# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_jmk193_3_rt _database_code_depnum_ccdc_archive 'CCDC 748038' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; (Fe C26 H16 N10 S4) ; _chemical_formula_sum 'C26 H16 Fe N10 S4' _chemical_formula_weight 652.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.937(5) _cell_length_b 8.0205(16) _cell_length_c 16.694(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.18(3) _cell_angle_gamma 90.00 _cell_volume 2882.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6599 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.850 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8157 _exptl_absorpt_correction_T_max 0.9508 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-Axis SPIDER' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48179 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6599 _reflns_number_gt 3851 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.9415P] 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 6599 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1022 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.0000 1.0000 0.5000 0.04377(15) Uani 1 2 d S . . N1 N 0.01292(10) 0.8056(3) 0.41325(13) 0.0465(6) Uani 1 1 d . . . N2 N 0.07103(10) 1.1008(3) 0.45335(14) 0.0441(5) Uani 1 1 d . . . N3 N 0.10304(10) 1.2492(3) 0.46964(14) 0.0459(6) Uani 1 1 d . . . N4 N 0.21522(13) 1.3897(3) 0.37993(16) 0.0683(8) Uani 1 1 d . . . S1 S 0.14380(3) 1.08440(10) 0.36831(5) 0.0518(2) Uani 1 1 d . . . C1 C -0.01650(14) 0.6583(4) 0.39491(19) 0.0576(8) Uani 1 1 d . . . H1 H -0.0471 0.6343 0.4179 0.069 Uiso 1 1 calc R . . C2 C -0.00302(15) 0.5407(4) 0.3430(2) 0.0595(8) Uani 1 1 d . . . H2 H -0.0243 0.4398 0.3318 0.071 Uiso 1 1 calc R . . C3 C 0.04181(14) 0.5743(4) 0.30849(19) 0.0582(8) Uani 1 1 d . . . H3 H 0.0513 0.4972 0.2733 0.070 Uiso 1 1 calc R . . C4 C 0.07278(13) 0.7257(4) 0.32703(17) 0.0500(7) Uani 1 1 d . . . H4 H 0.1037 0.7513 0.3047 0.060 Uiso 1 1 calc R . . C5 C 0.05721(12) 0.8375(3) 0.37894(16) 0.0416(6) Uani 1 1 d . . . C6 C 0.08730(12) 1.0019(3) 0.40265(16) 0.0416(6) Uani 1 1 d . . . C7 C 0.14263(12) 1.2569(3) 0.42917(15) 0.0416(6) Uani 1 1 d . . . C8 C 0.18481(12) 1.3982(3) 0.43480(17) 0.0454(7) Uani 1 1 d . . . C9 C 0.19243(14) 1.5244(4) 0.49340(19) 0.0587(8) Uani 1 1 d . . . H9 H 0.1702 1.5252 0.5307 0.070 Uiso 1 1 calc R . . C10 C 0.23421(16) 1.6504(4) 0.4951(2) 0.0714(9) Uani 1 1 d . . . H10 H 0.2409 1.7377 0.5340 0.086 Uiso 1 1 calc R . . C11 C 0.26536(18) 1.6442(5) 0.4389(2) 0.0848(12) Uani 1 1 d . . . H11 H 0.2934 1.7277 0.4384 0.102 Uiso 1 1 calc R . . C12 C 0.25473(18) 1.5135(5) 0.3831(2) 0.0893(13) Uani 1 1 d . . . H12 H 0.2763 1.5107 0.3451 0.107 Uiso 1 1 calc R . . N51 N -0.06971(12) 1.1173(3) 0.39965(16) 0.0628(7) Uani 1 1 d . . . C51 C -0.10941(13) 1.2062(4) 0.36256(18) 0.0469(7) Uani 1 1 d . . . S51 S -0.16446(4) 1.33083(13) 0.31094(6) 0.0756(3) Uani 1 1 d . . . Fe2 Fe 0.5000 0.0000 0.0000 0.04599(16) Uani 1 2 d S . . N21 N 0.49896(10) 0.2283(3) -0.07420(14) 0.0477(6) Uani 1 1 d . . . N22 N 0.43178(10) 0.1617(3) 0.02661(14) 0.0475(6) Uani 1 1 d . . . N23 N 0.39578(11) 0.1411(3) 0.07690(14) 0.0512(6) Uani 1 1 d . . . N24 N 0.26791(11) 0.3994(3) 0.07861(14) 0.0529(6) Uani 1 1 d . . . S21 S 0.35554(4) 0.40308(9) -0.01346(5) 0.0532(2) Uani 1 1 d . . . C21 C 0.53473(14) 0.2637(4) -0.12027(18) 0.0560(8) Uani 1 1 d . . . H21 H 0.5668 0.1909 -0.1181 0.067 Uiso 1 1 calc R . . C22 C 0.52621(16) 0.4040(4) -0.17117(19) 0.0626(8) Uani 1 1 d . . . H22 H 0.5519 0.4248 -0.2026 0.075 Uiso 1 1 calc R . . C23 C 0.47923(17) 0.5118(4) -0.1744(2) 0.0712(10) Uani 1 1 d . . . H23 H 0.4726 0.6071 -0.2081 0.085 Uiso 1 1 calc R . . C24 C 0.44179(15) 0.4775(4) -0.1270(2) 0.0618(8) Uani 1 1 d . . . H24 H 0.4096 0.5491 -0.1284 0.074 Uiso 1 1 calc R . . C25 C 0.45284(13) 0.3361(3) -0.07772(16) 0.0440(6) Uani 1 1 d . . . C26 C 0.41684(12) 0.2930(3) -0.02278(16) 0.0443(6) Uani 1 1 d . . . C27 C 0.35406(13) 0.2590(3) 0.06276(17) 0.0467(7) Uani 1 1 d . . . C28 C 0.30876(13) 0.2748(4) 0.10710(17) 0.0483(7) Uani 1 1 d . . . C29 C 0.30972(15) 0.1673(4) 0.17214(19) 0.0643(8) Uani 1 1 d . . . H29 H 0.3392 0.0828 0.1899 0.077 Uiso 1 1 calc R . . C30 C 0.26538(17) 0.1899(5) 0.2099(2) 0.0761(10) Uani 1 1 d . . . H30 H 0.2645 0.1205 0.2542 0.091 Uiso 1 1 calc R . . C31 C 0.22254(16) 0.3157(5) 0.1816(2) 0.0725(10) Uani 1 1 d . . . H31 H 0.1921 0.3326 0.2058 0.087 Uiso 1 1 calc R . . C32 C 0.22568(15) 0.4159(4) 0.1166(2) 0.0654(9) Uani 1 1 d . . . H32 H 0.1965 0.5007 0.0978 0.079 Uiso 1 1 calc R . . N61 N 0.57130(13) 0.0900(3) 0.10669(17) 0.0611(7) Uani 1 1 d . . . C61 C 0.60906(13) 0.1355(3) 0.16928(19) 0.0464(7) Uani 1 1 d . . . S61 S 0.66092(4) 0.20344(13) 0.25503(6) 0.0752(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0413(3) 0.0498(3) 0.0469(3) 0.0058(3) 0.0239(3) -0.0027(3) N1 0.0420(13) 0.0517(15) 0.0508(14) 0.0028(11) 0.0225(11) -0.0080(11) N2 0.0427(13) 0.0462(14) 0.0507(14) 0.0024(11) 0.0253(11) -0.0061(11) N3 0.0472(13) 0.0464(14) 0.0511(14) 0.0014(11) 0.0257(11) -0.0042(11) N4 0.0824(19) 0.0705(19) 0.0714(17) -0.0157(14) 0.0511(16) -0.0356(15) S1 0.0549(5) 0.0577(5) 0.0542(4) -0.0085(4) 0.0334(4) -0.0169(4) C1 0.0572(19) 0.059(2) 0.0634(19) 0.0011(16) 0.0292(16) -0.0176(16) C2 0.062(2) 0.052(2) 0.065(2) -0.0072(16) 0.0230(17) -0.0174(15) C3 0.063(2) 0.056(2) 0.0575(19) -0.0076(15) 0.0235(16) -0.0063(16) C4 0.0483(17) 0.0571(19) 0.0489(17) 0.0016(14) 0.0223(14) -0.0080(14) C5 0.0386(15) 0.0483(17) 0.0384(15) 0.0035(12) 0.0138(12) -0.0031(12) C6 0.0403(15) 0.0487(16) 0.0389(14) 0.0059(13) 0.0177(12) -0.0041(13) C7 0.0414(15) 0.0477(17) 0.0386(15) 0.0032(12) 0.0177(12) -0.0033(12) C8 0.0457(16) 0.0501(18) 0.0429(15) 0.0017(13) 0.0184(13) -0.0077(13) C9 0.062(2) 0.061(2) 0.0544(18) -0.0027(15) 0.0220(16) -0.0050(16) C10 0.075(2) 0.057(2) 0.079(2) -0.0147(18) 0.022(2) -0.0180(18) C11 0.093(3) 0.076(3) 0.092(3) -0.010(2) 0.040(2) -0.045(2) C12 0.109(3) 0.093(3) 0.090(3) -0.024(2) 0.065(2) -0.055(2) N51 0.0549(17) 0.076(2) 