(2) . . ? C9 C8 C7 119.2(2) . . ? C8 C9 C10 119.6(3) . . ? N2 C10 C9 122.9(3) . . ? N2 C11 C7 122.5(2) . . ? N2 C11 C12 117.6(2) . . ? C7 C11 C12 119.9(2) . . ? N1 C12 C4 123.3(2) . . ? N1 C12 C11 117.5(2) . . ? C4 C12 C11 119.2(2) . . ? N3 C13 C14 123.2(3) . . ? C15 C14 C13 119.2(3) . . ? C14 C15 C16 120.1(3) . . ? C15 C16 C24 117.0(3) . . ? C15 C16 C17 124.3(3) . . ? C24 C16 C17 118.7(3) . . ? C18 C17 C16 121.4(3) . . ? C17 C18 C19 121.5(3) . . ? C20 C19 C23 117.7(3) . . ? C20 C19 C18 123.5(3) . . ? C23 C19 C18 118.8(3) . . ? C21 C20 C19 119.3(3) . . ? C20 C21 C22 119.6(3) . . ? N4 C22 C21 122.9(3) . . ? N4 C23 C19 122.7(3) . . ? N4 C23 C24 117.4(2) . . ? C19 C23 C24 119.9(3) . . ? N3 C24 C16 123.0(3) . . ? N3 C24 C23 117.4(2) . . ? C16 C24 C23 119.6(3) . . ? C26 C25 C30 118.2(3) . . ? C26 C25 Se1 121.0(2) . . ? C30 C25 Se1 120.8(2) . . ? C25 C26 C27 120.9(3) . . ? C28 C27 C26 120.5(4) . . ? C27 C28 C29 119.6(4) . . ? C28 C29 C30 120.4(4) . . ? C29 C30 C25 120.4(3) . . ? C36 C31 C32 117.7(3) . . ? C36 C31 Se2 121.6(3) . . ? C32 C31 Se2 120.7(2) . . ? C33 C32 C31 122.0(3) . . ? C34 C33 C32 119.8(4) . . ? C33 C34 C35 119.9(4) . . ? C34 C35 C36 121.0(4) . . ? C31 C36 C35 119.6(4) . . ? C38 O1 C41 100.2(5) . . ? O1 C38 C39 105.2(5) . . ? C40 C39 C38 103.1(5) . . ? C39 C40 C41 101.9(5) . . ? O1 C41 C40 110.4(5) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.70 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.600 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.053 ##END data_4 _database_code_depnum_ccdc_archive 'CCDC 737600' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Fe(C12N2H8)3][Fe(SeC6H5)4]*(CH3)2NCO' _chemical_formula_sum 'C63 H51 Fe2 N7 O Se4' _chemical_formula_weight 1349.65 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.290(3) _cell_length_b 13.461(3) _cell_length_c 16.475(3) _cell_angle_alpha 88.85(3) _cell_angle_beta 77.74(3) _cell_angle_gamma 89.44(3) _cell_volume 2879.6(10) _cell_formula_units_Z 2 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used 15981 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 26.11 _exptl_crystal_description plates _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 3.080 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6935 _exptl_absorpt_correction_T_max 0.8945 _exptl_absorpt_process_details 'STOE X-RED' _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26364 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 24.89 _reflns_number_total 9954 _reflns_number_gt 8231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _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^)+(0.1143P)^2^+0.9566P] 