Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Hughes, David' 'Davies, Sian C.' 'Evans, D.' 'Konkol, Martin' 'Richards, R.' 'Sanders, J. Roger' 'Sobota, Piotr' _publ_contact_author_name 'Dr David Hughes' _publ_contact_author_address ; Dr David Hughes Department of Biological Chemistry John Innes Centre Colney Lane Norwich NR4 7UH UK ; _publ_contact_author_email 'HUGHES@BBSRC.AC.UK' _publ_section_title ; Mononuclear, binuclear, trinuclear and tetranuclear iron complexes of the N(CH2CH2S)3 3-(NS3) ligand with nitrosyl co-ligands ; data_roger42 _symmetry_Int_Tables_number 178000 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 1' _chemical_formula_moiety 'C8 H20 N, C6 H12 Fe N2 O S3' _chemical_formula_structural '(NEt4)[Fe(NO){N(CH2CH2S)3}]' _chemical_formula_analytical ? _chemical_formula_sum 'C14 H32 Fe N3 O S3' _chemical_formula_weight 410.46 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'Pbcm' _symmetry_Int_Tables_number 57 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 8.8770(11) _cell_length_b 14.2422(14) _cell_length_c 15.919(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2012.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _exptl_crystal_description 'fibrous needles' _exptl_crystal_colour brown _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method ? _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 1.065 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.16 _exptl_absorpt_correction_T_max 0.19 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 0 _diffrn_reflns_number 1841 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0873 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.00 _reflns_number_total '1841 (1296 to theta-max 22.0 deg)' _reflns_number_observed '784 (716 to theta-max 22.0 deg)' _reflns_observed_criterion I>2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_data_reduction 'CAD4 (Hursthouse, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0315P)^2^] 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 '1296 (all data to theta-max 22.0 deg)' _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0980 _refine_ls_R_factor_obs 0.0477 _refine_ls_wR_factor_all 0.1157 _refine_ls_wR_factor_obs 0.0888 _refine_ls_goodness_of_fit_all 1.018 _refine_ls_goodness_of_fit_obs 1.107 _refine_ls_restrained_S_all 1.018 _refine_ls_restrained_S_obs 1.107 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.18921(15) 0.06641(10) 0.2500 0.0465(5) Uani 1 d S . S1 S 0.1631(3) 0.2280(2) 0.2500 0.0607(8) Uani 1 d S . C14 C -0.0379(10) 0.2413(7) 0.2500 0.073(3) Uani 1 d S . H14A H -0.0649 0.2941 0.2853 0.087 Uiso 0.50 calc PR . H14B H -0.0716 0.2549 0.1933 0.087 Uiso 0.50 calc PR . C41 C -0.1148(13) 0.1572(9) 0.2804(8) 0.067(6) Uani 0.50 d P . H41A H -0.1080 0.1568 0.3412 0.080 Uiso 0.50 calc PR . H41B H -0.2206 0.1629 0.2660 0.080 Uiso 0.50 calc PR . S2 S 0.1637(2) -0.01338(14) 0.37593(12) 0.0707(7) Uani 1 d . . C24 C -0.0368(8) -0.0205(6) 0.3846(4) 0.079(2) Uani 1 d . . H24A H -0.0631 -0.0805 0.4094 0.095 Uiso 0.50 calc PR 1 H24B H -0.0712 0.0284 0.4225 0.095 Uiso 0.50 calc PR 1 H24C H -0.0697 -0.0811 0.3636 0.095 Uiso 0.50 calc PR 2 H24D H -0.0645 -0.0168 0.4435 0.095 Uiso 0.50 calc PR 2 C42 C -0.1196(18) -0.0105(11) 0.3023(9) 0.065(5) Uani 0.50 d P 1 H42A H -0.1111 -0.0689 0.2712 0.078 Uiso 0.50 calc PR 1 H42B H -0.2255 0.0002 0.3136 0.078 Uiso 0.50 calc PR 1 C43 C -0.1161(16) 0.0533(12) 0.1613(9) 0.055(4) Uani 0.50 d P 2 H43A H -0.2227 0.0384 0.1624 0.066 Uiso 0.50 calc PR 2 H43B H -0.1042 0.1120 0.1312 0.066 Uiso 0.50 calc PR 2 N4 N -0.0622(7) 0.0665(5) 0.2500 0.042(2) Uani 1 d S . N5 N 0.3830(9) 0.0684(6) 0.2500 0.062(3) Uani 1 d S . O5 O 0.4987(12) 0.0826(13) 0.2788(11) 0.180(10) Uani 0.50 d P . N6 N 0.4764(9) 0.2500 0.5000 0.055(2) Uani 1 d S . C61 C 0.4785(24) 0.2571(17) 0.6004(14) 0.079(8) Uiso 0.367(10) d P 3 H61A H 0.5615 0.2977 0.6162 0.095 Uiso 0.367(10) calc PR 3 H61B H 0.3864 0.2882 0.6179 0.095 Uiso 0.367(10) calc PR 3 C62 C 0.4911(25) 0.1764(18) 0.6452(15) 0.075(7) Uiso 0.367(10) d P 3 H62A H 0.4909 0.1906 0.7041 0.113 Uiso 0.367(10) calc PR 3 H62B H 0.5837 0.1454 0.6307 0.113 Uiso 0.367(10) calc PR 3 H62C H 0.4078 0.1359 0.6324 0.113 Uiso 0.367(10) calc PR 3 C63 C 0.4715(29) 0.3627(22) 0.4788(18) 0.081(8) Uiso 0.367(10) d P 4 H63A H 0.3836 0.3916 0.5042 0.097 Uiso 0.367(10) calc PR 4 H63B H 0.5610 0.3937 0.5001 0.097 Uiso 0.367(10) calc PR 4 C64 C 0.4643(29) 0.3705(22) 0.3832(23) 0.097(10) Uiso 0.367(10) d P 4 H64A H 0.4612 0.4355 0.3673 0.145 Uiso 0.367(10) calc PR 4 H64B H 0.3754 0.3394 0.3631 0.145 Uiso 0.367(10) calc PR 4 H64C H 0.5518 0.3414 0.3591 0.145 Uiso 0.367(10) calc PR 4 C65 C 0.6148(13) 0.2117(12) 0.4702(10) 0.087(6) Uani 0.50 d P . H65A H 0.6140 0.2170 0.4095 0.104 Uiso 0.50 calc PR . H65B H 0.6140 0.1452 0.4834 0.104 Uiso 0.50 calc PR . C66 C 0.7619(10) 0.2500 0.5000 0.072(3) Uani 1 d S . H66A H 0.8428 0.2162 0.4737 0.107 Uiso 0.50 calc PR . H66B H 0.7688 0.2431 0.5599 0.107 Uiso 0.50 calc PR . H66C H 0.7688 0.3153 0.4855 0.107 Uiso 0.50 calc PR . C67 C 0.3460(14) 0.2066(12) 0.4687(10) 0.092(6) Uani 0.50 d P . H67A H 0.3487 0.1408 0.4843 0.110 Uiso 0.50 calc PR . H67B H 0.3487 0.2098 0.4078 0.110 Uiso 0.50 calc PR . C68 C 0.1897(10) 0.2500 0.5000 0.079(4) Uani 1 d S . H68A H 0.1078 0.2158 0.4753 0.118 Uiso 0.50 calc PR . H68B H 0.1838 0.3147 0.4835 0.118 Uiso 0.50 calc PR . H68C H 0.1838 0.2456 0.5601 0.118 Uiso 0.50 calc PR . C61A C 0.4784(56) 0.3361(38) 0.5634(32) 0.052(17) Uiso 0.133(10) d P 5 C62A C 0.4790(72) 0.4379(52) 0.5038(47) 0.091(21) Uiso 0.133(10) d P 5 C61B C 0.4765(75) 0.1661(57) 0.5684(64) 0.082(23) Uiso 0.133(10) d P 6 C62B C 0.4549(64) 0.0790(52) 0.5579(49) 0.073(20) Uiso 0.133(10) d P 6 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0418(8) 0.0498(9) 0.0479(9) 0.000 0.000 0.0031(8) S1 0.059(2) 0.049(2) 0.073(2) 0.000 0.000 -0.0107(15) C14 0.056(7) 0.048(7) 0.114(9) 0.000 0.000 0.003(6) C41 0.051(8) 0.057(9) 0.094(16) -0.010(8) 0.015(7) -0.006(7) S2 0.0751(14) 0.0788(15) 0.0583(13) 0.0180(11) -0.0078(12) 0.0098(12) C24 0.099(7) 0.086(7) 0.052(5) 0.017(5) 0.004(5) 0.003(5) C42 0.066(11) 0.055(10) 0.074(12) 0.013(10) 0.001(10) -0.019(10) C43 0.041(8) 0.076(12) 0.047(10) 0.007(9) -0.012(8) -0.012(10) N4 0.044(4) 0.028(4) 0.053(5) 0.000 0.000 0.000(4) N5 0.042(5) 0.072(6) 0.073(6) 0.000 0.000 0.004(5) O5 0.049(6) 0.321(18) 0.168(28) -0.016(15) -0.019(10) -0.009(10) N6 0.048(6) 0.059(6) 0.058(6) 0.002(5) 0.000 0.000 C65 0.037(8) 0.143(19) 0.080(13) -0.039(11) 0.015(8) -0.023(10) C66 0.053(7) 0.092(9) 0.070(8) -0.022(7) 0.000 0.000 C67 0.041(9) 0.144(18) 0.090(13) -0.019(12) -0.006(9) -0.044(10) C68 0.029(6) 0.123(10) 0.083(8) 0.022(7) 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N5 1.721(8) . ? Fe N4 2.232(7) . ? Fe S1 2.313(3) . ? Fe S2 2.316(2) . ? Fe S2 2.316(2) 6_556 ? S1 C14 1.794(9) . ? C14 C41 1.460(13) . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? C41 N4 1.457(12) . ? C41 H41A 0.97 . ? C41 H41B 0.97 . ? S2 C24 1.788(7) . ? C24 C43 1.46(2) 6_556 ? C24 C42 1.51(2) . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C24 H24C 0.97 . ? C24 H24D 0.97 . ? C42 N4 1.468(14) . ? C42 H42A 0.97 . ? C42 H42B 0.97 . ? C43 C24 1.46(2) 6_556 ? C43 N4 1.503(14) . ? C43 H43A 0.97 . ? C43 H43B 0.97 . ? N4 C41 1.457(12) 6_556 ? N4 C42 1.468(14) 6_556 ? N4 C43 1.503(14) 6_556 ? N5 O5 1.143(12) . ? N5 O5 1.143(12) 6_556 ? O5 O5 0.92(4) 6_556 ? N6 C67 1.404(12) . ? N6 C65 1.425(12) . ? N6 C61A 1.59(5) . ? N6 C61 1.60(2) . ? N6 C61B 1.62(9) . ? N6 C63 1.64(3) . ? C61 C62 1.36(3) . ? C61 H61A 0.97 . ? C61 H61B 0.97 . ? C62 H62A 0.96 . ? C62 H62B 0.96 . ? C62 H62C 0.96 . ? C63 C64 1.53(4) . ? C63 H63A 0.97 . ? C63 H63B 0.97 . ? C64 H64A 0.96 . ? C64 H64B 0.96 . ? C64 H64C 0.96 . ? C65 C66 1.492(13) . ? C65 H65A 0.97 . ? C65 H65B 0.97 . ? C66 H66A 0.96 . ? C66 H66B 0.96 . ? C66 H66C 0.96 . ? C67 C68 1.598(14) . ? C67 H67A 0.97 . ? C67 H67B 0.97 . ? C68 H68A 0.96 . ? C68 H68B 0.96 . ? C68 H68C 0.96 . ? C61A C62A 1.73(9) . ? C61B C62B 1.27(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 N5 Fe N4 179.0(4) . . ? N5 Fe S1 94.8(3) . . ? N4 Fe S1 84.2(2) . . ? N5 Fe S2 96.1(2) . . ? N4 Fe S2 84.40(12) . . ? S1 Fe S2 118.59(6) . . ? N5 Fe S2 96.1(2) . 6_556 ? N4 Fe S2 84.40(12) . 6_556 ? S1 Fe S2 118.59(6) . 6_556 ? S2 Fe S2 119.94(11) . 6_556 ? C14 S1 Fe 101.8(4) . . ? C41 C14 S1 112.2(8) . . ? C41 C14 H14A 109.2 . . ? S1 C14 H14A 109.2 . . ? C41 C14 H14B 109.2 . . ? S1 C14 H14B 109.16 . . ? H14A C14 H14B 107.9 . . ? N4 C41 C14 117.9(9) . . ? N4 C41 H41A 107.8 . . ? C14 C41 H41A 107.8 . . ? N4 C41 H41B 107.8 . . ? C14 C41 H41B 107.8 . . ? H41A C41 H41B 107.2 . . ? C24 S2 Fe 101.1(3) . . ? C43 C24 S2 113.6(7) 6_556 . ? C42 C24 S2 114.3(7) . . ? C42 C24 H24A 108.7 . . ? S2 C24 H24A 108.7 . . ? C42 C24 H24B 108.7 . . ? S2 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? C43 C24 H24C 108.8 6_556 . ? S2 C24 H24C 108.8 . . ? C43 C24 H24D 108.8 6_556 . ? S2 C24 H24D 108.8 . . ? H24C C24 H24D 107.7 . . ? N4 C42 C24 113.2(11) . . ? N4 C42 H42A 108.9 . . ? C24 C42 H42A 108.9 . . ? N4 C42 H42B 108.9 . . ? C24 C42 H42B 108.9 . . ? H42A C42 H42B 107.8 . . ? C24 C43 N4 114.0(11) 6_556 . ? C24 C43 H43A 108.8 6_556 . ? N4 C43 H43A 108.8 . . ? C24 C43 H43B 108.8 6_556 . ? N4 C43 H43B 108.8 . . ? H43A C43 H43B 107.6 . . ? C41 N4 C42 111.3(9) . . ? C41 N4 C43 108.7(10) . . ? C42 N4 C43 109.2(12) . . ? C41 N4 Fe 108.7(6) . . ? C42 N4 Fe 110.3(7) . . ? C43 N4 Fe 108.6(6) . . ? O5 N5 Fe 154.4(9) . . ? C67 N6 C65 115.1(8) . . ? C67 N6 C61A 125.1(21) . . ? C65 N6 C61A 119.8(20) . . ? C67 N6 C61 113.1(12) . . ? C65 N6 C61 110.3(12) . . ? C67 N6 C61B 95.0(27) . 3_556 ? C65 N6 C61B 93.3(28) . 3_556 ? C61A N6 C61B 82(4) . 3_556 ? C67 N6 C61B 85.1(28) . . ? C65 N6 C61B 86.6(27) . . ? C61A N6 C61B 98(4) . . ? C67 N6 C63 109.6(13) . . ? C65 N6 C63 109.2(13) . . ? C61 N6 C63 98.2(13) . . ? C62 C61 N6 118.1(19) . . ? C62 C61 H61A 107.8 . . ? N6 C61 H61A 107.8 . . ? C62 C61 H61B 107.8 . . ? N6 C61 H61B 107.8 . . ? H61A C61 H61B 107.1 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 N6 106.1(25) . . ? C64 C63 H63A 110.5 . . ? N6 C63 H63A 110.5 . . ? C64 C63 H63B 110.5 . . ? N6 C63 H63B 110.5 . . ? H63A C63 H63B 108.7 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N6 C65 C66 120.6(10) . . ? N6 C65 H65A 107.2 . . ? C66 C65 H65A 107.2 . . ? N6 C65 H65B 107.2 . . ? C66 C65 H65B 107.2 . . ? H65A C65 H65B 106.8 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N6 C67 C68 115.8(10) . . ? N6 C67 H67A 108.3 . . ? C68 C67 H67A 108.3 . . ? N6 C67 H67B 108.3 . . ? C68 C67 H67B 108.3 . . ? H67A C67 H67B 107.4 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N6 C61A C62A 107.4(38) . . ? C62B C61B N6 129.5(86) . . ? _refine_diff_density_max 0.329 _refine_diff_density_min -0.277 _refine_diff_density_rms 0.070 #===END data_roger99 _symmetry_Int_Tables_number 178001 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 6' _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 Fe4 N6 O4 S6' _chemical_formula_sum 'C12 H24 Fe4 N6 O4 S6' _chemical_formula_structural '[{Fe(NO)2{Fe(NS3)}}2]' _chemical_formula_weight 732.