# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Chou-Fu Sheu' _publ_contact_author_email hiav8d.tw@yahoo.com.tw loop_ _publ_author_name 'Yu Wang' 'Szu-Miao Chen' 'Gene-Hsiang Lee' 'Yi-Hung Liu' ; Chou-Fu Sheu ; 'Shih-Chi Wang' data_PhaseD-300K _database_code_depnum_ccdc_archive 'CCDC 732121' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H20 Fe N14 S2' _chemical_formula_sum 'C26 H20 Fe N14 S2' _chemical_formula_weight 648.53 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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.8028(10) _cell_length_b 15.9264(7) _cell_length_c 17.4513(18) _cell_angle_alpha 90.000 _cell_angle_beta 106.809(7) _cell_angle_gamma 90.000 _cell_volume 2874.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 10541 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 27.50 _exptl_crystal_description Needle _exptl_crystal_colour Red-brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.715 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(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 KappaCCD _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28211 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.0751 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6581 _reflns_number_gt 3630 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD server software (Nonius, 1997)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL/PC & Mercury 1.4.1 (CCDC)' _computing_publication_material 'XIF in SHELXTL/PC' _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^)+(0.0404P)^2^+1.2809P] 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 6581 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1225 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 1.0000 0.0000 0.0000 0.03568(15) Uani 1 2 d S . . S1 S 1.44232(9) 0.05034(8) 0.16922(6) 0.0894(4) Uani 1 1 d . . . N1 N 0.9837(2) -0.10175(13) 0.08015(14) 0.0372(6) Uani 1 1 d . . . N2 N 0.9155(2) 0.05804(13) 0.08432(13) 0.0379(6) Uani 1 1 d . . . N3 N 1.1911(3) 0.02572(17) 0.07359(15) 0.0537(7) Uani 1 1 d . . . N4 N 0.8727(2) 0.13669(14) 0.09720(14) 0.0405(6) Uani 1 1 d . . . N5 N 0.7080(2) 0.18214(16) 0.24564(15) 0.0503(7) Uani 1 1 d . . . N6 N 0.8278(2) 0.04773(14) 0.18117(13) 0.0350(5) Uani 1 1 d . . . N7 N 0.7858(4) 0.01063(19) 0.2431(2) 0.0551(8) Uani 1 1 d . . . H1N H 0.725(5) 0.038(3) 0.246(3) 0.12(2) Uiso 1 1 d . . . H2N H 0.846(5) 0.028(3) 0.287(3) 0.13(2) Uiso 1 1 d . . . C1 C 1.0240(3) -0.18000(18) 0.07623(18) 0.0465(8) Uani 1 1 d . . . H1A H 1.0652 -0.1927 0.0377 0.056 Uiso 1 1 calc R . . C2 C 1.0081(3) -0.24314(19) 0.1262(2) 0.0516(8) Uani 1 1 d . . . H2A H 1.0369 -0.2973 0.1213 0.062 Uiso 1 1 calc R . . C3 C 0.9487(3) -0.22403(19) 0.1834(2) 0.0547(9) Uani 1 1 d . . . H3A H 0.9361 -0.2655 0.2180 0.066 Uiso 1 1 calc R . . C4 C 0.9075(3) -0.14298(18) 0.18958(18) 0.0494(8) Uani 1 1 d . . . H4B H 0.8678 -0.1289 0.2286 0.059 Uiso 1 1 calc R . . C5 C 0.9261(2) -0.08336(16) 0.13699(16) 0.0361(7) Uani 1 1 d . . . C6 C 0.8883(2) 0.00543(17) 0.13508(15) 0.0338(6) Uani 1 1 d . . . C7 C 0.8202(3) 0.12928(17) 0.15611(16) 0.0361(7) Uani 1 1 d . . . C8 C 0.7654(3) 0.19959(18) 0.18926(17) 0.0385(7) Uani 1 1 d . . . C9 C 0.7757(3) 0.28016(19) 0.1626(2) 0.0521(8) Uani 1 1 d . . . H9A H 0.8140 0.2899 0.1221 0.063 Uiso 1 1 calc R . . C10 C 0.7285(3) 0.3457(2) 0.1970(2) 0.0647(10) Uani 1 1 d . . . H10A H 0.7349 0.4007 0.1804 0.078 Uiso 1 1 calc R . . C11 C 0.6721(3) 0.3290(2) 0.2558(2) 0.0628(10) Uani 1 1 d . . . H11A H 0.6410 0.3723 0.2808 0.075 Uiso 1 1 calc R . . C12 C 0.6623(4) 0.2479(3) 0.2771(2) 0.0671(10) Uani 1 1 d . . . H12A H 0.6212 0.2372 0.3161 0.080 Uiso 1 1 calc R . . C13 C 1.2951(3) 0.03450(19) 0.11345(19) 0.0468(8) Uani 1 1 d . . . Fe2 Fe 1.0000 0.0000 0.5000 0.03520(15) Uani 1 2 d S . . S2 S 1.16722(8) 0.06799(5) 0.27670(5) 0.0512(2) Uani 1 1 d . . . N8 N 0.8687(2) -0.09753(13) 0.42912(13) 0.0371(6) Uani 1 1 d . . . N9 N 0.8143(2) 0.06013(14) 0.45791(14) 0.0417(6) Uani 1 1 d . . . N10 N 1.0534(3) 0.03632(16) 0.39741(16) 0.0528(7) Uani 1 1 d . . . N11 N 0.7646(2) 0.13486(15) 0.47492(14) 0.0454(6) Uani 1 1 d . . . N12 N 0.4278(3) 0.16707(18) 0.45321(16) 0.0603(8) Uani 1 1 d . . . N13 N 0.6050(2) 0.05028(15) 0.41543(14) 0.0406(6) Uani 1 1 d . . . N14 N 0.4802(3) 0.01622(19) 0.3794(2) 0.0595(8) Uani 1 1 d . . . H3N H 0.434(3) 0.045(2) 0.401(2) 0.071(13) Uiso 1 1 d . . . H4N H 0.469(4) 0.030(3) 0.327(3) 0.118(19) Uiso 1 1 d . . . C14 C 0.9040(3) -0.17462(18) 0.41317(17) 0.0451(8) Uani 1 1 d . . . H14A H 0.9909 -0.1892 0.4319 0.054 Uiso 1 1 calc R . . C15 C 0.8180(3) -0.23330(19) 0.3704(2) 0.0566(9) Uani 1 1 d . . . H15A H 0.8457 -0.2862 0.3600 0.068 Uiso 1 1 calc R . . C16 C 0.6904(4) -0.2112(2) 0.3436(2) 0.0687(10) Uani 1 1 d . . . H16A H 0.6295 -0.2497 0.3154 0.082 Uiso 1 1 calc R . . C17 C 0.6517(3) -0.1320(2) 0.3584(2) 0.0575(9) Uani 1 1 d . . . H17A H 0.5654 -0.1162 0.3393 0.069 Uiso 1 1 calc R . . C18 C 0.7426(3) -0.07674(17) 0.40180(16) 0.0378(7) Uani 1 1 d . . . C19 C 0.7180(2) 0.00929(17) 0.42320(16) 0.0366(7) Uani 1 1 d . . . C20 C 0.6381(3) 0.12765(18) 0.44862(16) 0.0405(7) Uani 1 1 d . . . C21 C 0.5476(3) 0.1932(2) 0.45744(17) 0.0474(8) Uani 1 1 d . . . C22 C 0.5877(3) 0.2754(2) 0.4708(2) 0.0637(10) Uani 1 1 d . . . H22A H 0.6714 0.2911 0.4725 0.076 Uiso 1 1 calc R . . C23 C 0.4991(4) 0.3341(3) 0.4815(2) 0.0831(13) Uani 1 1 d . . . H23A H 0.5225 0.3901 0.4913 0.100 Uiso 1 1 calc R . . C24 C 0.3766(4) 0.3078(3) 0.4773(2) 0.0845(14) Uani 1 1 d . . . H24A H 0.3156 0.3458 0.4843 0.101 Uiso 1 1 calc R . . C25 C 0.3450(4) 0.2250(3) 0.4627(2) 0.0773(12) Uani 1 1 d . . . H25A H 0.2610 0.2084 0.4592 0.093 Uiso 1 1 calc R . . C26 C 1.1019(3) 0.04968(17) 0.34764(18) 0.0403(7) 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 0.0379(3) 0.0339(3) 0.0355(3) 0.0008(3) 0.0110(2) 0.0001(3) S1 0.0412(5) 0.1368(10) 0.0787(7) 0.0266(7) -0.0006(5) -0.0190(6) N1 0.0366(13) 0.0314(13) 0.0414(14) 0.0001(11) 0.0078(11) 0.0001(11) N2 0.0457(14) 0.0304(13) 0.0397(14) 0.0042(11) 0.0156(11) 0.0031(11) N3 0.0443(16) 0.0663(18) 0.0469(17) 0.0006(13) 0.0075(13) -0.0050(14) N4 0.0490(15) 0.0328(14) 0.0418(15) 0.0025(11) 0.0164(12) 0.0042(11) N5 0.0543(16) 0.0520(17) 0.0470(16) -0.0025(13) 0.0188(13) 0.0072(13) N6 0.0353(13) 0.0362(14) 0.0342(13) 0.0062(11) 0.0112(10) 0.0000(11) N7 0.0592(19) 0.060(2) 0.055(2) 0.0176(16) 0.0297(16) 0.0080(18) C1 0.0480(19) 0.0379(18) 0.050(2) -0.0037(16) 0.0088(15) 0.0020(15) C2 0.0515(19) 0.0326(17) 0.061(2) -0.0001(17) 0.0014(17) -0.0024(15) C3 0.063(2) 0.0381(19) 0.059(2) 0.0154(16) 0.0106(18) -0.0056(16) C4 0.056(2) 0.0426(19) 0.049(2) 0.0090(15) 0.0154(16) -0.0023(16) C5 0.0332(15) 0.0324(17) 0.0385(17) 0.0002(13) 0.0038(13) -0.0032(13) C6 0.0328(14) 0.0360(16) 0.0307(15) 0.0009(14) 0.0063(11) -0.0017(13) C7 0.0337(15) 0.0381(17) 0.0352(17) 0.0013(14) 0.0083(13) 0.0003(13) C8 0.0310(15) 0.0442(19) 0.0370(17) -0.0016(14) 0.0046(13) 0.0032(13) C9 0.055(2) 0.0421(18) 0.061(2) 0.0038(16) 0.0192(17) 0.0072(16) C10 0.060(2) 0.044(2) 0.082(3) 0.0001(19) 0.009(2) 0.0126(17) C11 0.061(2) 0.063(3) 0.057(2) -0.0141(19) 0.0044(19) 0.0234(19) C12 0.075(3) 0.077(3) 0.054(2) -0.001(2) 0.0257(19) 0.023(2) C13 0.0480(19) 0.0485(18) 0.0449(19) 0.0073(15) 0.0149(16) -0.0037(16) Fe2 0.0272(3) 0.0385(3) 0.0398(3) -0.0027(3) 0.0095(2) 0.0025(3) S2 0.0520(5) 0.0561(5) 0.0500(5) 0.0043(4) 0.0220(4) 0.0047(4) N8 0.0354(13) 0.0353(14) 0.0417(14) 0.0009(11) 0.0131(11) 0.0028(11) N9 0.0311(13) 0.0407(14) 0.0514(16) -0.0083(12) 0.0088(11) 0.0036(12) N10 0.0554(17) 0.0579(17) 0.0502(17) 0.0015(14) 0.0233(14) 0.0002(14) N11 0.0342(14) 0.0434(15) 0.0547(16) -0.0106(12) 0.0068(12) 0.0072(11) N12 0.0414(17) 0.081(2) 0.0573(18) 0.0020(15) 0.0125(13) 0.0227(15) N13 0.0265(13) 0.0473(16) 0.0441(15) -0.0012(12) 0.0039(11) 0.0016(11) N14 0.0288(15) 0.064(2) 0.079(3) -0.0100(19) 0.0037(15) -0.0001(14) C14 0.0449(18) 0.0455(19) 0.0474(19) 0.0004(15) 0.0171(15) 0.0069(15) C15 0.065(2) 0.039(2) 0.067(2) -0.0112(17) 0.0211(19) -0.0001(17) C16 0.065(3) 0.053(2) 0.082(3) -0.019(2) 0.011(2) -0.0111(19) C17 0.0400(18) 0.053(2) 0.072(2) -0.0113(18) 0.0039(16) -0.0032(16) C18 0.0357(16) 0.0380(17) 0.0385(17) 0.0000(13) 0.0091(13) -0.0003(13) C19 0.0277(14) 0.0431(18) 0.0367(16) 0.0009(14) 0.0055(12) 0.0035(14) C20 0.0345(17) 0.0469(18) 0.0379(17) -0.0015(14) 0.0069(13) 0.0085(14) C21 0.0391(18) 0.062(2) 0.0378(18) -0.0058(16) 0.0056(14) 0.0148(16) C22 0.056(2) 0.064(2) 0.066(2) -0.0166(19) 0.0091(18) 0.0147(18) C23 0.088(3) 0.069(3) 0.080(3) -0.025(2) 0.005(2) 0.033(2) C24 0.069(3) 0.110(4) 0.068(3) -0.014(2) 0.009(2) 0.055(3) C25 0.052(2) 0.108(3) 0.070(3) -0.005(2) 0.0152(19) 0.031(2) C26 0.0369(16) 0.0372(17) 0.0438(19) -0.0044(15) 