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 9954 _refine_ls_number_parameters 669 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1558 _refine_ls_wR_factor_gt 0.1471 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Se1 Se -0.50676(4) 0.65474(4) 0.28410(3) 0.03543(15) Uani 1 1 d . . . Se2 Se -0.29913(4) 0.46381(4) 0.14690(3) 0.03615(15) Uani 1 1 d . . . Se3 Se -0.26167(4) 0.61123(4) 0.35488(3) 0.03621(15) Uani 1 1 d . . . Se4 Se -0.26991(4) 0.75668(4) 0.12599(4) 0.04281(16) Uani 1 1 d . . . Fe2 Fe 0.17374(5) 1.08576(5) 0.22208(4) 0.02650(16) Uani 1 1 d . . . Fe1 Fe -0.32586(5) 0.61765(5) 0.22533(4) 0.02944(17) Uani 1 1 d . . . N1 N 0.1997(4) 1.0382(3) 0.1063(3) 0.0391(10) Uani 1 1 d . . . N2 N 0.3036(3) 1.0144(3) 0.2222(3) 0.0331(9) Uani 1 1 d . . . N3 N 0.0880(3) 0.9677(3) 0.2573(2) 0.0296(8) Uani 1 1 d . . . N4 N 0.0388(3) 1.1497(3) 0.2237(3) 0.0331(9) Uani 1 1 d . . . N5 N 0.2496(3) 1.2106(3) 0.1895(2) 0.0295(8) Uani 1 1 d . . . N6 N 0.1681(3) 1.1331(3) 0.3345(2) 0.0300(8) Uani 1 1 d . . . C1 C -0.5774(4) 0.6545(3) 0.1945(3) 0.0326(10) Uani 1 1 d . . . C2 C -0.6813(4) 0.6809(4) 0.2094(4) 0.0442(13) Uani 1 1 d . . . H2 H -0.7145 0.7021 0.2631 0.053 Uiso 1 1 calc R . . C3 C -0.7367(4) 0.6768(5) 0.1475(4) 0.0493(14) Uani 1 1 d . . . H3 H -0.8073 0.6960 0.1590 0.059 Uiso 1 1 calc R . . C4 C -0.6907(4) 0.6451(4) 0.0685(4) 0.0433(12) Uani 1 1 d . . . H4 H -0.7295 0.6408 0.0265 0.052 Uiso 1 1 calc R . . C5 C -0.5869(4) 0.6199(4) 0.0522(3) 0.0395(12) Uani 1 1 d . . . H5 H -0.5538 0.5991 -0.0017 0.047 Uiso 1 1 calc R . . C6 C -0.5310(4) 0.6250(4) 0.1146(3) 0.0347(11) Uani 1 1 d . . . H6 H -0.4599 0.6081 0.1024 0.042 Uiso 1 1 calc R . . C7 C -0.3743(4) 0.3646(4) 0.2178(3) 0.0340(11) Uani 1 1 d . . . C8 C -0.4093(4) 0.2813(4) 0.1820(4) 0.0421(12) Uani 1 1 d . . . H8 H -0.3983 0.2776 0.1233 0.050 Uiso 1 1 calc R . . C9 C -0.4594(5) 0.2048(4) 0.2308(4) 0.0482(14) Uani 1 1 d . . . H9 H -0.4816 0.1487 0.2054 0.058 Uiso 1 1 calc R . . C10 C -0.4773(5) 0.2090(4) 0.3162(4) 0.0509(14) Uani 1 1 d . . . H10 H -0.5112 0.1560 0.3497 0.061 Uiso 1 1 calc R . . C11 C -0.4451(5) 0.2919(5) 0.3526(4) 0.0540(15) Uani 1 1 d . . . H11 H -0.4581 0.2960 0.4114 0.065 Uiso 1 1 calc R . . C12 C -0.3946(5) 0.3682(4) 0.3040(4) 0.0459(13) Uani 1 1 d . . . H12 H -0.3732 0.4243 0.3300 0.055 Uiso 1 1 calc R . . C13 C -0.1219(4) 0.5676(4) 0.3251(3) 0.0344(11) Uani 1 1 d . . . C14 C -0.0684(4) 0.5619(4) 0.2424(4) 0.0425(12) Uani 1 1 d . . . H14 H -0.1028 0.5773 0.1987 0.051 Uiso 1 1 calc R . . C15 C 0.0342(5) 0.5339(5) 0.2240(5) 0.0549(16) Uani 1 