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 '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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9285(7) _cell_length_b 10.9103(8) _cell_length_c 11.9760(8) _cell_angle_alpha 98.430(2) _cell_angle_beta 109.149(2) _cell_angle_gamma 90.726(2) _cell_volume 1209.69(15) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4918 _cell_measurement_theta_min 3.96 _cell_measurement_theta_max 68.78 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.010 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 24.001 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.0654 _exptl_absorpt_correction_T_max 0.1976 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6818 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.10 _diffrn_reflns_theta_max 68.68 _reflns_number_total 3806 _reflns_number_observed 3285 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 w=1/[\s^2^(Fo^2^)+(0.0531P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3806 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_obs 0.0386 _refine_ls_wR_factor_all 0.0937 _refine_ls_wR_factor_obs 0.0917 _refine_ls_goodness_of_fit_all 1.011 _refine_ls_goodness_of_fit_obs 1.082 _refine_ls_restrained_S_all 1.022 _refine_ls_restrained_S_obs 1.082 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.22754(7) 0.29484(6) 0.42178(6) 0.0137(2) Uani 1 d . . S11 S 0.09029(11) 0.11766(9) 0.36693(9) 0.0170(2) Uani 1 d . . C114 C 0.2040(5) 0.0228(4) 0.3005(4) 0.0199(9) Uani 1 d . . H11A H 0.2738 -0.0156 0.3633 0.024 Uiso 1 calc R . H11B H 0.1442 -0.0447 0.2390 0.024 Uiso 1 calc R . C141 C 0.2827(5) 0.0997(4) 0.2440(4) 0.0185(9) Uani 1 d . . H14A H 0.3563 0.0504 0.2227 0.022 Uiso 1 calc R . H14B H 0.2149 0.1217 0.1695 0.022 Uiso 1 calc R . S12 S 0.13451(12) 0.40692(10) 0.27123(9) 0.0184(2) Uani 1 d . . C124 C 0.2506(5) 0.3625(4) 0.1823(4) 0.0188(9) Uani 1 d . . H12A H 0.1983 0.3001 0.1119 0.023 Uiso 1 calc R . H12B H 0.2774 0.4363 0.1530 0.023 Uiso 1 calc R . C142 C 0.3844(5) 0.3090(4) 0.2569(4) 0.0177(9) Uani 1 d . . H14C H 0.4339 0.2681 0.2033 0.021 Uiso 1 calc R . H14D H 0.4497 0.3774 0.3125 0.021 Uiso 1 calc R . S13 S 0.42815(10) 0.38904(9) 0.55565(9) 0.0140(2) Uani 1 d . . C134 C 0.5600(5) 0.2953(4) 0.5121(4) 0.0184(9) Uani 1 d . . H13A H 0.6189 0.3481 0.4829 0.022 Uiso 1 calc R . H13B H 0.6243 0.2642 0.5832 0.022 Uiso 1 calc R . C143 C 0.4900(5) 0.1868(4) 0.4157(4) 0.0188(9) Uani 1 d . . H14E H 0.5567 0.1602 0.3722 0.023 Uiso 1 calc R . H14F H 0.4714 0.1165 0.4535 0.023 Uiso 1 calc R . N14 N 0.3527(4) 0.2162(3) 0.3281(3) 0.0151(7) Uani 1 d . . Fe2 Fe 0.31563(7) 0.30323(6) 0.65958(6) 0.0131(2) Uani 1 d . . S21 S 0.41993(11) 0.12407(9) 0.67222(9) 0.0177(2) Uani 1 d . . C214 C 0.2899(5) 0.0401(4) 0.7172(4) 0.0217(10) Uani 1 d . . H21A H 0.2138 -0.0024 0.6449 0.026 Uiso 1 calc R . H21B H 0.3381 -0.0240 0.7642 0.026 Uiso 1 calc R . C241 C 0.2242(5) 0.1278(4) 0.7915(4) 0.0195(9) Uani 1 d . . H24A H 0.1415 0.0841 0.8009 0.023 Uiso 1 calc R . H24B H 0.2953 0.1540 0.8722 0.023 Uiso 1 calc R . S22 S 0.42727(11) 0.42719(10) 0.83665(9) 0.0177(2) Uani 1 d . . C224 C 0.3028(5) 0.3986(4) 0.9158(4) 0.0216(10) Uani 1 d . . H22A H 0.3441 0.3417 0.9736 0.026 Uiso 1 calc R . H22B H 0.2883 0.4779 0.9612 0.026 Uiso 1 calc R . C242 C 0.1600(5) 0.3419(4) 0.8284(4) 0.0180(9) Uani 1 d . . H24C H 0.1045 0.3075 0.8732 0.022 Uiso 1 calc R . H24D H 0.1054 0.4078 0.7884 0.022 Uiso 1 calc R . S23 S 0.13384(10) 0.39792(9) 0.54941(8) 0.0133(2) Uani 1 d . . C234 C -0.0157(4) 0.3133(4) 0.5682(4) 0.0152(8) Uani 1 d . . H23A H -0.0652 0.3714 0.6107 0.018 Uiso 1 calc R . H23B H -0.0849 0.2796 0.4884 0.018 Uiso 1 calc R . C243 C 0.0339(4) 0.2077(4) 0.6382(4) 0.0167(9) Uani 1 d . . H24E H -0.0377 0.1872 0.6750 0.020 Uiso 1 calc R . H24F H 0.0408 0.1332 0.5827 0.020 Uiso 1 calc R . N24 N 0.1759(4) 0.2402(3) 0.7343(3) 0.0146(7) Uani 1 d . . Fe3 Fe -0.02798(7) 0.24052(7) 0.22937(6) 0.0202(2) Uani 1 d . . N36 N -0.1701(4) 0.2885(4) 0.2667(3) 0.0232(8) Uani 1 d . . O36 O -0.2826(4) 0.3084(4) 0.2753(4) 0.0374(9) Uani 1 d . . N37 N -0.0577(5) 0.1635(4) 0.0909(4) 0.0309(10) Uani 1 d . . O37 O -0.0951(6) 0.1088(5) -0.0066(4) 0.067(2) Uani 1 d . . Fe4 Fe 0.55804(7) 0.25523(7) 0.84119(6) 0.0196(2) Uani 1 d . . N46 N 0.7117(4) 0.2945(4) 0.8209(4) 0.0272(9) Uani 1 d . . O46 O 0.8324(4) 0.3119(4) 0.8290(5) 0.0487(11) Uani 1 d . . N47 N 0.5647(4) 0.1874(4) 0.9598(4) 0.0292(9) Uani 1 d . . O47 O 0.5753(5) 0.1382(4) 1.0428(4) 0.0531(12) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0180(3) 0.0122(3) 0.0107(3) -0.0010(3) 0.0056(3) 0.0029(3) S11 0.0216(5) 0.0143(5) 0.0140(5) -0.0032(4) 0.0068(4) -0.0006(4) C114 0.028(2) 0.013(2) 0.017(2) -0.006(2) 0.008(2) 0.000(2) C141 0.023(2) 0.018(2) 0.013(2) -0.001(2) 0.006(2) 0.002(2) S12 0.0261(5) 0.0175(5) 0.0137(5) 0.0038(4) 0.0084(4) 0.0091(4) C124 0.025(2) 0.020(2) 0.013(2) 0.001(2) 0.008(2) 0.002(2) C142 0.025(2) 0.017(2) 0.017(2) 0.003(2) 0.014(2) 0.004(2) S13 0.0176(4) 0.0126(4) 0.0119(4) -0.0010(4) 0.0062(4) 0.0016(4) C134 0.017(2) 0.023(2) 0.018(2) 0.003(2) 0.009(2) 0.006(2) C143 0.019(2) 0.021(2) 0.019(2) 0.002(2) 0.010(2) 0.006(2) N14 0.018(2) 0.013(2) 0.013(2) -0.001(2) 0.005(2) 0.0023(15) Fe2 0.0163(3) 0.0128(3) 0.0106(3) 0.0007(3) 0.0054(3) 0.0037(3) S21 0.0227(5) 0.0145(5) 0.0178(5) 0.0031(4) 0.0086(5) 0.0075(4) C214 0.025(2) 0.013(2) 0.026(2) 0.005(2) 0.008(2) 0.004(2) C241 0.021(2) 0.021(2) 0.017(2) 0.004(2) 0.007(2) 0.003(2) S22 0.0191(5) 0.0200(5) 0.0113(4) -0.0038(4) 0.0041(4) -0.0001(4) C224 0.025(2) 0.026(2) 0.013(2) -0.004(2) 0.008(2) 0.001(2) C242 0.023(2) 0.019(2) 0.011(2) -0.006(2) 0.008(2) 0.003(2) S23 0.0169(4) 0.0128(4) 0.0100(4) -0.0001(4) 0.0048(4) 0.0052(4) C234 0.017(2) 0.019(2) 0.010(2) -0.002(2) 0.006(2) 0.003(2) C243 0.014(2) 0.021(2) 0.012(2) -0.005(2) 0.004(2) -0.002(2) N24 0.015(2) 0.016(2) 0.011(2) -0.0017(15) 0.003(2) 0.0020(15) Fe3 0.0210(3) 0.0233(4) 0.0140(3) -0.0017(3) 0.0045(3) 0.0047(3) N36 0.022(2) 0.025(2) 0.019(2) -0.001(2) 0.003(2) 0.003(2) O36 0.020(2) 0.045(2) 0.043(2) -0.004(2) 0.010(2) 0.006(2) N37 0.035(2) 0.036(2) 0.017(2) 0.002(2) 0.002(2) 0.015(2) O37 0.091(4) 0.070(3) 0.018(2) -0.010(2) -0.005(2) 0.037(3) Fe4 0.0177(3) 0.0235(4) 0.0169(3) 0.0034(3) 0.0046(3) 0.0036(3) N46 0.025(2) 0.030(2) 0.028(2) 0.008(2) 0.008(2) 0.005(2) O46 0.023(2) 0.051(2) 0.079(3) 0.019(2) 0.023(2) 0.005(2) N47 0.026(2) 0.037(2) 0.018(2) 0.007(2) -0.002(2) 0.003(2) O47 0.068(3) 0.060(3) 0.025(2) 0.021(2) 0.001(2) -0.011(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N14 2.049(3) . ? Fe1 S23 2.2186(11) . ? Fe1 S13 2.2280(12) . ? Fe1 S11 2.2359(12) . ? Fe1 S12 2.2763(12) . ? Fe1 Fe2 2.6779(9) . ? Fe1 Fe3 2.7970(10) . ? S11 C114 1.832(4) . ? S11 Fe3 2.3039(13) . ? C114 C141 1.506(6) . ? C141 N14 1.502(5) . ? S12 C124 1.834(4) . ? S12 Fe3 2.2975(13) . ? C124 C142 1.516(6) . ? C142 N14 1.508(5) . ? S13 C134 1.832(4) . ? S13 Fe2 2.2139(12) . ? C134 C143 1.507(6) . ? C143 N14 1.495(5) . ? Fe2 N24 2.041(4) . ? Fe2 S23 2.2250(11) . ? Fe2 S21 2.2251(12) . ? Fe2 S22 2.2658(12) . ? Fe2 Fe4 2.7801(9) . ? S21 C214 1.835(5) . ? S21 Fe4 2.3030(13) . ? C214 C241 1.510(6) . ? C241 N24 1.500(6) . ? S22 C224 1.836(4) . ? S22 Fe4 2.2921(13) . ? C224 C242 1.518(6) . ? C242 N24 1.511(5) . ? S23 C234 1.831(4) . ? C234 C243 1.517(6) . ? C243 N24 1.497(5) . ? Fe3 N37 1.676(4) . ? Fe3 N36 1.682(4) . ? N36 O36 1.175(5) . ? N37 O37 1.167(6) . ? Fe4 N47 1.678(4) . ? Fe4 N46 1.681(4) . ? N46 O46 1.181(5) . ? N47 O47 1.174(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 N14 Fe1 S23 168.33(11) . . ? N14 Fe1 S13 86.86(10) . . ? S23 Fe1 S13 81.47(4) . . ? N14 Fe1 S11 88.95(10) . . ? S23 Fe1 S11 100.33(4) . . ? S13 Fe1 S11 143.19(5) . . ? N14 Fe1 S12 87.96(10) . . ? S23 Fe1 S12 96.34(4) . . ? S13 Fe1 S12 111.33(5) . . ? S11 Fe1 S12 105.04(5) . . ? N14 Fe1 Fe2 118.82(10) . . ? S23 Fe1 Fe2 53.05(3) . . ? S13 Fe1 Fe2 52.68(3) . . ? S11 Fe1 Fe2 99.02(4) . . ? S12 Fe1 Fe2 144.28(4) . . ? N14 Fe1 Fe3 94.59(10) . . ? S23 Fe1 Fe3 96.64(4) . . ? S13 Fe1 Fe3 163.73(4) . . ? S11 Fe1 Fe3 53.07(3) . . ? S12 Fe1 Fe3 52.64(3) . . ? Fe2 Fe1 Fe3 137.43(3) . . ? C114 S11 Fe1 97.82(15) . . ? C114 S11 Fe3 106.9(2) . . ? Fe1 S11 Fe3 76.05(4) . . ? C141 C114 S11 111.3(3) . . ? N14 C141 C114 110.9(3) . . ? C124 S12 Fe1 99.11(14) . . ? C124 S12 Fe3 105.45(15) . . ? Fe1 S12 Fe3 75.40(4) . . ? C142 C124 S12 110.6(3) . . ? N14 C142 C124 112.5(3) . . ? C134 S13 Fe2 115.77(15) . . ? C134 S13 Fe1 99.88(15) . . ? Fe2 S13 Fe1 74.15(4) . . ? C143 C134 S13 111.9(3) . . ? N14 C143 C134 112.9(3) . . ? C143 N14 C141 109.2(3) . . ? C143 N14 C142 108.9(3) . . ? C141 N14 C142 108.9(3) . . ? C143 N14 Fe1 108.4(3) . . ? C141 N14 Fe1 112.7(3) . . ? C142 N14 Fe1 108.7(2) . . ? N24 Fe2 S13 168.15(10) . . ? N24 Fe2 S23 86.52(10) . . ? S13 Fe2 S23 81.64(4) . . ? N24 Fe2 S21 89.31(10) . . ? S13 Fe2 S21 100.01(4) . . ? S23 Fe2 S21 144.09(5) . . ? N24 Fe2 S22 88.28(10) . . ? S13 Fe2 S22 96.13(4) . . ? S23 Fe2 S22 109.82(4) . . ? S21 Fe2 S22 105.68(5) . . ? N24 Fe2 Fe1 118.34(10) . . ? S13 Fe2 Fe1 53.16(3) . . ? S23 Fe2 Fe1 52.83(3) . . ? S21 Fe2 Fe1 99.48(4) . . ? S22 Fe2 Fe1 143.53(4) . . ? N24 Fe2 Fe4 94.54(10) . . ? S13 Fe2 Fe4 96.89(4) . . ? S23 Fe2 Fe4 162.50(4) . . ? S21 Fe2 Fe4 53.40(3) . . ? S22 Fe2 Fe4 52.85(3) . . ? Fe1 Fe2 Fe4 138.45(3) . . ? C214 S21 Fe2 98.06(14) . . ? C214 S21 Fe4 106.2(2) . . ? Fe2 S21 Fe4 75.73(4) . . ? C241 C214 S21 110.9(3) . . ? N24 C241 C214 111.3(4) . . ? C224 S22 Fe2 99.24(15) . . ? C224 S22 Fe4 105.3(2) . . ? Fe2 S22 Fe4 75.17(4) . . ? C242 C224 S22 110.9(3) . . ? N24 C242 C224 112.6(3) . . ? C234 S23 Fe1 114.43(14) . . ? C234 S23 Fe2 99.98(14) . . ? Fe1 S23 Fe2 74.12(4) . . ? C243 C234 S23 111.8(3) . . ? N24 C243 C234 111.9(3) . . ? C243 