0.0624(17) 0.0140(14) 0.0258(14) 0.0021(15) C51 0.0452(17) 0.0568(19) 0.0468(17) -0.0017(14) 0.0263(14) -0.0093(14) S51 0.0663(6) 0.0941(7) 0.0761(6) 0.0237(5) 0.0370(5) 0.0294(5) Fe2 0.0499(3) 0.0358(3) 0.0533(3) 0.0038(3) 0.0192(3) 0.0110(3) N21 0.0518(14) 0.0381(13) 0.0564(14) 0.0012(11) 0.0230(12) 0.0066(11) N22 0.0534(14) 0.0400(13) 0.0535(14) 0.0040(11) 0.0240(12) 0.0093(11) N23 0.0576(15) 0.0435(14) 0.0578(15) 0.0066(11) 0.0269(13) 0.0101(12) N24 0.0469(14) 0.0582(16) 0.0534(15) -0.0095(12) 0.0169(12) 0.0070(12) S21 0.0557(5) 0.0469(4) 0.0603(5) 0.0081(4) 0.0242(4) 0.0177(4) C21 0.0591(19) 0.0509(19) 0.063(2) -0.0004(15) 0.0277(16) 0.0075(15) C22 0.079(2) 0.058(2) 0.062(2) 0.0058(16) 0.0385(18) 0.0033(18) C23 0.099(3) 0.054(2) 0.073(2) 0.0209(17) 0.045(2) 0.0166(19) C24 0.074(2) 0.0496(19) 0.068(2) 0.0160(16) 0.0329(18) 0.0193(16) C25 0.0515(17) 0.0364(16) 0.0430(15) 0.0011(12) 0.0147(13) 0.0087(13) C26 0.0500(17) 0.0366(16) 0.0464(16) -0.0003(12) 0.0166(13) 0.0087(13) C27 0.0495(17) 0.0430(17) 0.0473(16) -0.0031(13) 0.0162(14) 0.0038(13) C28 0.0477(17) 0.0490(18) 0.0482(17) -0.0083(14) 0.0167(14) -0.0017(14) C29 0.067(2) 0.065(2) 0.064(2) 0.0067(17) 0.0267(18) 0.0003(17) C30 0.082(3) 0.089(3) 0.065(2) -0.002(2) 0.036(2) -0.020(2) C31 0.063(2) 0.096(3) 0.071(2) -0.023(2) 0.0381(19) -0.015(2) C32 0.053(2) 0.077(2) 0.067(2) -0.0213(19) 0.0223(17) 0.0047(17) N61 0.0646(18) 0.0501(16) 0.0643(17) -0.0025(13) 0.0167(14) 0.0086(13) C61 0.0447(17) 0.0391(17) 0.0588(19) 0.0033(14) 0.0223(15) 0.0106(13) S61 0.0555(5) 0.0863(7) 0.0703(6) -0.0117(5) 0.0042(4) 0.0159(5) _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 N51 2.098(3) . ? Fe1 N51 2.098(3) 3_576 ? Fe1 N2 2.188(2) . ? Fe1 N2 2.188(2) 3_576 ? Fe1 N1 2.216(2) . ? Fe1 N1 2.216(2) 3_576 ? N1 C1 1.342(3) . ? N1 C5 1.352(3) . ? N2 C6 1.305(3) . ? N2 N3 1.376(3) . ? N3 C7 1.307(3) . ? N4 C8 1.331(3) . ? N4 C12 1.333(4) . ? S1 C6 1.720(2) . ? S1 C7 1.722(3) . ? C1 C2 1.386(4) . ? C2 C3 1.368(4) . ? C3 C4 1.386(4) . ? C4 C5 1.377(4) . ? C5 C6 1.477(4) . ? C7 C8 1.472(4) . ? C8 C9 1.377(4) . ? C9 C10 1.386(4) . ? C10 C11 1.363(5) . ? C11 C12 1.368(5) . ? N51 C51 1.154(3) . ? C51 S51 1.608(3) . ? Fe2 N61 2.088(3) . ? Fe2 N61 2.088(3) 3_655 ? Fe2 N22 2.192(2) . ? Fe2 N22 2.192(2) 3_655 ? Fe2 N21 2.206(2) . ? Fe2 N21 2.206(2) 3_655 ? N21 C21 1.334(3) . ? N21 C25 1.352(3) . ? N22 C26 1.308(3) . ? N22 N23 1.376(3) . ? N23 C27 1.308(3) . ? N24 C32 1.335(4) . ? N24 C28 1.340(3) . ? S21 C26 1.712(3) . ? S21 C27 1.728(3) . ? C21 C22 1.383(4) . ? C22 C23 1.368(4) . ? C23 C24 1.381(4) . ? C24 C25 1.372(4) . ? C25 C26 1.472(4) . ? C27 C28 1.474(4) . ? C28 C29 1.381(4) . ? C29 C30 1.381(4) . ? C30 C31 1.374(5) . ? C31 C32 1.371(5) . ? N61 C61 1.162(3) . ? C61 S61 1.608(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 N51 Fe1 N51 179.997(1) . 3_576 ? N51 Fe1 N2 90.35(9) . . ? N51 Fe1 N2 89.65(9) 3_576 . ? N51 Fe1 N2 89.65(9) . 3_576 ? N51 Fe1 N2 90.35(9) 3_576 3_576 ? N2 Fe1 N2 180.00(6) . 3_576 ? N51 Fe1 N1 91.75(10) . . ? N51 Fe1 N1 88.25(10) 3_576 . ? N2 Fe1 N1 75.15(8) . . ? N2 Fe1 N1 104.85(8) 3_576 . ? N51 Fe1 N1 88.25(10) . 3_576 ? N51 Fe1 N1 91.75(10) 3_576 3_576 ? N2 Fe1 N1 104.85(8) . 3_576 ? N2 Fe1 N1 75.15(8) 3_576 3_576 ? N1 Fe1 N1 180.0 . 3_576 ? C1 N1 C5 117.5(2) . . ? C1 N1 Fe1 126.74(18) . . ? C5 N1 Fe1 115.66(18) . . ? C6 N2 N3 113.7(2) . . ? C6 N2 Fe1 114.89(17) . . ? N3 N2 Fe1 131.40(16) . . ? C7 N3 N2 110.9(2) . . ? C8 N4 C12 116.5(3) . . ? C6 S1 C7 86.89(13) . . ? N1 C1 C2 122.6(3) . . ? C3 C2 C1 119.4(3) . . ? C2 C3 C4 118.7(3) . . ? C5 C4 C3 119.1(3) . . ? N1 C5 C4 122.6(2) . . ? N1 C5 C6 113.9(2) . . ? C4 C5 C6 123.5(2) . . ? N2 C6 C5 120.3(2) . . ? N2 C6 S1 113.5(2) . . ? C5 C6 S1 126.2(2) . . ? N3 C7 C8 124.2(2) . . ? N3 C7 S1 115.0(2) . . ? C8 C7 S1 120.83(18) . . ? N4 C8 C9 124.0(3) . . ? N4 C8 C7 113.9(2) . . ? C9 C8 C7 122.1(2) . . ? C8 C9 C10 117.9(3) . . ? C11 C10 C9 118.8(3) . . ? C10 C11 C12 119.0(3) . . ? N4 C12 C11 123.8(3) . . ? C51 N51 Fe1 161.5(3) . . ? N51 C51 S51 179.7(3) . . ? N61 Fe2 N61 180.0 . 3_655 ? N61 Fe2 N22 91.52(9) . . ? N61 Fe2 N22 88.48(9) 3_655 . ? N61 Fe2 N22 88.48(9) . 3_655 ? N61 Fe2 N22 91.52(9) 3_655 3_655 ? N22 Fe2 N22 180.00(11) . 3_655 ? N61 Fe2 N21 92.62(9) . . ? N61 Fe2 N21 87.38(9) 3_655 . ? N22 Fe2 N21 75.67(8) . . ? N22 Fe2 N21 104.33(8) 3_655 . ? N61 Fe2 N21 87.38(9) . 3_655 ? N61 Fe2 N21 92.62(9) 3_655 3_655 ? N22 Fe2 N21 104.33(8) . 3_655 ? N22 Fe2 N21 75.67(8) 3_655 3_655 ? N21 Fe2 N21 180.00(14) . 3_655 ? C21 N21 C25 117.8(2) . . ? C21 N21 Fe2 127.64(19) . . ? C25 N21 Fe2 114.35(17) . . ? C26 N22 N23 113.5(2) . . ? C26 N22 Fe2 113.49(17) . . ? N23 N22 Fe2 132.32(17) . . ? C27 N23 N22 111.0(2) . . ? C32 N24 C28 116.0(3) . . ? C26 S21 C27 86.98(13) . . ? N21 C21 C22 122.9(3) . . ? C23 C22 C21 118.7(3) . . ? C22 C23 C24 119.2(3) . . ? C25 C24 C23 119.0(3) . . ? N21 C25 C24 122.3(3) . . ? N21 C25 C26 114.9(2) . . ? C24 C25 C26 122.7(2) . . ? N22 C26 C25 120.1(2) . . ? N22 C26 S21 113.7(2) . . ? C25 C26 S21 126.2(2) . . ? N23 C27 C28 124.8(3) . . ? N23 C27 S21 114.7(2) . . ? C28 C27 S21 120.6(2) . . ? N24 C28 C29 124.4(3) . . ? N24 C28 C27 114.4(2) . . ? C29 C28 C27 121.2(3) . . ? C28 C29 C30 117.6(3) . . ? C31 C30 C29 119.4(3) . . ? C32 C31 C30 118.5(3) . . ? N24 C32 C31 124.2(3) . . ? C61 N61 Fe2 175.7(3) . . ? N61 C61 S61 178.5(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 N51 Fe1 N1 C1 -90.7(2) . . . . ? N51 Fe1 N1 C1 89.3(2) 3_576 . . . ? N2 Fe1 N1 C1 179.4(2) . . . . ? N2 Fe1 N1 C1 -0.6(2) 3_576 . . . ? N1 Fe1 N1 C1 136(100) 3_576 . . . ? N51 Fe1 N1 C5 92.59(19) . . . . ? N51 Fe1 N1 C5 -87.41(19) 3_576 . . . ? N2 Fe1 N1 C5 2.69(17) . . . . ? N2 Fe1 N1 C5 -177.31(17) 3_576 . . . ? N1 Fe1 N1 C5 -41(100) 3_576 . . . ? N51 Fe1 N2 C6 -93.9(2) . . . . ? N51 Fe1 N2 C6 86.1(2) 3_576 . . . ? N2 Fe1 N2 C6 -154(100) 3_576 . . . ? N1 Fe1 N2 C6 -2.19(18) . . . . ? N1 Fe1 N2 C6 177.81(18) 3_576 . . . ? N51 Fe1 N2 N3 88.0(2) . . . . ? N51 Fe1 N2 N3 -92.0(2) 3_576 . . . ? N2 Fe1 N2 N3 28(100) 