1 d . . . H15 H 0.0696 0.5305 0.1676 0.066 Uiso 1 1 calc R . . C16 C 0.0859(5) 0.5108(5) 0.2863(6) 0.0627(19) Uani 1 1 d . . . H16 H 0.1563 0.4914 0.2730 0.075 Uiso 1 1 calc R . . C17 C 0.0353(6) 0.5162(6) 0.3662(6) 0.072(2) Uani 1 1 d . . . H17 H 0.0707 0.5002 0.4092 0.086 Uiso 1 1 calc R . . C18 C -0.0671(5) 0.5445(5) 0.3869(4) 0.0552(16) Uani 1 1 d . . . H18 H -0.1007 0.5484 0.4438 0.066 Uiso 1 1 calc R . . C19 C -0.1330(4) 0.7232(4) 0.0701(3) 0.0336(10) Uani 1 1 d . . . C20 C -0.1137(5) 0.6447(4) 0.0149(4) 0.0458(13) Uani 1 1 d . . . H20 H -0.1687 0.6051 0.0055 0.055 Uiso 1 1 calc R . . C21 C -0.0127(5) 0.6246(5) -0.0264(4) 0.0590(17) Uani 1 1 d . . . H21 H 0.0003 0.5710 -0.0639 0.071 Uiso 1 1 calc R . . C22 C 0.0677(5) 0.6802(6) -0.0142(4) 0.0595(17) Uani 1 1 d . . . H22 H 0.1358 0.6657 -0.0432 0.071 Uiso 1 1 calc R . . C23 C 0.0494(5) 0.7570(5) 0.0402(4) 0.0543(15) Uani 1 1 d . . . H23 H 0.1051 0.7960 0.0491 0.065 Uiso 1 1 calc R . . C24 C -0.0501(4) 0.7784(4) 0.0824(3) 0.0426(12) Uani 1 1 d . . . H24 H -0.0617 0.8316 0.1203 0.051 Uiso 1 1 calc R . . C25 C 0.1429(5) 1.0486(4) 0.0487(3) 0.0462(13) Uani 1 1 d . . . H25 H 0.0802 1.0851 0.0611 0.055 Uiso 1 1 calc R . . C26 C 0.1753(6) 1.0054(5) -0.0314(4) 0.0573(17) Uani 1 1 d . . . H26 H 0.1342 1.0138 -0.0717 0.069 Uiso 1 1 calc R . . C27 C 0.2641(6) 0.9527(4) -0.0501(4) 0.0571(17) Uani 1 1 d . . . H27 H 0.2849 0.9239 -0.1032 0.068 Uiso 1 1 calc R . . C28 C 0.3253(5) 0.9406(4) 0.0085(4) 0.0510(15) Uani 1 1 d . . . C29 C 0.4231(5) 0.8870(4) -0.0032(4) 0.0544(17) Uani 1 1 d . . . H29 H 0.4493 0.8580 -0.0556 0.065 Uiso 1 1 calc R . . C30 C 0.4771(5) 0.8765(4) 0.0551(4) 0.0540(16) Uani 1 1 d . . . H30 H 0.5404 0.8407 0.0441 0.065 Uiso 1 1 calc R . . C31 C 0.4404(4) 0.9190(4) 0.1344(4) 0.0479(15) Uani 1 1 d . . . C32 C 0.4900(5) 0.9088(4) 0.2002(5) 0.0564(17) Uani 1 1 d . . . H32 H 0.5535 0.8736 0.1932 0.068 Uiso 1 1 calc R . . C33 C 0.4475(5) 0.9493(5) 0.2750(5) 0.0536(15) Uani 1 1 d . . . H33 H 0.4809 0.9425 0.3205 0.064 Uiso 1 1 calc R . . C34 C 0.3546(4) 1.0009(4) 0.2838(4) 0.0431(12) Uani 1 1 d . . . H34 H 0.3256 1.0281 0.3364 0.052 Uiso 1 1 calc R . . C35 C 0.2896(4) 0.9843(4) 0.0861(3) 0.0414(13) Uani 1 1 d . . . C36 C 0.3470(4) 0.9722(4) 0.1484(3) 0.0372(11) Uani 1 1 d . . . C37 C 0.1150(4) 0.8750(4) 0.2729(3) 0.0377(11) Uani 1 1 d . . . H37 H 0.1857 0.8605 0.2703 0.045 Uiso 1 1 calc R . . C38 C 0.0437(5) 0.7980(4) 0.2928(3) 0.0452(13) Uani 1 1 d . . . H38 H 0.0666 0.7327 0.3030 0.054 Uiso 1 1 calc R . . C39 C -0.0588(5) 0.8159(4) 0.2979(3) 0.0440(13) Uani 1 1 d . . . H39 H -0.1075 0.7638 0.3112 0.053 