N24 C241 108.8(3) . . ? C243 N24 C242 109.1(3) . . ? C241 N24 C242 108.7(3) . . ? C243 N24 Fe2 108.6(3) . . ? C241 N24 Fe2 112.6(3) . . ? C242 N24 Fe2 109.1(3) . . ? N37 Fe3 N36 118.0(2) . . ? N37 Fe3 S12 111.0(2) . . ? N36 Fe3 S12 108.75(14) . . ? N37 Fe3 S11 109.20(15) . . ? N36 Fe3 S11 106.51(14) . . ? S12 Fe3 S11 102.19(5) . . ? N37 Fe3 Fe1 129.91(15) . . ? N36 Fe3 Fe1 112.04(14) . . ? S12 Fe3 Fe1 51.96(3) . . ? S11 Fe3 Fe1 50.88(3) . . ? O36 N36 Fe3 168.5(4) . . ? O37 N37 Fe3 172.0(5) . . ? N47 Fe4 N46 119.0(2) . . ? N47 Fe4 S22 110.7(2) . . ? N46 Fe4 S22 108.11(15) . . ? N47 Fe4 S21 107.4(2) . . ? N46 Fe4 S21 108.0(2) . . ? S22 Fe4 S21 102.32(4) . . ? N47 Fe4 Fe2 127.43(15) . . ? N46 Fe4 Fe2 113.49(15) . . ? S22 Fe4 Fe2 51.99(3) . . ? S21 Fe4 Fe2 50.87(3) . . ? O46 N46 Fe4 165.7(4) . . ? O47 N47 Fe4 177.0(4) . . ? _refine_diff_density_max 0.703 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.126 #===END data_roger50 _symmetry_Int_Tables_number 178002 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 7' _chemical_formula_moiety 'C7 H12 Fe2 N3 O3 S3' _chemical_formula_structural '[{Fe(CO)(N{CH2CH2S}3)-S,S'}Fe(NO)2]' _chemical_formula_analytical ? _chemical_formula_sum 'C7 H12 Fe2 N3 O3 S3' _chemical_formula_weight 394.08 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'F2/d' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, y, -z+1/4' 'x, y+1/2, z+1/2' '-x+1/4, y+1/2, -z+3/4' 'x+1/2, y, z+1/2' '-x+3/4, y, -z+3/4' 'x+1/2, y+1/2, z' '-x+3/4, y+1/2, -z+1/4' '-x, -y, -z' 'x-1/4, -y, z-1/4' '-x, -y+1/2, -z+1/2' 'x-1/4, -y+1/2, z+1/4' '-x+1/2, -y, -z+1/2' 'x+1/4, -y, z+1/4' '-x+1/2, -y+1/2, -z' 'x+1/4, -y+1/2, z-1/4' _cell_length_a 18.092(2) _cell_length_b 13.4423(13) _cell_length_c 22.510(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.454(9) _cell_angle_gamma 90.00 _cell_volume 5414.8(10) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _exptl_crystal_description 'irregular octahedra' _exptl_crystal_colour Black _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.934 _exptl_crystal_density_method ? _exptl_crystal_F_000 3184 _exptl_absorpt_coefficient_mu 2.606 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.818 _exptl_absorpt_correction_T_max 0.998 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 0 _diffrn_reflns_number 4636 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 30.0 _reflns_number_total 3946 _reflns_number_observed 3429 _reflns_observed_criterion I>2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_data_reduction 'CAD4 (Hursthouse, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+6.2789P] 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 ; Hydrogen coordinates were initially located in idealised postions and subsequently refined freely. Isotropic thermal displacement parameters were refined freely. ; _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00060(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3946 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_obs 0.0270 _refine_ls_wR_factor_all 0.0730 _refine_ls_wR_factor_obs 0.0694 _refine_ls_goodness_of_fit_all 1.084 _refine_ls_goodness_of_fit_obs 1.110 _refine_ls_restrained_S_all 1.084 _refine_ls_restrained_S_obs 1.110 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.411466(13) 0.29225(2) 0.514459(10) 0.02774(7) Uani 1 d . . Fe2 Fe 0.511699(15) 0.18407(2) 0.586647(12) 0.03597(8) Uani 1 d . . S1 S 0.53277(3) 0.33277(3) 0.54217(2) 0.03570(10) Uani 1 d . . S2 S 0.38563(3) 0.16294(3) 0.57024(2) 0.03478(10) Uani 1 d . . S3 S 0.33164(3) 0.37610(4) 0.45045(2) 0.04490(13) Uani 1 d . . N4 N 0.38554(8) 0.38501(11) 0.58085(6) 0.0300(3) Uani 1 d . . C14 C 0.52153(12) 0.4301(2) 0.59717(10) 0.0420(4) Uani 1 d . . H14A H 0.5560(14) 0.4866(20) 0.5899(11) 0.054(7) Uiso 1 d . . H14B H 0.5391(14) 0.4010(19) 0.6370(11) 0.050(7) Uiso 1 d . . C41 C 0.44184(12) 0.46708(14) 0.58822(9) 0.0390(4) Uani 1 d . . H41A H 0.4322(13) 0.5087(19) 0.5524(11) 0.044(6) Uiso 1 d . . H41B H 0.4328(13) 0.5101(19) 0.6232(11) 0.047(6) Uiso 1 d . . C24 C 0.35213(12) 0.2301(2) 0.63173(9) 0.0412(4) Uani 1 d . . H24A H 0.3646(15) 0.1924(19) 0.6675(11) 0.050(7) Uiso 1 d . . H24B H 0.2986(14) 0.2346(18) 0.6209(10) 0.044(6) Uiso 1 d . . C42 C 0.38644(12) 0.3325(2) 0.63960(8) 0.0378(4) Uani 1 d . . H42A H 0.4380(13) 0.3265(17) 0.6575(10) 0.036(6) Uiso 1 d . . H42B H 0.3572(14) 0.3743(18) 0.6681(10) 0.041(6) Uiso 1 d . . C34 C 0.29810(13) 0.4672(2) 0.49977(10) 0.0465(5) Uani 1 d . . H34A H 0.2429(15) 0.4818(19) 0.4865(11) 0.050(7) Uiso 1 d . . H34B H 0.3221(13) 0.5287(20) 0.4971(10) 0.046(7) Uiso 1 d . . C43 C 0.30878(11) 0.4271(2) 0.56317(9) 0.0421(4) Uani 1 d . . H43A H 0.2742(13) 0.3696(19) 0.5652(10) 0.043(6) Uiso 1 d . . H43B H 0.2994(13) 0.4782(18) 0.5926(10) 0.039(6) Uiso 1 d . . C5 C 0.43211(11) 0.21674(15) 0.45461(8) 0.0370(4) Uani 1 d . . O5 O 0.44679(10) 0.16855(14) 0.41632(7) 0.0571(4) Uani 1 d . . N6 N 0.55054(10) 0.09535(14) 0.54874(9) 0.0491(4) Uani 1 d . . O6 O 0.58451(12) 0.03078(15) 0.53184(13) 0.0858(7) Uani 1 d . . N7 N 0.53397(10) 0.19220(15) 0.66095(8) 0.0469(4) Uani 1 d . . O7 O 0.54872(12) 0.1911(2) 0.71318(8) 0.0767(6) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02855(12) 0.03025(13) 0.02499(12) -0.00150(8) 0.00578(8) -0.00353(9) Fe2 0.03227(14) 0.03500(14) 0.04056(15) 0.00102(10) 0.00501(10) 0.00157(10) S1 0.0311(2) 0.0363(2) 0.0411(2) -0.0049(2) 0.0102(2) -0.0075(2) S2 0.0357(2) 0.0320(2) 0.0384(2) 0.0009(2) 0.0112(2) -0.0066(2) S3 0.0492(3) 0.0534(3) 0.0302(2) 0.0036(2) -0.0003(2) 0.0073(2) N4 0.0319(7) 0.0317(7) 0.0269(6) -0.0009(5) 0.0054(5) 0.0008(5) C14 0.0404(10) 0.0376(9) 0.0472(10) -0.0120(8) 0.0039(8) -0.0095(8) C41 0.0448(10) 0.0309(8) 0.0415(9) -0.0067(7) 0.0070(8) -0.0043(7) C24 0.0465(11) 0.0456(10) 0.0354(9) 0.0043(8) 0.0186(8) -0.0019(8) C42 0.0436(10) 0.0426(10) 0.0286(8) -0.0005(7) 0.0098(7) 0.0015(8) C34 0.0471(11) 0.0463(11) 0.0444(10) 0.0057(9) 0.0011(8) 0.0114(9) C43 0.0378(10) 0.0479(11) 0.0414(10) -0.0017(8) 0.0078(8) 0.0096(8) C5 0.0364(9) 0.0424(9) 0.0336(8) -0.0031(7) 0.0098(7) -0.0060(7) O5 0.0656(11) 0.0636(10) 0.0460(9) -0.0197(7) 0.0214(8) -0.0034(8) N6 0.0416(9) 0.0380(9) 0.0698(12) -0.0061(8) 0.0150(8) -0.0019(7) O6 0.0721(13) 0.0490(10) 0.144(2) -0.0261(12) 0.0404(14) 0.0063(9) N7 0.0381(9) 0.0566(11) 0.0447(9) 0.0043(8) 0.0018(7) 0.0077(8) O7 0.0662(12) 0.120(2) 0.0424(9) 0.0040(10) 0.0037(8) 0.0221(12) _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 C5 1.770(2) . ? Fe1 N4 2.0529(14) . ? Fe1 S3 2.1955(6) . ? Fe1 S2 2.2336(5) . ? Fe1 S1 2.2582(5) . ? Fe1 Fe2 2.6790(4) . ? Fe2 N7 1.665(2) . ? Fe2 N6 1.679(2) . ? Fe2 S2 2.2741(6) . ? Fe2 S1 2.2925(6) . ? S1 C14 1.833(2) . ? S2 C24 1.829(2) . ? S3 C34 1.816(2) . ? N4 C41 1.494(2) . ? N4 C42 1.497(2) . ? N4 C43 1.498(2) . ? C14 C41 1.510(3) . ? C14 H14A 1.01(3) . ? C14 H14B 0.99(2) . ? C41 H41A 0.98(3) . ? C41 H41B 1.01(2) . ? C24 C42 1.510(3) . ? C24 H24A 0.95(3) . ? C24 H24B 0.97(2) . ? C42 H42A 0.96(2) . ? C42 H42B 1.05(2) . ? C34 C43 1.511(3) . ? C34 H34A 1.02(3) . ? C34 H34B 0.94(3) . ? C43 H43A 1.00(2) . ? C43 H43B 0.99(2) . ? C5 O5 1.140(2) . ? N6 O6 1.160(2) . ? N7 O7 1.167(2) . ? 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 C5 Fe1 N4 177.20(8) . . ? C5 Fe1 S3 89.25(7) . . ? N4 Fe1 S3 88.13(4) . . ? C5 Fe1 S2 93.82(7) . . ? N4 Fe1 S2 88.53(4) . . ? S3 Fe1 S2 126.63(2) . . ? C5 Fe1 S1 92.49(6) . . ? N4 Fe1 S1 88.23(4) . . ? S3 Fe1 S1 125.19(2) . . ? S2 Fe1 S1 107.92(2) . . ? C5 Fe1 Fe2 87.17(7) . . ? N4 Fe1 Fe2 95.44(4) . . ? S3 Fe1 Fe2 176.38(2) . . ? S2 Fe1 Fe2 54.23(2) . . ? S1 Fe1 Fe2 54.53(2) . . ? N7 Fe2 N6 119.96(10) . . ? N7 Fe2 S2 105.08(7) . . ? N6 Fe2 S2 108.26(7) . . ? N7 Fe2 S1 110.49(7) . . ? N6 Fe2 S1 106.77(7) . . ? S2 Fe2 S1 105.38(2) . . ? N7 Fe2 Fe1 128.01(6) . . ? N6 Fe2 Fe1 111.95(7) . . ? S2 Fe2 Fe1 52.844(15) . . ? S1 Fe2 Fe1 53.343(14) . . ? C14 S1 Fe1 99.15(7) . . ? C14 S1 Fe2 106.59(8) . . ? Fe1 S1 Fe2 72.13(2) . . ? C24 S2 Fe1 99.28(7) . . ? C24 S2 Fe2 104.56(7) . . ? Fe1 S2 Fe2 72.92(2) . . ? C34 S3 Fe1 101.04(7) . . ? C41 N4 C42 109.35(14) . . ? C41 N4 C43 109.9(2) . . ? C42 N4 C43 107.56(14) . . ? C41 N4 Fe1 107.72(11) . . ? C42 N4 Fe1 112.51(11) . . ? C43 N4 Fe1 109.75(11) . . ? C41 C14 S1 110.08(13) . . ? C41 C14 H14A 109.3(15) . . ? S1 C14 H14A 107.2(15) . . ? C41 C14 H14B 115.1(14) . . ? S1 C14 H14B 106.1(15) . . ? H14A C14 H14B 108.7(20) . . ? N4 C41 C14 113.2(2) . . ? N4 C41 H41A 107.2(14) . . ? C14 C41 H41A 110.5(14) . . ? N4 C41 H41B 108.9(14) . . ? C14 C41 H41B 110.2(14) . . ? H41A C41 H41B 106.7(19) . . ? C42 C24 S2 111.27(13) . . ? C42 C24 H24A 110.1(16) . . ? S2 C24 H24A 108.4(15) . . ? C42 C24 H24B 110.7(15) . . ? S2 C24 H24B 105.7(14) . . ? H24A C24 H24B 110.6(21) . . ? N4 C42 C24 112.0(2) . . ? N4 C42 H42A 107.1(13) . . ? C24 C42 H42A 109.2(14) . . ? N4 C42 H42B 110.2(13) . . ? C24 C42 H42B 108.9(13) . . ? H42A C42 H42B 109.4(18) . . ? C43 C34 S3 109.21(15) . . ? C43 C34 H34A 109.2(14) . . ? S3 C34 H34A 110.6(14) . . ? C43 C34 H34B 112.2(15) . . ? S3 C34 H34B 110.8(14) . . ? H34A C34 H34B 104.6(21) . . ? N4 C43 C34 111.7(2) . . ? N4 C43 H43A 104.9(14) . . ? C34 C43 H43A 109.0(13) . . ? N4 C43 H43B 109.2(13) . . ? C34 C43 H43B 112.0(13) . . ? H43A C43 H43B 109.7(18) . . ? O5 C5 Fe1 178.7(2) . . ? O6 N6 Fe2 168.5(2) . . ? O7 N7 Fe2 175.4(2) . . ? _refine_diff_density_max 0.451 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.066 #===END data_roger46 _symmetry_Int_Tables_number 178003 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 9' _chemical_formula_moiety 'C6 H12 Fe2 N4 O3 S3' _chemical_formula_structural '[{Fe(NO){N(CH2CH2S)3}}Fe(NO)2]' _chemical_formula_analytical ? _chemical_formula_sum 'C6 H12 Fe2 N4 O3 S3' _chemical_formula_weight 396.08 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'C -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, y+1/2, z' '-x, -y, -z' '-x+1/2, -y+1/2, -z' _cell_length_a 8.1707(6) _cell_length_b 14.314(2) _cell_length_c 12.1054(12) _cell_angle_alpha 82.108(10) _cell_angle_beta 91.536(7) _cell_angle_gamma 83.088(9) _cell_volume 1390.