0.0069(14) 0.0016(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N3 2.132(3) 3_755 ? Fe1 N3 2.132(3) . ? Fe1 N2 2.152(2) . ? Fe1 N2 2.152(2) 3_755 ? Fe1 N1 2.181(2) . ? Fe1 N1 2.181(2) 3_755 ? S1 C13 1.627(3) . ? N1 C1 1.329(3) . ? N1 C5 1.347(3) . ? N2 C6 1.313(3) . ? N2 N4 1.376(3) . ? N3 C13 1.146(4) . ? N4 C7 1.316(3) . ? N5 C8 1.335(3) . ? N5 C12 1.341(4) . ? N6 C6 1.353(3) . ? N6 C7 1.365(3) . ? N6 N7 1.416(3) . ? N7 H1N 0.81(5) . ? N7 H2N 0.89(5) . ? C1 C2 1.374(4) . ? C1 H1A 0.9300 . ? C2 C3 1.368(4) . ? C2 H2A 0.9300 . ? C3 C4 1.380(4) . ? C3 H3A 0.9300 . ? C4 C5 1.375(4) . ? C4 H4B 0.9300 . ? C5 C6 1.470(4) . ? C7 C8 1.462(4) . ? C8 C9 1.380(4) . ? C9 C10 1.375(4) . ? C9 H9A 0.9300 . ? C10 C11 1.362(5) . ? C10 H10A 0.9300 . ? C11 C12 1.355(5) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? Fe2 N10 2.114(3) 3_756 ? Fe2 N10 2.114(3) . ? Fe2 N9 2.152(2) 3_756 ? Fe2 N9 2.152(2) . ? Fe2 N8 2.222(2) . ? Fe2 N8 2.222(2) 3_756 ? S2 C26 1.619(3) . ? N8 C14 1.339(3) . ? N8 C18 1.349(3) . ? N9 C19 1.319(3) . ? N9 N11 1.373(3) . ? N10 C26 1.156(3) . ? N11 C20 1.315(3) . ? N12 C25 1.328(4) . ? N12 C21 1.341(4) . ? N13 C19 1.356(3) . ? N13 C20 1.365(3) . ? N13 N14 1.421(3) . ? N14 H3N 0.84(3) . ? N14 H4N 0.91(4) . ? C14 C15 1.376(4) . ? C14 H14A 0.9300 . ? C15 C16 1.368(5) . ? C15 H15A 0.9300 . ? C16 C17 1.376(4) . ? C16 H16A 0.9300 . ? C17 C18 1.371(4) . ? C17 H17A 0.9300 . ? C18 C19 1.465(4) . ? C20 C21 1.468(4) . ? C21 C22 1.377(4) . ? C22 C23 1.388(5) . ? C22 H22A 0.9300 . ? C23 C24 1.370(6) . ? C23 H23A 0.9300 . ? C24 C25 1.367(6) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? 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 N3 Fe1 N3 180.0(2) 3_755 . ? N3 Fe1 N2 88.06(9) 3_755 . ? N3 Fe1 N2 91.94(9) . . ? N3 Fe1 N2 91.94(9) 3_755 3_755 ? N3 Fe1 N2 88.06(9) . 3_755 ? N2 Fe1 N2 180.00(14) . 3_755 ? N3 Fe1 N1 89.99(9) 3_755 . ? N3 Fe1 N1 90.01(9) . . ? N2 Fe1 N1 75.62(8) . . ? N2 Fe1 N1 104.38(8) 3_755 . ? N3 Fe1 N1 90.01(9) 3_755 3_755 ? N3 Fe1 N1 89.99(9) . 3_755 ? N2 Fe1 N1 104.38(8) . 3_755 ? N2 Fe1 N1 75.62(8) 3_755 3_755 ? N1 Fe1 N1 180.00(15) . 3_755 ? C1 N1 C5 118.1(2) . . ? C1 N1 Fe1 125.1(2) . . ? C5 N1 Fe1 116.81(17) . . ? C6 N2 N4 108.6(2) . . ? C6 N2 Fe1 114.15(17) . . ? N4 N2 Fe1 137.03(17) . . ? C13 N3 Fe1 175.9(3) . . ? C7 N4 N2 106.7(2) . . ? C8 N5 C12 116.3(3) . . ? C6 N6 C7 106.1(2) . . ? C6 N6 N7 124.2(2) . . ? C7 N6 N7 129.7(2) . . ? N6 N7 H1N 106(3) . . ? N6 N7 H2N 102(3) . . ? H1N N7 H2N 100(4) . . ? N1 C1 C2 123.4(3) . . ? N1 C1 H1A 118.3 . . ? C2 C1 H1A 118.3 . . ? C3 C2 C1 118.1(3) . . ? C3 C2 H2A 120.9 . . ? C1 C2 H2A 120.9 . . ? C2 C3 C4 119.7(3) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 118.8(3) . . ? C5 C4 H4B 120.6 . . ? C3 C4 H4B 120.6 . . ? N1 C5 C4 122.0(3) . . ? N1 C5 C6 112.2(2) . . ? C4 C5 C6 125.9(3) . . ? N2 C6 N6 108.9(2) . . ? N2 C6 C5 121.0(2) . . ? N6 C6 C5 130.1(2) . . ? N4 C7 N6 109.6(2) . . ? N4 C7 C8 123.8(3) . . ? N6 C7 C8 126.6(2) . . ? N5 C8 C9 122.8(3) . . ? N5 C8 C7 117.4(3) . . ? C9 C8 C7 119.8(3) . . ? C10 C9 C8 118.9(3) . . ? C10 C9 H9A 120.6 . . ? C8 C9 H9A 120.6 . . ? C11 C10 C9 118.9(3) . . ? C11 C10 H10A 120.6 . . ? C9 C10 H10A 120.6 . . ? C12 C11 C10 118.7(3) . . ? C12 C11 H11A 120.7 . . ? C10 C11 H11A 120.7 . . ? N5 C12 C11 124.4(3) . . ? N5 C12 H12A 117.8 . . ? C11 C12 H12A 117.8 . . ? N3 C13 S1 178.0(3) . . ? N10 Fe2 N10 180.000(1) 3_756 . ? N10 Fe2 N9 92.58(9) 3_756 3_756 ? N10 Fe2 N9 87.42(9) . 3_756 ? N10 Fe2 N9 87.42(9) 3_756 . ? N10 Fe2 N9 92.58(9) . . ? N9 Fe2 N9 180.0 3_756 . ? N10 Fe2 N8 89.64(9) 3_756 . ? N10 Fe2 N8 90.36(9) . . ? N9 Fe2 N8 105.12(8) 3_756 . ? N9 Fe2 N8 74.88(8) . . ? N10 Fe2 N8 90.36(9) 3_756 3_756 ? N10 Fe2 N8 89.64(9) . 3_756 ? N9 Fe2 N8 74.88(8) 3_756 3_756 ? N9 Fe2 N8 105.12(8) . 3_756 ? N8 Fe2 N8 180.00(11) . 3_756 ? C14 N8 C18 118.1(2) . . ? C14 N8 Fe2 125.63(19) . . ? C18 N8 Fe2 116.24(17) . . ? C19 N9 N11 109.0(2) . . ? C19 N9 Fe2 114.66(17) . . ? N11 N9 Fe2 134.13(17) . . ? C26 N10 Fe2 168.6(3) . . ? C20 N11 N9 106.3(2) . . ? C25 N12 C21 116.8(3) . . ? C19 N13 C20 106.0(2) . . ? C19 N13 N14 124.9(2) . . ? C20 N13 N14 129.1(2) . . ? N13 N14 H3N 102(2) . . ? N13 N14 H4N 101(3) . . ? H3N N14 H4N 113(4) . . ? N8 C14 C15 123.2(3) . . ? N8 C14 H14A 118.4 . . ? C15 C14 H14A 118.4 . . ? C16 C15 C14 117.8(3) . . ? C16 C15 H15A 121.1 . . ? C14 C15 H15A 121.1 . . ? C15 C16 C17 120.2(3) . . ? C15 C16 H16A 119.9 . . ? C17 C16 H16A 119.9 . . ? C18 C17 C16 119.0(3) . . ? C18 C17 H17A 120.5 . . ? C16 C17 H17A 120.5 . . ? N8 C18 C17 121.8(3) . . ? N8 C18 C19 112.3(2) . . ? C17 C18 C19 126.0(3) . . ? N9 C19 N13 108.5(2) . . ? N9 C19 C18 120.9(2) . . ? N13 C19 C18 130.5(2) . . ? N11 C20 N13 110.2(2) . . ? N11 C20 C21 123.9(3) . . ? N13 C20 C21 125.9(3) . . ? N12 C21 C22 123.8(3) . . ? N12 C21 C20 115.7(3) . . ? C22 C21 C20 120.5(3) . . ? C21 C22 C23 117.9(3) . . ? C21 C22 H22A 121.1 . . ? C23 C22 H22A 121.1 . . ? C24 C23 C22 118.7(4) . . ? C24 C23 H23A 120.7 . . ? C22 C23 H23A 120.7 . . ? C25 C24 C23 119.4(3) . . ? C25 C24 H24A 120.3 . . ? C23 C24 H24A 120.3 . . ? N12 C25 C24 123.5(4) . . ? N12 C25 H25A 118.2 . . ? C24 C25 H25A 118.2 . . ? N10 C26 S2 178.9(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.545 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.056 # Attachment 'CCDC 732122_PhaseD_90K_F_v.cif' data_PhaseD-90K _database_code_depnum_ccdc_archive 'CCDC 732122' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H20 Fe N14 S2' _chemical_formula_sum 'C26 H20 Fe N14 S2' _chemical_formula_weight 648.53 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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.8074(5) _cell_length_b 15.7251(10) _cell_length_c 17.0180(7) _cell_angle_alpha 90.000 _cell_angle_beta 107.652(4) _cell_angle_gamma 90.000 _cell_volume 2755.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 11263 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.5 _exptl_crystal_description Needle _exptl_crystal_colour Red-brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.879 _exptl_absorpt_correction_T_max 0.941 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 KappaCCD _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25192 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.0767 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6302 _reflns_number_gt 4185 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD server software (Nonius, 1997)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL/PC & Mercury 1.4.1 (CCDC)' _computing_publication_material 'XIF in SHELXTL/PC' _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^)+(0.0359P)^2^+2.4570P] 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 6302 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0906 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.0961 _refine_ls_wR_factor_gt 0.0813 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 1.0000 0.0000 0.0000 0.00857(12) Uani 1 2 d S . . S1 S 1.43445(7) 0.04867(5) 0.16766(4) 0.02148(18) Uani 1 1 d . . . N1 N 0.9928(2) -0.10112(13) 0.06930(13) 0.0101(5) Uani 1 1 d . . . N2 N 0.9207(2) 0.05289(13) 0.07866(13) 0.0095(5) Uani 1 1 d . . . N3 N 1.1758(2) 0.02411(13) 0.07093(13) 0.0110(5) Uani 1 1 d . . . N4 N 0.8764(2) 0.13185(13) 0.09224(13) 0.0111(5) Uani 1 1 d . . . N5 N 0.7054(2) 0.17221(14) 0.24240(13) 0.0143(5) Uani 1 1 d . . . N6 N 0.8313(2) 0.03937(13) 0.17675(12) 0.0102(5) Uani 1 1 d . . . N7 N 0.7894(3) -0.00126(17) 0.23865(15) 0.0158(5) Uani 1 1 d . . . H1N H 0.722(4) 0.027(3) 0.242(3) 0.070(15) Uiso 1 1 d . . . H2N H 0.844(4) 0.015(2) 0.283(2) 0.051(13) Uiso 1 1 d . . . C1 C 1.0394(3) -0.17873(16) 0.06265(16) 0.0117(6) Uani 1 1 d . . . H1A H 1.0820 -0.1876 0.0234 0.014 Uiso 1 1 calc R . . C2 C 1.0269(2) -0.24647(17) 0.11176(15) 0.0124(5) Uani 1 1 d . . . H2A H 1.0596 -0.2997 0.1048 0.015 Uiso 1 1 calc R . . C3 C 0.9652(3) -0.23412(16) 0.17132(16) 0.0135(6) Uani 1 1 d . . . H3A H 0.9553 -0.2789 0.2046 0.016 Uiso 1 1 calc R . . C4 C 0.9184(2) -0.15348(16) 0.18030(16) 0.0121(6) Uani 1 1 d . . . H4B H 0.8774 -0.1430 0.2201 0.015 Uiso 1 1 calc R . . C5 C 0.9342(2) -0.08940(16) 0.12891(15) 0.0105(6) Uani 1 1 d . . . C6 C 0.8929(2) -0.00171(16) 0.12967(14) 0.0093(5) Uani 1 1 d . . . C7 C 0.8235(2) 0.12274(16) 0.15244(15) 0.0102(5) Uani 1 1 d . . . C8 C 0.7664(2) 0.19255(16) 0.18685(15) 0.0106(6) Uani 1 1 d . . . C9 C 0.7794(3) 0.27560(16) 0.16233(17) 0.0143(6) Uani 1 1 d . . . H9A H 0.8194 0.2869 0.1222 0.017 Uiso 1 1 calc R . . C10 C 0.7314(3) 0.34084(18) 0.19897(17) 0.0183(6) Uani 1 1 d . . . H10A H 0.7395 0.3971 0.1843 0.022 Uiso 1 1 calc R . . C11 C 0.6714(3) 0.32166(18) 0.25760(16) 0.0170(6) Uani 1 1 d . . . H11A H 0.6406 0.3646 0.2843 