Uiso 1 1 calc R . . C40 C -0.0910(4) 0.9138(4) 0.2828(3) 0.0383(11) Uani 1 1 d . . . C41 C -0.1959(5) 0.9414(5) 0.2878(4) 0.0538(15) Uani 1 1 d . . . H41 H -0.2483 0.8925 0.3005 0.065 Uiso 1 1 calc R . . C42 C -0.2211(5) 1.0372(5) 0.2742(4) 0.0575(16) Uani 1 1 d . . . H42 H -0.2915 1.0545 0.2783 0.069 Uiso 1 1 calc R . . C43 C -0.1447(4) 1.1130(4) 0.2541(4) 0.0441(13) Uani 1 1 d . . . C44 C -0.1670(5) 1.2131(5) 0.2420(5) 0.0570(16) Uani 1 1 d . . . H44 H -0.2361 1.2356 0.2481 0.068 Uiso 1 1 calc R . . C45 C -0.0861(5) 1.2783(5) 0.2210(5) 0.0555(16) Uani 1 1 d . . . H45 H -0.0994 1.3469 0.2131 0.067 Uiso 1 1 calc R . . C46 C 0.0146(4) 1.2447(4) 0.2113(4) 0.0462(13) Uani 1 1 d . . . H46 H 0.0688 1.2912 0.1952 0.055 Uiso 1 1 calc R . . C47 C -0.0144(4) 0.9856(4) 0.2624(3) 0.0316(10) Uani 1 1 d . . . C48 C -0.0419(4) 1.0851(4) 0.2457(3) 0.0332(10) Uani 1 1 d . . . C49 C 0.2867(4) 1.2509(4) 0.1142(3) 0.0347(11) Uani 1 1 d . . . H49 H 0.2775 1.2166 0.0665 0.042 Uiso 1 1 calc R . . C50 C 0.3378(4) 1.3404(4) 0.1037(3) 0.0410(12) Uani 1 1 d . . . H50 H 0.3609 1.3672 0.0492 0.049 Uiso 1 1 calc R . . C51 C 0.3559(4) 1.3912(4) 0.1697(4) 0.0415(12) Uani 1 1 d . . . H51 H 0.3936 1.4515 0.1616 0.050 Uiso 1 1 calc R . . C52 C 0.3174(4) 1.3522(4) 0.2506(3) 0.0335(11) Uani 1 1 d . . . C53 C 0.3290(4) 1.3991(4) 0.3253(4) 0.0402(12) Uani 1 1 d . . . H53 H 0.3661 1.4595 0.3219 0.048 Uiso 1 1 calc R . . C54 C 0.2878(4) 1.3581(4) 0.4009(4) 0.0421(12) Uani 1 1 d . . . H54 H 0.2962 1.3906 0.4496 0.050 Uiso 1 1 calc R . . C55 C 0.2314(4) 1.2664(4) 0.4087(3) 0.0381(11) Uani 1 1 d . . . C56 C 0.1872(5) 1.2196(5) 0.4835(4) 0.0533(15) Uani 1 1 d . . . H56 H 0.1933 1.2477 0.5347 0.064 Uiso 1 1 calc R . . C57 C 0.1350(6) 1.1327(5) 0.4829(4) 0.0554(16) Uani 1 1 d . . . H57 H 0.1043 1.1005 0.5338 0.066 Uiso 1 1 calc R . . C58 C 0.1265(4) 1.0909(4) 0.4079(3) 0.0401(12) Uani 1 1 d . . . H58 H 0.0899 1.0304 0.4090 0.048 Uiso 1 1 calc R . . C59 C 0.2644(3) 1.2621(3) 0.2566(3) 0.0284(10) Uani 1 1 d . . . C60 C 0.2197(4) 1.2202(3) 0.3354(3) 0.0299(10) Uani 1 1 d . . . N7 N 0.7966(6) 0.2746(6) 0.5057(5) 0.0798(18) Uiso 1 1 d . . . O1 O 0.8056(10) 0.1203(11) 0.5546(8) 0.191(5) Uiso 1 1 d . . . C61 C 0.8993(10) 0.2716(10) 0.4607(8) 0.126(4) Uiso 1 1 d . . . H61A H 0.9156 0.3340 0.4292 0.189 Uiso 1 1 calc R . . H61B H 0.9082 0.2160 0.4223 0.189 Uiso 1 1 calc R . . H61C H 0.9456 0.2626 0.4994 0.189 Uiso 1 1 calc R . . C62 C 0.7392(8) 0.3644(8) 0.5106(7) 0.101(3) Uiso 1 1 d . . . H62A H 0.7781 0.4143 0.4728 0.152 Uiso 1 1 calc R . . H62B H 0.7263 0.3886 0.5676 0.152 Uiso 1 1 calc R . . H62C H 