3_576 . . . ? N1 Fe1 N2 N3 179.7(2) . . . . ? N1 Fe1 N2 N3 -0.3(2) 3_576 . . . ? C6 N2 N3 C7 0.5(3) . . . . ? Fe1 N2 N3 C7 178.64(18) . . . . ? C5 N1 C1 C2 0.1(4) . . . . ? Fe1 N1 C1 C2 -176.6(2) . . . . ? N1 C1 C2 C3 -0.2(5) . . . . ? C1 C2 C3 C4 0.4(5) . . . . ? C2 C3 C4 C5 -0.5(4) . . . . ? C1 N1 C5 C4 -0.2(4) . . . . ? Fe1 N1 C5 C4 176.9(2) . . . . ? C1 N1 C5 C6 -179.8(2) . . . . ? Fe1 N1 C5 C6 -2.7(3) . . . . ? C3 C4 C5 N1 0.4(4) . . . . ? C3 C4 C5 C6 180.0(3) . . . . ? N3 N2 C6 C5 180.0(2) . . . . ? Fe1 N2 C6 C5 1.5(3) . . . . ? N3 N2 C6 S1 -0.8(3) . . . . ? Fe1 N2 C6 S1 -179.30(11) . . . . ? N1 C5 C6 N2 0.8(4) . . . . ? C4 C5 C6 N2 -178.8(3) . . . . ? N1 C5 C6 S1 -178.21(19) . . . . ? C4 C5 C6 S1 2.1(4) . . . . ? C7 S1 C6 N2 0.7(2) . . . . ? C7 S1 C6 C5 179.8(2) . . . . ? N2 N3 C7 C8 -178.7(2) . . . . ? N2 N3 C7 S1 0.1(3) . . . . ? C6 S1 C7 N3 -0.4(2) . . . . ? C6 S1 C7 C8 178.4(2) . . . . ? C12 N4 C8 C9 -0.5(5) . . . . ? C12 N4 C8 C7 -179.1(3) . . . . ? N3 C7 C8 N4 -171.6(3) . . . . ? S1 C7 C8 N4 9.7(3) . . . . ? N3 C7 C8 C9 9.8(4) . . . . ? S1 C7 C8 C9 -168.9(2) . . . . ? N4 C8 C9 C10 0.2(5) . . . . ? C7 C8 C9 C10 178.6(3) . . . . ? C8 C9 C10 C11 0.4(5) . . . . ? C9 C10 C11 C12 -0.5(6) . . . . ? C8 N4 C12 C11 0.4(6) . . . . ? C10 C11 C12 N4 0.1(7) . . . . ? N51 Fe1 N51 C51 -117(4) 3_576 . . . ? N2 Fe1 N51 C51 -112.6(8) . . . . ? N2 Fe1 N51 C51 67.4(8) 3_576 . . . ? N1 Fe1 N51 C51 172.3(8) . . . . ? N1 Fe1 N51 C51 -7.7(8) 3_576 . . . ? Fe1 N51 C51 S51 78(61) . . . . ? N61 Fe2 N21 C21 85.2(2) . . . . ? N61 Fe2 N21 C21 -94.8(2) 3_655 . . . ? N22 Fe2 N21 C21 176.1(3) . . . . ? N22 Fe2 N21 C21 -3.9(3) 3_655 . . . ? N21 Fe2 N21 C21 0.00(17) 3_655 . . . ? N61 Fe2 N21 C25 -100.64(19) . . . . ? N61 Fe2 N21 C25 79.36(19) 3_655 . . . ? N22 Fe2 N21 C25 -9.74(18) . . . . ? N22 Fe2 N21 C25 170.26(18) 3_655 . . . ? N21 Fe2 N21 C25 0.00(13) 3_655 . . . ? N61 Fe2 N22 C26 103.0(2) . . . . ? N61 Fe2 N22 C26 -77.0(2) 3_655 . . . ? N22 Fe2 N22 C26 62(100) 3_655 . . . ? N21 Fe2 N22 C26 10.72(19) . . . . ? N21 Fe2 N22 C26 -169.28(19) 3_655 . . . ? N61 Fe2 N22 N23 -87.0(2) . . . . ? N61 Fe2 N22 N23 93.0(2) 3_655 . . . ? N22 Fe2 N22 N23 -128(100) 3_655 . . . ? N21 Fe2 N22 N23 -179.3(2) . . . . ? N21 Fe2 N22 N23 0.7(2) 3_655 . . . ? C26 N22 N23 C27 0.5(3) . . . . ? Fe2 N22 N23 C27 -169.46(19) . . . . ? C25 N21 C21 C22 -0.4(4) . . . . ? Fe2 N21 C21 C22 173.6(2) . . . . ? N21 C21 C22 C23 0.2(5) . . . . ? C21 C22 C23 C24 -0.1(5) . . . . ? C22 C23 C24 C25 0.2(5) . . . . ? C21 N21 C25 C24 0.5(4) . . . . ? Fe2 N21 C25 C24 -174.2(2) . . . . ? C21 N21 C25 C26 -177.7(2) . . . . ? Fe2 N21 C25 C26 7.6(3) . . . . ? C23 C24 C25 N21 -0.4(5) . . . . ? C23 C24 C25 C26 177.7(3) . . . . ? N23 N22 C26 C25 177.3(2) . . . . ? Fe2 N22 C26 C25 -10.7(3) . . . . ? N23 N22 C26 S21 -1.1(3) . . . . ? Fe2 N22 C26 S21 170.83(12) . . . . ? N21 C25 C26 N22 2.2(4) . . . . ? C24 C25 C26 N22 -176.0(3) . . . . ? N21 C25 C26 S21 -179.6(2) . . . . ? C24 C25 C26 S21 2.2(4) . . . . ? C27 S21 C26 N22 1.0(2) . . . . ? C27 S21 C26 C25 -177.3(3) . . . . ? N22 N23 C27 C28 -179.0(2) . . . . ? N22 N23 C27 S21 0.3(3) . . . . ? C26 S21 C27 N23 -0.8(2) . . . . ? C26 S21 C27 C28 178.6(2) . . . . ? C32 N24 C28 C29 -0.6(4) . . . . ? C32 N24 C28 C27 179.1(2) . . . . ? N23 C27 C28 N24 -176.1(3) . . . . ? S21 C27 C28 N24 4.6(3) . . . . ? N23 C27 C28 C29 3.7(4) . . . . ? S21 C27 C28 C29 -175.6(2) . . . . ? N24 C28 C29 C30 0.2(5) . . . . ? C27 C28 C29 C30 -179.5(3) . . . . ? C28 C29 C30 C31 0.3(5) . . . . ? C29 C30 C31 C32 -0.4(5) . . . . ? C28 N24 C32 C31 0.5(4) . . . . ? C30 C31 C32 N24 0.0(5) . . . . ? N61 Fe2 N61 C61 -133(4) 3_655 . . . ? N22 Fe2 N61 C61 65(3) . . . . ? N22 Fe2 N61 C61 -115(3) 3_655 . . . ? N21 Fe2 N61 C61 141(3) . . . . ? N21 Fe2 N61 C61 -39(3) 3_655 . . . ? Fe2 N61 C61 S61 -120(10) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.341 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.063 # Attachment 'jmk193_3.cif' data_jmk193_3 _database_code_depnum_ccdc_archive 'CCDC 748039' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; (Fe C26 H16 N10 S4) ; _chemical_formula_sum 'C26 H16 Fe N10 S4' _chemical_formula_weight 652.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.760(5) _cell_length_b 7.8903(16) _cell_length_c 16.533(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.84(3) _cell_angle_gamma 90.00 _cell_volume 2774.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 6352 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.883 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8095 _exptl_absorpt_correction_T_max 0.9489 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-Axis SPIDER' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47697 _diffrn_reflns_av_R_equivalents 0.0923 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6352 _reflns_number_gt 4505 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+0.9604P] 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 6352 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0714 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1074 _refine_ls_wR_factor_gt 0.0966 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.0000 0.0000 0.5000 0.02314(14) Uani 1 2 d S . . N1 N 0.01280(10) -0.1996(3) 0.41351(14) 0.0254(5) Uani 1 1 d . . . N2 N 0.07221(10) 0.0991(3) 0.45503(14) 0.0254(5) Uani 1 1 d . . . N3 N 0.10479(10) 0.2496(3) 0.47180(14) 0.0255(5) Uani 1 1 d . . . N4 N 0.21824(11) 0.3898(3) 0.38117(16) 0.0355(6) Uani 1 1 d . . . S1 S 0.14620(3) 0.07968(9) 0.37031(5) 0.02759(17) Uani 1 1 d . . . C1 C -0.01789(13) -0.3481(4) 0.39432(19) 0.0314(7) Uani 1 1 d . . . H1 H -0.0499 -0.3712 0.4172 0.038 Uiso 1 1 calc R . . C2 C -0.00454(13) -0.4696(4) 0.34213(19) 0.0323(7) Uani 1 1 d . . . H2 H -0.0270 -0.5737 0.3300 0.039 Uiso 1 1 calc R . . C3 C 0.04167(13) -0.4368(4) 0.30832(18) 0.0308(6) Uani 1 1 d . . . H3 H 0.0512 -0.5174 0.2721 0.037 Uiso 1 1 calc R . . C4 C 0.07418(12) -0.2835(3) 0.32818(17) 0.0269(6) Uani 1 1 d . . . H4 H 0.1067 -0.2584 0.3066 0.032 Uiso 1 1 calc R . . C5 C 0.05800(12) -0.1689(3) 0.37996(16) 0.0230(6) Uani 1 1 d . . . C6 C 0.08865(12) -0.0023(3) 0.40409(16) 0.0223(6) Uani 1 1 d . . . C7 C 0.14494(12) 0.2564(3) 0.43177(17) 0.0246(6) Uani 1 1 d . . . C8 C 0.18843(12) 0.3985(3) 0.43765(17) 0.0241(6) Uani 1 1 d . . . C9 C 0.19675(13) 0.5275(4) 0.49765(19) 0.0306(6) Uani 1 1 d . . . H9 H 0.1739 0.5290 0.5359 0.037 Uiso 1 1 calc R . . C10 C 0.23958(13) 0.6544(4) 0.4999(2) 0.0361(7) Uani 1 1 d . . . H10 H 0.2474 0.7438 0.5409 0.043 Uiso 1 1 calc R . . C11 C 0.27046(15) 0.6489(4) 0.4421(2) 0.0428(8) Uani 1 1 d . . . H11 H 0.2996 0.7351 0.4419 0.051 Uiso 1 1 calc R . . C12 C 0.25830(16) 0.5151(4) 0.3838(2) 0.0446(8) Uani 1 1 d . . . H12 H 0.2796 0.5126 0.3437 0.053 Uiso 1 1 calc R . . Fe2 Fe 0.5000 0.0000 0.0000 0.02182(14) Uani 1 2 d S . . N21 N 0.50461(10) 0.2023(3) -0.07154(14) 0.0238(5) Uani 1 1 d . . . N22 N 0.43536(10) 0.1451(3) 0.02044(14) 0.0251(5) Uani 1 1 d . . . N23 N 0.40102(10) 0.1289(3) 0.07356(14) 0.0260(5) Uani 1 1 d . . . N24 N 0.27487(10) 0.4003(3) 0.07805(15) 0.0295(5) Uani 1 1 d . . . S21 S 0.35960(3) 0.39567(9) -0.01890(5) 0.02953(17) Uani 1 1 d . . . C21 C 0.54507(13) 0.2348(4) -0.11186(18) 0.0295(6) Uani 1 1 d . . . H21 H 0.5782 0.1568 -0.1054 0.035 Uiso 1 1 calc R . . C22 C 0.54063(14) 0.3776(4) -0.16273(19) 0.0332(7) Uani 1 1 d . . . H22 H 0.5706 0.3968 -0.1897 0.040 Uiso 1 1 calc R . . C23 C 0.49244(15) 0.4915(4) -0.1738(2) 0.0366(7) Uani 1 1 d . . . H23 H 0.4881 0.5887 -0.2094 0.044 Uiso 1 1 calc R . . C24 C 0.45068(14) 0.4611(4) -0.13205(19) 0.0331(7) Uani 1 1 d . . . H24 H 0.4173 0.5379 -0.1378 0.040 Uiso 1 1 calc R . . C25 C 0.45816(12) 0.3181(3) -0.08202(17) 0.0255(6) Uani 1 1 d . . . C26 C 0.41996(12) 0.2803(3) -0.02974(17) 0.0249(6) Uani 1 1 d . . . C27 C 0.35943(12) 0.2516(3) 0.06001(17) 0.0262(6) Uani 1 1 d . . . C28 C 0.31543(12) 0.2703(3) 0.10641(17) 0.0263(6) Uani 1 1 d . . . C29 C 0.31688(13) 0.1620(4) 0.17260(19) 0.0330(7) Uani 1 1 d . . . H29 H 0.3470 0.0734 0.1908 0.040 Uiso 1 1 calc R . . C30 C 0.27265(14) 0.1869(4) 0.21186(19) 0.0372(7) Uani 1 1 d . . . H30 H 0.2719 0.1152 0.2577 0.045 Uiso 1 1 calc R . . C31 C 0.23004(14) 0.3170(4) 0.1833(2) 0.0367(7) Uani 1 1 d . . . H31 H 0.1989 0.3352 0.2084 0.044 Uiso 1 1 calc R . . C32 C 0.23305(13) 0.4213(4) 0.11739(19) 0.0333(7) Uani 1 1 d . . . H32 H 0.2040 0.5123 0.0992 0.040 Uiso 1 1 calc R . . N61 N 0.56504(10) 0.0936(3) 0.10095(15) 0.0256(5) Uani 1 1 d . . . C61 C 0.60533(12) 0.1454(3) 0.16154(17) 0.0227(6) Uani 1 1 d . . . S61 S 0.66192(3) 0.22378(10) 0.24468(5) 0.03362(19) Uani 1 1 d . . . N51 N -0.07041(11) 0.1158(3) 0.39711(15) 0.0330(6) Uani 1 1 d . . . C51 C -0.11192(12) 0.2056(4) 0.35942(17) 0.0247(6) Uani 1 1 d . . . S51 S -0.16927(3) 0.32970(11) 0.30572(5) 0.0386(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0221(3) 0.0264(3) 0.0253(3) 0.0035(2) 0.0137(2) -0.0003(2) N1 0.0236(11) 0.0281(13) 0.0276(12) 0.0033(10) 0.0128(10) -0.0031(10) N2 0.0229(11) 0.0276(13) 0.0272(12) 0.0009(10) 0.0109(10) -0.0010(9) N3 0.0258(12) 0.0277(13) 0.0270(12) 0.0013(10) 0.0142(10) -0.0055(9) N4 0.0433(15) 0.0364(15) 0.0366(14) -0.0054(11) 0.0263(12) -0.0152(12) S1 0.0290(4) 0.0312(4) 0.0292(4) -0.0043(3) 0.0185(3) -0.0081(3) C1 0.0292(15) 0.0339(17) 0.0358(16) 0.0005(13) 0.0174(13) -0.0105(13) C2 0.0351(16) 0.0286(16) 0.0333(16) -0.0030(13) 0.0123(13) -0.0113(13) C3 0.0341(15) 0.0314(16) 0.0280(15) -0.0012(13) 0.0126(13) -0.0017(13) C4 0.0254(14) 0.0298(16) 0.0274(14) 0.0023(12) 0.0119(12) -0.0029(12) C5 0.0229(13) 0.0260(15) 0.0208(13) 0.0038(11) 0.0088(11) -0.0008(11) C6 0.0221(13) 0.0274(15) 0.0208(13) 0.0048(11) 0.0115(11) -0.0016(11) C7 0.0264(14) 0.0266(15) 0.0203(13) 0.0038(11) 0.0079(11) -0.0015(11) C8 0.0239(13) 0.0256(15) 0.0235(14) 0.0018(11) 0.0094(11) -0.0019(11) C9 0.0316(15) 0.0315(16) 0.0310(15) 0.0004(13) 0.0140(13) -0.0005(12) C10 0.0386(17) 0.0265(16) 0.0418(18) -0.0069(14) 0.0125(15) -0.0040(13) C11 0.0468(19) 0.0372(19) 0.0468(19) -0.0035(16) 0.0197(16) -0.0173(15) C12 0.055(2) 0.047(2) 0.0449(19) -0.0055(16) 0.0333(17) -0.0215(16) Fe2 0.0234(3) 0.0185(3) 0.0236(3) 0.0004(2) 0.0085(2) 0.0025(2) N21 0.0285(12) 0.0196(12) 0.0230(11) 0.0003(9) 0.0087(10) 0.0017(9) N22 0.0274(12) 0.0258(12) 0.0235(12) 0.0002(10) 0.0108(10) 0.0005(10) N23 0.0268(12) 0.0239(13) 0.0278(12) 0.0003(10) 0.0104(10) 0.0021(10) N24 0.0294(13) 0.0280(13) 0.0332(13) -0.0046(11) 0.0136(11) 0.0015(10) S21 0.0317(4) 0.0272(4) 0.0311(4) 0.0027(3) 0.0128(3) 0.0085(3) C21 0.0362(16) 0.0251(15) 0.0310(15) -0.0016(12) 0.0167(13) -0.0023(12) C22 0.0436(17) 0.0288(17) 0.0315(16) -0.0004(13) 0.0186(14) -0.0045(13) C23 0.0475(19) 0.0288(17) 0.0327(17) 0.0083(13) 0.0132(15) 0.0033(14) C24 0.0387(17) 0.0286(16) 0.0321(16) 0.0055(13) 0.0129(14) 0.0064(13) C25 0.0292(14) 0.0215(14) 0.0240(14) -0.0006(11) 0.0073(12) 0.0027(11) C26 0.0273(14) 0.0200(14) 0.0247(14) -0.0001(11) 0.0060(12) 0.0029(11) C27 0.0260(14) 0.0229(15) 0.0274(15) -0.0006(11) 0.0068(12) 0.0013(11) C28 0.0273(14) 0.0253(15) 0.0257(14) -0.0046(12) 0.0085(12) -0.0013(12) C29 0.0305(15) 0.0320(16) 0.0334(16) 0.0077(13) 0.0077(13) 0.0014(13) C30 0.0427(18) 0.0410(19) 0.0312(16) 0.0000(14) 0.0172(14) -0.0115(15) C31 0.0361(17) 0.0425(19) 0.0393(18) -0.0113(15) 0.0228(15) -0.0095(14) C32 0.0324(16) 0.0346(17) 0.0347(17) -0.0050(13) 0.0141(14) 0.0015(13) N61 0.0260(12) 0.0227(12) 0.0288(13) 0.0016(10) 0.0105(11) 0.0032(10) C61 0.0227(14) 0.0204(14) 0.0276(15) 0.0024(11) 0.0119(12) 0.0064(11) S61 0.0254(4) 0.0374(4) 0.0333(4) -0.0084(3) 0.0047(3) 0.0052(3) N51 0.0300(13) 0.0400(16) 0.0319(14) 0.0048(12) 0.0145(11) 0.0009(12) C51 0.0240(14) 0.0313(16) 0.0242(14) -0.0005(12) 0.0151(12) -0.0041(12) S51 0.0321(4) 0.0510(5) 0.0380(4) 0.0111(4) 0.0190(4) 0.0138(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 N51 2.087(3) 3_556 ? Fe1 N51 2.087(3) . ? Fe1 N2 2.176(2) 3_556 ? Fe1 N2 2.176(2) . ? Fe1 N1 2.215(2) . ? Fe1 N1 2.215(2) 3_556 ? N1 C1 1.343(3) . ? N1 C5 1.353(3) . ? N2 C6 1.309(3) . ? N2 N3 1.375(3) . ? N3 C7 1.306(3) . ? N4 