0.020 Uiso 1 1 calc R . . C12 C 0.6582(3) 0.23721(18) 0.27567(17) 0.0177(6) Uani 1 1 d . . . H12A H 0.6138 0.2246 0.3133 0.021 Uiso 1 1 calc R . . C13 C 1.2828(3) 0.03278(17) 0.11145(16) 0.0118(6) Uani 1 1 d . . . Fe2 Fe 1.0000 0.0000 0.5000 0.00885(12) Uani 1 2 d S . . S2 S 1.16896(7) 0.06697(4) 0.27276(4) 0.01438(16) Uani 1 1 d . . . N8 N 0.8684(2) -0.09877(13) 0.42709(13) 0.0103(5) Uani 1 1 d . . . N9 N 0.8120(2) 0.05905(13) 0.45998(13) 0.0117(5) Uani 1 1 d . . . N10 N 1.0455(2) 0.03930(14) 0.39325(14) 0.0156(5) Uani 1 1 d . . . N11 N 0.7614(2) 0.13432(14) 0.47823(13) 0.0131(5) Uani 1 1 d . . . N12 N 0.4231(2) 0.16556(15) 0.45624(14) 0.0163(5) Uani 1 1 d . . . N13 N 0.6007(2) 0.04777(14) 0.41603(13) 0.0112(5) Uani 1 1 d . . . N14 N 0.4758(2) 0.01301(16) 0.37917(17) 0.0168(5) Uani 1 1 d . . . H3N H 0.426(3) 0.0423(18) 0.3964(17) 0.015(8) Uiso 1 1 d . . . H4N H 0.456(3) 0.027(2) 0.325(2) 0.032(10) Uiso 1 1 d . . . C14 C 0.9051(3) -0.17574(16) 0.40843(16) 0.0124(6) Uani 1 1 d . . . H14A H 0.9930 -0.1893 0.4260 0.015 Uiso 1 1 calc R . . C15 C 0.8182(3) -0.23597(17) 0.36425(16) 0.0159(6) Uani 1 1 d . . . H15A H 0.8469 -0.2889 0.3528 0.019 Uiso 1 1 calc R . . C16 C 0.6880(3) -0.21557(18) 0.33762(18) 0.0201(7) Uani 1 1 d . . . H16A H 0.6274 -0.2550 0.3082 0.024 Uiso 1 1 calc R . . C17 C 0.6481(3) -0.13564(17) 0.35509(17) 0.0179(6) Uani 1 1 d . . . H17A H 0.5609 -0.1204 0.3369 0.022 Uiso 1 1 calc R . . C18 C 0.7409(2) -0.07915(16) 0.40006(15) 0.0113(6) Uani 1 1 d . . . C19 C 0.7150(2) 0.00724(16) 0.42349(15) 0.0110(5) Uani 1 1 d . . . C20 C 0.6342(3) 0.12645(17) 0.45102(15) 0.0122(6) Uani 1 1 d . . . C21 C 0.5424(3) 0.19238(17) 0.45934(16) 0.0141(6) Uani 1 1 d . . . C22 C 0.5820(3) 0.27698(18) 0.47106(17) 0.0206(7) Uani 1 1 d . . . H22A H 0.6650 0.2931 0.4714 0.025 Uiso 1 1 calc R . . C23 C 0.4942(3) 0.3365(2) 0.48227(18) 0.0263(8) Uani 1 1 d . . . H23A H 0.5174 0.3934 0.4914 0.032 Uiso 1 1 calc R . . C24 C 0.3717(3) 0.3093(2) 0.47957(18) 0.0268(8) Uani 1 1 d . . . H24A H 0.3110 0.3479 0.4871 0.032 Uiso 1 1 calc R . . C25 C 0.3401(3) 0.22483(19) 0.46569(17) 0.0227(7) Uani 1 1 d . . . H25A H 0.2563 0.2080 0.4627 0.027 Uiso 1 1 calc R . . C26 C 1.0986(2) 0.05098(16) 0.34349(16) 0.0117(6) 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 0.0086(3) 0.0079(3) 0.0099(3) 0.0004(2) 0.0038(2) -0.0003(2) S1 0.0094(3) 0.0324(5) 0.0214(4) 0.0049(3) 0.0028(3) -0.0026(3) N1 0.0078(11) 0.0111(12) 0.0104(11) -0.0018(9) 0.0013(9) -0.0008(9) N2 0.0081(11) 0.0074(11) 0.0124(11) 0.0005(9) 0.0024(9) -0.0001(9) N3 0.0138(12) 0.0094(12) 0.0124(11) 0.0008(9) 0.0076(10) 0.0000(9) N4 0.0102(12) 0.0102(11) 0.0135(11) -0.0011(9) 0.0045(10) 0.0020(9) N5 0.0147(12) 0.0149(12) 0.0155(12) -0.0006(10) 0.0079(10) 0.0026(10) N6 0.0111(11) 0.0111(11) 0.0098(11) 0.0013(9) 0.0051(9) 0.0001(9) N7 0.0172(13) 0.0196(13) 0.0149(13) 0.0052(11) 0.0112(11) 0.0022(12) C1 0.0111(14) 0.0125(14) 0.0123(14) -0.0011(11) 0.0049(11) 0.0003(11) C2 0.0110(13) 0.0094(13) 0.0157(13) 0.0015(12) 0.0024(11) -0.0005(12) C3 0.0130(14) 0.0124(15) 0.0137(13) 0.0034(11) 0.0019(11) -0.0034(11) C4 0.0099(14) 0.0140(15) 0.0135(13) 0.0017(11) 0.0049(11) -0.0018(11) C5 0.0069(13) 0.0109(14) 0.0126(13) -0.0007(11) 0.0014(11) -0.0020(11) C6 0.0080(12) 0.0101(13) 0.0102(12) 0.0001(11) 0.0032(10) -0.0011(11) C7 0.0081(13) 0.0098(14) 0.0110(13) -0.0007(11) 0.0005(11) -0.0018(11) C8 0.0055(13) 0.0149(14) 0.0103(13) -0.0022(11) 0.0010(11) -0.0007(11) C9 0.0117(14) 0.0139(14) 0.0178(15) 0.0004(11) 0.0053(12) 0.0015(11) C10 0.0144(15) 0.0138(15) 0.0242(16) -0.0015(12) 0.0021(13) 0.0015(12) C11 0.0163(15) 0.0146(15) 0.0177(15) -0.0052(12) 0.0017(13) 0.0061(12) C12 0.0160(15) 0.0229(17) 0.0156(14) -0.0003(12) 0.0070(12) 0.0061(13) C13 0.0133(15) 0.0112(14) 0.0119(13) 0.0019(11) 0.0053(12) 0.0012(12) Fe2 0.0070(3) 0.0096(3) 0.0111(3) -0.0003(2) 0.0044(2) -0.0002(2) S2 0.0139(4) 0.0161(4) 0.0155(3) 0.0019(3) 0.0080(3) 0.0021(3) N8 0.0107(12) 0.0107(12) 0.0116(11) 0.0010(9) 0.0063(9) 0.0004(9) N9 0.0104(11) 0.0105(11) 0.0143(11) -0.0019(9) 0.0039(10) 0.0027(10) N10 0.0160(12) 0.0153(13) 0.0160(12) -0.0015(10) 0.0059(10) -0.0015(10) N11 0.0116(12) 0.0120(12) 0.0170(12) -0.0022(10) 0.0064(10) 0.0045(10) N12 0.0090(12) 0.0244(13) 0.0152(12) 0.0023(10) 0.0033(10) 0.0065(10) N13 0.0053(11) 0.0140(12) 0.0141(12) 0.0003(9) 0.0025(9) -0.0001(9) N14 0.0065(12) 0.0198(14) 0.0236(14) -0.0014(11) 0.0038(11) 0.0001(10) C14 0.0117(14) 0.0126(14) 0.0143(14) 0.0015(11) 0.0060(11) 0.0035(11) C15 0.0217(16) 0.0102(15) 0.0180(14) -0.0031(11) 0.0096(12) 0.0001(12) C16 0.0165(16) 0.0200(16) 0.0230(16) -0.0054(13) 0.0049(13) -0.0051(13) C17 0.0116(14) 0.0193(16) 0.0208(15) -0.0016(12) 0.0018(12) -0.0029(12) C18 0.0102(14) 0.0133(14) 0.0115(13) 0.0023(11) 0.0051(11) 0.0007(11) C19 0.0090(13) 0.0129(14) 0.0107(13) 0.0012(11) 0.0024(11) 0.0015(12) C20 0.0116(14) 0.0150(14) 0.0109(13) 0.0000(11) 0.0051(11) 0.0014(11) C21 0.0117(14) 0.0195(15) 0.0094(13) -0.0010(11) 0.0010(12) 0.0054(12) C22 0.0170(16) 0.0210(16) 0.0233(16) -0.0059(13) 0.0055(13) 0.0037(13) C23 0.0275(18) 0.0209(17) 0.0253(18) -0.0082(13) 0.0006(15) 0.0103(14) C24 0.0222(17) 0.036(2) 0.0181(16) -0.0047(14) 0.0004(14) 0.0190(15) C25 0.0137(15) 0.0351(19) 0.0196(16) 0.0008(13) 0.0053(13) 0.0088(14) C26 0.0105(13) 0.0098(14) 0.0135(14) -0.0007(11) 0.0018(11) 0.0023(11) _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 N3 1.955(2) 3_755 ? Fe1 N3 1.955(2) . ? Fe1 N2 1.978(2) . ? Fe1 N2 1.978(2) 3_755 ? Fe1 N1 1.995(2) . ? Fe1 N1 1.995(2) 3_755 ? S1 C13 1.647(3) . ? N1 C1 1.338(3) . ? N1 C5 1.362(3) . ? N2 C6 1.319(3) . ? N2 N4 1.375(3) . ? N3 C13 1.161(3) . ? N4 C7 1.324(3) . ? N5 C12 1.342(3) . ? N5 C8 1.345(3) . ? N6 C6 1.351(3) . ? N6 C7 1.370(3) . ? N6 N7 1.418(3) . ? N7 H1N 0.86(4) . ? N7 H2N 0.84(4) . ? C1 C2 1.386(4) . ? C1 H1A 0.9300 . ? C2 C3 1.385(4) . ? C2 H2A 0.9300 . ? C3 C4 1.391(4) . ? C3 H3A 0.9300 . ? C4 C5 1.378(3) . ? C4 H4B 0.9300 . ? C5 C6 1.451(4) . ? C7 C8 1.466(4) . ? C8 C9 1.391(4) . ? C9 C10 1.381(4) . ? C9 H9A 0.9300 . ? C10 C11 1.378(4) . ? C10 H10A 0.9300 . ? C11 C12 1.380(4) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? Fe2 N10 2.113(2) 3_756 ? Fe2 N10 2.113(2) . ? Fe2 N9 2.148(2) . ? Fe2 N9 2.148(2) 3_756 ? Fe2 N8 2.215(2) . ? Fe2 N8 2.215(2) 3_756 ? S2 C26 1.626(3) . ? N8 C14 1.341(3) . ? N8 C18 1.350(3) . ? N9 C19 1.324(3) . ? N9 N11 1.378(3) . ? N10 C26 1.173(3) . ? N11 C20 1.317(3) . ? N12 C25 1.337(3) . ? N12 C21 1.342(3) . ? N13 C19 1.361(3) . ? N13 C20 1.373(3) . ? N13 N14 1.415(3) . ? N14 H3N 0.83(3) . ? N14 H4N 0.91(3) . ? C14 C15 1.384(4) . ? C14 H14A 0.9300 . ? C15 C16 1.379(4) . ? C15 H15A 0.9300 . ? C16 C17 1.390(4) . ? C16 H16A 0.9300 . ? C17 C18 1.384(4) . ? C17 H17A 0.9300 . ? C18 C19 1.466(4) . ? C20 C21 1.471(4) . ? C21 C22 1.393(4) . ? C22 C23 1.387(4) . ? C22 H22A 0.9300 . ? C23 C24 1.378(5) . ? C23 H23A 0.9300 . ? C24 C25 1.375(4) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? 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 N3 Fe1 N3 180.0(2) 3_755 . ? N3 Fe1 N2 87.70(8) 3_755 . ? N3 Fe1 N2 92.30(8) . . ? N3 Fe1 N2 92.30(8) 3_755 3_755 ? N3 Fe1 N2 87.70(8) . 3_755 ? N2 Fe1 N2 180.00(15) . 3_755 ? N3 Fe1 N1 90.32(8) 3_755 . ? N3 Fe1 N1 89.68(8) . . ? N2 Fe1 N1 80.37(8) . . ? N2 Fe1 N1 99.63(8) 3_755 . ? N3 Fe1 N1 89.68(8) 3_755 3_755 ? N3 Fe1 N1 90.32(8) . 3_755 ? N2 Fe1 N1 99.63(8) . 3_755 ? N2 Fe1 N1 80.37(8) 3_755 3_755 ? N1 Fe1 N1 180.00(12) . 3_755 ? C1 N1 C5 117.3(2) . . ? C1 N1 Fe1 126.44(17) . . ? C5 N1 Fe1 116.28(17) . . ? C6 N2 N4 108.5(2) . . ? C6 N2 Fe1 113.80(17) . . ? N4 N2 Fe1 137.51(16) . . ? C13 N3 Fe1 175.1(2) . . ? C7 N4 N2 106.6(2) . . ? C12 N5 C8 116.5(2) . . ? C6 N6 C7 105.9(2) . . ? C6 N6 N7 123.4(2) . . ? C7 N6 N7 130.6(2) . . ? N6 N7 H1N 106(3) . . ? N6 N7 H2N 104(3) . . ? H1N N7 H2N 100(4) . . ? N1 C1 C2 122.8(2) . . ? N1 C1 H1A 118.6 . . ? C2 C1 H1A 118.6 . . ? C3 C2 C1 119.4(2) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C2 C3 C4 118.7(2) . . ? C2 C3 H3A 120.7 . . ? C4 C3 H3A 120.7 . . ? C5 C4 C3 118.5(2) . . ? C5 C4 H4B 120.7 . . ? C3 C4 H4B 120.7 . . ? N1 C5 C4 123.3(2) . . ? N1 C5 C6 110.4(2) . . ? C4 C5 C6 126.3(2) . . ? N2 C6 N6 109.3(2) . . ? N2 C6 C5 118.7(2) . . ? N6 C6 C5 131.9(2) . . ? N4 C7 N6 109.6(2) . . ? N4 C7 C8 124.1(2) . . ? N6 C7 C8 126.2(2) . . ? N5 C8 C9 123.3(2) . . ? N5 C8 C7 117.3(2) . . ? C9 C8 C7 119.4(2) . . ? C10 C9 C8 118.5(3) . . ? C10 C9 H9A 120.8 . . ? C8 C9 H9A 120.8 . . ? C11 C10 C9 119.2(3) . . ? C11 C10 H10A 120.4 . . ? C9 C10 H10A 120.4 . . ? C10 C11 C12 118.4(3) . . ? C10 C11 H11A 120.8 . . ? C12 C11 H11A 120.8 . . ? N5 C12 C11 124.1(3) . . ? N5 C12 H12A 118.0 . . ? C11 C12 H12A 118.0 . . ? N3 C13 S1 177.9(3) . . ? N10 Fe2 N10 180.0 3_756 . ? N10 Fe2 N9 87.39(8) 3_756 . ? N10 Fe2 N9 92.61(8) . . ? N10 Fe2 N9 92.61(8) 3_756 3_756 ? N10 Fe2 N9 87.39(8) . 