0.6733 0.3524 0.4948 0.152 Uiso 1 1 calc R . . C63 C 0.7515(12) 0.1990(11) 0.5550(9) 0.130(4) Uiso 1 1 d . . . H63 H 0.6837 0.2042 0.5879 0.156 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 Se1 0.0279(3) 0.0417(3) 0.0357(3) -0.0015(2) -0.0045(2) 0.0009(2) Se2 0.0366(3) 0.0326(3) 0.0389(3) -0.0059(2) -0.0068(2) 0.0009(2) Se3 0.0344(3) 0.0405(3) 0.0355(3) -0.0038(2) -0.0109(2) -0.0055(2) Se4 0.0338(3) 0.0359(3) 0.0526(3) 0.0096(2) 0.0036(2) 0.0053(2) Fe2 0.0290(3) 0.0203(3) 0.0294(3) 0.0012(2) -0.0046(3) 0.0006(2) Fe1 0.0264(4) 0.0280(3) 0.0345(4) -0.0012(3) -0.0077(3) -0.0007(3) N1 0.052(3) 0.026(2) 0.040(2) 0.0037(18) -0.009(2) -0.0094(19) N2 0.033(2) 0.025(2) 0.038(2) 0.0039(17) -0.0011(17) 0.0020(16) N3 0.038(2) 0.0241(19) 0.0266(19) 0.0004(15) -0.0056(16) -0.0003(16) N4 0.032(2) 0.026(2) 0.042(2) 0.0069(17) -0.0091(18) -0.0015(16) N5 0.027(2) 0.0248(19) 0.035(2) 0.0014(16) -0.0032(16) 0.0033(15) N6 0.030(2) 0.026(2) 0.032(2) 0.0006(16) -0.0031(16) 0.0000(16) C1 0.032(3) 0.025(2) 0.039(3) 0.003(2) -0.005(2) -0.0016(19) C2 0.033(3) 0.052(3) 0.046(3) -0.005(3) -0.004(2) 0.008(2) C3 0.029(3) 0.065(4) 0.055(4) -0.007(3) -0.012(2) 0.005(3) C4 0.032(3) 0.049(3) 0.051(3) 0.001(3) -0.015(2) 0.000(2) C5 0.039(3) 0.039(3) 0.039(3) 0.003(2) -0.006(2) -0.003(2) C6 0.022(2) 0.040(3) 0.041(3) 0.005(2) -0.005(2) -0.0005(19) C7 0.029(2) 0.033(3) 0.041(3) -0.007(2) -0.010(2) 0.0059(19) C8 0.038(3) 0.037(3) 0.054(3) -0.008(2) -0.014(2) -0.001(2) C9 0.048(3) 0.037(3) 0.063(4) -0.002(3) -0.019(3) -0.008(2) C10 0.052(3) 0.040(3) 0.059(4) 0.006(3) -0.007(3) -0.004(3) C11 0.064(4) 0.046(3) 0.051(4) 0.001(3) -0.012(3) -0.007(3) C12 0.050(3) 0.040(3) 0.049(3) -0.004(2) -0.012(3) -0.004(2) C13 0.036(3) 0.027(2) 0.043(3) 0.005(2) -0.016(2) -0.0042(19) C14 0.039(3) 0.041(3) 0.051(3) -0.006(2) -0.017(2) -0.001(2) C15 0.038(3) 0.047(3) 0.080(5) -0.019(3) -0.011(3) 0.000(3) C16 0.042(3) 0.048(4) 0.104(6) -0.001(4) -0.029(4) 0.012(3) C17 0.059(4) 0.068(5) 0.101(6) 0.030(4) -0.048(4) 0.003(3) C18 0.052(4) 0.059(4) 0.060(4) 0.025(3) -0.026(3) -0.009(3) C19 0.033(3) 0.033(3) 0.032(2) 0.005(2) -0.003(2) 0.004(2) C20 0.053(3) 0.041(3) 0.046(3) -0.003(2) -0.014(3) 0.007(2) C21 0.066(4) 0.063(4) 0.045(3) -0.012(3) -0.004(3) 0.023(3) C22 0.038(3) 0.086(5) 0.050(4) 0.006(3) -0.002(3) 0.022(3) C23 0.035(3) 0.073(4) 0.055(4) 0.011(3) -0.011(3) 0.000(3) C24 0.043(3) 0.044(3) 0.041(3) 0.001(2) -0.011(2) 0.000(2) C25 0.068(4) 0.035(3) 0.039(3) 0.005(2) -0.021(3) -0.007(3) C26 0.088(5) 0.049(4) 0.039(3) 0.009(3) -0.024(3) -0.019(3) C27 0.086(5) 0.037(3) 0.042(3) -0.007(3) 0.000(3) -0.011(3) C28 