C12 1.335(4) . ? N4 C8 1.337(3) . ? S1 C6 1.722(2) . ? S1 C7 1.732(3) . ? C1 C2 1.394(4) . ? C2 C3 1.380(4) . ? C3 C4 1.395(4) . ? C4 C5 1.382(4) . ? C5 C6 1.475(4) . ? C7 C8 1.476(4) . ? C8 C9 1.387(4) . ? C9 C10 1.388(4) . ? C10 C11 1.374(4) . ? C11 C12 1.390(4) . ? Fe2 N61 1.940(2) 3_655 ? Fe2 N61 1.940(2) . ? Fe2 N22 1.986(2) 3_655 ? Fe2 N22 1.986(2) . ? Fe2 N21 2.011(2) . ? Fe2 N21 2.011(2) 3_655 ? N21 C21 1.340(3) . ? N21 C25 1.361(3) . ? N22 C26 1.320(3) . ? N22 N23 1.374(3) . ? N23 C27 1.316(3) . ? N24 C32 1.340(4) . ? N24 C28 1.348(3) . ? S21 C26 1.710(3) . ? S21 C27 1.731(3) . ? C21 C22 1.388(4) . ? C22 C23 1.378(4) . ? C23 C24 1.380(4) . ? C24 C25 1.373(4) . ? C25 C26 1.458(4) . ? C27 C28 1.469(4) . ? C28 C29 1.380(4) . ? C29 C30 1.392(4) . ? C30 C31 1.375(4) . ? C31 C32 1.386(4) . ? N61 C61 1.165(3) . ? C61 S61 1.634(3) . ? N51 C51 1.168(3) . ? C51 S51 1.621(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 N51 Fe1 N51 179.998(1) 3_556 . ? N51 Fe1 N2 91.06(9) 3_556 3_556 ? N51 Fe1 N2 88.94(9) . 3_556 ? N51 Fe1 N2 88.94(9) 3_556 . ? N51 Fe1 N2 91.06(9) . . ? N2 Fe1 N2 180.00(6) 3_556 . ? N51 Fe1 N1 88.61(9) 3_556 . ? N51 Fe1 N1 91.38(9) . . ? N2 Fe1 N1 104.70(8) 3_556 . ? N2 Fe1 N1 75.30(8) . . ? N51 Fe1 N1 91.39(9) 3_556 3_556 ? N51 Fe1 N1 88.62(9) . 3_556 ? N2 Fe1 N1 75.30(8) 3_556 3_556 ? N2 Fe1 N1 104.70(8) . 3_556 ? N1 Fe1 N1 180.0 . 3_556 ? C1 N1 C5 117.8(2) . . ? C1 N1 Fe1 126.60(18) . . ? C5 N1 Fe1 115.52(17) . . ? C6 N2 N3 113.6(2) . . ? C6 N2 Fe1 115.09(17) . . ? N3 N2 Fe1 131.31(16) . . ? C7 N3 N2 111.0(2) . . ? C12 N4 C8 116.7(3) . . ? C6 S1 C7 86.49(13) . . ? N1 C1 C2 122.5(2) . . ? C3 C2 C1 119.2(3) . . ? C2 C3 C4 119.0(3) . . ? C5 C4 C3 118.5(2) . . ? N1 C5 C4 123.1(2) . . ? N1 C5 C6 113.8(2) . . ? C4 C5 C6 123.1(2) . . ? N2 C6 C5 120.2(2) . . ? N2 C6 S1 113.8(2) . . ? C5 C6 S1 126.00(19) . . ? N3 C7 C8 124.9(2) . . ? N3 C7 S1 115.1(2) . . ? C8 C7 S1 119.99(19) . . ? N4 C8 C9 124.3(2) . . ? N4 C8 C7 114.2(2) . . ? C9 C8 C7 121.5(2) . . ? C8 C9 C10 117.7(3) . . ? C11 C10 C9 119.1(3) . . ? C10 C11 C12 118.8(3) . . ? N4 C12 C11 123.4(3) . . ? N61 Fe2 N61 179.994(2) 3_655 . ? N61 Fe2 N22 91.08(9) 3_655 3_655 ? N61 Fe2 N22 88.92(9) . 3_655 ? N61 Fe2 N22 88.92(9) 3_655 . ? N61 Fe2 N22 91.08(9) . . ? N22 Fe2 N22 180.00(16) 3_655 . ? N61 Fe2 N21 88.82(9) 3_655 . ? N61 Fe2 N21 91.17(9) . . ? N22 Fe2 N21 99.25(9) 3_655 . ? N22 Fe2 N21 80.75(9) . . ? N61 Fe2 N21 91.18(9) 3_655 3_655 ? N61 Fe2 N21 88.83(9) . 3_655 ? N22 Fe2 N21 80.75(9) 3_655 3_655 ? N22 Fe2 N21 99.25(9) . 3_655 ? N21 Fe2 N21 180.00(15) . 3_655 ? C21 N21 C25 116.6(2) . . ? C21 N21 Fe2 129.32(18) . . ? C25 N21 Fe2 114.01(17) . . ? C26 N22 N23 113.1(2) . . ? C26 N22 Fe2 113.97(18) . . ? N23 N22 Fe2 132.82(17) . . ? C27 N23 N22 111.2(2) . . ? C32 N24 C28 116.2(3) . . ? C26 S21 C27 86.95(13) . . ? N21 C21 C22 122.9(3) . . ? C23 C22 C21 119.5(3) . . ? C22 C23 C24 118.5(3) . . ? C25 C24 C23 119.0(3) . . ? N21 C25 C24 123.5(3) . . ? N21 C25 C26 112.8(2) . . ? C24 C25 C26 123.6(2) . . ? N22 C26 C25 117.2(2) . . ? N22 C26 S21 114.1(2) . . ? C25 C26 S21 128.6(2) . . ? N23 C27 C28 124.6(2) . . ? N23 C27 S21 114.6(2) . . ? C28 C27 S21 120.8(2) . . ? N24 C28 C29 124.6(3) . . ? N24 C28 C27 113.9(2) . . ? C29 C28 C27 121.6(3) . . ? C28 C29 C30 117.7(3) . . ? C31 C30 C29 118.9(3) . . ? C30 C31 C32 119.1(3) . . ? N24 C32 C31 123.4(3) . . ? C61 N61 Fe2 177.8(2) . . ? N61 C61 S61 178.1(3) . . ? C51 N51 Fe1 160.2(2) . . ? N51 C51 S51 179.1(2) . . ? 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 N51 Fe1 N1 C1 90.7(2) 3_556 . . . ? N51 Fe1 N1 C1 -89.3(2) . . . . ? N2 Fe1 N1 C1 -0.1(2) 3_556 . . . ? N2 Fe1 N1 C1 179.9(2) . . . . ? N1 Fe1 N1 C1 0(100) 3_556 . . . ? N51 Fe1 N1 C5 -86.68(19) 3_556 . . . ? N51 Fe1 N1 C5 93.32(19) . . . . ? N2 Fe1 N1 C5 -177.41(18) 3_556 . . . ? N2 Fe1 N1 C5 2.59(18) . . . . ? N1 Fe1 N1 C5 0(100) 3_556 . . . ? N51 Fe1 N2 C6 87.0(2) 3_556 . . . ? N51 Fe1 N2 C6 -93.0(2) . . . . ? N2 Fe1 N2 C6 0(100) 3_556 . . . ? N1 Fe1 N2 C6 -1.85(18) . . . . ? N1 Fe1 N2 C6 178.15(18) 3_556 . . . ? N51 Fe1 N2 N3 -91.8(2) 3_556 . . . ? N51 Fe1 N2 N3 88.2(2) . . . . ? N2 Fe1 N2 N3 0(100) 3_556 . . . ? N1 Fe1 N2 N3 179.4(2) . . . . ? N1 Fe1 N2 N3 -0.6(2) 3_556 . . . ? C6 N2 N3 C7 0.4(3) . . . . ? Fe1 N2 N3 C7 179.16(18) . . . . ? C5 N1 C1 C2 0.3(4) . . . . ? Fe1 N1 C1 C2 -177.0(2) . . . . ? N1 C1 C2 C3 -0.3(5) . . . . ? C1 C2 C3 C4 0.7(4) . . . . ? C2 C3 C4 C5 -1.1(4) . . . . ? C1 N1 C5 C4 -0.8(4) . . . . ? Fe1 N1 C5 C4 176.8(2) . . . . ? C1 N1 C5 C6 179.6(2) . . . . ? Fe1 N1 C5 C6 -2.9(3) . . . . ? C3 C4 C5 N1 1.2(4) . . . . ? C3 C4 C5 C6 -179.2(2) . . . . ? N3 N2 C6 C5 180.0(2) . . . . ? Fe1 N2 C6 C5 1.0(3) . . . . ? N3 N2 C6 S1 -0.6(3) . . . . ? Fe1 N2 C6 S1 -179.62(11) . . . . ? N1 C5 C6 N2 1.3(4) . . . . ? C4 C5 C6 N2 -178.4(3) . . . . ? N1 C5 C6 S1 -178.01(19) . . . . ? C4 C5 C6 S1 2.3(4) . . . . ? C7 S1 C6 N2 0.5(2) . . . . ? C7 S1 C6 C5 179.9(2) . . . . ? N2 N3 C7 C8 -178.4(2) . . . . ? N2 N3 C7 S1 0.0(3) . . . . ? C6 S1 C7 N3 -0.3(2) . . . . ? C6 S1 C7 C8 178.2(2) . . . . ? C12 N4 C8 C9 -0.2(4) . . . . ? C12 N4 C8 C7 -179.9(3) . . . . ? N3 C7 C8 N4 -170.3(3) . . . . ? S1 C7 C8 N4 11.3(3) . . . . ? N3 C7 C8 C9 10.0(4) . . . . ? S1 C7 C8 C9 -168.4(2) . . . . ? N4 C8 C9 C10 -1.0(4) . . . . ? C7 C8 C9 C10 178.7(3) . . . . ? C8 C9 C10 C11 1.4(4) . . . . ? C9 C10 C11 C12 -0.8(5) . . . . ? C8 N4 C12 C11 0.9(5) . . . . ? C10 C11 C12 N4 -0.4(5) . . . . ? N61 Fe2 N21 C21 -97.9(2) 3_655 . . . ? N61 Fe2 N21 C21 82.0(2) . . . . ? N22 Fe2 N21 C21 -7.0(2) 3_655 . . . ? N22 Fe2 N21 C21 173.0(2) . . . . ? N21 Fe2 N21 C21 0.00(15) 3_655 . . . ? N61 Fe2 N21 C25 79.52(19) 3_655 . . . ? N61 Fe2 N21 C25 -100.49(19) . . . . ? N22 Fe2 N21 C25 170.42(18) 3_655 . . . ? N22 Fe2 N21 C25 -9.58(18) . . . . ? N21 Fe2 N21 C25 0.00(15) 3_655 . . . ? N61 Fe2 N22 C26 -78.87(19) 3_655 . . . ? N61 Fe2 N22 C26 101.13(19) . . . . ? N22 Fe2 N22 C26 -117(100) 3_655 . . . ? N21 Fe2 N22 C26 10.12(19) . . . . ? N21 Fe2 N22 C26 -169.88(19) 3_655 . . . ? N61 