3_756 ? N9 Fe2 N9 180.0 . 3_756 ? N10 Fe2 N8 89.96(8) 3_756 . ? N10 Fe2 N8 90.04(8) . . ? N9 Fe2 N8 74.97(8) . . ? N9 Fe2 N8 105.03(8) 3_756 . ? N10 Fe2 N8 90.04(8) 3_756 3_756 ? N10 Fe2 N8 89.96(8) . 3_756 ? N9 Fe2 N8 105.03(8) . 3_756 ? N9 Fe2 N8 74.97(8) 3_756 3_756 ? N8 Fe2 N8 180.000(1) . 3_756 ? C14 N8 C18 118.1(2) . . ? C14 N8 Fe2 125.42(18) . . ? C18 N8 Fe2 116.52(17) . . ? C19 N9 N11 108.8(2) . . ? C19 N9 Fe2 114.88(16) . . ? N11 N9 Fe2 134.53(16) . . ? C26 N10 Fe2 163.6(2) . . ? C20 N11 N9 106.4(2) . . ? C25 N12 C21 116.6(2) . . ? C19 N13 C20 105.6(2) . . ? C19 N13 N14 125.3(2) . . ? C20 N13 N14 129.1(2) . . ? N13 N14 H3N 105(2) . . ? N13 N14 H4N 105(2) . . ? H3N N14 H4N 105(3) . . ? N8 C14 C15 123.0(2) . . ? N8 C14 H14A 118.5 . . ? C15 C14 H14A 118.5 . . ? C16 C15 C14 118.4(3) . . ? C16 C15 H15A 120.8 . . ? C14 C15 H15A 120.8 . . ? C15 C16 C17 119.5(3) . . ? C15 C16 H16A 120.3 . . ? C17 C16 H16A 120.3 . . ? C18 C17 C16 118.6(3) . . ? C18 C17 H17A 120.7 . . ? C16 C17 H17A 120.7 . . ? N8 C18 C17 122.4(2) . . ? N8 C18 C19 112.2(2) . . ? C17 C18 C19 125.4(2) . . ? N9 C19 N13 108.8(2) . . ? N9 C19 C18 120.6(2) . . ? N13 C19 C18 130.6(2) . . ? N11 C20 N13 110.3(2) . . ? N11 C20 C21 124.2(2) . . ? N13 C20 C21 125.5(2) . . ? N12 C21 C22 123.7(3) . . ? N12 C21 C20 116.3(2) . . ? C22 C21 C20 120.0(2) . . ? C23 C22 C21 118.1(3) . . ? C23 C22 H22A 121.0 . . ? C21 C22 H22A 121.0 . . ? C24 C23 C22 118.5(3) . . ? C24 C23 H23A 120.8 . . ? C22 C23 H23A 120.8 . . ? C25 C24 C23 119.5(3) . . ? C25 C24 H24A 120.3 . . ? C23 C24 H24A 120.3 . . ? N12 C25 C24 123.6(3) . . ? N12 C25 H25A 118.2 . . ? C24 C25 H25A 118.2 . . ? N10 C26 S2 178.6(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.386 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.089 # Attachment 'CCDC 732123_PhaseC_300K_F_v.cif' data_PhaseC-300K _database_code_depnum_ccdc_archive 'CCDC 732123' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H20 Fe N14 S2' _chemical_formula_sum 'C26 H20 Fe N14 S2' _chemical_formula_weight 648.53 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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.4000(3) _cell_length_b 17.5754(3) _cell_length_c 9.9940(2) _cell_angle_alpha 90.000 _cell_angle_beta 90.7480(10) _cell_angle_gamma 90.000 _cell_volume 2880.33(9) _cell_formula_units_Z 4 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 14330 _cell_measurement_theta_min 1.24 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Red-Brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.714 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.765 _exptl_absorpt_correction_T_max 0.875 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(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 KappaCCD _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26033 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6573 _reflns_number_gt 4330 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD server software (Nonius, 1997)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL/PC & Mercury 1.4.1 (CCDC)' _computing_publication_material 'XIF in SHELXTL/PC' _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^)+(0.0534P)^2^+0.2062P] 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 6573 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.1044 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.5000 0.5000 0.05194(12) Uani 1 2 d S . . S1 S 0.07703(5) 0.73787(4) 0.71491(8) 0.1000(2) Uani 1 1 d . . . N1 N -0.09858(9) 0.53994(9) 0.36576(15) 0.0539(4) Uani 1 1 d . . . N2 N 0.06001(9) 0.52810(9) 0.31606(14) 0.0545(4) Uani 1 1 d . . . N3 N 0.02313(12) 0.61184(11) 0.57179(19) 0.0755(5) Uani 1 1 d . . . N4 N 0.13886(9) 0.52896(9) 0.27109(15) 0.0562(4) Uani 1 1 d . . . N5 N 0.19485(11) 0.60062(10) -0.05355(16) 0.0706(5) Uani 1 1 d . . . N6 N 0.05773(9) 0.57774(8) 0.11737(13) 0.0481(3) Uani 1 1 d . . . N7 N 0.02749(12) 0.61557(13) 0.00138(18) 0.0650(5) Uani 1 1 d . . . H1N H 0.0716(15) 0.6092(14) -0.057(3) 0.098(8) Uiso 1 1 d . . . H2N H 0.0321(15) 0.6634(16) 0.036(3) 0.103(10) Uiso 1 1 d . . . C1 C -0.17786(12) 0.54013(12) 0.3936(2) 0.0644(5) Uani 1 1 d . . . H1A H -0.1938 0.5252 0.4786 0.077 Uiso 1 1 calc R . . C2 C -0.23731(13) 0.56143(13) 0.3024(2) 0.0746(6) Uani 1 1 d . . . H2A H -0.2921 0.5602 0.3250 0.090 Uiso 1 1 calc R . . C3 C -0.21390(13) 0.58451(14) 0.1776(2) 0.0783(7) Uani 1 1 d . . . H3A H -0.2528 0.5997 0.1146 0.094 Uiso 1 1 calc R . . C4 C -0.13241(12) 0.58498(12) 0.1464(2) 0.0683(6) Uani 1 1 d . . . H4A H -0.1155 0.6005 0.0622 0.082 Uiso 1 1 calc R . . C5 C -0.07634(11) 0.56212(10) 0.24209(18) 0.0505(4) Uani 1 1 d . . . C6 C 0.01181(11) 0.55697(10) 0.22296(16) 0.0482(4) Uani 1 1 d . . . C7 C 0.13614(11) 0.55949(10) 0.15089(16) 0.0497(4) Uani 1 1 d . . . C8 C 0.20820(12) 0.57023(10) 0.06692(17) 0.0534(4) Uani 1 1 d . . . C9 C 0.28366(12) 0.54787(13) 0.1128(2) 0.0669(5) Uani 1 1 d . . . H9A H 0.2900 0.5253 0.1964 0.080 Uiso 1 1 calc R . . C10 C 0.34998(14) 0.55966(15) 0.0315(2) 0.0807(6) Uani 1 1 d . . . H10A H 0.4020 0.5453 0.0597 0.097 Uiso 1 1 calc R . . C11 C 0.33794(17) 0.59251(15) -0.0903(3) 0.0895(8) Uani 1 1 d . . . H11A H 0.3818 0.6021 -0.1459 0.107 Uiso 1 1 calc R . . C12 C 0.26025(16) 0.61120(15) -0.1296(2) 0.0886(7) Uani 1 1 d . . . H12A H 0.2526 0.6325 -0.2140 0.106 Uiso 1 1 calc R . . C13 C 0.04599(13) 0.66386(13) 0.6296(2) 0.0642(5) Uani 1 1 d . . . Fe2 Fe 0.5000 0.5000 0.5000 0.05237(12) Uani 1 2 d S . . S2 S 0.43198(4) 0.38263(4) 0.92732(6) 0.0868(2) Uani 1 1 d . . . N8 N 0.40937(9) 0.59248(9) 0.52793(15) 0.0569(4) Uani 1 1 d . . . N9 N 0.56760(10) 0.59022(9) 0.59577(16) 0.0571(4) Uani 1 1 d . . . N10 N 0.47263(11) 0.45737(10) 0.69324(17) 0.0673(4) Uani 1 1 d . . . N11 N 0.64402(10) 0.59613(9) 0.65243(16) 0.0582(4) Uani 1 1 d . . . N12 N 0.70240(11) 0.74138(10) 0.89143(16) 0.0697(5) Uani 1 1 d . . . N13 N 0.56572(10) 0.68703(8) 0.73032(15) 0.0563(4) Uani 1 1 d . . . N14 N 0.53370(16) 0.74717(13) 0.8082(3) 0.0840(6) Uani 1 1 d . . . H4N H 0.5457(17) 0.7884(18) 0.754(3) 0.117(11) Uiso 1 1 d . . . H3N H 0.573(2) 0.758(2) 0.865(4) 0.146(14) Uiso 1 1 d . . . C14 C 0.33347(13) 0.59435(14) 0.4774(2) 0.0699(6) Uani 1 1 d . . . H14A H 0.3145 0.5524 0.4297 0.084 Uiso 1 1 calc R . . C15 C 0.28240(14) 0.65558(16) 0.4927(2) 0.0812(7) Uani 1 1 d . . . H15A H 0.2300 0.6548 0.4562 0.097 Uiso 1 1 calc R . . C16 C 0.30960(14) 0.71734(15) 0.5620(3) 0.0828(7) Uani 1 1 d . . . H16A H 0.2757 0.7592 0.5735 0.099 Uiso 1 1 calc R . . C17 C 0.38788(14) 0.71764(12) 0.6155(2) 0.0740(6) Uani 1 1 d . . . H17A H 0.4075 0.7595 0.6629 0.089 Uiso 1 1 calc R . . C18 C 0.43634(11) 0.65388(11) 0.59674(18) 0.0572(5) Uani 1 1 d . . . C19 C 0.52122(11) 0.64523(10) 0.64248(18) 0.0523(4) Uani 1 1 d . . . C20 C 0.64232(11) 0.65555(10) 0.73306(17) 0.0535(4) Uani 1 1 d . . . C21 C 0.71415(12) 0.68434(10) 0.80509(17) 0.0560(5) Uani 1 1 d . . . C22 C 0.79023(13) 0.65525(12) 0.77678(18) 0.0655(5) Uani 1 1 d . . . H22A H 0.7957 0.6143 0.7186 0.079 Uiso 1 1 calc R . . C23 C 0.85781(14) 0.68804(14) 0.8364(2) 0.0777(6) Uani 1 1 d . . . H23A H 0.9099 0.6704 0.8177 0.093 Uiso 1 1 calc R . . C24 C 0.84680(17) 0.74729(15) 0.9239(2) 0.0832(7) Uani 1 1 d . . . H24A H 0.8913 0.7710 0.9648 0.100 Uiso 1 1 calc R . . C25 C 0.76961(18) 0.77047(14) 0.9492(2) 0.0826(7) Uani 1 1 d . . . H25A H 0.7629 0.8094 1.0112 0.099 Uiso 1 1 calc R . . C26 C 0.45573(11) 0.42722(11) 0.7914(2) 0.0577(5) 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 0.0562(2) 0.0532(2) 0.0465(2) 0.01259(16) 0.00718(16) 0.00561(17) S1 0.1298(6) 0.0687(4) 0.1011(5) 0.0010(4) -0.0197(4) -0.0147(4) N1 0.0523(9) 0.0546(9) 0.0550(9) 0.0078(7) 0.0057(7) 0.0007(7) N2 0.0531(9) 0.0616(9) 0.0491(8) 0.0142(8) 0.0081(7) 0.0064(8) N3 0.0953(14) 0.0587(11) 0.0728(12) 0.0068(10) 0.0058(10) 0.0009(10) N4 0.0542(9) 0.0651(9) 0.0496(8) 0.0131(8) 0.0081(7) 0.0113(8) N5 0.0777(12) 0.0839(12) 0.0506(9) 0.0145(9) 0.0164(8) 0.0083(9) N6 0.0541(9) 0.0499(8) 0.0403(7) 0.0078(7) -0.0006(6) 0.0018(7) N7 0.0668(11) 0.0809(14) 0.0472(9) 0.0201(9) -0.0043(8) -0.0022(10) C1 0.0554(12) 0.0695(13) 0.0685(12) 0.0071(11) 0.0074(10) -0.0041(10) C2 0.0489(12) 0.0873(15) 0.0876(16) 0.0063(13) -0.0006(11) -0.0068(11) C3 0.0550(13) 0.1027(18) 0.0768(15) 0.0119(13) -0.0146(11) -0.0036(12) C4 0.0609(13) 0.0846(15) 0.0591(12) 0.0142(11) -0.0070(10) -0.0071(11) C5 0.0536(10) 0.0468(10) 0.0512(10) 0.0052(8) -0.0007(8) -0.0027(8) C6 0.0541(10) 0.0468(9) 0.0436(9) 0.0080(8) 0.0012(8) 0.0002(8) C7 0.0591(11) 0.0492(10) 0.0408(9) 0.0046(8) 0.0044(8) 0.0023(8) C8 0.0626(12) 0.0518(10) 