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _exptl_crystal_description prisms _exptl_crystal_colour 'black, irregular hexagonal' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.891 _exptl_crystal_density_method ? _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 2.539 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.913 _exptl_absorpt_correction_T_max 0.997 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 0 _diffrn_reflns_number 3474 _diffrn_reflns_av_R_equivalents 0.013 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 28.0 _reflns_number_total 3341 _reflns_number_observed 2236 _reflns_observed_criterion I>2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_data_reduction 'CAD4 (Hursthouse, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3341 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_obs 0.0312 _refine_ls_wR_factor_all 0.0699 _refine_ls_wR_factor_obs 0.0579 _refine_ls_goodness_of_fit_all 0.994 _refine_ls_goodness_of_fit_obs 1.025 _refine_ls_restrained_S_all 0.994 _refine_ls_restrained_S_obs 1.025 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.73796(5) 0.02499(3) 0.16986(3) 0.03722(11) Uani 1 d . . S1 S 0.51660(9) -0.01401(6) 0.28051(6) 0.0462(2) Uani 1 d . . C14 C 0.5283(4) -0.1416(2) 0.2727(3) 0.0476(7) Uani 1 d . . H14A H 0.5693(33) -0.1781(20) 0.3438(24) 0.048(8) Uiso 1 d . . H14B H 0.4059(40) -0.1511(21) 0.2586(25) 0.063(9) Uiso 1 d . . C41 C 0.6280(4) -0.1707(2) 0.1767(3) 0.0442(7) Uani 1 d . . H41A H 0.6437(33) -0.2421(20) 0.1857(22) 0.044(8) Uiso 1 d . . H41B H 0.5659(33) -0.1451(19) 0.1080(23) 0.042(8) Uiso 1 d . . S2 S 0.96108(10) 0.00427(6) 0.29575(6) 0.0501(2) Uani 1 d . . C24 C 1.0383(4) -0.1190(2) 0.2859(3) 0.0531(8) Uani 1 d . . H24A H 1.1159(38) -0.1189(21) 0.2280(26) 0.059(10) Uiso 1 d . . H24B H 1.0934(38) -0.1459(22) 0.3567(26) 0.060(9) Uiso 1 d . . C42 C 0.9026(4) -0.1778(2) 0.2648(3) 0.0442(7) Uani 1 d . . H42A H 0.9480(32) -0.2391(19) 0.2514(21) 0.037(7) Uiso 1 d . . H42B H 0.8403(32) -0.1891(18) 0.3285(23) 0.036(7) Uiso 1 d . . S3 S 0.74065(10) 0.03544(5) -0.01562(6) 0.0443(2) Uani 1 d . . C34 C 0.7748(5) -0.0882(2) -0.0366(3) 0.0478(7) Uani 1 d . . H34A H 0.6721(39) -0.1113(21) -0.0537(24) 0.055(9) Uiso 1 d . . H34B H 0.8398(36) -0.0918(20) -0.1009(24) 0.050(9) Uiso 1 d . . C43 C 0.8658(4) -0.1486(2) 0.0634(2) 0.0426(7) Uani 1 d . . H43A H 0.8709(32) -0.2145(20) 0.0539(21) 0.039(7) Uiso 1 d . . H43B H 0.9809(34) -0.1372(18) 0.0701(21) 0.036(7) Uiso 1 d . . N4 N 0.7889(3) -0.1317(2) 0.1705(2) 0.0370(5) Uani 1 d . . N5 N 0.7174(3) 0.1480(2) 0.1620(2) 0.0522(7) Uani 1 d . . O5 O 0.7843(29) 0.2156(12) 0.1441(19) 0.092(6) Uani 0.50 d P . O5A O 0.7508(29) 0.2216(14) 0.1252(17) 0.085(5) Uani 0.50 d P . Fe2 Fe 0.73066(6) 0.00120(3) 0.40025(3) 0.04791(13) Uani 1 d . . N6 N 0.6846(4) 0.1083(2) 0.4398(2) 0.0574(7) Uani 1 d . . O6 O 0.6346(33) 0.1665(16) 0.4884(16) 0.079(5) Uani 0.50 d P . O6A O 0.6591(32) 0.1800(16) 0.4850(16) 0.081(5) Uani 0.50 d P . N7 N 0.7560(4) -0.0921(2) 0.4998(2) 0.0576(7) Uani 1 d . . O7 O 0.7684(4) -0.1510(2) 0.5764(2) 0.0959(10) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0381(2) 0.0355(2) 0.0363(2) 0.0003(2) -0.0003(2) -0.0041(2) S1 0.0392(4) 0.0534(4) 0.0450(4) -0.0054(3) 0.0047(3) -0.0031(3) C14 0.039(2) 0.054(2) 0.051(2) -0.0040(15) 0.0051(14) -0.0134(14) C41 0.040(2) 0.041(2) 0.051(2) -0.0014(14) 0.0025(14) -0.0113(13) S2 0.0444(4) 0.0594(5) 0.0468(4) -0.0003(4) -0.0053(3) -0.0177(4) C24 0.037(2) 0.066(2) 0.051(2) 0.006(2) -0.005(2) -0.001(2) C42 0.042(2) 0.040(2) 0.045(2) 0.0075(13) -0.0017(14) 0.0016(13) S3 0.0504(4) 0.0423(4) 0.0376(4) 0.0038(3) 0.0006(3) -0.0067(3) C34 0.059(2) 0.045(2) 0.040(2) -0.0061(13) 0.004(2) -0.008(2) C43 0.045(2) 0.036(2) 0.046(2) -0.0061(13) 0.0062(14) -0.0032(13) N4 0.0335(12) 0.0376(12) 0.0380(12) 0.0013(10) 0.0011(10) -0.0046(10) N5 0.064(2) 0.0411(15) 0.049(2) -0.0043(13) 0.0007(13) 0.0014(13) O5 0.086(7) 0.032(6) 0.158(13) -0.007(6) -0.014(6) -0.024(6) O5A 0.108(12) 0.045(5) 0.095(6) 0.008(4) 0.026(9) 0.007(6) Fe2 0.0549(3) 0.0526(3) 0.0366(2) -0.0033(2) 0.0008(2) -0.0121(2) N6 0.072(2) 0.059(2) 0.0429(15) -0.0048(13) -0.0001(13) -0.019(2) O6 0.119(9) 0.054(7) 0.082(7) -0.037(6) 0.038(6) -0.039(5) O6A 0.124(11) 0.051(7) 0.068(6) -0.004(5) -0.014(7) -0.025(7) N7 0.070(2) 0.061(2) 0.0430(14) -0.0024(13) 0.0001(13) -0.0171(14) O7 0.140(3) 0.074(2) 0.068(2) 0.0195(15) -0.003(2) -0.027(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N5 1.738(3) . ? Fe1 S3 2.2305(8) . ? Fe1 N4 2.231(2) . ? Fe1 S2 2.3089(9) . ? Fe1 S1 2.3547(9) . ? Fe1 Fe2 2.7660(6) . ? S1 C14 1.833(3) . ? S1 Fe2 2.2913(9) . ? C14 C41 1.513(4) . ? C14 H14A 0.97(3) . ? C14 H14B 1.04(3) . ? C41 N4 1.488(3) . ? C41 H41A 1.01(3) . ? C41 H41B 0.97(3) . ? S2 C24 1.822(4) . ? S2 Fe2 2.2976(9) . ? C24 C42 1.507(4) . ? C24 H24A 0.96(3) . ? C24 H24B 0.97(3) . ? C42 N4 1.480(3) . ? C42 H42A 0.95(3) . ? C42 H42B 0.94(3) . ? S3 C34 1.812(3) . ? C34 C43 1.509(4) . ? C34 H34A 0.97(3) . ? C34 H34B 0.96(3) . ? C43 N4 1.492(4) . ? C43 H43A 0.96(3) . ? C43 H43B 0.98(3) . ? N5 O5A 1.15(2) . ? N5 O5 1.16(2) . ? Fe2 N7 1.660(3) . ? Fe2 N6 1.672(3) . ? N6 O6 1.13(2) . ? N6 O6A 1.23(2) . ? N7 O7 1.158(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 N5 Fe1 S3 91.16(9) . . ? N5 Fe1 N4 173.94(10) . . ? S3 Fe1 N4 85.68(6) . . ? N5 Fe1 S2 92.82(9) . . ? S3 Fe1 S2 127.88(3) . . ? N4 Fe1 S2 85.08(6) . . ? N5 Fe1 S1 101.95(9) . . ? S3 Fe1 S1 125.83(3) . . ? N4 Fe1 S1 84.07(6) . . ? S2 Fe1 S1 103.96(3) . . ? N5 Fe1 Fe2 92.04(9) . . ? S3 Fe1 Fe2 176.65(3) . . ? N4 Fe1 Fe2 91.22(6) . . ? S2 Fe1 Fe2 52.91(2) . . ? S1 Fe1 Fe2 52.41(2) . . ? C14 S1 Fe2 105.39(11) . . ? C14 S1 Fe1 100.34(10) . . ? Fe2 S1 Fe1 73.06(3) . . ? C41 C14 S1 112.6(2) . . ? C41 C14 H14A 112.1(16) . . ? S1 C14 H14A 110.1(17) . . ? C41 C14 H14B 109.3(17) . . ? S1 C14 H14B 103.0(17) . . ? H14A C14 H14B 109.3(23) . . ? N4 C41 C14 112.8(3) . . ? N4 C41 H41A 111.5(16) . . ? C14 C41 H41A 107.4(15) . . ? N4 C41 H41B 106.8(16) . . ? C14 C41 H41B 108.1(16) . . ? H41A C41 H41B 110.2(23) . . ? C24 S2 Fe2 106.63(11) . . ? C24 S2 Fe1 99.54(11) . . ? Fe2 S2 Fe1 73.80(3) . . ? C42 C24 S2 112.8(2) . . ? C42 C24 H24A 111.4(19) . . ? S2 C24 H24A 107.7(19) . . ? C42 C24 H24B 107.8(19) . . ? S2 C24 H24B 107.2(19) . . ? H24A C24 H24B 109.8(25) . . ? N4 C42 C24 112.1(2) . . ? N4 C42 H42A 110.0(16) . . ? C24 C42 H42A 110.3(16) . . ? N4 C42 H42B 108.3(16) . . ? C24 C42 H42B 111.2(16) . . ? H42A C42 H42B 104.6(22) . . ? C34 S3 Fe1 102.43(10) . . ? C43 C34 S3 110.9(2) . . ? C43 C34 H34A 111.3(18) . . ? S3 C34 H34A 111.1(18) . . ? C43 C34 H34B 109.4(17) . . ? S3 C34 H34B 107.5(18) . . ? H34A C34 H34B 106.4(25) . . ? N4 C43 C34 112.5(2) . . ? N4 C43 H43A 110.7(16) . . ? C34 C43 H43A 109.1(16) . . ? N4 C43 H43B 107.2(15) . . ? C34 C43 H43B 112.3(15) . . ? H43A C43 H43B 104.8(22) . . ? C42 N4 C41 110.8(2) . . ? C42 N4 C43 109.1(2) . . ? C41 N4 C43 109.6(2) . . ? C42 N4 Fe1 111.8(2) . . ? C41 N4 Fe1 107.7(2) . . ? C43 N4 Fe1 107.9(2) . . ? O5A N5 O5 17.2(25) . . ? O5A N5 Fe1 151.8(9) . . ? O5 N5 Fe1 145.3(12) . . ? N7 Fe2 N6 117.32(13) . . ? N7 Fe2 S1 109.16(10) . . ? N6 Fe2 S1 105.05(10) . . ? N7 Fe2 S2 110.08(10) . . ? N6 Fe2 S2 108.23(10) . . ? S1 Fe2 S2 106.38(3) . . ? N7 Fe2 Fe1 134.59(10) . . ? N6 Fe2 Fe1 108.07(9) . . ? S1 Fe2 Fe1 54.53(2) . . ? S2 Fe2 Fe1 53.28(2) . . ? O6 N6 O6A 13.6(27) . . ? O6 N6 Fe2 161.6(13) . . ? O6A N6 Fe2 170.1(9) . . ? O7 N7 Fe2 173.3(3) . . ? _refine_diff_density_max 0.262 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.073 #===END data_roger52 _symmetry_Int_Tables_number 178004 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 10' _chemical_formula_moiety 'C8 H20 N, C7 H12 Fe2 N4 O2 S3' _chemical_formula_structural '(NEt4)[{Fe(CN)(N{CH2CH2S}3)-S,S'}Fe(NO)2]' _chemical_formula_analytical ? _chemical_formula_sum 'C15 H32 Fe2 N5 O2 S3' _chemical_formula_weight 522.34 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' _symmetry_Int_Tables_number 14 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 10.6164(11) _cell_length_b 17.184(2) _cell_length_c 12.649(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.229(10) _cell_angle_gamma 90.00 _cell_volume 2289.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _exptl_crystal_description rhombs _exptl_crystal_colour Black _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method ? _exptl_crystal_F_000 1092 _exptl_absorpt_coefficient_mu 1.56 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.817 _exptl_absorpt_correction_T_max 0.939 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 0 _diffrn_reflns_number 5046 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_av_sigmaI/netI 0.1095 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 26.0 _reflns_number_total '4483 (3190 to theta of 23.0)' _reflns_number_observed '1602 (1488 to theta of 23.0)' _reflns_observed_criterion I>2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_data_reduction 'CAD4 (Hursthouse, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0178P)^2^] 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 ; Coordinates were of idealised positions and set to ride on the parent carbon atoms. All isotropic thermal displacement parameters were set to be 1.2 x Ueq of the parent atom except those of the methyl hydrogens which were set to be 1.5 x Ueq. ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3190 _refine_ls_number_parameters 257 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1270 _refine_ls_R_factor_obs 0.0528 _refine_ls_wR_factor_all 0.1108 _refine_ls_wR_factor_obs 0.0792 _refine_ls_goodness_of_fit_all 1.010 _refine_ls_goodness_of_fit_obs 1.110 _refine_ls_restrained_S_all 1.010 _refine_ls_restrained_S_obs 1.110 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.15769(10) 0.37051(7) 0.38297(8) 0.0377(3) Uani 1 d . . Fe2 Fe 0.40353(11) 0.36461(7) 0.36153(8) 0.0442(4) Uani 1 d . . S1 S 0.2915(2) 0.47012(12) 0.40968(15) 0.0462(6) Uani 1 d . . C14 C 0.3165(8) 0.4732(5) 0.5550(5) 0.053(2) Uani 1 d . . H14A H 0.3988 0.4511 0.5805 0.064 Uiso 0.760(13) calc PR 1 H14B H 0.3158 0.5269 0.5788 0.064 Uiso 0.760(13) calc PR 1 H14C H 0.4029 0.4892 0.5791 0.064 Uiso 0.240(13) calc PR 2 H14D H 0.2593 0.5109 0.5806 0.064 Uiso 0.240(13) calc PR 2 C41A C 0.2119(12) 0.4272(7) 0.6016(7) 0.049(4) Uani 0.760(13) d P 1 H41A H 0.2393 0.4166 0.6763 0.059 Uiso 0.760(13) calc PR 1 H41B H 0.1357 0.4588 0.5973 0.059 Uiso 0.760(13) calc PR 1 C41B C 0.2941(41) 0.3992(22) 0.5961(28) 0.053(12) Uiso 0.240(13) d P 2 H41C H 0.2856 0.4054 0.6711 0.064 Uiso 0.240(13) calc PR 2 H41D H 0.3692 0.3679 0.5918 0.064 Uiso 0.240(13) calc PR 2 S2 S 0.2663(2) 0.26205(11) 0.36721(15) 0.0425(5) Uani 1 d . . C24 C 0.2866(8) 0.2297(5) 0.5050(5) 0.054(2) Uani 1 d . . H24A H 0.2180 0.1946 0.5163 0.065 Uiso 0.760(13) calc PR 1 H24B H 0.3658 0.2012 0.5194 0.065 Uiso 0.760(13) calc PR 1 H24C H 0.2732 0.1740 0.5086 0.065 Uiso 0.240(13) calc PR 2 H24D H 0.3718 0.2413 0.5385 0.065 Uiso 0.240(13) calc PR 2 C42A C 0.2879(11) 0.2960(7) 0.5799(7) 0.046(4) Uani 0.760(13) d P 1 H42A H 0.3691 0.3225 0.5836 0.055 Uiso 0.760(13) calc PR 1 H42B H 0.2789 0.2765 0.6505 0.055 Uiso 0.760(13) calc PR 1 C42B C 0.1835(47) 0.2753(24) 0.5645(32) 0.073(14) Uiso 0.240(13) d P 2 H42C H 0.1000 0.2542 0.5410 0.087 Uiso 0.240(13) calc PR 2 H42D H 0.2017 0.2663 0.6406 0.087 Uiso 0.240(13) calc PR 2 S3 S -0.0476(2) 0.37909(14) 0.3905(2) 0.0550(6) Uani 1 d . . C34 C -0.0542(8) 0.3671(5) 0.5327(6) 0.063(3) Uani 1 d . . H34A H -0.0535 0.4177 0.5670 0.075 Uiso 0.760(13) calc PR 1 H34B H -0.1319 0.3405 0.5443 0.075 Uiso 0.760(13) calc PR 1 H34C H -0.1218 0.3991 0.5544 0.075 Uiso 0.240(13) calc PR 2 H34D H -0.0723 0.3133 0.5480 0.075 Uiso 0.240(13) calc PR 2 C43A C 0.0644(11) 0.3181(7) 0.5816(8) 0.056(4) Uani 0.760(13) d P 1 H43A H 0.0707 0.3185 0.6588 0.068 Uiso 0.760(13) calc PR 1 H43B H 0.0556 0.2646 0.5574 0.068 Uiso 0.760(13) calc PR 1 C43B C 0.0728(28) 0.3911(19) 0.5950(22) 0.033(10) Uiso 0.240(13) d P 2 H43C H 0.0812 0.4473 0.5936 0.040 Uiso 0.240(13) calc PR 2 H43D H 0.0757 0.3748 0.6687 0.040 Uiso 0.240(13) calc PR 2 N4 N 0.1818(6) 0.3538(4) 0.5461(4) 0.041(2) Uani 1 d . . C5 C 0.1240(7) 0.3843(4) 0.2338(7) 0.044(2) Uani 1 d . . N5 N 0.0991(8) 0.3928(4) 0.1430(5) 0.070(2) Uani 1 d . . N6 N 0.4394(6) 0.3786(4) 0.2389(5) 0.046(2) Uani 1 d . . O6 O 0.4972(6) 0.3884(4) 0.1661(4) 0.080(2) Uani 1 d . . N7 N 0.5242(7) 0.3496(4) 0.4558(5) 0.054(2) Uani 1 d . . O7 O 0.6122(6) 0.3390(4) 0.5204(5) 0.084(2) Uani 1 d . . N8 N 0.2454(6) 0.6233(4) 0.1132(5) 0.048(2) Uani 1 d . . C81 C 0.1328(8) 0.5915(5) 0.1636(6) 0.059(3) Uani 1 d . . H81A H 0.1228 0.5368 0.1459 0.071 Uiso 1 calc R . H81B H 0.1517 0.5955 0.2404 0.071 Uiso 1 calc R . C82 C 0.0083(8) 0.6327(6) 0.1288(6) 0.070(3) Uani 1 d . . H82A H -0.0577 0.6096 0.1637 0.105 Uiso 1 calc R . H82B H -0.0127 0.6279 0.0530 0.105 Uiso 1 calc R . H82C H 0.0162 0.6868 0.1477 0.105 Uiso 1 calc R . C83 C 0.3583(8) 0.5758(5) 0.1612(7) 0.070(3) Uani 1 d . . H83A H 0.3667 0.5820 0.2379 0.084 Uiso 1 calc R . H83B H 0.3398 0.5214 0.1458 0.084 Uiso 1 calc R . C84 C 0.4842(9) 0.5947(7) 0.1245(8) 0.109(4) Uani 1 d . . H84A H 0.5485 0.5611 0.1599 0.164 Uiso 1 calc R . H84B H 0.5057 0.6479 0.1412 0.164 Uiso 1 calc R . H84C H 0.4788 0.5870 0.0489 0.164 Uiso 1 calc R . C85 C 0.2251(9) 0.6147(6) -0.0073(6) 0.074(3) Uani 1 d . . H85A H 0.1502 0.6441 -0.0348 0.088 Uiso 1 calc R . H85B H 0.2969 0.6379 -0.0359 0.088 Uiso 1 calc R . C86 C 0.2094(9) 0.5324(7) -0.0485(7) 0.096(4) Uani 1 d . . H86A H 0.1972 0.5329 -0.1250 0.144 Uiso 1 calc R . H86B H 0.1369 0.5090 -0.0228 0.144 Uiso 1 calc R . H86C H 0.2840 0.5028 -0.0239 0.144 Uiso 1 calc R . C87 C 0.2671(9) 0.7084(5) 0.1353(6) 0.064(3) Uani 1 d . . H87A H 0.1954 0.7371 0.0995 0.077 Uiso 1 calc R . H87B H 0.3419 0.7244 0.1040 0.077 Uiso 1 calc R . C88 C 0.2847(11) 0.7312(6) 0.2510(7) 0.110(4) Uani 1 d . . H88A H 0.2979 0.7863 0.2570 0.165 Uiso 1 calc R . H88B H 0.3571 0.7045 0.2872 0.165 Uiso 1 calc R . H88C H 0.2103 0.7172 0.2827 0.165 Uiso 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 0.0392(7) 0.0387(7) 0.0347(7) -0.0001(6) 0.0029(5) -0.0010(6) Fe2 0.0416(8) 0.0502(8) 0.0406(7) 0.0028(6) 0.0043(6) -0.0025(7) S1 0.0502(15) 0.0402(13) 0.0479(13) -0.0001(10) 0.0049(11) -0.0045(12) C14 0.070(7) 0.053(6) 0.036(5) -0.018(4) 0.005(4) -0.010(5) C41A 0.048(8) 0.065(9) 0.034(7) -0.016(6) 0.006(6) -0.004(7) S2 0.0512(14) 0.0387(12) 0.0381(11) 0.0006(10) 0.0072(10) 0.0010(12) C24 0.067(6) 0.049(6) 0.044(5) 0.016(4) 0.002(5) 0.013(5) C42A 0.036(7) 0.069(9) 0.030(6) 0.010(6) 0.000(5) 0.007(7) S3 0.0433(14) 0.059(2) 0.0626(15) -0.0020(13) 0.0054(11) 0.0048(13) C34 0.054(6) 0.054(6) 0.084(7) -0.013(5) 0.024(5) 0.004(6) C43A 0.075(10) 0.059(9) 0.041(7) -0.018(6) 0.030(7) -0.026(8) N4 0.042(4) 0.044(4) 0.037(4) -0.002(3) 0.006(3) -0.006(4) C5 0.042(5) 0.034(5) 0.059(5) -0.010(4) 0.014(4) 0.002(4) N5 0.102(7) 0.055(5) 0.048(4) 0.004(4) -0.008(5) 0.013(5) N6 0.041(4) 0.046(5) 0.054(4) 0.009(4) 0.014(4) -0.003(4) O6 0.078(5) 0.099(6) 0.067(4) 0.013(4) 0.030(4) -0.010(4) N7 0.055(5) 0.053(5) 0.052(5) 0.001(4) 0.002(4) -0.003(4) O7 0.061(5) 0.107(6) 0.076(5) -0.004(4) -0.021(4) 0.007(4) N8 0.049(5) 0.044(5) 0.051(4) 0.017(4) 0.007(3) 0.012(4) C81 0.066(7) 0.052(6) 0.062(6) 0.008(5) 0.018(5) -0.011(5) C82 0.061(7) 0.078(7) 0.071(6) -0.012(6) 0.011(5) 0.003(6) C83 0.058(7) 0.061(7) 0.089(7) 0.013(5) 0.005(6) 0.009(6) C84 0.060(8) 0.134(12) 0.133(10) 0.024(8) 0.014(7) 0.007(8) C85 0.091(8) 0.091(9) 0.037(5) -0.002(5) 0.000(5) 0.001(7) C86 0.069(8) 0.131(11) 0.093(8) -0.046(8) 0.028(6) -0.002(8) C87 0.084(8) 0.035(5) 0.071(6) 0.006(5) 0.001(6) -0.001(5) C88 0.149(12) 0.082(9) 0.087(8) -0.029(7) -0.029(8) -0.019(8) _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 C5 1.890(8) . ? Fe1 N4 2.067(6) . ? Fe1 S3 2.198(2) . ? Fe1 S2 2.214(2) . ? Fe1 S1 2.223(2) . ? Fe1 Fe2 2.660(2) . ? Fe2 N7 1.657(7) . ? Fe2 N6 1.661(6) . ? Fe2 S1 2.293(2) . ? Fe2 S2 2.293(2) . ? S1 C14 1.824(7) . ? C14 C41B 1.41(4) . ? C14 C41A 1.540(12) . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? C14 H14C 0.97 . ? C14 H14D 0.97 . ? C41A H41A 0.97 . ? C41A H41B 0.97 . ? C41B H41C 0.97 . ? C41B H41D 0.97 . ? S2 C24 1.816(6) . ? C24 C42A 1.481(12) . ? C24 C42B 1.61(4) . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C24 H24C 0.97 . ? C24 H24D 0.97 . ? C42A H42A 0.97 . ? C42A H42B 0.97 . ? C42B H42C 0.97 . ? C42B H42D 0.97 . ? S3 C34 1.821(8) . ? C34 C43B 1.53(3) . ? C34 C43A 1.576(14) . ? C34 H34A 0.97 . ? C34 H34B 0.97 . ? C34 H34C 0.97 . ? C34 H34D 0.97 . ? C43A H43A 0.97 . ? C43A H43B 0.97 . ? C43B H43C 0.97 . ? C43B H43D 0.97 . ? N4 C42B 1.37(4) . ? N4 C41A 1.459(11) . ? N4 C41B 1.50(4) . ? N4 C43A 1.507(12) . ? N4 C43B 1.52(3) . ? N4 C42A 1.522(11) . ? C5 N5 1.156(8) . ? N6 O6 1.182(6) . ? N7 O7 1.175(7) . ? N8 C87 1.501(9) . ? N8 C83 1.512(10) . ? N8 C85 1.520(8) . ? N8 C81 1.524(9) . ? C81 C82 1.515(11) . ? C81 H81A 0.97 . ? C81 H81B 0.97 . ? C82 H82A 0.96 . ? C82 H82B 0.96 . ? C82 H82C 0.96 . ? C83 C84 1.505(11) . ? C83 H83A 0.97 . ? C83 H83B 0.97 . ? C84 H84A 0.96 . ? C84 H84B 0.96 . ? C84 H84C 0.96 . ? C85 C86 1.509(12) . ? C85 H85A 0.97 . ? C85 H85B 0.97 . ? C86 H86A 0.96 . ? C86 H86B 0.96 . ? C86 H86C 0.96 . ? C87 C88 1.504(9) . ? C87 H87A 0.97 . ? C87 H87B 0.97 . ? C88 H88A 0.96 . ? C88 H88B 0.96 . ? C88 H88C 0.96 . ? 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 C5 Fe1 N4 176.2(3) . . ? C5 Fe1 S3 88.3(2) . . ? N4 Fe1 S3 88.0(2) . . ? C5 Fe1 S2 92.9(2) . . ? N4 Fe1 S2 88.4(2) . . ? S3 Fe1 S2 126.22(10) . . ? C5 Fe1 S1 95.3(2) . . ? N4 Fe1 S1 87.6(2) . . ? S3 Fe1 S1 124.04(10) . . ? S2 Fe1 S1 109.38(9) . . ? C5 Fe1 Fe2 88.2(2) . . ? N4 Fe1 Fe2 95.5(2) . . ? S3 Fe1 Fe2 176.27(8) . . ? S2 Fe1 Fe2 55.23(7) . . ? S1 Fe1 Fe2 55.14(7) . . ? N7 Fe2 N6 116.6(3) . . ? N7 Fe2 S1 108.2(2) . . ? N6 Fe2 S1 108.8(2) . . ? N7 Fe2 S2 107.1(2) . . ? N6 Fe2 S2 111.2(2) . . ? S1 Fe2 S2 104.27(9) . . ? N7 Fe2 Fe1 127.7(2) . . ? N6 Fe2 Fe1 115.7(2) . . ? S1 Fe2 Fe1 52.70(6) . . ? S2 Fe2 Fe1 52.47(6) . . ? C14 S1 Fe1 100.6(3) . . ? C14 S1 Fe2 106.0(3) . . ? Fe1 S1 Fe2 72.16(7) . . ? C41B C14 S1 109.7(16) . . ? C41A C14 S1 110.5(6) . . ? C41A C14 H14A 109.5 . . ? S1 C14 H14A 109.5 . . ? C41A C14 H14B 109.5 . . ? S1 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C41B C14 H14C 109.7 . . ? S1 C14 H14C 109.7 . . ? C41B C14 H14D 109.7 . . ? S1 C14 H14D 109.7 . . ? H14C C14 H14D 108.2 . . ? N4 C41A C14 112.6(8) . . ? N4 C41A H41A 109.1 . . ? C14 C41A H41A 109.1 . . ? N4 C41A H41B 109.1 . . ? C14 C41A H41B 109.1 . . ? H41A C41A H41B 107.8 . . ? C14 C41B N4 118.6(26) . . ? C14 C41B H41C 107.7 . . ? N4 C41B H41C 107.7 . . ? C14 C41B H41D 107.7 . . ? N4 C41B H41D 107.7 . . ? H41C C41B H41D 107.1 . . ? C24 S2 Fe1 99.9(3) . . ? C24 S2 Fe2 105.4(3) . . ? Fe1 S2 Fe2 72.30(7) . . ? C42A C24 S2 111.6(6) . . ? C42B C24 S2 107.1(16) . . ? C42A C24 H24A 109.3 . . ? S2 C24 H24A 109.3 . . ? C42A C24 H24B 109.3 . . ? S2 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? C42B C24 H24C 110.3 . . ? S2 C24 H24C 110.3 . . ? C42B C24 H24D 110.3 . . ? S2 C24 H24D 110.3 . . ? H24C C24 H24D 108.5 . . ? C24 C42A N4 112.1(8) . . ? C24 C42A H42A 109.2 . . ? N4 C42A H42A 109.2 . . ? C24 C42A H42B 109.2 . . ? N4 C42A H42B 109.2 . . ? H42A C42A H42B 107.9 . . ? N4 C42B C24 113.4(29) . . ? N4 C42B H42C 108.9 . . ? C24 C42B H42C 108.9 . . ? N4 C42B H42D 108.9 . . ? C24 C42B H42D 108.9 . . ? H42C C42B H42D 107.7 . . ? C34 S3 Fe1 101.4(3) . . ? C43B C34 S3 109.7(12) . . ? C43A C34 S3 108.6(6) . . ? C43A C34 H34A 110.0 . . ? S3 C34 H34A 110.0 . . ? C43A C34 H34B 110.0 . . ? S3 C34 H34B 110.0 . . ? H34A C34 H34B 108.3 . . ? C43B C34 H34C 109.7 . . ? S3 C34 H34C 109.7 . . ? C43B C34 H34D 109.7 . . ? S3 C34 H34D 109.7 . . ? H34C C34 H34D 108.2 . . ? N4 C43A C34 108.4(8) . . ? N4 C43A H43A 110.0 . . ? C34 C43A H43A 110.0 . . ? N4 C43A H43B 110.0 . . ? C34 C43A H43B 110.0 . . ? H43A C43A H43B 108.4 . . ? N4 C43B C34 110.1(19) . . ? N4 C43B H43C 109.6 . . ? C34 C43B H43C 109.6 . . ? N4 C43B H43D 109.6 . . ? C34 C43B H43D 109.6 . . ? H43C C43B H43D 108.1 . . ? C42B N4 C41B 116.7(26) . . ? C41A N4 C43A 110.3(7) . . ? C42B N4 C43B 109.9(22) . . ? C41B N4 C43B 102.4(20) . . ? C41A N4 C42A 108.6(8) . . ? C43A N4 C42A 105.2(8) . . ? C42B N4 Fe1 107.7(18) . . ? C41A N4 Fe1 110.6(5) . . ? C41B N4 Fe1 110.0(14) . . ? C43A N4 Fe1 110.5(6) . . ? C43B N4 Fe1 110.0(11) . . ? C42A N4 Fe1 111.4(5) . . ? N5 C5 Fe1 177.7(8) . . ? O6 N6 Fe2 162.1(6) . . ? O7 N7 Fe2 178.0(7) . . ? C87 N8 C83 110.8(7) . . ? C87 N8 C85 106.3(6) . . ? C83 N8 C85 110.8(6) . . ? C87 N8 C81 112.4(6) . . ? C83 N8 C81 105.2(6) . . ? C85 N8 C81 111.4(7) . . ? C82 C81 N8 114.4(7) . . ? C82 C81 H81A 108.7 . . ? N8 C81 H81A 108.7 . . ? C82 C81 H81B 108.7 . . ? N8 C81 H81B 108.7 . . ? H81A C81 H81B 107.6 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C84 C83 N8 116.7(8) . . ? C84 C83 H83A 108.1 . . ? N8 C83 H83A 108.1 . . ? C84 C83 H83B 108.1 . . ? N8 C83 H83B 108.1 . . ? H83A C83 H83B 107.3 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C86 C85 N8 115.7(8) . . ? C86 C85 H85A 108.4 . . ? N8 C85 H85A 108.4 . . ? C86 C85 H85B 108.4 . . ? N8 C85 H85B 108.4 . . ? H85A C85 H85B 107.4 . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? N8 C87 C88 115.6(7) . . ? N8 C87 H87A 108.4 . . ? C88 C87 H87A 108.4 . . ? N8 C87 H87B 108.4 . . ? C88 C87 H87B 108.4 . . ? H87A C87 H87B 107.4 . . ? C87 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C87 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? _refine_diff_density_max 0.376 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.093 #===END data_roger54 _symmetry_Int_Tables_number 178005 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 13' _chemical_formula_moiety 'C8 H15 Fe3 I1 N6 O4 S3' _chemical_formula_structural '[{Fe(NO)2}{Fe(NS3)(CNMe)}{FeI(NO)2}]' _chemical_formula_analytical ? _chemical_formula_sum 'C8 H15 Fe3 I1 N6 O4 S3' _chemical_formula_weight 649.89 _chemical_melting_point ? _chemical_compound_source ? 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' 'I' 'I' -0.4742 1.8119 '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' 'S' 'S' 0.1246 0.1234 '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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.1107(15) _cell_length_b 14.2334(15) _cell_length_c 10.0102(11) _cell_angle_alpha 98.701(9) _cell_angle_beta 110.566(8) _cell_angle_gamma 94.203(8) _cell_volume 1973.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _exptl_crystal_description rhombs _exptl_crystal_colour black _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.187 _exptl_crystal_density_method ? _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 4.082 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.760 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% ? _diffrn_reflns_number 12066 _diffrn_reflns_av_R_equivalents 0.012 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 30.0 _reflns_number_total 11451 _reflns_number_observed 8036 _reflns_observed_criterion I>2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_data_reduction 'CAD4 (Hursthouse, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+0.4067P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11451 _refine_ls_number_parameters 483 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_obs 0.0346 _refine_ls_wR_factor_all 0.0846 _refine_ls_wR_factor_obs 0.0732 _refine_ls_goodness_of_fit_all 1.054 _refine_ls_goodness_of_fit_obs 1.098 _refine_ls_restrained_S_all 1.054 _refine_ls_restrained_S_obs 1.098 _refine_ls_shift/esd_max -0.020 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe11 Fe 0.59741(3) 0.24014(3) 0.37422(5) 0.02669(9) Uani 1 d . . S11 S 0.59560(6) 0.22802(6) 0.14834(9) 0.0369(2) Uani 1 d . . C114 C 0.6938(3) 0.3203(3) 0.1736(4) 0.0421(8) Uani 1 d . . H11A H 0.7503 0.2908 0.1774 0.052(12) Uiso 1 calc R . H11B H 0.6768 0.3538 0.0925 0.063(13) Uiso 1 calc R . C141 C 0.7141(3) 0.3905(2) 0.3140(4) 0.0384(8) Uani 1 d . . H14A H 0.7750 0.4297 0.3394 0.049(11) Uiso 1 calc R . H14B H 0.6654 0.4328 0.2988 0.041(10) Uiso 1 calc R . S12 S 0.69053(6) 0.13871(6) 0.48182(9) 0.0319(2) Uani 1 d . . C124 C 0.8017(2) 0.2212(2) 0.5712(4) 0.0345(7) Uani 1 d . . H12A H 0.8061 0.2504 0.6678 0.037(10) Uiso 1 calc R . H12B H 0.8554 0.1857 0.5814 0.050(11) Uiso 1 calc R . C142 C 0.8071(2) 0.2988(2) 0.4860(4) 0.0339(7) Uani 1 d . . H14C H 0.8592 0.3487 0.5457 0.040(10) Uiso 1 calc R . H14D H 0.8206 0.2719 0.4014 0.028(8) Uiso 1 calc R . S13 S 0.52384(6) 0.35571(6) 0.44276(9) 0.0332(2) Uani 1 d . . C134 C 0.6213(2) 0.4553(2) 0.5219(4) 0.0367(7) Uani 1 d . . H13A H 0.6160 0.4981 0.4534 0.044(11) Uiso 1 calc R . H13B H 0.6172 0.4915 0.6092 0.040(10) Uiso 1 calc R . C143 C 0.7165(2) 0.4176(2) 0.5585(3) 0.0325(7) Uani 1 d . . H14E H 0.7666 0.4701 0.5771 0.043(10) Uiso 1 calc R . H14F H 0.7300 0.3910 0.6462 0.046(11) Uiso 1 calc R . N14 N 0.7164(2) 0.3422(2) 0.4376(3) 0.0268(5) Uani 1 d . . C15 C 0.4874(2) 0.1521(2) 0.3062(4) 0.0379(7) Uani 1 d . . N15 N 0.4195(2) 0.0967(2) 0.2583(4) 0.0513(8) Uani 1 d . . C151 C 0.3390(4) 0.0233(4) 0.2064(7) 0.082(2) Uani 1 d . . H15A H 0.2878(14) 0.0420(18) 0.1309(40) 0.139(28) Uiso 1 calc R . H15B H 0.3188(23) 0.0141(27) 0.2849(14) 0.129(27) Uiso 1 calc R . H15C H 0.3565(11) -0.0356(11) 0.1685(53) 0.241(53) Uiso 1 calc R . Fe12 Fe 0.66748(4) 0.10538(3) 0.24257(5) 0.03550(11) Uani 1 d . . N16 N 0.5900(2) 0.0050(2) 0.1714(3) 0.0484(8) Uani 1 d . . O16 O 0.5495(3) -0.0709(2) 0.1143(4) 0.0831(12) Uani 1 d . . N17 N 0.7693(2) 0.1061(2) 0.2154(4) 0.0476(8) Uani 1 d . . O17 O 0.8361(3) 0.0963(3) 0.1864(5) 0.0896(12) Uani 1 d . . Fe13 Fe 0.54915(4) 0.27194(4) 0.62951(6) 0.04237(12) Uani 1 d . . I1 I 0.50448(2) 0.40731(2) 0.79977(3) 0.04587(7) Uani 1 d . . N18 N 0.4661(3) 0.1778(3) 0.5911(5) 0.0736(12) Uani 1 d . . O18 O 0.4225(4) 0.1048(3) 0.5817(5) 0.126(2) Uani 1 d . . N19 N 0.6536(3) 0.2648(3) 0.7581(4) 0.0691(12) Uani 1 d . . O19 O 0.7183(3) 0.2532(4) 0.8555(4) 0.126(2) Uani 1 d . . Fe21 Fe 0.13071(3) 0.23072(3) 0.89545(4) 0.02465(9) Uani 1 d . . S21 S 0.05815(6) 0.26339(6) 0.67651(9) 0.0320(2) Uani 1 d . . C214 C 0.1131(3) 0.3872(2) 0.7004(4) 0.0381(8) Uani 1 d . . H21A H 0.1626 0.3872 0.6595 0.046(11) Uiso 1 calc R . H21B H 0.0653 0.4241 0.6487 0.076(15) Uiso 1 calc R . C241 C 0.1555(3) 0.4329(2) 0.8576(4) 0.0392(8) Uani 1 d . . H24A H 0.1049 0.4527 0.8895 0.033(9) Uiso 1 calc R . H24B H 0.1989 0.4899 0.8695 0.050(11) Uiso 1 calc R . S22 S 0.25965(6) 0.16616(6) 0.89533(10) 0.0368(2) Uani 1 d . . C224 C 0.3471(2) 0.2748(3) 0.9711(4) 0.0468(9) Uani 1 d . . H22A H 0.3741 0.2824 1.0761 0.057(12) Uiso 1 calc R . H22B H 0.3985 0.2687 0.9349 0.058(12) Uiso 1 calc R . C242 C 0.3014(2) 0.3618(3) 0.9304(4) 0.0396(8) Uani 1 d . . H24C H 0.3453 0.4189 0.9878 0.065(13) Uiso 1 calc R . H24D H 0.2903 0.3622 0.8290 0.033(9) Uiso 1 calc R . S23 S 0.15307(5) 0.23685(5) 1.12626(8) 0.0288(2) Uani 1 d . . C234 C 0.2406(3) 0.3437(2) 1.2086(3) 0.0370(8) Uani 1 d . . H23A H 0.2352 0.3738 1.2985 0.037(10) Uiso 1 calc R . H23B H 0.3044 0.3263 1.2309 0.087(17) Uiso 1 calc R . C243 C 0.2237(2) 0.4127(2) 1.1048(3) 0.0352(7) Uani 1 d . . H24E H 0.1679 0.4427 1.1038 0.041(10) Uiso 1 calc R . H24F H 0.2779 0.4629 1.1397 0.035(9) Uiso 1 calc R . N24 N 0.2091(2) 0.3663(2) 0.9530(3) 0.0312(6) Uani 1 d . . C25 C 0.0580(2) 0.1112(2) 0.8445(3) 0.0303(6) Uani 1 d . . N25 N 0.0130(2) 0.0371(2) 0.8124(3) 0.0379(6) Uani 1 d . . C251 C -0.0465(3) -0.0521(3) 0.7789(5) 0.0564(11) Uani 1 d . . H25A H -0.0278(15) -0.0982(7) 0.7169(28) 0.073(15) Uiso 1 calc R . H25B H -0.1117(4) -0.0437(5) 0.7300(31) 0.063(14) Uiso 1 calc R . H25C H -0.0401(18) -0.0747(12) 0.8670(6) 0.132(25) Uiso 1 calc R . Fe22 Fe 0.17301(4) 0.17172(4) 0.66226(5) 0.03544(11) Uani 1 d . . N26 N 0.1251(2) 0.0576(2) 0.5862(3) 0.0436(7) Uani 1 d . . O26 O 0.1025(3) -0.0200(2) 0.5188(3) 0.0696(10) Uani 1 d . . N27 N 0.2335(2) 0.2277(3) 0.5804(3) 0.0509(8) Uani 1 d . . O27 O 0.2692(3) 0.2606(4) 0.5098(4) 0.0963(14) Uani 1 d . . Fe23 Fe 0.00388(3) 0.28088(3) 1.02718(5) 0.03059(10) Uani 1 d . . I2 I 0.00183(2) 0.35948(2) 1.28269(3) 0.05654(8) Uani 1 d . . N28 N -0.0764(2) 0.1818(2) 0.9691(3) 0.0417(7) Uani 1 d . . O28 O -0.1420(2) 0.1241(2) 0.9025(4) 0.0668(9) Uani 1 d . . N29 N -0.0339(2) 0.3660(2) 0.9328(3) 0.0371(6) Uani 1 d . . O29 O -0.0748(2) 0.4153(2) 0.8543(3) 0.0588(8) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe11 0.0225(2) 0.0249(2) 0.0295(2) 0.0014(2) 0.0074(2) 0.0029(2) S11 0.0379(4) 0.0370(4) 0.0284(4) 0.0013(3) 0.0053(3) 0.0043(3) C114 0.050(2) 0.048(2) 0.034(2) 0.012(2) 0.020(2) 0.005(2) C141 0.043(2) 0.033(2) 0.040(2) 0.0094(14) 0.016(2) -0.0004(15) S12 0.0316(4) 0.0285(4) 0.0339(4) 0.0053(3) 0.0102(3) 0.0054(3) C124 0.0249(15) 0.037(2) 0.036(2) 0.0029(13) 0.0059(13) 0.0059(13) C142 0.0215(14) 0.037(2) 0.039(2) -0.0005(14) 0.0098(13) 0.0012(12) S13 0.0283(4) 0.0345(4) 0.0366(4) 0.0043(3) 0.0116(3) 0.0103(3) C134 0.040(2) 0.027(2) 0.041(2) -0.0002(13) 0.0148(15) 0.0072(13) C143 0.031(2) 0.028(2) 0.032(2) -0.0046(12) 0.0084(13) 0.0018(12) N14 0.0259(12) 0.0257(12) 0.0281(12) 0.0020(10) 0.0105(10) 0.0035(10) C15 0.031(2) 0.038(2) 0.042(2) 0.0070(14) 0.0104(14) 0.0033(14) N15 0.035(2) 0.050(2) 0.057(2) 0.006(2) 0.0076(15) -0.0108(14) C151 0.058(3) 0.080(4) 0.083(4) 0.020(3) 0.003(3) -0.035(3) Fe12 0.0373(3) 0.0303(2) 0.0339(2) -0.0033(2) 0.0105(2) 0.0072(2) N16 0.049(2) 0.035(2) 0.047(2) -0.0067(13) 0.0062(15) 0.0046(14) O16 0.079(2) 0.044(2) 0.087(3) -0.014(2) -0.002(2) -0.010(2) N17 0.054(2) 0.047(2) 0.049(2) 0.0080(15) 0.026(2) 0.016(2) O17 0.086(3) 0.102(3) 0.123(3) 0.038(3) 0.077(3) 0.042(2) Fe13 0.0478(3) 0.0426(3) 0.0432(3) 0.0124(2) 0.0219(2) 0.0110(2) I1 0.04617(14) 0.05255(15) 0.04411(13) 0.00680(11) 0.02388(11) 0.00678(11) N18 0.107(3) 0.056(2) 0.070(3) 0.008(2) 0.054(3) -0.013(2) O18 0.193(5) 0.076(3) 0.119(4) 0.008(3) 0.088(4) -0.051(3) N19 0.075(3) 0.109(3) 0.044(2) 0.025(2) 0.035(2) 0.055(2) O19 0.103(3) 0.241(6) 0.058(2) 0.052(3) 0.033(2) 0.112(4) Fe21 0.0249(2) 0.0229(2) 0.0253(2) 0.0025(2) 0.0098(2) -0.0007(2) S21 0.0282(4) 0.0334(4) 0.0311(4) 0.0058(3) 0.0073(3) 0.0027(3) C214 0.044(2) 0.034(2) 0.038(2) 0.0128(14) 0.014(2) 0.0039(15) C241 0.042(2) 0.028(2) 0.049(2) 0.0137(14) 0.018(2) 0.0021(14) S22 0.0311(4) 0.0394(4) 0.0414(4) 0.0105(4) 0.0128(3) 0.0102(3) C224 0.023(2) 0.063(2) 0.052(2) 0.015(2) 0.010(2) 0.003(2) C242 0.033(2) 0.041(2) 0.045(2) 0.007(2) 0.0174(15) -0.0030(14) S23 0.0311(4) 0.0277(4) 0.0269(3) 0.0064(3) 0.0099(3) 0.0002(3) C234 0.041(2) 0.037(2) 0.026(2) -0.0001(13) 0.0087(14) -0.0093(14) C243 0.038(2) 0.0256(15) 0.037(2) -0.0028(13) 0.0130(14) -0.0051(13) N24 0.0337(14) 0.0286(13) 0.0295(13) 0.0029(10) 0.0121(11) -0.0040(11) C25 0.033(2) 0.030(2) 0.0266(14) 0.0019(12) 0.0115(12) -0.0007(12) N25 0.043(2) 0.0277(14) 0.042(2) 0.0039(12) 0.0171(13) -0.0056(12) C251 0.061(3) 0.033(2) 0.062(3) 0.006(2) 0.012(2) -0.018(2) Fe22 0.0375(3) 0.0393(3) 0.0315(2) 0.0025(2) 0.0165(2) 0.0067(2) N26 0.052(2) 0.042(2) 0.036(2) 0.0023(13) 0.0161(14) 0.0136(14) O26 0.091(2) 0.042(2) 0.056(2) -0.0083(14) 0.008(2) 0.021(2) N27 0.043(2) 0.075(2) 0.040(2) 0.014(2) 0.0212(15) 0.009(2) O27 0.072(2) 0.164(4) 0.071(2) 0.052(3) 0.039(2) -0.001(2) Fe23 0.0306(2) 0.0302(2) 0.0334(2) 0.0072(2) 0.0142(2) 0.0046(2) I2 0.0756(2) 0.0648(2) 0.04342(14) 0.01162(12) 0.03527(14) 0.02591(15) N28 0.0328(15) 0.040(2) 0.053(2) 0.0069(14) 0.0179(14) 0.0024(13) O28 0.040(2) 0.054(2) 0.093(2) -0.001(2) 0.018(2) -0.0114(14) N29 0.039(2) 0.037(2) 0.0367(15) 0.0078(12) 0.0139(12) 0.0104(12) O29 0.062(2) 0.051(2) 0.061(2) 0.0253(14) 0.0118(15) 0.0194(14) _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 