Fe2 N22 N23 97.4(2) 3_655 . . . ? N61 Fe2 N22 N23 -82.6(2) . . . . ? N22 Fe2 N22 N23 59(100) 3_655 . . . ? N21 Fe2 N22 N23 -173.7(2) . . . . ? N21 Fe2 N22 N23 6.3(2) 3_655 . . . ? C26 N22 N23 C27 1.5(3) . . . . ? Fe2 N22 N23 C27 -174.75(19) . . . . ? C25 N21 C21 C22 -0.5(4) . . . . ? Fe2 N21 C21 C22 176.9(2) . . . . ? N21 C21 C22 C23 -0.7(4) . . . . ? C21 C22 C23 C24 1.4(4) . . . . ? C22 C23 C24 C25 -0.8(5) . . . . ? C21 N21 C25 C24 1.2(4) . . . . ? Fe2 N21 C25 C24 -176.6(2) . . . . ? C21 N21 C25 C26 -174.8(2) . . . . ? Fe2 N21 C25 C26 7.4(3) . . . . ? C23 C24 C25 N21 -0.5(4) . . . . ? C23 C24 C25 C26 175.0(3) . . . . ? N23 N22 C26 C25 173.9(2) . . . . ? Fe2 N22 C26 C25 -9.2(3) . . . . ? N23 N22 C26 S21 -2.3(3) . . . . ? Fe2 N22 C26 S21 174.66(12) . . . . ? N21 C25 C26 N22 1.1(4) . . . . ? C24 C25 C26 N22 -174.9(3) . . . . ? N21 C25 C26 S21 176.6(2) . . . . ? C24 C25 C26 S21 0.7(4) . . . . ? C27 S21 C26 N22 1.9(2) . . . . ? C27 S21 C26 C25 -173.8(3) . . . . ? N22 N23 C27 C28 180.0(2) . . . . ? N22 N23 C27 S21 0.0(3) . . . . ? C26 S21 C27 N23 -1.0(2) . . . . ? C26 S21 C27 C28 179.0(2) . . . . ? C32 N24 C28 C29 -0.9(4) . . . . ? C32 N24 C28 C27 179.0(2) . . . . ? N23 C27 C28 N24 -176.4(2) . . . . ? S21 C27 C28 N24 3.6(3) . . . . ? N23 C27 C28 C29 3.5(4) . . . . ? S21 C27 C28 C29 -176.5(2) . . . . ? N24 C28 C29 C30 1.1(4) . . . . ? C27 C28 C29 C30 -178.7(3) . . . . ? C28 C29 C30 C31 -0.1(4) . . . . ? C29 C30 C31 C32 -1.1(4) . . . . ? C28 N24 C32 C31 -0.4(4) . . . . ? C30 C31 C32 N24 1.4(5) . . . . ? N61 Fe2 N61 C61 -51(6) 3_655 . . . ? N22 Fe2 N61 C61 -17(6) 3_655 . . . ? N22 Fe2 N61 C61 163(6) . . . . ? N21 Fe2 N61 C61 -116(6) . . . . ? N21 Fe2 N61 C61 64(6) 3_655 . . . ? Fe2 N61 C61 S61 118(7) . . . . ? N51 Fe1 N51 C51 -169(5) 3_556 . . . ? N2 Fe1 N51 C51 64.0(6) 3_556 . . . ? N2 Fe1 N51 C51 -116.0(6) . . . . ? N1 Fe1 N51 C51 168.6(6) . . . . ? N1 Fe1 N51 C51 -11.4(6) 3_556 . . . ? Fe1 N51 C51 S51 160(100) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.523 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.085 # Attachment 'jmk193_3_tt.cif' data_jmk193_3_tt _database_code_depnum_ccdc_archive 'CCDC 748040' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; (Fe C26 H16 N10 S4) ; _chemical_formula_sum 'C26 H16 Fe N10 S4' _chemical_formula_weight 652.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.698(5) _cell_length_b 7.8613(16) _cell_length_c 16.210(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.89(3) _cell_angle_gamma 90.00 _cell_volume 2719.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6163 _cell_measurement_theta_min 3.13 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.900 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8062 _exptl_absorpt_correction_T_max 0.9480 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-Axis SPIDER' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43709 _diffrn_reflns_av_R_equivalents 0.1104 _diffrn_reflns_av_sigmaI/netI 0.0728 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6163 _reflns_number_gt 4180 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1031P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6163 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0968 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.1841 _refine_ls_wR_factor_gt 0.1614 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe2 Fe 1.0000 0.5000 0.5000 0.0228(2) Uani 1 2 d S . . N21 N 0.99491(14) 0.2960(4) 0.5719(2) 0.0253(7) Uani 1 1 d . . . N23 N 1.10025(14) 0.3740(4) 0.4253(2) 0.0272(7) Uani 1 1 d . . . N24 N 1.22820(15) 0.1081(4) 0.4206(2) 0.0293(8) Uani 1 1 d . . . C21 C 0.95355(18) 0.2608(5) 0.6113(3) 0.0278(9) Uani 1 1 d . . . H21 H 0.9201 0.3383 0.6042 0.033 Uiso 1 1 calc R . . C22 C 0.95695(19) 0.1154(5) 0.6625(3) 0.0306(9) Uani 1 1 d . . . H22 H 0.9260 0.0941 0.6887 0.037 Uiso 1 1 calc R . . C23 C 1.0063(2) 0.0025(6) 0.6745(3) 0.0343(10) Uani 1 1 d . . . H23 H 1.0106 -0.0955 0.7103 0.041 Uiso 1 1 calc R . . C24 C 1.04933(19) 0.0367(5) 0.6326(3) 0.0310(9) Uani 1 1 d . . . H24 H 1.0833 -0.0386 0.6387 0.037 Uiso 1 1 calc R . . C25 C 1.04179(17) 0.1822(5) 0.5821(3) 0.0262(8) Uani 1 1 d . . . C26 C 1.08094(17) 0.2220(5) 0.5302(3) 0.0254(8) Uani 1 1 d . . . C27 C 1.14258(18) 0.2537(5) 0.4396(3) 0.0283(9) Uani 1 1 d . . . C28 C 1.18740(17) 0.2381(5) 0.3923(3) 0.0271(9) Uani 1 1 d . . . C29 C 1.18643(18) 0.3472(5) 0.3252(3) 0.0304(9) Uani 1 1 d . . . H29 H 1.1563 0.4357 0.3071 0.036 Uiso 1 1 calc R . . C30 C 1.23104(19) 0.3234(6) 0.2848(3) 0.0342(10) Uani 1 1 d . . . H30 H 1.2319 0.3957 0.2383 0.041 Uiso 1 1 calc R . . C31 C 1.2739(2) 0.1929(6) 0.3134(3) 0.0357(10) Uani 1 1 d . . . H31 H 1.3051 0.1749 0.2873 0.043 Uiso 1 1 calc R . . C32 C 1.27083(19) 0.0884(5) 0.3809(3) 0.0304(9) Uani 1 1 d . . . H32 H 1.3003 -0.0015 0.3998 0.037 Uiso 1 1 calc R . . S21 S 1.14238(4) 0.10896(13) 0.51950(7) 0.0289(3) Uani 1 1 d . . . N22 N 1.06521(14) 0.3566(4) 0.4785(2) 0.0259(7) Uani 1 1 d . . . N61 N 0.93511(14) 0.4070(4) 0.3984(2) 0.0264(7) Uani 1 1 d . . . C61 C 0.89349(17) 0.3571(5) 0.3388(3) 0.0244(8) Uani 1 1 d . . . S61 S 0.83538(4) 0.28071(14) 0.25722(7) 0.0318(3) Uani 1 1 d . . . Fe1 Fe 0.5000 1.0000 0.5000 0.0222(2) Uani 1 2 d S . . N1 N 0.50660(14) 1.1886(4) 0.4191(2) 0.0243(7) Uani 1 1 d . . . N2 N 0.56547(14) 0.9020(4) 0.4582(2) 0.0247(7) Uani 1 1 d . . . N3 N 0.59740(14) 0.7504(4) 0.4761(2) 0.0242(7) Uani 1 1 d . . . N4 N 0.71407(15) 0.6109(4) 0.3866(2) 0.0315(8) Uani 1 1 d . . . S1 S 0.64206(4) 0.91857(13) 0.37396(7) 0.0272(3) Uani 1 1 d . . . C1 C 0.47382(18) 1.3334(5) 0.3987(3) 0.0303(9) Uani 1 1 d . . . H1 H 0.4410 1.3521 0.4215 0.036 Uiso 1 1 calc R . . C2 C 0.48583(19) 1.4578(5) 0.3453(3) 0.0307(9) Uani 1 1 d . . . H2 H 0.4613 1.5585 0.3322 0.037 Uiso 1 1 calc R . . C3 C 0.53352(18) 1.4347(6) 0.3114(3) 0.0287(9) Uani 1 1 d . . . H3 H 0.5426 1.5191 0.2756 0.034 Uiso 1 1 calc R . . C4 C 0.56775(18) 1.2848(5) 0.3312(3) 0.0284(9) Uani 1 1 d . . . H4 H 0.6008 1.2643 0.3091 0.034 Uiso 1 1 calc R . . C5 C 0.55288(16) 1.1661(5) 