0.0462(10) 0.0000(8) 0.0101(8) 0.0013(9) C9 0.0625(13) 0.0816(15) 0.0567(11) 0.0045(11) 0.0093(9) 0.0022(11) C10 0.0610(13) 0.1025(18) 0.0790(15) -0.0046(14) 0.0137(11) -0.0016(12) C11 0.0881(18) 0.1032(19) 0.0783(16) 0.0009(14) 0.0406(14) -0.0024(15) C12 0.099(2) 0.1055(19) 0.0621(13) 0.0180(13) 0.0291(13) 0.0040(16) C13 0.0727(14) 0.0557(12) 0.0644(12) 0.0144(11) 0.0043(10) 0.0071(11) Fe2 0.0548(2) 0.0515(2) 0.0509(2) 0.00077(17) 0.00714(16) -0.00269(17) S2 0.0858(4) 0.1007(5) 0.0747(4) 0.0328(3) 0.0255(3) 0.0110(3) N8 0.0554(10) 0.0629(10) 0.0526(8) 0.0076(8) 0.0083(7) -0.0009(8) N9 0.0531(9) 0.0536(9) 0.0648(9) -0.0054(8) 0.0046(7) -0.0014(7) N10 0.0741(12) 0.0686(11) 0.0594(10) 0.0083(9) 0.0090(8) -0.0013(9) N11 0.0569(10) 0.0554(9) 0.0624(9) -0.0056(8) 0.0023(8) -0.0017(7) N12 0.0869(13) 0.0668(11) 0.0554(9) -0.0082(9) 0.0038(9) -0.0110(9) N13 0.0699(10) 0.0459(8) 0.0533(8) 0.0011(7) 0.0073(8) 0.0065(8) N14 0.1081(17) 0.0675(13) 0.0760(13) -0.0168(12) -0.0053(13) 0.0288(12) C14 0.0583(13) 0.0871(16) 0.0642(12) 0.0112(11) 0.0031(10) -0.0008(11) C15 0.0623(13) 0.0948(18) 0.0866(16) 0.0237(15) 0.0044(11) 0.0092(14) C16 0.0671(15) 0.0736(15) 0.1078(19) 0.0210(15) 0.0110(13) 0.0184(12) C17 0.0742(15) 0.0544(12) 0.0935(16) 0.0092(11) 0.0085(12) 0.0078(11) C18 0.0599(12) 0.0548(11) 0.0572(11) 0.0143(10) 0.0117(9) 0.0024(9) C19 0.0589(11) 0.0433(9) 0.0547(10) 0.0056(9) 0.0077(9) -0.0010(9) C20 0.0656(12) 0.0466(10) 0.0486(10) 0.0040(9) 0.0056(8) -0.0014(9) C21 0.0744(13) 0.0505(10) 0.0430(9) 0.0052(9) -0.0015(9) -0.0031(10) C22 0.0778(14) 0.0653(12) 0.0532(11) 0.0003(10) -0.0132(10) 0.0088(11) C23 0.0751(15) 0.0900(17) 0.0674(13) 0.0087(13) -0.0227(11) 0.0056(13) C24 0.0920(19) 0.0889(17) 0.0680(14) 0.0023(13) -0.0252(13) -0.0170(14) C25 0.110(2) 0.0780(16) 0.0602(13) -0.0101(12) -0.0064(13) -0.0140(15) C26 0.0519(11) 0.0613(12) 0.0599(12) 0.0068(10) 0.0075(9) 0.0050(9) _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 N3 2.125(2) 3_566 ? Fe1 N3 2.125(2) . ? Fe1 N2 2.1538(14) 3_566 ? Fe1 N2 2.1538(14) . ? Fe1 N1 2.2022(15) . ? Fe1 N1 2.2022(15) 3_566 ? S1 C13 1.633(3) . ? N1 C1 1.333(2) . ? N1 C5 1.351(2) . ? N2 C6 1.315(2) . ? N2 N4 1.3747(19) . ? N3 C13 1.142(3) . ? N4 C7 1.316(2) . ? N5 C8 1.333(2) . ? N5 C12 1.335(3) . ? N6 C6 1.355(2) . ? N6 C7 1.363(2) . ? N6 N7 1.420(2) . ? N7 H1N 0.94(3) . ? N7 H2N 0.91(3) . ? C1 C2 1.378(3) . ? C1 H1A 0.9300 . ? C2 C3 1.371(3) . ? C2 H2A 0.9300 . ? C3 C4 1.376(3) . ? C3 H3A 0.9300 . ? C4 C5 1.378(3) . ? C4 H4A 0.9300 . ? C5 C6 1.464(3) . ? C7 C8 1.471(2) . ? C8 C9 1.371(3) . ? C9 C10 1.382(3) . ? C9 H9A 0.9300 . ? C10 C11 1.359(3) . ? C10 H10A 0.9300 . ? C11 C12 1.368(3) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? Fe2 N10 2.1249(17) . ? Fe2 N10 2.1249(17) 3_666 ? Fe2 N9 2.1522(15) 3_666 ? Fe2 N9 2.1522(15) . ? Fe2 N8 2.2225(16) 3_666 ? Fe2 N8 2.2225(16) . ? S2 C26 1.620(2) . ? N8 C14 1.338(2) . ? N8 C18 1.351(2) . ? N9 C19 1.319(2) . ? N9 N11 1.372(2) . ? N10 C26 1.152(2) . ? N11 C20 1.320(2) . ? N12 C21 1.338(2) . ? N12 C25 1.339(3) . ? N13 C19 1.351(2) . ? N13 C20 1.373(2) . ? N13 N14 1.418(2) . ? N14 H4N 0.93(3) . ? N14 H3N 0.87(4) . ? C14 C15 1.373(3) . ? C14 H14A 0.9300 . ? C15 C16 1.360(4) . ? C15 H15A 0.9300 . ? C16 C17 1.384(3) . ? C16 H16A 0.9300 . ? C17 C18 1.388(3) . ? C17 H17A 0.9300 . ? C18 C19 1.468(3) . ? C20 C21 1.463(3) . ? C21 C22 1.381(3) . ? C22 C23 1.378(3) . ? C22 H22A 0.9300 . ? C23 C24 1.373(3) . ? C23 H23A 0.9300 . ? C24 C25 1.357(3) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? 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 N3 Fe1 N3 180.00(4) 3_566 . ? N3 Fe1 N2 89.69(7) 3_566 3_566 ? N3 Fe1 N2 90.31(7) . 3_566 ? N3 Fe1 N2 90.31(7) 3_566 . ? N3 Fe1 N2 89.69(7) . . ? N2 Fe1 N2 180.000(1) 3_566 . ? N3 Fe1 N1 87.87(7) 3_566 . ? N3 Fe1 N1 92.13(7) . . ? N2 Fe1 N1 104.66(5) 3_566 . ? N2 Fe1 N1 75.34(5) . . ? N3 Fe1 N1 92.13(7) 3_566 3_566 ? N3 Fe1 N1 87.87(7) . 3_566 ? N2 Fe1 N1 75.34(5) 3_566 3_566 ? N2 Fe1 N1 104.66(5) . 3_566 ? N1 Fe1 N1 180.0 . 3_566 ? C1 N1 C5 117.78(16) . . ? C1 N1 Fe1 125.72(13) . . ? C5 N1 Fe1 116.39(12) . . ? C6 N2 N4 108.89(14) . . ? C6 N2 Fe1 114.54(12) . . ? N4 N2 Fe1 136.37(11) . . ? C13 N3 Fe1 165.29(17) . . ? C7 N4 N2 106.39(14) . . ? C8 N5 C12 116.5(2) . . ? C6 N6 C7 106.10(13) . . ? C6 N6 N7 124.78(15) . . ? C7 N6 N7 128.99(15) . . ? N6 N7 H1N 100.6(15) . . ? N6 N7 H2N 95.3(17) . . ? H1N N7 H2N 107(2) . . ? N1 C1 C2 123.12(19) . . ? N1 C1 H1A 118.4 . . ? C2 C1 H1A 118.4 . . ? C3 C2 C1 118.54(19) . . ? C3 C2 H2A 120.7 . . ? C1 C2 H2A 120.7 . . ? C2 C3 C4 119.49(19) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C3 C4 C5 118.82(19) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? N1 C5 C4 122.24(17) . . ? N1 C5 C6 112.38(15) . . ? C4 C5 C6 125.37(17) . . ? N2 C6 N6 108.67(15) . . ? N2 C6 C5 121.14(15) . . ? N6 C6 C5 130.18(15) . . ? N4 C7 N6 109.94(15) . . ? N4 C7 C8 123.74(16) . . ? N6 C7 C8 126.32(15) . . ? N5 C8 C9 123.61(18) . . ? N5 C8 C7 116.31(17) . . ? C9 C8 C7 120.06(16) . . ? C8 C9 C10 118.3(2) . . ? C8 C9 H9A 120.8 . . ? C10 C9 H9A 120.8 . . ? C11 C10 C9 118.9(2) . . ? C11 C10 H10A 120.5 . . ? C9 C10 H10A 120.5 . . ? C10 C11 C12 118.9(2) . . ? C10 C11 H11A 120.6 . . ? C12 C11 H11A 120.6 . . ? N5 C12 C11 123.7(2) . . ? N5 C12 H12A 118.1 . . ? C11 C12 H12A 118.1 . . ? N3 C13 S1 178.6(2) . . ? N10 Fe2 N10 180.000(1) . 3_666 ? N10 Fe2 N9 91.76(6) . 3_666 ? N10 Fe2 N9 88.24(6) 3_666 3_666 ? N10 Fe2 N9 88.24(6) . . ? N10 Fe2 N9 91.76(6) 3_666 . ? N9 Fe2 N9 180.00(6) 3_666 . ? N10 Fe2 N8 90.33(6) . 3_666 ? N10 Fe2 N8 89.67(6) 3_666 3_666 ? N9 Fe2 N8 75.33(6) 3_666 3_666 ? N9 Fe2 N8 104.67(6) . 3_666 ? N10 Fe2 N8 89.67(6) . . ? N10 Fe2 N8 90.33(6) 3_666 . ? N9 Fe2 N8 104.67(6) 3_666 . ? N9 Fe2 N8 75.33(6) . . ? N8 Fe2 N8 180.000(1) 3_666 . ? C14 N8 C18 118.00(18) . . ? C14 N8 Fe2 126.24(15) . . ? C18 N8 Fe2 115.66(12) . . ? C19 N9 N11 109.04(15) . . ? C19 N9 Fe2 113.66(13) . . ? N11 N9 Fe2 134.55(12) . . ? C26 N10 Fe2 172.84(17) . . ? C20 N11 N9 106.58(15) . . ? C21 N12 C25 116.1(2) . . ? C19 N13 C20 106.27(15) . . ? C19 N13 N14 124.15(18) . . ? C20 N13 N14 129.42(18) . . ? N13 N14 H4N 100.4(18) . . ? N13 N14 H3N 104(2) . . ? H4N N14 H3N 93(3) . . ? N8 C14 C15 122.9(2) . . ? N8 C14 H14A 118.6 . . ? C15 C14 H14A 118.6 . . ? C16 C15 C14 119.1(2) . . ? C16 C15 H15A 120.5 . . ? C14 C15 H15A 120.5 . . ? C15 C16 C17 119.8(2) . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? C16 C17 C18 118.3(2) . . ? C16 C17 H17A 120.8 . . ? C18 C17 H17A 120.8 . . ? N8 C18 C17 121.98(19) . . ? N8 C18 C19 112.25(16) . . ? C17 C18 C19 125.73(19) . . ? N9 C19 N13 108.62(16) . . ? N9 C19 C18 120.98(17) . . ? N13 C19 C18 130.40(17) . . ? N11 C20 N13 109.48(16) . . ? N11 C20 C21 123.43(17) . . ? N13 C20 C21 126.97(17) . . ? N12 C21 C22 123.19(18) . . ? N12 C21 C20 117.03(18) . . ? C22 C21 C20 119.68(17) . . ? C23 C22 C21 118.7(2) . . ? C23 C22 H22A 120.6 . . ? C21 C22 H22A 120.6 . . ? C24 C23 C22 118.7(2) . . ? C24 C23 H23A 120.6 . . ? C22 C23 H23A 120.6 . . ? C25 C24 C23 118.5(2) . . ? C25 C24 H24A 120.7 . . ? C23 C24 H24A 120.7 . . ? N12 C25 C24 124.7(2) . . ? N12 C25 H25A 117.6 . . ? C24 C25 H25A 117.6 . . ? N10 C26 S2 178.43(19) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.313 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.039 # Attachment 'CCDC 732124_PhaseC_130K_F_v.cif' data_PhaseC-130K _database_code_depnum_ccdc_archive 'CCDC 732124' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H20 Fe N14 S2' _chemical_formula_sum 'C26 H20 Fe N14 S2' _chemical_formula_weight 648.53 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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.3109(4) _cell_length_b 17.4820(5) _cell_length_c 29.6431(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.8470(11) _cell_angle_gamma 90.000 _cell_volume 8452.0(3) _cell_formula_units_Z 12 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 19212 _cell_measurement_theta_min 1.25 _cell_measurement_theta_max 27.47 _exptl_crystal_description Block _exptl_crystal_colour Red-Brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3984 _exptl_absorpt_coefficient_mu 0.730 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.806 _exptl_absorpt_correction_T_max 0.865 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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 KappaCCD _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46348 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 27.47 _reflns_number_total 18410 _reflns_number_gt 11301 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD server software (Nonius, 1997)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL/PC & Mercury 1.4.1 (CCDC)' _computing_publication_material 'XIF in SHELXTL/PC' _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^)+(0.0454P)^2^+1.0931P] 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 18410 _refine_ls_number_parameters 1201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0968 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1149 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe11 Fe 1.0000 0.5000 0.0000 0.02021(12) Uani 1 2 d S . . S1 S 0.92110(5) 0.25986(4) -0.07182(2) 0.0442(2) Uani 1 1 d . . . N1 N 1.09959(12) 0.46272(11) 0.04565(6) 0.0221(5) Uani 1 1 d . . . N2 N 0.93938(12) 0.47327(12) 0.06171(6) 0.0229(5) Uani 1 1 d . . . N3 N 0.97724(13) 0.38712(12) -0.02339(7) 0.0290(5) Uani 1 1 d . . . N4 N 0.86024(12) 0.47144(12) 0.07646(6) 0.0235(5) Uani 1 1 d . . . N5 N 0.80229(13) 0.39587(13) 0.18514(7) 0.0304(5) Uani 1 1 d . . . N6 N 0.94170(12) 0.42378(11) 0.12913(6) 0.0201(5) Uani 1 1 d . . . N7 N 0.97200(14) 0.38558(14) 0.16816(7) 0.0281(5) Uani 1 1 d . . . H1N H 0.9286(16) 0.3920(15) 0.1879(8) 0.034 Uiso 1 1 d . . . H2N H 0.9699(16) 0.3384(16) 0.1596(8) 0.034 Uiso 1 1 d . . . C1 C 1.17938(15) 0.46396(14) 0.03650(9) 0.0283(6) Uani 1 1 d . . . H1A H 1.1954 0.4792 0.0079 0.034 Uiso 1 1 calc R . . C2 C 1.23976(16) 0.44335(15) 0.06795(9) 0.0320(6) Uani 1 1 d . . . H2A H 1.2949 0.4448 0.0605 0.038 Uiso 1 1 calc R . . C3 C 1.21591(16) 0.42083(16) 0.11033(9) 0.0332(7) Uani 1 1 d . . . H3A H 1.2549 0.4063 0.1319 0.040 Uiso 1 1 calc R . . C4 C 1.13332(15) 0.42001(15) 0.12051(8) 0.0287(6) Uani 1 1 d . . . H4A H 1.1162 0.4057 0.1491 0.034 Uiso 1 1 calc R . . C5 C 1.07678(14) 0.44086(13) 0.08753(8) 0.0214(5) Uani 1 1 d . . . C6 C 0.98789(14) 0.44486(13) 0.09364(8) 0.0202(5) Uani 1 1 d . . . C7 C 0.86242(14) 0.44116(14) 0.11704(8) 0.0219(6) Uani 1 1 d . . . C8 C 0.79005(15) 0.43057(14) 0.14513(8) 0.0241(6) Uani 1 1 d . . . C9 C 0.71405(15) 0.45662(15) 0.13008(8) 0.0270(6) Uani 1 1 d . . . H9A H 0.7083 0.4811 0.1024 0.032 Uiso 1 1 calc R . . C10 C 0.64696(16) 0.44514(16) 0.15743(8) 0.0343(7) Uani 1 1 d . . . H10A H 0.5952 0.4623 0.1486 0.041 Uiso 1 1 calc R . . C11 C 0.65822(17) 0.40789(17) 0.19790(9) 0.0402(7) Uani 1 1 d . . . H11A H 0.6139 0.3982 0.2164 0.048 Uiso 1 1 calc R . . C12 C 0.73662(18) 0.38496(17) 0.21068(9) 0.0393(7) Uani 1 1 d . . . H12A H 0.7438 0.3608 0.2384 0.047 Uiso 1 1 calc R . . C13 C 0.95323(15) 0.33424(15) -0.04303(8) 0.0265(6) Uani 1 1 d . . . Fe12 Fe -0.01546(2) 1.002874(19) 0.165773(10) 0.02102(9) Uani 1 1 d . . . S2 S 0.06918(5) 0.76424(4) 0.23780(2) 0.0422(2) Uani 1 1 d . . . S3 S -0.09025(5) 1.24559(4) 0.09492(3) 0.0414(2) Uani 1 1 d . . . N8 N -0.11381(12) 0.95902(12) 0.12176(6) 0.0241(5) Uani 1 1 d . . . N9 N 0.04449(12) 0.97643(12) 0.10425(6) 0.0232(5) Uani 1 1 d . . . N10 N 0.00986(14) 0.89118(13) 0.18972(7) 0.0310(5) Uani 1 1 d . . . N11 N 0.12319(12) 0.97899(12) 0.08879(6) 0.0241(5) Uani 1 1 d . . . N12 N 0.18021(13) 0.90742(12) -0.02127(7) 0.0296(5) Uani 1 1 d . . . N13 N 0.04349(12) 0.92375(11) 0.03785(6) 0.0201(5) Uani 1 1 d . . . N14 N 0.01469(14) 0.88232(14) -0.00037(7) 0.0281(5) Uani 1 1 d . . . H4N H 0.0206(17) 0.8376(16) 0.0103(8) 0.034 Uiso 1 1 d . . . H3N H 0.0577(16) 0.8874(15) -0.0208(8) 0.034 Uiso 1 1 d . . . N15 N 0.08463(12) 1.04091(12) 0.21032(7) 0.0247(5) Uani 1 1 d . . . N16 N -0.07467(12) 1.02997(11) 0.22760(6) 0.0227(5) Uani 1 1 d . . . N17 N -0.04166(14) 1.11427(13) 0.14223(7) 0.0336(6) Uani 1 1 d . . . N18 N -0.15394(12) 1.03292(12) 0.24280(6) 0.0246(5) Uani 1 1 d . . . N19 N -0.20793(13) 1.10449(12) 0.35321(7) 0.0298(5) Uani 1 1 d . . . N20 N -0.07068(12) 1.07912(11) 0.29530(6) 0.0217(5) Uani 1 1 d . . . N21 N -0.03859(14) 1.11535(13) 0.33468(7) 0.0266(5) Uani 1 1 d . . . H6N H -0.0395(16) 1.1608(15) 0.3243(8) 0.032 Uiso 1 1 d . . . H5N H -0.0839(16) 1.1098(14) 0.3542(8) 0.032 Uiso 1 1 d . . . C14 C -0.19324(15) 0.95690(15) 0.13204(9) 0.0286(6) Uani 1 1 d . . . H14A H -0.2092 0.9741 0.1603 0.034 Uiso 1 1 calc R . . C15 C -0.25294(16) 0.92989(15) 0.10206(9) 0.0331(7) Uani 1 1 d . . . H15A H -0.3079 0.9295 0.1100 0.040 Uiso 1 1 calc R . . C16 C -0.22916(16) 0.90369(15) 0.06028(9) 0.0332(7) Uani 1 1 d . . . H16A H -0.2679 0.8849 0.0398 0.040 Uiso 1 1 calc R . . C17 C -0.14705(15) 0.90572(15) 0.04921(9) 0.0297(6) Uani 1 1 d . . . H17A H -0.1298 0.8885 0.0212 0.036 Uiso 1 1 calc R . . C18 C -0.09131(14) 0.93387(14) 0.08060(8) 0.0223(6) Uani 1 1 d . . . C19 C -0.00293(14) 0.94308(14) 0.07354(8) 0.0206(5) Uani 1 1 d . . . C20 C 0.12150(15) 0.94658(14) 0.04861(8) 0.0222(6) Uani 1 1 d . . . C21 C 0.19360(15) 0.93746(14) 0.01990(8) 0.0235(6) Uani 1 1 d . . . C22 C 0.27040(15) 0.96007(15) 0.03564(8) 0.0269(6) Uani 1 1 d . . . H22A H 0.2770 0.9822 0.0640 0.032 Uiso 1 1 calc R . . C23 C 0.33666(16) 0.94869(15) 0.00799(9) 0.0325(7) Uani 1 1 d . . . H23A H 0.3891 0.9627 0.0176 0.039 Uiso 1 1 calc R . . C24 C 0.32442(17) 0.91664(16) -0.03362(9) 0.0385(7) Uani 1 1 d . . . H24A H 0.3685 0.9078 -0.0525 0.046 Uiso 1 1 calc R . . C25 C 0.24544(18) 0.89750(16) -0.04731(9) 0.0358(7) Uani 1 1 d . . . H25A H 0.2375 0.8768 -0.0759 0.043 Uiso 1 1 calc R . . C26 C 0.03490(16) 0.83852(15) 0.20931(8) 0.0274(6) Uani 1 1 d . . . C27 C 0.16442(15) 1.03895(15) 0.20079(9) 0.0299(6) Uani 1 1 d . . . H27A H 0.1797 1.0247 0.1719 0.036 Uiso 1 1 calc R . . C28 C 0.22583(16) 1.05722(15) 0.23214(9) 0.0348(7) Uani 1 1 d . . . H28A H 0.2808 1.0555 0.2243 0.042 Uiso 1 1 calc R . . C29 C 0.20319(16) 1.07792(16) 0.27501(9) 0.0354(7) Uani 1 1 d . . . H29A H 0.2428 1.0909 0.2966 0.042 Uiso 1 1 calc R . . C30 C 0.12074(15) 1.07923(15) 0.28574(8) 0.0306(6) Uani 1 1 d . . . H30A H 0.1043 1.0922 0.3147 0.037 Uiso 1 1 calc R . . C31 C 0.06341(15) 1.06096(14) 0.25266(8) 0.0233(6) Uani 1 1 d . . . C32 C -0.02542(15) 1.05788(14) 0.25938(8) 0.0212(5) Uani 1 1 d . . . C33 C -0.15046(15) 1.06275(14) 0.28360(8) 0.0219(6) Uani 1 1 d . . . C34 C -0.22215(15) 1.07532(14) 0.31203(8) 0.0246(6) Uani 1 1 d . . . C35 C -0.29948(16) 1.05611(16) 0.29560(8) 0.0315(7) Uani 1 1 d . . . H35A H -0.3065 1.0346 0.2671 0.038 Uiso 1 1 calc R . . C36 C -0.36605(17) 1.06992(16) 0.32296(9) 0.0368(7) Uani 1 1 d . . . H36A H -0.4189 1.0577 0.3132 0.044 Uiso 1 1 calc R . . C37 C -0.35291(17) 1.10186(17) 0.36471(9) 0.0393(7) Uani 1 1 d . . . H37A H -0.3967 1.1130 0.3833 0.047 Uiso 1 1 calc R . . C38 C -0.27290(18) 1.11718(17) 0.37864(9) 0.0382(7) Uani 1 1 d . . . H38A H -0.2644 1.1374 0.4073 0.046 Uiso 1 1 calc R . . C39 C -0.06243(16) 1.16889(16) 0.12319(8) 0.0295(6) Uani 1 1 d . . . Fe21 Fe 0.5000 0.5000 0.0000 0.02105(12) Uani 1 2 d S . . S4 S 0.43132(4) 0.38855(4) 0.14618(2) 0.03528(18) Uani 1 1 d . . . N22 N 0.41044(12) 0.59448(12) 0.00691(6) 0.0234(5) Uani 1 1 d . . . N23 N 0.57006(12) 0.59250(12) 0.02852(6) 0.0241(5) Uani 1 1 d . . . N24 N 0.47469(13) 0.46437(12) 0.06687(7) 0.0280(5) Uani 1 1 d . . . N25 N 0.64643(12) 0.59722(12) 0.04855(6) 0.0246(5) Uani 1 1 d . . . N26 N 0.70408(13) 0.74131(12) 0.13124(6) 0.0272(5) Uani 1 1 d . . . N27 N 0.56873(12) 0.69064(11) 0.07389(6) 0.0221(5) Uani 1 1 d . . . N28 N 0.53716(15) 0.75163(14) 0.09946(8) 0.0347(6) Uani 1 1 d . . . H8N H 0.5489(17) 0.7914(16) 0.0805(9) 0.042 Uiso 1 1 d . . . H7N H 0.5741(17) 0.7582(15) 0.1225(9) 0.042 Uiso 1 1 d . . . C40 C 0.33402(15) 0.59593(16) -0.01025(8) 0.0289(6) Uani 1 1 d . . . H40A H 0.3144 0.5527 -0.0251 0.035 Uiso 1 1 calc R . . C41 C 0.28299(16) 0.65882(16) -0.00683(8) 0.0335(7) Uani 1 1 d . . . H41A H 0.2301 0.6577 -0.0189 0.040 Uiso 1 1 calc R . . C42 C 0.31221(16) 0.72310(16) 0.01486(9) 0.0342(7) Uani 1 1 d . . . H42A H 0.2791 0.7661 0.0176 0.041 Uiso 1 1 calc R . . C43 C 0.39151(16) 0.72338(15) 0.03259(8) 0.0311(6) Uani 1 1 d . . . H43A H 0.4126 0.7665 0.0470 0.037 Uiso 1 1 calc R . . C44 C 0.43842(14) 0.65792(14) 0.02828(8) 0.0232(6) Uani 1 1 d . . . C45 C 0.52399(14) 0.64876(14) 0.04396(8) 0.0216(5) Uani 1 1 d . . . C46 C 0.64460(15) 0.65723(14) 0.07571(8) 0.0223(6) Uani 1 1 d . . . C47 C 0.71633(15) 0.68442(14) 0.10135(7) 0.0227(6) Uani 1 1 d . . . C48 C 0.79338(15) 0.65374(14) 0.09296(8) 0.0252(6) Uani 1 1 d . . . H48A H 0.7993 0.6129 0.0732 0.030 Uiso 1 1 calc R . . C49 C 0.86079(16) 0.68519(15) 0.11457(8) 0.0320(7) Uani 1 1 d . . . H49A H 0.9132 0.6668 0.1089 0.038 Uiso 1 1 calc R . . C50 C 0.84940(17) 0.74447(16) 0.14478(8) 0.0363(7) Uani 1 1 d . . . H50A H 0.8938 0.7671 0.1596 0.044 Uiso 1 1 calc R . . C51 C 0.77052(17) 0.76910(16) 0.15231(8) 0.0346(7) Uani 1 1 d . . . H51A H 0.7631 0.8076 0.1735 0.042 Uiso 1 1 calc R . . C52 C 0.45699(14) 0.43352(14) 0.10028(8) 0.0237(6) Uani 1 1 d . . . Fe22 Fe 0.49265(2) 0.00456(2) 0.162853(10) 0.02180(10) Uani 1 1 d . . . S5 S 0.55040(4) -0.11539(4) 0.01684(2) 0.03254(17) Uani 1 1 d . . . S6 S 