0.072(4) 0.032(3) 0.042(3) -0.007(2) 0.005(3) -0.016(3) C29 0.060(4) 0.029(3) 0.058(4) -0.018(3) 0.025(3) -0.006(3) C30 0.049(4) 0.036(3) 0.068(4) -0.008(3) 0.008(3) -0.002(3) C31 0.046(3) 0.021(2) 0.066(4) -0.003(2) 0.013(3) -0.006(2) C32 0.042(3) 0.036(3) 0.090(5) 0.015(3) -0.014(3) 0.003(2) C33 0.042(3) 0.044(3) 0.076(4) 0.003(3) -0.017(3) 0.010(3) C34 0.043(3) 0.035(3) 0.052(3) 0.007(2) -0.012(2) 0.004(2) C35 0.049(3) 0.020(2) 0.047(3) -0.003(2) 0.008(2) -0.009(2) C36 0.038(3) 0.024(2) 0.045(3) 0.001(2) 0.002(2) -0.002(2) C37 0.048(3) 0.023(2) 0.040(3) 0.003(2) -0.004(2) 0.002(2) C38 0.067(4) 0.020(2) 0.043(3) 0.001(2) 0.000(3) -0.005(2) C39 0.056(4) 0.031(3) 0.040(3) -0.006(2) 0.002(2) -0.014(2) C40 0.041(3) 0.035(3) 0.038(3) -0.004(2) -0.006(2) -0.010(2) C41 0.040(3) 0.061(4) 0.059(4) 0.000(3) -0.007(3) -0.017(3) C42 0.037(3) 0.065(4) 0.072(4) 0.002(3) -0.014(3) -0.008(3) C43 0.032(3) 0.047(3) 0.054(3) 0.005(3) -0.011(2) -0.002(2) C44 0.038(3) 0.052(4) 0.079(5) 0.012(3) -0.011(3) 0.012(3) C45 0.043(3) 0.040(3) 0.081(5) 0.016(3) -0.011(3) 0.012(3) C46 0.039(3) 0.033(3) 0.066(4) 0.010(3) -0.010(3) 0.003(2) C47 0.035(3) 0.028(2) 0.031(2) -0.0004(19) -0.0060(19) -0.0008(19) C48 0.035(3) 0.031(2) 0.033(2) 0.002(2) -0.007(2) -0.004(2) C49 0.032(3) 0.036(3) 0.034(3) 0.003(2) -0.001(2) 0.001(2) C50 0.044(3) 0.036(3) 0.039(3) 0.009(2) -0.001(2) -0.001(2) C51 0.037(3) 0.027(2) 0.057(3) 0.007(2) -0.004(2) -0.006(2) C52 0.025(2) 0.027(2) 0.047(3) 0.001(2) -0.006(2) -0.0004(18) C53 0.036(3) 0.031(3) 0.057(3) -0.006(2) -0.016(2) -0.002(2) C54 0.047(3) 0.033(3) 0.050(3) -0.006(2) -0.015(3) -0.006(2) C55 0.043(3) 0.035(3) 0.038(3) -0.003(2) -0.011(2) -0.002(2) C56 0.073(4) 0.051(4) 0.034(3) -0.007(3) -0.009(3) -0.011(3) C57 0.081(5) 0.053(4) 0.030(3) 0.002(3) -0.006(3) -0.019(3) C58 0.049(3) 0.038(3) 0.031(3) 0.001(2) -0.001(2) -0.012(2) C59 0.024(2) 0.022(2) 0.039(3) 0.0006(19) -0.0071(19) 0.0008(17) C60 0.030(2) 0.023(2) 0.036(3) -0.0023(19) -0.0062(19) 0.0023(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 Se1 C1 1.911(5) . ? Se1 Fe1 2.4443(11) . ? Se2 C7 1.901(5) . ? Se2 Fe1 2.4459(11) . ? Se3 C13 1.908(5) . ? Se3 Fe1 2.4608(10) . ? Se4 C19 1.910(5) . ? Se4 Fe1 2.4741(12) . ? Fe2 N6 1.956(4) . ? Fe2 N2 1.967(4) . ? Fe2 N3 1.969(4) . ? Fe2 N5 1.974(4) . ? Fe2 N4 1.977(4) . ? Fe2 N1 1.983(4) . ? N1 C25 1.337(7) . ? N1 C35 1.374(7) . ? N2 C34 1.343(7) . ? N2 C36 1.364(7) . ? N3 C37 1.331(6) . ? N3 C47 1.364(6) . ? N4 C46 1.338(7) . ? N4 C48 1.370(6) . ? N5 C49 1.340(6) . ? N5 C59 1.366(6) . ? N6 C58 1.336(6) . ? N6 C60 1.366(6) . ? C1 C6 1.393(7) . ? C1 C2 