0.3836(2) 0.0240(8) Uani 1 1 d . . . C6 C 0.58413(17) 1.0019(5) 0.4076(3) 0.0244(8) Uani 1 1 d . . . C7 C 0.63872(17) 0.7427(5) 0.4360(2) 0.0242(8) Uani 1 1 d . . . C8 C 0.68182(17) 0.6005(5) 0.4423(3) 0.0249(8) Uani 1 1 d . . . C9 C 0.68980(18) 0.4698(5) 0.5033(3) 0.0292(9) Uani 1 1 d . . . H9 H 0.6664 0.4677 0.5420 0.035 Uiso 1 1 calc R . . C10 C 0.73312(18) 0.3422(5) 0.5059(3) 0.0323(9) Uani 1 1 d . . . H10 H 0.7398 0.2508 0.5465 0.039 Uiso 1 1 calc R . . C11 C 0.7659(2) 0.3516(6) 0.4486(3) 0.0357(10) Uani 1 1 d . . . H11 H 0.7958 0.2666 0.4492 0.043 Uiso 1 1 calc R . . C12 C 0.7549(2) 0.4866(6) 0.3895(3) 0.0354(10) Uani 1 1 d . . . H12 H 0.7773 0.4904 0.3496 0.042 Uiso 1 1 calc R . . N51 N 0.43398(14) 0.8875(4) 0.4063(2) 0.0257(7) Uani 1 1 d . . . C51 C 0.39127(17) 0.8105(5) 0.3616(3) 0.0255(8) Uani 1 1 d . . . S51 S 0.33173(4) 0.70098(14) 0.29779(7) 0.0300(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe2 0.0182(4) 0.0260(5) 0.0268(4) 0.0002(3) 0.0111(3) 0.0011(3) N21 0.0195(16) 0.0276(18) 0.0294(18) -0.0026(14) 0.0093(14) -0.0004(12) N23 0.0212(16) 0.0324(19) 0.0321(19) -0.0003(14) 0.0143(14) 0.0028(13) N24 0.0231(17) 0.032(2) 0.036(2) -0.0053(15) 0.0142(15) 0.0008(13) C21 0.027(2) 0.030(2) 0.032(2) -0.0015(17) 0.0182(17) -0.0003(16) C22 0.032(2) 0.033(2) 0.031(2) -0.0020(17) 0.0178(18) -0.0059(17) C23 0.038(2) 0.036(3) 0.032(2) 0.0051(18) 0.0159(19) -0.0005(18) C24 0.030(2) 0.035(2) 0.029(2) -0.0005(18) 0.0119(17) 0.0031(17) C25 0.025(2) 0.030(2) 0.026(2) 0.0001(16) 0.0113(16) 0.0004(15) C26 0.0224(19) 0.024(2) 0.031(2) 0.0001(16) 0.0102(16) 0.0015(14) C27 0.022(2) 0.033(2) 0.032(2) -0.0010(17) 0.0106(17) -0.0010(16) C28 0.023(2) 0.028(2) 0.034(2) -0.0036(17) 0.0138(17) -0.0014(15) C29 0.028(2) 0.033(2) 0.032(2) 0.0022(18) 0.0123(17) -0.0018(16) C30 0.029(2) 0.044(3) 0.032(2) 0.0025(19) 0.0129(18) -0.0053(18) C31 0.031(2) 0.046(3) 0.038(3) -0.008(2) 0.0220(19) -0.0040(18) C32 0.028(2) 0.032(2) 0.035(2) -0.0057(18) 0.0160(18) 0.0009(16) S21 0.0248(5) 0.0334(6) 0.0325(6) 0.0016(4) 0.0148(4) 0.0057(4) N22 0.0203(16) 0.0290(18) 0.0321(19) 0.0007(14) 0.0137(14) 0.0017(13) N61 0.0196(16) 0.0300(19) 0.0335(19) -0.0017(14) 0.0140(15) 0.0012(13) C61 0.023(2) 0.026(2) 0.028(2) 0.0012(16) 0.0148(17) 0.0033(15) S61 0.0204(5) 0.0406(7) 0.0344(6) -0.0076(5) 0.0092(4) 0.0024(4) Fe1 0.0169(4) 0.0286(5) 0.0258(4) -0.0012(3) 0.0132(3) 0.0016(3) N1 0.0180(16) 0.0334(19) 0.0241(17) -0.0014(14) 0.0105(13) 0.0016(13) N2 0.0176(15) 0.0337(19) 0.0261(17) -0.0029(14) 0.0117(13) 0.0032(13) N3 0.0191(16) 0.0302(18) 0.0270(17) -0.0026(14) 0.0127(13) 0.0022(13) N4 0.0281(18) 0.037(2) 0.036(2) 0.0001(15) 0.0193(16) 0.0077(14) S1 0.0238(5) 0.0343(6) 0.0305(6) 0.0032(4) 0.0182(4) 0.0061(4) C1 0.021(2) 0.040(2) 0.035(2) 0.0016(19) 0.0171(17) 0.0055(16) C2 0.029(2) 0.033(2) 0.037(2) 0.0033(19) 0.0207(18) 0.0063(17) C3 0.027(2) 0.037(2) 0.026(2) 0.0019(17) 0.0144(16) 0.0004(17) C4 0.023(2) 0.033(2) 0.034(2) 0.0014(17) 0.0161(17) 0.0022(15) C5 0.0192(18) 0.033(2) 0.024(2) -0.0017(16) 0.0131(15) -0.0008(15) C6 0.0185(18) 0.030(2) 0.031(2) -0.0054(16) 0.0164(16) 0.0016(14) C7 0.0235(19) 0.030(2) 0.0220(19) 0.0004(16) 0.0114(15) 0.0018(15) C8 0.0212(19) 0.029(2) 0.027(2) -0.0008(16) 0.0115(16) 0.0018(15) C9 0.023(2) 0.034(2) 0.035(2) -0.0014(18) 0.0164(17) 0.0032(16) C10 0.031(2) 0.028(2) 0.042(3) 0.0030(18) 0.0169(19) 0.0021(16) C11 0.032(2) 0.038(3) 0.042(3) -0.002(2) 0.0178(19) 0.0125(18) C12 0.034(2) 0.045(3) 0.033(2) -0.0027(19) 0.0196(19) 0.0092(18) N51 0.0202(16) 0.0324(19) 0.0298(18) -0.0023(14) 0.0154(14) 0.0030(13) C51 0.021(2) 0.032(2) 0.030(2) -0.0004(17) 0.0164(17) 0.0061(16) S51 0.0213(5) 0.0395(6) 0.0340(6) -0.0051(4) 0.0155(4) -0.0043(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 Fe2 N61 1.940(3) . ? Fe2 N61 1.940(3) 3_766 ? Fe2 N22 1.984(3) . ? Fe2 N22 1.984(3) 3_766 ? Fe2 N21 2.008(3) 3_766 ? Fe2 N21 2.008(3) . ? N21 C21 1.332(5) . ? N21 C25 1.357(5) . ? N23 C27 1.312(5) . ? N23 N22 1.364(4) . ? N24 C32 1.342(5) . ? N24 C28 1.350(5) . ? C21 C22 1.400(6) . ? C22 C23 1.390(6) . ? C23 C24 1.391(6) . ? C24 C25 1.384(6) . ? C25 C26 1.450(5) . ? C26 N22 1.321(5) . ? C26 S21 1.711(4) . ? C27 C28 1.472(5) . ? C27 S21 1.725(4) . ? C28 C29 1.379(6) . ? C29 C30 1.393(6) . ? C30 C31 1.381(6) . ? C31 C32 1.388(6) . ? N61 C61 1.166(5) . ? C61 S61 1.631(4) . ? Fe1 N51 1.946(3) . ? Fe1 N51 1.946(3) 3_676 ? Fe1 N2 1.986(3) 3_676 ? Fe1 N2 1.986(3) . ? Fe1 N1 2.019(3) 3_676 ? Fe1 N1 2.019(3) . ? N1 C1 1.338(5) . ? N1 C5 1.369(4) . ? N2 C6 1.305(5) . ? N2 N3 1.374(4) . ? N3 C7 1.313(5) . ? N4 C12 1.336(5) . ? N4 C8 1.345(5) . ? S1 C6 1.716(4) . ? S1 C7 1.726(4) . ? C1 C2 1.392(6) . ? C2 C3 1.382(5) . ? C3 C4 1.388(6) . ? C4 C5 1.378(5) . ? C5 C6 1.461(5) . ? C7 C8 1.465(5) . ? C8 C9 1.394(6) . ? C9 C10 1.395(5) . ? C10 C11 1.377(6) . ? C11 C12 1.394(6) . ? N51 C51 1.163(5) . ? C51 S51 1.639(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 N61 Fe2 N61 179.998(1) . 3_766 ? N61 Fe2 N22 91.88(13) . . ? N61 Fe2 N22 88.12(13) 3_766 . ? N61 Fe2 N22 88.12(13) . 3_766 ? N61 Fe2 N22 91.88(13) 3_766 3_766 ? N22 Fe2 N22 180.00(19) . 3_766 ? N61 Fe2 N21 89.16(13) . 3_766 ? N61 Fe2 N21 90.83(13) 3_766 3_766 ? N22 Fe2 N21 99.09(13) . 3_766 ? N22 Fe2 N21 80.91(13) 3_766 3_766 ? N61 Fe2 N21 90.84(13) . . ? N61 Fe2 N21 89.16(13) 3_766 . ? N22 Fe2 N21 80.91(13) . . ? N22 Fe2 N21 99.09(13) 3_766 . ? N21 Fe2 N21 180.0 3_766 . ? C21 N21 C25 117.1(3) . . ? C21 N21 Fe2 129.3(3) . . ? C25 N21 Fe2 113.6(3) . . ? C27 N23 N22 111.4(3) . . ? C32 N24 C28 116.6(4) . . ? N21 C21 C22 123.3(4) . . ? C23 C22 C21 118.9(4) . . ? C22 C23 C24 118.4(4) . . ? C25 C24 C23 118.8(4) . . ? N21 C25 C24 123.5(4) . . ? N21 C25 C26 113.4(3) . . ? C24 C25 C26 123.0(4) . . ? N22 C26 C25 117.0(3) . . ? N22 C26 S21 113.9(3) . . ? C25 C26 S21 128.9(3) . . ? N23 C27 C28 124.2(4) . . ? N23 C27 S21 114.8(3) . . ? C28 C27 S21 121.0(3) . . ? N24 C28 C29 124.3(4) . . ? N24 C28 C27 113.7(4) . . ? C29 C28 C27 122.0(4) . . ? C28 C29 C30 117.9(4) . . ? C31 C30 C29 118.9(4) . . ? C30 C31 C32 119.0(4) . . ? N24 C32 C31 123.2(4) . . ? C26 S21 C27 86.79(19) . . ? C26 N22 N23 113.1(3) . . ? C26 N22 Fe2 113.6(3) . . ? N23 N22 Fe2 133.2(3) . . ? C61 N61 Fe2 175.8(3) . . ? N61 C61 S61 177.9(4) . . ? N51 Fe1 N51 179.997(1) . 