0.41716(5) 0.12569(5) 0.30537(2) 0.0414(2) Uani 1 1 d . . . N29 N 0.40079(12) -0.08702(12) 0.17217(6) 0.0237(5) Uani 1 1 d . . . N30 N 0.55997(12) -0.08653(12) 0.19522(6) 0.0250(5) Uani 1 1 d . . . N31 N 0.52154(13) -0.03835(12) 0.09794(7) 0.0286(5) Uani 1 1 d . . . N32 N 0.63696(12) -0.09301(12) 0.21487(6) 0.0263(5) Uani 1 1 d . . . N33 N 0.69331(13) -0.24219(12) 0.29466(6) 0.0290(5) Uani 1 1 d . . . N34 N 0.55579(12) -0.18256(12) 0.24176(6) 0.0238(5) Uani 1 1 d . . . N35 N 0.52067(16) -0.24070(15) 0.26843(8) 0.0390(6) Uani 1 1 d . . . H10N H 0.5441(18) -0.2806(17) 0.2534(9) 0.047 Uiso 1 1 d . . . H9N H 0.5524(18) -0.2456(16) 0.2908(9) 0.047 Uiso 1 1 d . . . N36 N 0.58170(12) 0.09920(12) 0.15337(6) 0.0265(5) Uani 1 1 d . . . N37 N 0.42408(12) 0.09311(12) 0.12955(7) 0.0252(5) Uani 1 1 d . . . N38 N 0.46415(13) 0.04755(13) 0.22758(7) 0.0309(5) Uani 1 1 d . . . N39 N 0.34623(12) 0.09844(12) 0.11188(6) 0.0246(5) Uani 1 1 d . . . N40 N 0.28063(14) 0.24629(12) 0.03360(7) 0.0318(5) Uani 1 1 d . . . N41 N 0.42116(13) 0.19398(12) 0.08674(6) 0.0252(5) Uani 1 1 d . . . N42 N 0.44883(16) 0.25854(14) 0.06263(8) 0.0363(6) Uani 1 1 d . . . H11N H 0.4119(17) 0.2664(16) 0.0410(9) 0.044 Uiso 1 1 d . . . H12N H 0.4385(17) 0.2977(16) 0.0827(9) 0.044 Uiso 1 1 d . . . C53 C 0.32454(16) -0.08835(16) 0.15501(8) 0.0301(6) Uani 1 1 d . . . H53A H 0.3057 -0.0458 0.1392 0.036 Uiso 1 1 calc R . . C54 C 0.27256(17) -0.15006(17) 0.15977(8) 0.0346(7) Uani 1 1 d . . . H54A H 0.2197 -0.1488 0.1476 0.041 Uiso 1 1 calc R . . C55 C 0.30030(16) -0.21358(16) 0.18289(9) 0.0355(7) Uani 1 1 d . . . H55A H 0.2664 -0.2558 0.1865 0.043 Uiso 1 1 calc R . . C56 C 0.37928(16) -0.21391(15) 0.20079(8) 0.0326(7) Uani 1 1 d . . . H56A H 0.3995 -0.2564 0.2162 0.039 Uiso 1 1 calc R . . C57 C 0.42752(15) -0.14936(15) 0.19515(8) 0.0263(6) Uani 1 1 d . . . C58 C 0.51276(15) -0.14113(14) 0.21111(8) 0.0230(6) Uani 1 1 d . . . C59 C 0.63339(15) -0.15173(14) 0.24279(7) 0.0226(6) Uani 1 1 d . . . C60 C 0.70509(15) -0.18188(14) 0.26774(8) 0.0245(6) Uani 1 1 d . . . C61 C 0.78194(16) -0.15003(15) 0.25990(8) 0.0277(6) Uani 1 1 d . . . H61A H 0.7872 -0.1067 0.2420 0.033 Uiso 1 1 calc R . . C62 C 0.85018(17) -0.18427(16) 0.27932(8) 0.0326(7) Uani 1 1 d . . . H62A H 0.9025 -0.1654 0.2741 0.039 Uiso 1 1 calc R . . C63 C 0.83887(17) -0.24729(16) 0.30670(8) 0.0347(7) Uani 1 1 d . . . H63A H 0.8835 -0.2720 0.3200 0.042 Uiso 1 1 calc R . . C64 C 0.76019(17) -0.27278(16) 0.31392(8) 0.0332(7) Uani 1 1 d . . . H64A H 0.7532 -0.3139 0.3334 0.040 Uiso 1 1 calc R . . C65 C 0.53389(14) -0.06914(14) 0.06367(8) 0.0240(6) Uani 1 1 d . . . C66 C 0.65837(15) 0.10246(17) 0.17020(8) 0.0329(7) Uani 1 1 d . . . H66A H 0.6778 0.0612 0.1870 0.039 Uiso 1 1 calc R . . C67 C 0.70996(17) 0.16411(17) 0.16381(9) 0.0384(7) Uani 1 1 d . . . H67A H 0.7626 0.1643 0.1763 0.046 Uiso 1 1 calc R . . C68 C 0.68214(17) 0.22511(17) 0.13873(10) 0.0411(8) Uani 1 1 d . . . H68A H 0.7160 0.2669 0.1335 0.049 Uiso 1 1 calc R . . C69 C 0.60258(17) 0.22354(16) 0.12124(9) 0.0353(7) Uani 1 1 d . . . H69A H 0.5822 0.2646 0.1045 0.042 Uiso 1 1 calc R . . C70 C 0.55423(15) 0.16000(15) 0.12904(8) 0.0260(6) Uani 1 1 d . . . C71 C 0.46868(15) 0.15043(14) 0.11451(8) 0.0240(6) Uani 1 1 d . . . C72 C 0.34490(15) 0.16043(14) 0.08628(8) 0.0236(6) Uani 1 1 d . . . C73 C 0.27074(16) 0.19071(15) 0.06412(8) 0.0255(6) Uani 1 1 d . . . C74 C 0.19465(16) 0.16406(15) 0.07740(8) 0.0282(6) Uani 1 1 d . . . H74A H 0.1906 0.1235 0.0975 0.034 Uiso 1 1 calc R . . C75 C 0.12532(17) 0.19900(16) 0.06013(8) 0.0351(7) Uani 1 1 d . . . H75A H 0.0734 0.1833 0.0689 0.042 Uiso 1 1 calc R . . C76 C 0.13465(18) 0.25811(16) 0.02944(9) 0.0368(7) Uani 1 1 d . . . H76A H 0.0892 0.2835 0.0176 0.044 Uiso 1 1 calc R . . C77 C 0.21228(19) 0.27828(16) 0.01698(9) 0.0377(7) Uani 1 1 d . . . H77A H 0.2177 0.3167 -0.0045 0.045 Uiso 1 1 calc R . . C78 C 0.44439(15) 0.07928(15) 0.26042(9) 0.0277(6) 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 Fe11 0.0205(2) 0.0202(3) 0.0200(3) 0.0054(2) 0.00215(19) 0.0025(2) S1 0.0602(5) 0.0293(4) 0.0427(5) 0.0019(3) -0.0130(4) -0.0086(4) N1 0.0224(11) 0.0196(12) 0.0245(12) 0.0023(9) 0.0034(9) 0.0002(9) N2 0.0220(11) 0.0249(12) 0.0220(11) 0.0047(9) 0.0025(9) 0.0015(9) N3 0.0334(13) 0.0242(13) 0.0294(13) 0.0045(10) 0.0010(10) 0.0014(10) N4 0.0213(11) 0.0257(12) 0.0235(12) 0.0036(9) 0.0036(9) 0.0021(9) N5 0.0326(13) 0.0356(14) 0.0231(12) 0.0070(10) 0.0054(10) 0.0024(11) N6 0.0233(11) 0.0203(12) 0.0168(11) 0.0037(9) -0.0003(8) -0.0004(9) N7 0.0305(13) 0.0328(14) 0.0208(13) 0.0110(11) -0.0026(9) -0.0016(11) C1 0.0246(14) 0.0272(16) 0.0330(16) -0.0008(12) 0.0026(11) -0.0009(12) C2 0.0214(14) 0.0341(17) 0.0404(17) -0.0021(13) 0.0005(12) -0.0019(12) C3 0.0259(14) 0.0378(18) 0.0355(17) 0.0006(13) -0.0088(12) -0.0013(13) C4 0.0297(15) 0.0293(16) 0.0271(15) 0.0040(12) -0.0019(11) -0.0002(12) C5 0.0224(13) 0.0175(14) 0.0243(14) 0.0022(11) 0.0004(10) -0.0016(10) C6 0.0215(13) 0.0175(13) 0.0216(14) 0.0034(11) -0.0009(10) -0.0005(10) C7 0.0235(13) 0.0215(14) 0.0207(14) 0.0002(11) 0.0000(10) 0.0027(11) C8 0.0251(14) 0.0230(15) 0.0244(15) -0.0016(11) 0.0032(11) -0.0029(11) C9 0.0263(14) 0.0336(17) 0.0213(14) -0.0011(12) -0.0005(11) -0.0023(12) C10 0.0227(14) 0.0499(19) 0.0302(16) -0.0069(14) 0.0031(11) -0.0017(13) C11 0.0342(16) 0.054(2) 0.0324(17) -0.0017(15) 0.0162(13) -0.0108(15) C12 0.0431(18) 0.051(2) 0.0244(16) 0.0073(14) 0.0096(13) -0.0042(15) C13 0.0269(14) 0.0257(16) 0.0269(15) 0.0089(12) -0.0002(11) 0.0055(12) Fe12 0.02313(19) 0.0212(2) 0.0189(2) -0.00419(16) 0.00271(14) -0.00175(17) S2 0.0566(5) 0.0279(4) 0.0417(5) -0.0021(3) -0.0111(4) 0.0090(4) S3 0.0465(5) 0.0253(4) 0.0523(5) -0.0003(4) -0.0062(4) 0.0024(3) N8 0.0227(11) 0.0237(12) 0.0259(12) -0.0001(9) 0.0023(9) 0.0031(9) N9 0.0212(11) 0.0256(12) 0.0227(11) -0.0059(9) 0.0033(9) -0.0024(9) N10 0.0361(13) 0.0274(14) 0.0296(13) -0.0031(11) 0.0007(10) -0.0032(11) N11 0.0224(11) 0.0267(13) 0.0233(12) -0.0048(9) 0.0037(9) -0.0033(9) N12 0.0356(13) 0.0317(14) 0.0215(12) -0.0052(10) 0.0054(10) -0.0088(11) N13 0.0234(11) 0.0214(12) 0.0154(11) -0.0033(9) -0.0009(8) 0.0001(9) N14 0.0312(13) 0.0319(14) 0.0211(13) -0.0079(11) -0.0022(10) -0.0024(11) N15 0.0247(11) 0.0226(12) 0.0270(12) -0.0011(10) 0.0028(9) 0.0010(9) N16 0.0220(11) 0.0225(12) 0.0236(12) -0.0035(9) 0.0044(9) -0.0028(9) N17 0.0406(14) 0.0286(15) 0.0319(13) -0.0013(11) 0.0046(11) -0.0012(11) N18 0.0238(11) 0.0266(13) 0.0234(12) -0.0038(10) 0.0028(9) -0.0037(9) N19 0.0365(13) 0.0319(14) 0.0211(12) -0.0026(10) 0.0053(10) -0.0006(11) N20 0.0228(11) 0.0229(12) 0.0195(11) -0.0023(9) -0.0030(9) -0.0002(9) N21 0.0305(13) 0.0283(14) 0.0208(13) -0.0056(10) -0.0029(9) -0.0004(11) C14 0.0265(14) 0.0269(16) 0.0324(15) 0.0025(12) 0.0035(11) 0.0048(12) C15 0.0189(13) 0.0357(17) 0.0446(18) 0.0024(14) -0.0005(12) 0.0027(12) C16 0.0230(14) 0.0354(17) 0.0410(17) -0.0014(14) -0.0103(12) 0.0006(12) C17 0.0262(14) 0.0316(16) 0.0311(15) -0.0052(12) -0.0025(11) 0.0041(12) C18 0.0233(13) 0.0208(14) 0.0228(14) -0.0024(11) -0.0001(10) 0.0030(11) C19 0.0234(13) 0.0194(14) 0.0189(13) -0.0022(11) 0.0001(10) -0.0003(11) C20 0.0258(13) 0.0197(14) 0.0210(14) -0.0002(11) -0.0013(10) -0.0017(11) C21 0.0273(14) 0.0221(14) 0.0214(14) 0.0021(11) 0.0048(11) -0.0002(11) C22 0.0253(14) 0.0284(16) 0.0270(15) 0.0010(12) -0.0003(11) -0.0012(12) C23 0.0264(14) 0.0354(17) 0.0359(17) 0.0057(13) 0.0033(12) 0.0004(13) C24 0.0370(17) 0.0406(19) 0.0383(18) 0.0028(14) 0.0161(13) -0.0014(14) C25 0.0452(18) 0.0400(19) 0.0227(15) -0.0072(13) 0.0133(13) -0.0065(14) C26 0.0295(15) 0.0277(16) 0.0249(15) -0.0091(12) -0.0012(11) -0.0047(12) C27 0.0237(14) 0.0289(16) 0.0373(16) 0.0000(13) 0.0050(12) 0.0021(12) C28 0.0224(14) 0.0356(18) 0.0465(18) 0.0009(14) -0.0006(12) 0.0006(12) C29 0.0261(15) 0.0401(18) 0.0396(17) -0.0040(14) -0.0084(12) 0.0025(13) C30 0.0284(15) 0.0359(17) 0.0273(15) -0.0026(12) -0.0055(11) 0.0030(13) C31 0.0270(14) 0.0179(14) 0.0248(14) 0.0004(11) 0.0008(11) -0.0001(11) C32 0.0256(13) 0.0174(14) 0.0206(14) -0.0021(11) -0.0012(10) 0.0008(11) C33 0.0258(13) 0.0197(14) 0.0202(14) -0.0007(11) 0.0006(10) -0.0005(11) C34 0.0282(14) 0.0213(15) 0.0242(14) 0.0033(11) 0.0037(11) -0.0005(11) C35 0.0316(15) 0.0404(18) 0.0227(15) 0.0013(13) 0.0042(11) -0.0016(13) C36 0.0297(15) 0.045(2) 0.0361(17) 0.0042(14) 0.0061(12) -0.0010(14) C37 0.0382(17) 0.044(2) 0.0363(18) 0.0066(14) 0.0175(13) 0.0075(14) C38 0.0493(19) 0.0404(19) 0.0253(16) -0.0023(13) 0.0131(13) 0.0039(15) C39 0.0317(15) 0.0296(17) 0.0272(15) -0.0077(13) 0.0051(12) -0.0027(13) Fe21 0.0219(3) 0.0213(3) 0.0199(3) 0.0004(2) 0.00064(19) -0.0031(2) S4 0.0320(4) 0.0433(5) 0.0308(4) 0.0130(3) 0.0085(3) 0.0033(3) N22 0.0245(11) 0.0265(13) 