Fe11 C15 1.853(3) . ? Fe11 N14 2.069(2) . ? Fe11 S13 2.2078(9) . ? Fe11 S12 2.2199(9) . ? Fe11 S11 2.2318(10) . ? Fe11 Fe12 2.6552(7) . ? Fe11 Fe13 2.8766(8) . ? S11 C114 1.828(4) . ? S11 Fe12 2.2744(10) . ? C114 C141 1.515(5) . ? C114 H11A 0.97 . ? C114 H11B 0.97 . ? C141 N14 1.496(4) . ? C141 H14A 0.97 . ? C141 H14B 0.97 . ? S12 C124 1.827(3) . ? S12 Fe12 2.2645(10) . ? C124 C142 1.508(5) . ? C124 H12A 0.97 . ? C124 H12B 0.97 . ? C142 N14 1.498(4) . ? C142 H14C 0.97 . ? C142 H14D 0.97 . ? S13 C134 1.828(3) . ? S13 Fe13 2.3025(10) . ? C134 C143 1.515(5) . ? C134 H13A 0.97 . ? C134 H13B 0.97 . ? C143 N14 1.490(4) . ? C143 H14E 0.97 . ? C143 H14F 0.97 . ? C15 N15 1.152(4) . ? N15 C151 1.431(5) . ? C151 H15A 0.96 . ? C151 H15B 0.96 . ? C151 H15C 0.96 . ? Fe12 N17 1.654(3) . ? Fe12 N16 1.667(3) . ? N16 O16 1.157(4) . ? N17 O17 1.157(4) . ? Fe13 N18 1.666(4) . ? Fe13 N19 1.671(4) . ? Fe13 I1 2.6605(7) . ? N18 O18 1.162(5) . ? N19 O19 1.156(5) . ? Fe21 C25 1.852(3) . ? Fe21 N24 2.075(3) . ? Fe21 S23 2.2014(9) . ? Fe21 S22 2.2146(10) . ? Fe21 S21 2.2174(9) . ? Fe21 Fe22 2.6639(7) . ? Fe21 Fe23 2.7591(7) . ? S21 C214 1.836(3) . ? S21 Fe22 2.2770(10) . ? C214 C241 1.493(5) . ? C214 H21A 0.97 . ? C214 H21B 0.97 . ? C241 N24 1.520(4) . ? C241 H24A 0.97 . ? C241 H24B 0.97 . ? S22 C224 1.832(4) . ? S22 Fe22 2.2558(10) . ? C224 C242 1.502(5) . ? C224 H22A 0.97 . ? C224 H22B 0.97 . ? C242 N24 1.493(4) . ? C242 H24C 0.97 . ? C242 H24D 0.97 . ? S23 C234 1.817(3) . ? S23 Fe23 2.2984(9) . ? C234 C243 1.507(5) . ? C234 H23A 0.97 . ? C234 H23B 0.97 . ? C243 N24 1.495(4) . ? C243 H24E 0.97 . ? C243 H24F 0.97 . ? C25 N25 1.148(4) . ? N25 C251 1.423(4) . ? C251 H25A 0.96 . ? C251 H25B 0.96 . ? C251 H25C 0.96 . ? Fe22 N27 1.661(3) . ? Fe22 N26 1.675(3) . ? N26 O26 1.162(4) . ? N27 O27 1.158(4) . ? Fe23 N29 1.660(3) . ? Fe23 N28 1.674(3) . ? Fe23 I2 2.6438(6) . ? N28 O28 1.164(4) . ? N29 O29 1.175(4) . ? 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 C15 Fe11 N14 176.14(13) . . ? C15 Fe11 S13 92.07(11) . . ? N14 Fe11 S13 87.06(7) . . ? C15 Fe11 S12 94.03(11) . . ? N14 Fe11 S12 89.20(7) . . ? S13 Fe11 S12 135.97(4) . . ? C15 Fe11 S11 89.94(12) . . ? N14 Fe11 S11 87.05(8) . . ? S13 Fe11 S11 115.37(4) . . ? S12 Fe11 S11 108.20(4) . . ? C15 Fe11 Fe12 84.86(11) . . ? N14 Fe11 Fe12 95.32(7) . . ? S13 Fe11 Fe12 169.44(3) . . ? S12 Fe11 Fe12 54.47(3) . . ? S11 Fe11 Fe12 54.64(3) . . ? C15 Fe11 Fe13 82.01(12) . . ? N14 Fe11 Fe13 100.35(7) . . ? S13 Fe11 Fe13 51.84(3) . . ? S12 Fe11 Fe13 85.99(3) . . ? S11 Fe11 Fe13 164.21(3) . . ? Fe12 Fe11 Fe13 137.17(2) . . ? C114 S11 Fe11 101.60(11) . . ? C114 S11 Fe12 104.86(13) . . ? Fe11 S11 Fe12 72.20(3) . . ? C141 C114 S11 109.1(2) . . ? C141 C114 H11A 109.9 . . ? S11 C114 H11A 109.85 . . ? C141 C114 H11B 109.9 . . ? S11 C114 H11B 109.85 . . ? H11A C114 H11B 108.3 . . ? N14 C141 C114 113.0(3) . . ? N14 C141 H14A 109.0 . . ? C114 C141 H14A 109.0 . . ? N14 C141 H14B 109.0 . . ? C114 C141 H14B 109.0 . . ? H14A C141 H14B 107.8 . . ? C124 S12 Fe11 98.74(11) . . ? C124 S12 Fe12 106.64(12) . . ? Fe11 S12 Fe12 72.61(3) . . ? C142 C124 S12 111.4(2) . . ? C142 C124 H12A 109.3 . . ? S12 C124 H12A 109.35 . . ? C142 C124 H12B 109.3 . . ? S12 C124 H12B 109.35 . . ? H12A C124 H12B 108.0 . . ? N14 C142 C124 112.2(3) . . ? N14 C142 H14C 109.2 . . ? C124 C142 H14C 109.2 . . ? N14 C142 H14D 109.2 . . ? C124 C142 H14D 109.2 . . ? H14C C142 H14D 107.9 . . ? C134 S13 Fe11 101.23(11) . . ? C134 S13 Fe13 102.21(12) . . ? Fe11 S13 Fe13 79.22(3) . . ? C143 C134 S13 110.1(2) . . ? C143 C134 H13A 109.6 . . ? S13 C134 H13A 109.64 . . ? C143 C134 H13B 109.6 . . ? S13 C134 H13B 109.64 . . ? H13A C134 H13B 108.2 . . ? N14 C143 C134 111.2(2) . . ? N14 C143 H14E 109.4 . . ? C134 C143 H14E 109.4 . . ? N14 C143 H14F 109.4 . . ? C134 C143 H14F 109.4 . . ? H14E C143 H14F 108.0 . . ? C143 N14 C141 107.4(2) . . ? C143 N14 C142 109.1(2) . . ? C141 N14 C142 108.4(3) . . ? C143 N14 Fe11 110.0(2) . . ? C141 N14 Fe11 110.0(2) . . ? C142 N14 Fe11 111.8(2) . . ? N15 C15 Fe11 177.1(4) . . ? C15 N15 C151 175.5(4) . . ? N15 C151 H15A 109.5 . . ? N15 C151 H15B 109.5 . . ? H15A C151 H15B 109.5 . . ? N15 C151 H15C 109.5 . . ? H15A C151 H15C 109.5 . . ? H15B C151 H15C 109.5 . . ? N17 Fe12 N16 116.8(2) . . ? N17 Fe12 S12 112.11(12) . . ? N16 Fe12 S12 106.52(13) . . ? N17 Fe12 S11 107.21(12) . . ? N16 Fe12 S11 108.29(11) . . ? S12 Fe12 S11 105.22(4) . . ? N17 Fe12 Fe11 131.67(12) . . ? N16 Fe12 Fe11 111.43(12) . . ? S12 Fe12 Fe11 52.92(3) . . ? S11 Fe12 Fe11 53.16(3) . . ? O16 N16 Fe12 167.3(4) . . ? O17 N17 Fe12 172.0(4) . . ? N18 Fe13 N19 114.6(2) . . ? N18 Fe13 S13 113.2(2) . . ? N19 Fe13 S13 127.1(2) . . ? N18 Fe13 I1 105.2(2) . . ? N19 Fe13 I1 93.64(13) . . ? S13 Fe13 I1 94.63(3) . . ? N18 Fe13 Fe11 100.45(14) . . ? N19 Fe13 Fe11 100.79(12) . . ? S13 Fe13 Fe11 48.94(2) . . ? I1 Fe13 Fe11 141.94(2) . . ? O18 N18 Fe13 166.9(5) . . ? O19 N19 Fe13 170.5(5) . . ? C25 Fe21 N24 178.50(13) . . ? C25 Fe21 S23 91.33(10) . . ? N24 Fe21 S23 88.35(8) . . ? C25 Fe21 S22 91.84(11) . . ? N24 Fe21 S22 89.66(8) . . ? S23 Fe21 S22 97.95(4) . . ? C25 Fe21 S21 91.93(10) . . ? N24 Fe21 S21 87.71(8) . . ? S23 Fe21 S21 153.85(4) . . ? S22 Fe21 S21 107.86(4) . . ? C25 Fe21 Fe22 84.46(10) . . ? N24 Fe21 Fe22 96.51(8) . . ? S23 Fe21 Fe22 151.45(3) . . ? S22 Fe21 Fe22 54.14(3) . . ? S21 Fe21 Fe22 54.69(3) . . ? C25 Fe21 Fe23 83.28(10) . . ? N24 Fe21 Fe23 95.35(8) . . ? S23 Fe21 Fe23 53.79(3) . . ? S22 Fe21 Fe23 150.97(3) . . ? S21 Fe21 Fe23 100.91(3) . . ? Fe22 Fe21 Fe23 152.20(2) . . ? C214 S21 Fe21 101.27(11) . . ? C214 S21 Fe22 104.60(13) . . ? Fe21 S21 Fe22 72.69(3) . . ? C241 C214 S21 110.9(2) . . ? C241 C214 H21A 109.5 . . ? S21 C214 H21A 109.47 . . ? C241 C214 H21B 109.5 . . ? S21 C214 H21B 109.47 . . ? H21A C214 H21B 108.1 . . ? C214 C241 N24 112.8(3) . . ? C214 C241 H24A 109.0 . . ? N24 C241 H24A 109.0 . . ? C214 C241 H24B 109.0 . . ? N24 C241 H24B 109.0 . . ? H24A C241 H24B 107.8 . . ? C224 S22 Fe21 98.60(13) . . ? C224 S22 Fe22 107.87(13) . . ? Fe21 S22 Fe22 73.15(3) . . ? C242 C224 S22 110.9(2) . . ? C242 C224 H22A 109.5 . . ? S22 C224 H22A 109.47 . . ? C242 C224 H22B 109.5 . . ? S22 C224 H22B 109.47 . . ? H22A C224 H22B 108.1 . . ? N24 C242 C224 113.5(3) . . ? N24 C242 H24C 108.9 . . ? C224 C242 H24C 108.9 . . ? N24 C242 H24D 108.9 . . ? C224 C242 H24D 108.9 . . ? H24C C242 H24D 107.7 . . ? C234 S23 Fe21 100.43(11) . . ? C234 S23 Fe23 109.49(13) . . ? Fe21 S23 Fe23 75.60(3) . . ? C243 C234 S23 109.3(2) . . ? C243 C234 H23A 109.8 . . ? S23 C234 H23A 109.81 . . ? C243 C234 H23B 109.8 . . ? S23 C234 H23B 109.81 . . ? H23A C234 H23B 108.3 . . ? N24 C243 C234 113.4(3) . . ? N24 C243 H24E 108.9 . . ? C234 C243 H24E 108.9 . . ? N24 C243 H24F 108.9 . . ? C234 C243 H24F 108.9 . . ? H24E C243 H24F 107.7 . . ? C242 N24 C243 111.9(3) . . ? C242 N24 C241 106.6(3) . . ? C243 N24 C241 105.2(3) . . ? C242 N24 Fe21 110.7(2) . . ? C243 N24 Fe21 111.6(2) . . ? C241 N24 Fe21 110.6(2) . . ? N25 C25 Fe21 179.7(3) . . ? C25 N25 C251 175.9(4) . . ? N25 C251 H25A 109.5 . . ? N25 C251 H25B 109.5 . . ? H25A C251 H25B 109.5 . . ? N25 C251 H25C 109.5 . . ? H25A C251 H25C 109.5 . . ? H25B C251 H25C 109.5 . . ? N27 Fe22 N26 116.8(2) . . ? N27 Fe22 S22 113.80(12) . . ? N26 Fe22 S22 104.35(11) . . ? N27 Fe22 S21 106.13(13) . . ? N26 Fe22 S21 110.75(11) . . ? S22 Fe22 S21 104.43(4) . . ? N27 Fe22 Fe21 131.93(13) . . ? N26 Fe22 Fe21 111.26(11) . . ? S22 Fe22 Fe21 52.72(3) . . ? S21 Fe22 Fe21 52.62(3) . . ? O26 N26 Fe22 167.5(3) . . ? O27 N27 Fe22 172.7(4) . . ? N29 Fe23 N28 111.82(15) . . ? N29 Fe23 S23 131.61(11) . . ? N28 Fe23 S23 108.33(11) . . ? N29 Fe23 I2 100.51(10) . . ? N28 Fe23 I2 105.76(11) . . ? S23 Fe23 I2 93.40(3) . . ? N29 Fe23 Fe21 95.03(10) . . ? N28 Fe23 Fe21 101.63(11) . . ? S23 Fe23 Fe21 50.61(2) . . ? I2 Fe23 Fe21 140.48(2) . . ? O28 N28 Fe23 164.0(3) . . ? O29 N29 Fe23 168.4(3) . . ? 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 Fe11 S11 C114 C141 -20.1(3) . . . . ? S11 C114 C141 N14 44.9(4) . . . . ? C114 C141 N14 Fe11 -48.7(3) . . . . ? Fe11 S12 C124 C142 -30.1(2) . . . . ? S12 C124 C142 N14 46.3(3) . . . . ? C124 C142 N14 Fe11 -38.6(3) . . . . ? Fe11 S13 C134 C143 -19.1(3) . . . . ? S13 C134 C143 N14 44.9(3) . . . . ? C134 C143 N14 Fe11 -50.1(3) . . . . ? Fe21 S21 C214 C241 -20.4(3) . . . . ? S21 C214 C241 N24 42.7(4) . . . . ? C214 C241 N24 Fe21 -44.9(3) . . . . ? Fe21 S22 C224 C242 -30.0(3) . . . . ? S22 C224 C242 N24 46.8(4) . . . . ? C224 C242 N24 Fe21 -38.7(4) . . . . ? Fe21 S23 C234 C243 31.6(3) . . . . ? S23 C234 C243 N24 -46.6(4) . . . . ? C234 C243 N24 Fe21 37.9(3) . . . . ? Fe11 S13 Fe13 I1 167.73(3) . . . . ? Fe21 S23 Fe23 I2 -162.00(2) . . . . ? _refine_diff_density_max 1.164 _refine_diff_density_min -1.136 _refine_diff_density_rms 0.117 #===END data_roger53 _symmetry_Int_Tables_number 178006 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 14' _chemical_formula_moiety 'C6 H12 Fe3 I N6 O5 S3' _chemical_formula_structural '[{Fe(NO)2}{Fe(NS3)(NO)}{FeI(NO)2}]' _chemical_formula_analytical ? _chemical_formula_sum 'C6 H12 Fe3 I N6 O5 S3' _chemical_formula_weight 638.85 _chemical_melting_point ? _chemical_compound_source ? 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' 'I' 'I' -0.4742 1.8119 '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' 'S' 'S' 0.1246 0.1234 '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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6016(9) _cell_length_b 9.6695(15) _cell_length_c 12.678(2) _cell_angle_alpha 108.594(13) _cell_angle_beta 98.556(12) _cell_angle_gamma 101.865(11) _cell_volume 951.