3_676 ? N51 Fe1 N2 88.60(13) . 3_676 ? N51 Fe1 N2 91.40(13) 3_676 3_676 ? N51 Fe1 N2 91.40(13) . . ? N51 Fe1 N2 88.60(13) 3_676 . ? N2 Fe1 N2 179.998(2) 3_676 . ? N51 Fe1 N1 88.02(13) . 3_676 ? N51 Fe1 N1 91.97(13) 3_676 3_676 ? N2 Fe1 N1 80.42(13) 3_676 3_676 ? N2 Fe1 N1 99.58(13) . 3_676 ? N51 Fe1 N1 91.98(13) . . ? N51 Fe1 N1 88.03(13) 3_676 . ? N2 Fe1 N1 99.58(13) 3_676 . ? N2 Fe1 N1 80.42(13) . . ? N1 Fe1 N1 180.00(14) 3_676 . ? C1 N1 C5 116.6(3) . . ? C1 N1 Fe1 128.8(3) . . ? C5 N1 Fe1 114.5(3) . . ? C6 N2 N3 113.2(3) . . ? C6 N2 Fe1 114.9(3) . . ? N3 N2 Fe1 131.8(2) . . ? C7 N3 N2 110.5(3) . . ? C12 N4 C8 117.5(4) . . ? C6 S1 C7 86.01(18) . . ? N1 C1 C2 122.7(3) . . ? C3 C2 C1 120.0(4) . . ? C2 C3 C4 118.2(4) . . ? C5 C4 C3 118.8(4) . . ? N1 C5 C4 123.7(4) . . ? N1 C5 C6 112.0(3) . . ? C4 C5 C6 124.3(3) . . ? N2 C6 C5 117.8(3) . . ? N2 C6 S1 114.7(3) . . ? C5 C6 S1 127.4(3) . . ? N3 C7 C8 125.0(4) . . ? N3 C7 S1 115.6(3) . . ? C8 C7 S1 119.4(3) . . ? N4 C8 C9 123.5(3) . . ? N4 C8 C7 114.2(3) . . ? C9 C8 C7 122.3(3) . . ? C8 C9 C10 118.2(4) . . ? C11 C10 C9 118.6(4) . . ? C10 C11 C12 119.6(4) . . ? N4 C12 C11 122.7(4) . . ? C51 N51 Fe1 168.6(3) . . ? N51 C51 S51 179.2(4) . . ? 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 N61 Fe2 N21 C21 -79.9(3) . . . . ? N61 Fe2 N21 C21 100.1(4) 3_766 . . . ? N22 Fe2 N21 C21 -171.7(4) . . . . ? N22 Fe2 N21 C21 8.3(4) 3_766 . . . ? N21 Fe2 N21 C21 117(21) 3_766 . . . ? N61 Fe2 N21 C25 101.7(3) . . . . ? N61 Fe2 N21 C25 -78.3(3) 3_766 . . . ? N22 Fe2 N21 C25 10.0(3) . . . . ? N22 Fe2 N21 C25 -170.0(3) 3_766 . . . ? N21 Fe2 N21 C25 -61(21) 3_766 . . . ? C25 N21 C21 C22 0.8(6) . . . . ? Fe2 N21 C21 C22 -177.5(3) . . . . ? N21 C21 C22 C23 1.0(6) . . . . ? C21 C22 C23 C24 -1.9(6) . . . . ? C22 C23 C24 C25 0.9(6) . . . . ? C21 N21 C25 C24 -1.9(6) . . . . ? Fe2 N21 C25 C24 176.7(3) . . . . ? C21 N21 C25 C26 174.3(3) . . . . ? Fe2 N21 C25 C26 -7.1(4) . . . . ? C23 C24 C25 N21 1.0(6) . . . . ? C23 C24 C25 C26 -174.8(4) . . . . ? N21 C25 C26 N22 -2.4(5) . . . . ? C24 C25 C26 N22 173.8(4) . . . . ? N21 C25 C26 S21 -176.8(3) . . . . ? C24 C25 C26 S21 -0.6(6) . . . . ? N22 N23 C27 C28 179.9(3) . . . . ? N22 N23 C27 S21 0.2(4) . . . . ? C32 N24 C28 C29 1.3(6) . . . . ? C32 N24 C28 C27 -179.2(3) . . . . ? N23 C27 C28 N24 177.5(4) . . . . ? S21 C27 C28 N24 -2.8(5) . . . . ? N23 C27 C28 C29 -3.0(6) . . . . ? S21 C27 C28 C29 176.7(3) . . . . ? N24 C28 C29 C30 -1.0(6) . . . . ? C27 C28 C29 C30 179.5(4) . . . . ? C28 C29 C30 C31 0.0(6) . . . . ? C29 C30 C31 C32 0.7(6) . . . . ? C28 N24 C32 C31 -0.5(6) . . . . ? C30 C31 C32 N24 -0.4(7) . . . . ? N22 C26 S21 C27 -1.4(3) . . . . ? C25 C26 S21 C27 173.1(4) . . . . ? N23 C27 S21 C26 0.7(3) . . . . ? C28 C27 S21 C26 -179.0(3) . . . . ? C25 C26 N22 N23 -173.3(3) . . . . ? S21 C26 N22 N23 1.9(4) . . . . ? C25 C26 N22 Fe2 10.8(5) . . . . ? S21 C26 N22 Fe2 -174.00(18) . . . . ? C27 N23 N22 C26 -1.3(5) . . . . ? C27 N23 N22 Fe2 173.5(3) . . . . ? N61 Fe2 N22 C26 -101.8(3) . . . . ? N61 Fe2 N22 C26 78.2(3) 3_766 . . . ? N22 Fe2 N22 C26 -51(4) 3_766 . . . ? N21 Fe2 N22 C26 168.8(3) 3_766 . . . ? N21 Fe2 N22 C26 -11.2(3) . . . . ? N61 Fe2 N22 N23 83.4(3) . . . . ? N61 Fe2 N22 N23 -96.6(3) 3_766 . . . ? N22 Fe2 N22 N23 134(4) 3_766 . . . ? N21 Fe2 N22 N23 -6.0(4) 3_766 . . . ? N21 Fe2 N22 N23 174.0(4) . . . . ? N61 Fe2 N61 C61 -159(7) 3_766 . . . ? N22 Fe2 N61 C61 177(5) . . . . ? N22 Fe2 N61 C61 -3(5) 3_766 . . . ? N21 Fe2 N61 C61 -84(5) 3_766 . . . ? N21 Fe2 N61 C61 96(5) . . . . ? Fe2 N61 C61 S61 -105(10) . . . . ? N51 Fe1 N1 C1 86.8(3) . . . . ? N51 Fe1 N1 C1 -93.2(3) 3_676 . . . ? N2 Fe1 N1 C1 -2.1(4) 3_676 . . . ? N2 Fe1 N1 C1 177.9(4) . . . . ? N1 Fe1 N1 C1 -149(4) 3_676 . . . ? N51 Fe1 N1 C5 -96.1(3) . . . . ? N51 Fe1 N1 C5 83.9(3) 3_676 . . . ? N2 Fe1 N1 C5 175.0(3) 3_676 . . . ? N2 Fe1 N1 C5 -5.0(3) . . . . ? N1 Fe1 N1 C5 28(4) 3_676 . . . ? N51 Fe1 N2 C6 96.4(3) . . . . ? N51 Fe1 N2 C6 -83.6(3) 3_676 . . . ? N2 Fe1 N2 C6 -104(6) 3_676 . . . ? N1 Fe1 N2 C6 -175.4(3) 3_676 . . . ? N1 Fe1 N2 C6 4.6(3) . . . . ? N51 Fe1 N2 N3 -87.3(3) . . . . ? N51 Fe1 N2 N3 92.7(3) 3_676 . . . ? N2 Fe1 N2 N3 73(6) 3_676 . . . ? N1 Fe1 N2 N3 0.9(3) 3_676 . . . ? N1 Fe1 N2 N3 -179.1(3) . . . . ? C6 N2 N3 C7 -1.1(5) . . . . ? Fe1 N2 N3 C7 -177.4(3) . . . . ? C5 N1 C1 C2 -0.9(6) . . . . ? Fe1 N1 C1 C2 176.2(3) . . . . ? N1 C1 C2 C3 -0.4(7) . . . . ? C1 C2 C3 C4 0.8(6) . . . . ? C2 C3 C4 C5 -0.1(6) . . . . ? C1 N1 C5 C4 1.7(6) . . . . ? Fe1 N1 C5 C4 -175.8(3) . . . . ? C1 N1 C5 C6 -178.0(3) . . . . ? Fe1 N1 C5 C6 4.5(4) . . . . ? C3 C4 C5 N1 -1.3(6) . . . . ? C3 C4 C5 C6 178.5(4) . . . . ? N3 N2 C6 C5 179.4(3) . . . . ? Fe1 N2 C6 C5 -3.6(5) . . . . ? N3 N2 C6 S1 1.5(4) . . . . ? Fe1 N2 C6 S1 178.45(17) . . . . ? N1 C5 C6 N2 -0.6(5) . . . . ? C4 C5 C6 N2 179.6(4) . . . . ? N1 C5 C6 S1 177.0(3) . . . . ? C4 C5 C6 S1 -2.7(6) . . . . ? C7 S1 C6 N2 -1.1(3) . . . . ? C7 S1 C6 C5 -178.8(4) . . . . ? N2 N3 C7 C8 178.5(3) . . . . ? N2 N3 C7 S1 0.2(4) . . . . ? C6 S1 C7 N3 0.5(3) . . . . ? C6 S1 C7 C8 -177.9(3) . . . . ? C12 N4 C8 C9 1.3(6) . . . . ? C12 N4 C8 C7 179.2(4) . . . . ? N3 C7 C8 N4 171.7(4) . . . . ? S1 C7 C8 N4 -10.0(5) . . . . ? N3 C7 C8 C9 -10.3(6) . . . . ? S1 C7 C8 C9 167.9(3) . . . . ? N4 C8 C9 C10 -0.7(6) . . . . ? C7 C8 C9 C10 -178.4(4) . . . . ? C8 C9 C10 C11 0.1(6) . . . . ? C9 C10 C11 C12 -0.3(7) . . . . ? C8 N4 C12 C11 -1.5(6) . . . . ? C10 C11 C12 N4 1.1(7) . . . . ? N51 Fe1 N51 C51 -2(6) 3_676 . . . ? N2 Fe1 N51 C51 -51.6(16) 3_676 . . . ? N2 Fe1 N51 C51 128.4(16) . . . . ? N1 Fe1 N51 C51 28.9(16) 3_676 . . . ? N1 Fe1 N51 C51 -151.1(16) . . . . ? Fe1 N51 C51 S51 -137(29) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.219 _refine_diff_density_min -1.109 _refine_diff_density_rms 0.133