1.394(7) . ? C2 C3 1.382(8) . ? C3 C4 1.388(8) . ? C4 C5 1.389(8) . ? C5 C6 1.393(7) . ? C7 C12 1.390(8) . ? C7 C8 1.406(7) . ? C8 C9 1.380(8) . ? C9 C10 1.378(9) . ? C10 C11 1.390(9) . ? C11 C12 1.377(9) . ? C13 C14 1.400(8) . ? C13 C18 1.401(8) . ? C14 C15 1.382(8) . ? C15 C16 1.380(10) . ? C16 C17 1.349(11) . ? C17 C18 1.382(10) . ? C19 C24 1.387(8) . ? C19 C20 1.394(8) . ? C20 C21 1.396(9) . ? C21 C22 1.362(10) . ? C22 C23 1.368(10) . ? C23 C24 1.388(8) . ? C25 C26 1.433(9) . ? C26 C27 1.352(10) . ? C27 C28 1.393(10) . ? C28 C35 1.405(8) . ? C28 C29 1.459(10) . ? C29 C30 1.320(10) . ? C30 C31 1.424(9) . ? C31 C32 1.387(10) . ? C31 C36 1.406(8) . ? C32 C33 1.364(10) . ? C33 C34 1.392(8) . ? C35 C36 1.409(8) . ? C37 C38 1.398(8) . ? C38 C39 1.367(9) . ? C39 C40 1.415(8) . ? C40 C47 1.395(7) . ? C40 C41 1.425(8) . ? C41 C42 1.356(10) . ? C42 C43 1.431(8) . ? C43 C48 1.393(7) . ? C43 C44 1.395(8) . ? C44 C45 1.376(9) . ? C45 C46 1.386(8) . ? C47 C48 1.422(7) . ? C49 C50 1.379(7) . ? C50 C51 1.361(8) . ? C51 C52 1.415(8) . ? C52 C59 1.400(7) . ? C52 C53 1.431(8) . ? C53 C54 1.358(8) . ? C54 C55 1.440(7) . ? C55 C56 1.390(8) . ? C55 C60 1.407(7) . ? C56 C57 1.367(9) . ? C57 C58 1.394(8) . ? C59 C60 1.417(7) . ? N7 C63 1.353(15) . ? N7 C61 1.409(14) . ? N7 C62 1.417(12) . ? O1 C63 1.274(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Se1 Fe1 107.02(15) . . ? C7 Se2 Fe1 105.77(15) . . ? C13 Se3 Fe1 106.22(16) . . ? C19 Se4 Fe1 105.31(15) . . ? N6 Fe2 N2 91.23(17) . . ? N6 Fe2 N3 95.49(16) . . ? N2 Fe2 N3 93.78(17) . . ? N6 Fe2 N5 83.04(16) . . ? N2 Fe2 N5 90.60(16) . . ? N3 Fe2 N5 175.42(16) . . ? N6 Fe2 N4 89.31(17) . . ? N2 Fe2 N4 176.51(16) . . ? N3 Fe2 N4 82.74(16) . . ? N5 Fe2 N4 92.89(16) . . ? N6 Fe2 N1 172.35(18) . . ? N2 Fe2 N1 82.19(19) . . ? N3 Fe2 N1 88.86(17) . . ? N5 Fe2 N1 93.09(17) . . ? N4 Fe2 N1 97.49(19) . . ? Se1 Fe1 Se2 113.76(4) . . ? Se1 Fe1 Se3 98.76(4) . . ? Se2 Fe1 Se3 114.06(4) . . ? Se1 Fe1 Se4 104.07(4) . . ? Se2 Fe1 Se4 107.44(4) . . ? Se3 Fe1 Se4 118.25(4) . . ? C25 N1 C35 117.7(5) . . ? C25 N1 Fe2 130.1(4) . . ? C35 N1 Fe2 112.2(4) . . ? C34 N2 C36 116.0(4) . . ? C34 N2 Fe2 129.8(4) . . ? C36 N2 Fe2 114.2(4) . . ? C37 N3 C47 116.8(4) . . ? C37 N3 Fe2 130.2(4) . . ? C47 N3 Fe2 113.0(3) . . ? C46 N4 C48 116.5(4) . . ? C46 N4 Fe2 130.6(4) . . ? C48 N4 Fe2 112.8(3) . . ? C49 N5 C59 117.1(4) . . ? C49 N5 Fe2 130.5(3) . . ? C59 N5 Fe2 112.4(3) . . ? C58 N6 C60 117.2(4) . . ? C58 N6 Fe2 129.8(3) . . ? C60 N6 Fe2 112.9(3) . . ? C6 C1 C2 117.7(5) . . ? C6 C1 Se1 123.0(4) . . ? C2 C1 Se1 119.3(4) . . ? C3 C2 C1 121.2(5) . . ? C2 C3 