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 8 _cell_measurement_theta_max 10 _exptl_crystal_description 'square plates' _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.230 _exptl_crystal_density_method ? _exptl_crystal_F_000 618 _exptl_absorpt_coefficient_mu 4.236 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.820 _exptl_absorpt_correction_T_max 0.998 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 0 _diffrn_reflns_number 3714 _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_av_sigmaI/netI 0.0785 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 25.0 _reflns_number_total 3332 _reflns_number_observed 1920 _reflns_observed_criterion I>2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_data_reduction 'CAD4 (Hursthouse, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=[\s^-2^(Fo^2^)]' _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 3332 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0853 _refine_ls_R_factor_obs 0.0400 _refine_ls_wR_factor_all 0.0843 _refine_ls_wR_factor_obs 0.0662 _refine_ls_goodness_of_fit_all 0.991 _refine_ls_goodness_of_fit_obs 1.051 _refine_ls_restrained_S_all 0.991 _refine_ls_restrained_S_obs 1.051 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.24434(12) 0.49206(11) 0.30792(8) 0.0372(3) Uani 1 d . . S1 S 0.4652(2) 0.6854(2) 0.4230(2) 0.0467(5) Uani 1 d . . C14 C 0.6263(8) 0.6264(8) 0.3567(6) 0.049(2) Uani 1 d . . H14A H 0.6537 0.6834 0.3083 0.059 Uiso 0.741(12) calc PR 1 H14B H 0.7233 0.6478 0.4155 0.059 Uiso 0.741(12) calc PR 1 H14C H 0.7124 0.7155 0.3675 0.059 Uiso 0.259(12) calc PR 2 H14D H 0.6726 0.5660 0.3941 0.059 Uiso 0.259(12) calc PR 2 C41A C 0.5713(12) 0.4578(12) 0.2854(9) 0.054(3) Uani 0.741(12) d P 1 H41A H 0.6494 0.4329 0.2396 0.064 Uiso 0.741(12) calc PR 1 H41B H 0.5708 0.4011 0.3363 0.064 Uiso 0.741(12) calc PR 1 C41B C 0.5638(31) 0.5350(30) 0.2302(22) 0.037(8) Uiso 0.259(12) d P 2 H41C H 0.6466 0.4897 0.2009 0.044 Uiso 0.259(12) calc PR 2 H41D H 0.5411 0.6012 0.1898 0.044 Uiso 0.259(12) calc PR 2 S2 S 0.1429(2) 0.5636(2) 0.1657(2) 0.0450(5) Uani 1 d . . C24 C 0.2482(10) 0.4753(9) 0.0599(6) 0.052(2) Uani 1 d . . H24A H 0.1803 0.3744 0.0124 0.063 Uiso 0.741(12) calc PR 1 H24B H 0.2638 0.5337 0.0109 0.063 Uiso 0.741(12) calc PR 1 H24C H 0.1705 0.4249 -0.0135 0.063 Uiso 0.259(12) calc PR 2 H24D H 0.3312 0.5541 0.0524 0.063 Uiso 0.259(12) calc PR 2 C42A C 0.4071(13) 0.4639(13) 0.1109(8) 0.047(3) Uani 0.741(12) d P 1 H42A H 0.4849 0.5628 0.1368 0.057 Uiso 0.741(12) calc PR 1 H42B H 0.4441 0.3951 0.0522 0.057 Uiso 0.741(12) calc PR 1 C42B C 0.3314(42) 0.3572(40) 0.0875(26) 0.056(9) Uiso 0.259(12) d P 2 H42C H 0.2502 0.2611 0.0658 0.067 Uiso 0.259(12) calc PR 2 H42D H 0.4133 0.3414 0.0434 0.067 Uiso 0.259(12) calc PR 2 S3 S 0.1939(2) 0.2668(2) 0.3326(2) 0.0425(5) Uani 1 d . . C34 C 0.3176(9) 0.1712(8) 0.2457(6) 0.049(2) Uani 1 d . . H34A H 0.4203 0.1801 0.2944 0.059 Uiso 0.741(12) calc PR 1 H34B H 0.2611 0.0643 0.2082 0.059 Uiso 0.741(12) calc PR 1 H34C H 0.3579 0.1042 0.2790 0.059 Uiso 0.259(12) calc PR 2 H34D H 0.2516 0.1104 0.1693 0.059 Uiso 0.259(12) calc PR 2 C43A C 0.3500(14) 0.2372(11) 0.1589(9) 0.053(3) Uani 0.741(12) d P 1 H43A H 0.2511 0.2059 0.0995 0.064 Uiso 0.741(12) calc PR 1 H43B H 0.4327 0.1983 0.1240 0.064 Uiso 0.741(12) calc PR 1 C43B C 0.4561(38) 0.2842(33) 0.2394(28) 0.052(9) Uiso 0.259(12) d P 2 H43C H 0.5099 0.2334 0.1826 0.062 Uiso 0.259(12) calc PR 2 H43D H 0.5343 0.3275 0.3127 0.062 Uiso 0.259(12) calc PR 2 N4 N 0.4079(7) 0.4103(6) 0.2092(4) 0.0372(14) Uani 1 d . . N5 N 0.0965(9) 0.5482(8) 0.3828(6) 0.061(2) Uani 1 d . . O5 O -0.0119(8) 0.5803(8) 0.4130(6) 0.090(2) Uani 1 d . . Fe2 Fe 0.32897(14) 0.77206(12) 0.30000(9) 0.0481(3) Uani 1 d . . N6 N 0.2294(9) 0.8804(8) 0.3770(6) 0.060(2) Uani 1 d . . O6 O 0.1735(9) 0.9745(7) 0.4274(6) 0.091(2) Uani 1 d . . N7 N 0.4553(8) 0.8414(8) 0.2323(6) 0.062(2) Uani 1 d . . O7 O 0.5375(7) 0.8946(7) 0.1823(6) 0.084(2) Uani 1 d . . Fe3 Fe -0.07276(13) 0.13866(12) 0.23186(9) 0.0472(3) Uani 1 d . . I1 I -0.18157(7) 0.18407(7) 0.04885(5) 0.0629(2) Uani 1 d . . N8 N -0.1848(8) 0.1913(7) 0.3265(5) 0.054(2) Uani 1 d . . O8 O -0.2716(7) 0.1881(7) 0.3881(5) 0.082(2) Uani 1 d . . N9 N -0.0844(8) -0.0476(8) 0.1973(6) 0.061(2) Uani 1 d . . O9 O -0.1135(9) -0.1721(7) 0.1903(6) 0.093(2) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0350(6) 0.0404(6) 0.0391(6) 0.0156(5) 0.0080(5) 0.0146(5) S1 0.0416(12) 0.0541(12) 0.0403(11) 0.0104(9) 0.0050(9) 0.0178(10) C14 0.032(4) 0.066(5) 0.044(4) 0.014(4) 0.004(3) 0.015(4) C41A 0.035(6) 0.064(8) 0.061(7) 0.021(6) 0.009(5) 0.015(6) S2 0.0420(11) 0.0478(12) 0.0459(11) 0.0203(9) 0.0017(9) 0.0143(9) C24 0.067(6) 0.058(5) 0.032(4) 0.017(4) 0.008(4) 0.018(4) C42A 0.048(7) 0.056(8) 0.044(6) 0.014(5) 0.022(5) 0.025(6) S3 0.0434(11) 0.0465(11) 0.0424(11) 0.0182(9) 0.0126(9) 0.0169(9) C34 0.050(5) 0.047(5) 0.064(5) 0.027(4) 0.022(4) 0.025(4) C43A 0.061(8) 0.047(7) 0.059(7) 0.013(6) 0.025(6) 0.033(6) N4 0.042(4) 0.043(4) 0.032(3) 0.012(3) 0.014(3) 0.023(3) N5 0.052(5) 0.066(5) 0.069(5) 0.035(4) 0.006(4) 0.011(4) O5 0.059(4) 0.106(5) 0.111(6) 0.023(4) 0.052(4) 0.037(4) Fe2 0.0476(7) 0.0426(7) 0.0541(7) 0.0167(5) 0.0090(5) 0.0154(5) N6 0.073(5) 0.056(5) 0.064(5) 0.029(4) 0.019(4) 0.033(4) O6 0.120(6) 0.080(5) 0.097(5) 0.032(4) 0.045(5) 0.065(5) N7 0.052(5) 0.066(5) 0.064(5) 0.027(4) 0.010(4) 0.006(4) O7 0.061(4) 0.089(5) 0.092(5) 0.036(4) 0.014(4) -0.001(4) Fe3 0.0462(7) 0.0512(7) 0.0415(6) 0.0099(5) 0.0105(5) 0.0181(6) I1 0.0668(4) 0.0633(4) 0.0480(3) 0.0167(3) -0.0012(3) 0.0111(3) N8 0.059(5) 0.064(4) 0.040(4) 0.014(3) 0.013(3) 0.027(4) O8 0.069(4) 0.121(6) 0.053(4) 0.017(4) 0.028(3) 0.038(4) N9 0.051(4) 0.065(5) 0.056(4) 0.013(4) 0.007(3) 0.015(4) O9 0.105(6) 0.047(4) 0.116(6) 0.019(4) 0.010(4) 0.028(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 Fe1 N5 1.768(8) . ? Fe1 N4 2.126(5) . ? Fe1 S2 2.251(2) . ? Fe1 S3 2.263(2) . ? Fe1 S1 2.282(2) . ? Fe1 Fe2 2.693(2) . ? S1 C14 1.822(7) . ? S1 Fe2 2.280(2) . ? C14 C41B 1.51(2) . ? C14 C41A 1.522(12) . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? C14 H14C 0.97 . ? C14 H14D 0.97 . ? C41A N4 1.472(11) . ? C41A H41A 0.97 . ? C41A H41B 0.97 . ? C41B N4 1.53(3) . ? C41B H41C 0.97 . ? C41B H41D 0.97 . ? S2 C24 1.817(7) . ? S2 Fe2 2.280(2) . ? C24 C42A 1.463(12) . ? C24 C42B 1.57(3) . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C24 H24C 0.97 . ? C24 H24D 0.97 . ? C42A N4 1.495(11) . ? C42A H42A 0.97 . ? C42A H42B 0.97 . ? C42B N4 1.46(3) . ? C42B H42C 0.97 . ? C42B H42D 0.97 . ? S3 C34 1.818(7) . ? S3 Fe3 2.319(2) . ? C34 C43A 1.470(12) . ? C34 C43B 1.47(3) . ? C34 H34A 0.97 . ? C34 H34B 0.97 . ? C34 H34C 0.97 . ? C34 H34D 0.97 . ? C43A N4 1.529(11) . ? C43A H43A 0.97 . ? C43A H43B 0.97 . ? C43B N4 1.50(3) . ? C43B H43C 0.97 . ? C43B H43D 0.97 . ? N5 O5 1.123(8) . ? Fe2 N7 1.647(7) . ? Fe2 N6 1.658(7) . ? N6 O6 1.169(8) . ? N7 O7 1.166(8) . ? Fe3 N8 1.669(7) . ? Fe3 N9 1.690(8) . ? Fe3 I1 2.5739(13) . ? N8 O8 1.161(7) . ? N9 O9 1.149(8) . ? 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 N5 Fe1 N4 175.7(3) . . ? N5 Fe1 S2 90.9(2) . . ? N4 Fe1 S2 87.9(2) . . ? N5 Fe1 S3 91.9(2) . . ? N4 Fe1 S3 85.9(2) . . ? S2 Fe1 S3 132.18(8) . . ? N5 Fe1 S1 97.8(2) . . ? N4 Fe1 S1 86.5(2) . . ? S2 Fe1 S1 106.72(8) . . ? S3 Fe1 S1 120.10(8) . . ? N5 Fe1 Fe2 88.2(2) . . ? N4 Fe1 Fe2 94.5(2) . . ? S2 Fe1 Fe2 54.03(6) . . ? S3 Fe1 Fe2 173.79(7) . . ? S1 Fe1 Fe2 53.78(6) . . ? C14 S1 Fe2 104.7(3) . . ? C14 S1 Fe1 100.2(2) . . ? Fe2 S1 Fe1 72.37(7) . . ? C41B C14 S1 112.0(11) . . ? C41A C14 S1 110.5(6) . . ? C41A C14 H14A 109.6 . . ? S1 C14 H14A 109.6 . . ? C41A C14 H14B 109.6 . . ? S1 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? C41B C14 H14C 109.2 . . ? S1 C14 H14C 109.2 . . ? C41B C14 H14D 109.2 . . ? S1 C14 H14D 109.2 . . ? H14C C14 H14D 107.9 . . ? N4 C41A C14 113.1(8) . . ? N4 C41A H41A 109.0 . . ? C14 C41A H41A 109.0 . . ? N4 C41A H41B 109.0 . . ? C14 C41A H41B 109.0 . . ? H41A C41A H41B 107.8 . . ? C14 C41B N4 110.3(17) . . ? C14 C41B H41C 109.6 . . ? N4 C41B H41C 109.6 . . ? C14 C41B H41D 109.6 . . ? N4 C41B H41D 109.6 . . ? H41C C41B H41D 108.1 . . ? C24 S2 Fe1 98.9(2) . . ? C24 S2 Fe2 107.3(3) . . ? Fe1 S2 Fe2 72.95(7) . . ? C42A C24 S2 113.0(6) . . ? C42B C24 S2 114.8(12) . . ? C42A C24 H24A 109.0 . . ? S2 C24 H24A 109.0 . . ? C42A C24 H24B 109.0 . . ? S2 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C42B C24 H24C 108.6 . . ? S2 C24 H24C 108.6 . . ? C42B C24 H24D 108.6 . . ? S2 C24 H24D 108.6 . . ? H24C C24 H24D 107.5 . . ? C24 C42A N4 114.8(8) . . ? C24 C42A H42A 108.6 . . ? N4 C42A H42A 108.6 . . ? C24 C42A H42B 108.6 . . ? N4 C42A H42B 108.6 . . ? H42A C42A H42B 107.6 . . ? N4 C42B C24 110.8(21) . . ? N4 C42B H42C 109.5 . . ? C24 C42B H42C 109.5 . . ? N4 C42B H42D 109.5 . . ? C24 C42B H42D 109.5 . . ? H42C C42B H42D 108.1 . . ? C34 S3 Fe1 101.3(2) . . ? C34 S3 Fe3 104.3(3) . . ? Fe1 S3 Fe3 105.65(8) . . ? C43A C34 S3 110.9(6) . . ? C43B C34 S3 109.7(12) . . ? C43A C34 H34A 109.5 . . ? S3 C34 H34A 109.5 . . ? C43A C34 H34B 109.5 . . ? S3 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C43B C34 H34C 109.7 . . ? S3 C34 H34C 109.7 . . ? C43B C34 H34D 109.7 . . ? S3 C34 H34D 109.7 . . ? H34C C34 H34D 108.2 . . ? C34 C43A N4 112.4(8) . . ? C34 C43A H43A 109.1 . . ? N4 C43A H43A 109.1 . . ? C34 C43A H43B 109.1 . . ? N4 C43A H43B 109.1 . . ? H43A C43A H43B 107.9 . . ? C34 C43B N4 113.7(21) . . ? C34 C43B H43C 108.8 . . ? N4 C43B H43C 108.8 . . ? C34 C43B H43D 108.8 . . ? N4 C43B H43D 108.8 . . ? H43C C43B H43D 107.7 . . ? C41A N4 C42A 112.4(7) . . ? C42B N4 C43B 110.3(18) . . ? C41A N4 C43A 109.2(7) . . ? C42A N4 C43A 107.1(7) . . ? C42B N4 C41B 106.5(17) . . ? C43B N4 C41B 108.1(16) . . ? C42B N4 Fe1 109.9(13) . . ? C41A N4 Fe1 108.4(5) . . ? C42A N4 Fe1 111.0(5) . . ? C43B N4 Fe1 110.1(12) . . ? C43A N4 Fe1 108.6(5) . . ? C41B N4 Fe1 111.8(10) . . ? O5 N5 Fe1 168.5(7) . . ? N7 Fe2 N6 120.2(3) . . ? N7 Fe2 S2 106.6(2) . . ? N6 Fe2 S2 108.5(3) . . ? N7 Fe2 S1 109.7(2) . . ? N6 Fe2 S1 105.2(2) . . ? S2 Fe2 S1 105.80(8) . . ? N7 Fe2 Fe1 130.1(3) . . ? N6 Fe2 Fe1 109.7(2) . . ? S2 Fe2 Fe1 53.02(6) . . ? S1 Fe2 Fe1 53.84(6) . . ? O6 N6 Fe2 169.6(7) . . ? O7 N7 Fe2 175.8(7) . . ? N8 Fe3 N9 110.3(3) . . ? N8 Fe3 S3 104.2(2) . . ? N9 Fe3 S3 105.9(2) . . ? N8 Fe3 I1 109.5(2) . . ? N9 Fe3 I1 108.6(2) . . ? S3 Fe3 I1 118.29(7) . . ? O8 N8 Fe3 162.1(7) . . ? O9 N9 Fe3 165.2(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 Fe1 S1 C14 C41A -20.2(6) . . . . ? S1 C14 C41A N4 47.8(10) . . . . ? C14 C41A N4 Fe1 -51.1(9) . . . . ? Fe1 S2 C24 C42A -29.7(7) . . . . ? S2 C24 C42A N4 44.5(10) . . . . ? C24 C42A N4 Fe1 -35.1(10) . . . . ? Fe1 S3 C34 C43A -22.3(7) . . . . ? S3 C34 C43A N4 47.8(9) . . . . ? C34 C43A N4 Fe1 -49.9(9) . . . . ? Fe1 S1 C14 C41B 29.1(13) . . . . ? S1 C14 C41B N4 -48.5(20) . . . . ? C14 C41B N4 Fe1 44.1(20) . . . . ? Fe1 S2 C24 C42B 13.4(16) . . . . ? S2 C24 C42B N4 -40.0(27) . . . . ? C24 C42B N4 Fe1 46.6(25) . . . . ? Fe1 S3 C34 C43B 27.2(15) . . . . ? S3 C34 C43B N4 -48.8(23) . . . . ? C34 C43B N4 Fe1 45.9(23) . . . . ? Fe1 S3 Fe3 I1 32.52(10) . . . . ? _refine_diff_density_max 0.512 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.114 #===END