C4 120.8(5) . . ? C3 C4 C5 118.7(5) . . ? C4 C5 C6 120.3(5) . . ? C5 C6 C1 121.3(5) . . ? C12 C7 C8 117.5(5) . . ? C12 C7 Se2 123.6(4) . . ? C8 C7 Se2 118.8(4) . . ? C9 C8 C7 121.1(5) . . ? C10 C9 C8 120.5(5) . . ? C9 C10 C11 119.1(6) . . ? C12 C11 C10 120.5(6) . . ? C11 C12 C7 121.3(5) . . ? C14 C13 C18 117.3(5) . . ? C14 C13 Se3 122.5(4) . . ? C18 C13 Se3 120.2(5) . . ? C15 C14 C13 120.4(5) . . ? C16 C15 C14 121.0(7) . . ? C17 C16 C15 119.2(6) . . ? C16 C17 C18 121.3(6) . . ? C17 C18 C13 120.8(7) . . ? C24 C19 C20 118.2(5) . . ? C24 C19 Se4 120.3(4) . . ? C20 C19 Se4 121.4(4) . . ? C19 C20 C21 119.5(6) . . ? C22 C21 C20 121.5(6) . . ? C21 C22 C23 119.4(6) . . ? C22 C23 C24 120.3(6) . . ? C19 C24 C23 121.1(6) . . ? N1 C25 C26 120.9(6) . . ? C27 C26 C25 120.4(6) . . ? C26 C27 C28 120.2(6) . . ? C27 C28 C35 117.0(6) . . ? C27 C28 C29 126.2(6) . . ? C35 C28 C29 116.8(6) . . ? C30 C29 C28 123.6(6) . . ? C29 C30 C31 119.9(6) . . ? C32 C31 C36 117.5(6) . . ? C32 C31 C30 123.9(6) . . ? C36 C31 C30 118.6(6) . . ? C33 C32 C31 119.9(6) . . ? C32 C33 C34 119.0(6) . . ? N2 C34 C33 123.9(6) . . ? N1 C35 C28 123.8(6) . . ? N1 C35 C36 116.7(5) . . ? C28 C35 C36 119.4(6) . . ? N2 C36 C31 123.7(5) . . ? N2 C36 C35 114.7(5) . . ? C31 C36 C35 121.7(5) . . ? N3 C37 C38 122.8(5) . . ? C39 C38 C37 120.4(5) . . ? C38 C39 C40 118.7(5) . . ? C47 C40 C39 116.9(5) . . ? C47 C40 C41 119.7(5) . . ? C39 C40 C41 123.5(5) . . ? C42 C41 C40 120.1(5) . . ? C41 C42 C43 121.8(6) . . ? C48 C43 C44 118.1(5) . . ? C48 C43 C42 117.9(5) . . ? C44 C43 C42 124.0(6) . . ? C45 C44 C43 118.2(5) . . ? C44 C45 C46 120.5(6) . . ? N4 C46 C45 122.9(5) . . ? N3 C47 C40 124.5(5) . . ? N3 C47 C48 116.0(4) . . ? C40 C47 C48 119.5(5) . . ? N4 C48 C43 123.7(5) . . ? N4 C48 C47 115.4(4) . . ? C43 C48 C47 120.9(5) . . ? N5 C49 C50 122.2(5) . . ? C51 C50 C49 121.4(5) . . ? C50 C51 C52 118.6(5) . . ? C59 C52 C51 116.8(5) . . ? C59 C52 C53 119.0(5) . . ? C51 C52 C53 124.2(5) . . ? C54 C53 C52 120.8(5) . . ? C53 C54 C55 121.3(5) . . ? C56 C55 C60 117.2(5) . . ? C56 C55 C54 124.8(5) . . ? C60 C55 C54 118.0(5) . . ? C57 C56 C55 119.4(5) . . ? C56 C57 C58 120.4(5) . . ? N6 C58 C57 122.2(5) . . ? N5 C59 C52 123.9(4) . . ? N5 C59 C60 115.8(4) . . ? C52 C59 C60 120.3(4) . . ? N6 C60 C55 123.6(5) . . ? N6 C60 C59 115.8(4) . . ? C55 C60 C59 120.6(4) . . ? C63 N7 C61 123.4(10) . . ? C63 N7 C62 115.7(10) . . ? C61 N7 C62 120.4(9) . . ? O1 C63 N7 115.8(14) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.89 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.095 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.141