0.0193(11) 0.0031(9) 0.0011(9) -0.0020(9) N23 0.0201(11) 0.0251(12) 0.0270(12) -0.0011(10) -0.0012(9) -0.0036(9) N24 0.0308(12) 0.0290(13) 0.0242(12) 0.0016(10) 0.0012(9) -0.0002(10) N25 0.0212(11) 0.0266(13) 0.0259(12) -0.0002(10) -0.0016(9) -0.0032(9) N26 0.0353(13) 0.0238(13) 0.0223(12) -0.0003(10) -0.0010(9) -0.0053(10) N27 0.0270(12) 0.0167(12) 0.0226(11) 0.0019(9) 0.0007(9) 0.0010(9) N28 0.0425(15) 0.0290(14) 0.0326(14) -0.0068(11) -0.0041(11) 0.0151(12) C40 0.0232(14) 0.0397(17) 0.0237(14) 0.0043(12) -0.0011(11) -0.0056(12) C41 0.0223(14) 0.0460(19) 0.0321(16) 0.0107(14) -0.0013(11) 0.0003(13) C42 0.0298(15) 0.0291(17) 0.0438(17) 0.0110(13) 0.0016(13) 0.0041(13) C43 0.0306(15) 0.0228(15) 0.0400(16) 0.0054(12) 0.0006(12) -0.0008(12) C44 0.0229(13) 0.0234(15) 0.0234(14) 0.0069(11) 0.0037(10) -0.0029(11) C45 0.0240(13) 0.0160(14) 0.0249(14) 0.0044(11) 0.0006(10) -0.0027(11) C46 0.0274(14) 0.0192(14) 0.0202(13) 0.0037(11) 0.0001(10) -0.0006(11) C47 0.0310(14) 0.0209(14) 0.0161(13) 0.0038(11) -0.0013(10) -0.0043(11) C48 0.0310(14) 0.0237(15) 0.0207(14) 0.0019(11) -0.0053(11) 0.0001(12) C49 0.0299(15) 0.0356(17) 0.0302(15) 0.0054(13) -0.0094(12) 0.0035(13) C50 0.0411(17) 0.0406(19) 0.0267(15) 0.0022(13) -0.0132(13) -0.0086(14) C51 0.0461(18) 0.0320(17) 0.0256(15) -0.0038(13) -0.0062(13) -0.0060(14) C52 0.0192(13) 0.0254(15) 0.0263(15) -0.0003(12) -0.0013(11) 0.0015(11) Fe22 0.02241(19) 0.0223(2) 0.0208(2) -0.00060(16) 0.00271(14) 0.00094(16) S5 0.0320(4) 0.0373(4) 0.0286(4) -0.0104(3) 0.0067(3) -0.0009(3) S6 0.0365(4) 0.0509(5) 0.0371(4) -0.0213(4) 0.0138(3) -0.0074(4) N29 0.0221(11) 0.0277(13) 0.0215(11) -0.0024(9) 0.0042(9) -0.0012(9) N30 0.0252(12) 0.0242(12) 0.0257(12) 0.0010(10) 0.0010(9) 0.0015(10) N31 0.0304(12) 0.0294(13) 0.0260(13) -0.0020(10) 0.0012(9) 0.0034(10) N32 0.0250(12) 0.0273(13) 0.0267(12) 0.0012(10) 0.0000(9) 0.0007(10) N33 0.0369(13) 0.0295(14) 0.0206(12) -0.0002(10) 0.0013(10) 0.0024(11) N34 0.0300(12) 0.0191(12) 0.0223(12) 0.0007(9) 0.0010(9) -0.0027(9) N35 0.0463(16) 0.0343(16) 0.0360(16) 0.0113(12) -0.0071(12) -0.0110(12) N36 0.0266(12) 0.0306(13) 0.0226(12) -0.0053(10) 0.0060(9) -0.0009(10) N37 0.0200(11) 0.0247(13) 0.0310(12) -0.0003(10) 0.0026(9) 0.0013(9) N38 0.0315(13) 0.0327(14) 0.0287(13) -0.0046(11) 0.0039(10) -0.0024(10) N39 0.0244(11) 0.0220(12) 0.0276(12) 0.0022(10) 0.0017(9) 0.0016(9) N40 0.0453(14) 0.0270(13) 0.0230(12) 0.0035(10) 0.0026(10) 0.0069(11) N41 0.0349(13) 0.0172(12) 0.0237(12) 0.0002(9) 0.0048(9) -0.0017(10) N42 0.0499(16) 0.0222(14) 0.0370(16) 0.0060(11) 0.0030(12) -0.0082(12) C53 0.0301(15) 0.0372(17) 0.0231(14) -0.0039(12) 0.0013(11) 0.0021(13) C54 0.0292(15) 0.046(2) 0.0286(15) -0.0089(14) -0.0003(12) -0.0060(14) C55 0.0334(16) 0.0320(18) 0.0412(17) -0.0076(14) 0.0028(13) -0.0095(13) C56 0.0375(16) 0.0260(16) 0.0343(16) -0.0044(12) 0.0021(12) -0.0030(13) C57 0.0284(14) 0.0300(16) 0.0205(14) -0.0070(12) 0.0033(11) -0.0027(12) C58 0.0301(14) 0.0170(14) 0.0221(14) -0.0044(11) 0.0035(11) 0.0014(11) C59 0.0284(14) 0.0214(15) 0.0180(13) -0.0048(11) 0.0036(10) -0.0002(11) C60 0.0322(14) 0.0217(15) 0.0195(14) -0.0024(11) -0.0020(11) 0.0013(11) C61 0.0369(15) 0.0239(15) 0.0220(14) -0.0005(11) -0.0060(11) -0.0039(12) C62 0.0335(16) 0.0392(18) 0.0249(15) -0.0046(13) -0.0052(12) -0.0049(13) C63 0.0370(17) 0.0413(19) 0.0255(15) -0.0019(13) -0.0073(12) 0.0100(14) C64 0.0459(18) 0.0323(17) 0.0214(14) 0.0031(12) -0.0008(12) 0.0071(14) C65 0.0182(12) 0.0244(15) 0.0294(15) 0.0019(12) 0.0029(11) -0.0013(11) C66 0.0243(14) 0.0474(19) 0.0269(15) -0.0081(13) 0.0042(11) 0.0007(13) C67 0.0266(15) 0.050(2) 0.0391(17) -0.0170(15) 0.0068(12) -0.0045(14) C68 0.0289(16) 0.0369(19) 0.058(2) -0.0166(16) 0.0136(14) -0.0110(14) C69 0.0338(16) 0.0257(16) 0.0467(18) -0.0061(13) 0.0091(13) -0.0042(13) C70 0.0255(14) 0.0266(16) 0.0262(14) -0.0093(12) 0.0081(11) -0.0010(11) C71 0.0283(14) 0.0183(14) 0.0254(14) -0.0033(11) 0.0062(11) 0.0016(11) C72 0.0307(14) 0.0188(14) 0.0213(14) -0.0006(11) 0.0044(11) 0.0010(11) C73 0.0359(15) 0.0209(15) 0.0198(14) -0.0033(11) -0.0003(11) 0.0027(12) C74 0.0370(16) 0.0246(15) 0.0228(14) 0.0008(11) -0.0079(12) -0.0003(12) C75 0.0362(16) 0.0347(17) 0.0342(16) -0.0082(14) -0.0135(13) -0.0012(13) C76 0.0487(19) 0.0272(17) 0.0340(16) -0.0065(13) -0.0194(14) 0.0108(14) C77 0.060(2) 0.0252(17) 0.0280(16) 0.0013(12) -0.0053(14) 0.0091(15) C78 0.0202(13) 0.0312(16) 0.0319(16) -0.0015(13) 0.0023(11) -0.0040(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 Fe11 N3 2.122(2) 3_765 ? Fe11 N3 2.122(2) . ? Fe11 N2 2.1437(19) 3_765 ? Fe11 N2 2.1437(19) . ? Fe11 N1 2.1977(19) 3_765 ? Fe11 N1 2.1977(19) . ? S1 C13 1.637(3) . ? N1 C1 1.334(3) . ? N1 C5 1.356(3) . ? N2 C6 1.322(3) . ? N2 N4 1.369(3) . ? N3 C13 1.158(3) . ? N4 C7 1.314(3) . ? N5 C12 1.335(3) . ? N5 C8 1.344(3) . ? N6 C6 1.354(3) . ? N6 C7 1.371(3) . ? N6 N7 1.418(3) . ? N7 H1N 0.93(3) . ? N7 H2N 0.86(3) . ? C1 C2 1.394(3) . ? C1 H1A 0.9300 . ? C2 C3 1.378(3) . ? C2 H2A 0.9300 . ? C3 C4 1.385(3) . ? C3 H3A 0.9300 . ? C4 C5 1.383(3) . ? C4 H4A 0.9300 . ? C5 C6 1.465(3) . ? C7 C8 1.466(3) . ? C8 C9 1.388(3) . ? C9 C10 1.386(3) . ? C9 H9A 0.9300 . ? C10 C11 1.375(4) . ? C10 H10A 0.9300 . ? C11 C12 1.387(4) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? Fe12 N17 2.110(2) . ? Fe12 N10 2.116(2) . ? Fe12 N9 2.1327(19) . ? Fe12 N16 2.1374(19) . ? Fe12 N15 2.188(2) . ? Fe12 N8 2.191(2) . ? S2 C26 1.643(3) . ? S3 C39 1.642(3) . ? N8 C14 1.336(3) . ? N8 C18 1.353(3) . ? N9 C19 1.321(3) . ? N9 N11 1.370(3) . ? N10 C26 1.160(3) . ? N11 C20 1.319(3) . ? N12 C25 1.335(3) . ? N12 C21 1.344(3) . ? N13 C19 1.353(3) . ? N13 C20 1.367(3) . ? N13 N14 1.419(3) . ? N14 H4N 0.85(3) . ? N14 H3N 0.94(3) . ? N15 C27 1.336(3) . ? N15 C31 1.353(3) . ? N16 C32 1.322(3) . ? N16 N18 1.377(3) . ? N17 C39 1.157(3) . ? N18 C33 1.318(3) . ? N19 C38 1.328(3) . ? N19 C34 1.340(3) . ? N20 C32 1.356(3) . ? N20 C33 1.372(3) . ? N20 N21 1.421(3) . ? N21 H6N 0.85(3) . ? N21 H5N 0.95(3) . ? C14 C15 1.391(3) . ? C14 H14A 0.9300 . ? C15 C16 1.382(3) . ? C15 H15A 0.9300 . ? C16 C17 1.384(3) . ? C16 H16A 0.9300 . ? C17 C18 1.382(3) . ? C17 H17A 0.9300 . ? C18 C19 1.469(3) . ? C20 C21 1.470(3) . ? C21 C22 1.388(3) . ? C22 C23 1.380(3) . ? C22 H22A 0.9300 . ? C23 C24 1.367(4) . ? C23 H23A 0.9300 . ? C24 C25 1.386(4) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C27 C28 1.393(3) . ? C27 H27A 0.9300 . ? C28 C29 1.377(4) . ? C28 H28A 0.9300 . ? C29 C30 1.387(4) . ? C29 H29A 0.9300 . ? C30 C31 1.382(3) . ? C30 H30A 0.9300 . ? C31 C32 1.466(3) . ? C33 C34 1.468(3) . ? C34 C35 1.387(3) . ? C35 C36 1.386(3) . ? C35 H35A 0.9300 . ? C36 C37 1.372(4) . ? C36 H36A 0.9300 . ? C37 C38 1.389(4) . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? Fe21 N24 2.124(2) 3_665 ? Fe21 N24 2.124(2) . ? Fe21 N23 2.1463(19) . ? Fe21 N23 2.1463(19) 3_665 ? Fe21 N22 2.217(2) 3_665 ? Fe21 N22 2.217(2) . ? S4 C52 1.631(3) . ? N22 C40 1.339(3) . ? N22 C44 1.353(3) . ? N23 C45 1.324(3) . ? N23 N25 1.375(3) . ? N24 C52 1.168(3) . ? N25 C46 1.323(3) . ? N26 C51 1.335(3) . ? N26 C47 1.349(3) . ? N27 C45 1.355(3) . ? N27 C46 1.369(3) . ? N27 N28 1.410(3) . ? N28 H8N 0.92(3) . ? N28 H7N 0.91(3) . ? C40 C41 1.384(4) . ? C40 H40A 0.9300 . ? C41 C42 1.376(4) . ? C41 H41A 0.9300 . ? C42 C43 1.389(3) . ? C42 H42A 0.9300 . ? C43 C44 1.384(3) . ? C43 H43A 0.9300 . ? C44 C45 1.473(3) . ? C46 C47 1.465(3) . ? C47 C48 1.392(3) . ? C48 C49 1.379(3) . ? C48 H48A 0.9300 . ? C49 C50 1.384(4) . ? C49 H49A 0.9300 . ? C50 C51 1.378(4) . ? C50 H50A 0.9300 . ? C51 H51A 0.9300 . ? Fe22 N38 2.119(2) . ? Fe22 N31 2.125(2) . ? Fe22 N37 2.142(2) . ? Fe22 N30 2.152(2) . ? Fe22 N29 2.213(2) . ? Fe22 N36 2.222(2) . ? S5 C65 1.632(3) . ? S6 C78 1.627(3) . ? N29 C53 1.337(3) . ? N29 C57 1.354(3) . ? N30 C58 1.318(3) . ? N30 N32 1.381(3) . ? N31 C65 1.170(3) . ? N32 C59 1.321(3) . ? N33 C64 1.335(3) . ? N33 C60 1.338(3) . ? N34 C58 1.351(3) . ? N34 C59 1.376(3) . ? N34 N35 1.414(3) . ? N35 H10N 0.91(3) . ? N35 H9N 0.84(3) . ? N36 C66 1.341(3) . ? N36 C70 1.357(3) . ? N37 C71 1.320(3) . ? N37 N39 1.369(3) . ? N38 C78 1.170(3) . ? N39 C72 1.323(3) . ? N40 C77 1.335(3) . ? N40 C73 1.339(3) . ? N41 C71 1.356(3) . ? N41 C72 1.375(3) . ? N41 N42 1.413(3) . ? N42 H11N 0.88(3) . ? N42 H12N 0.92(3) . ? C53 C54 1.381(4) . ? C53 H53A 0.9300 . ? C54 C55 1.378(4) . ? C54 H54A 0.9300 . ? C55 C56 1.386(4) . ? C55 H55A 0.9300 . ? C56 C57 1.387(3) . ? C56 H56A 0.9300 . ? C57 C58 1.469(3) . ? C59 C60 1.472(3) . ? C60 C61 1.394(3) . ? C61 C62 1.382(3) . ? C61 H61A 0.9300 . ? C62 C63 1.382(4) . ? C62 H62A 0.9300 . ? C63 C64 1.378(4) . ? C63 H63A 0.9300 . ? C64 H64A 0.9300 . ? C66 C67 1.382(4) . ? C66 H66A 0.9300 . ? C67 C68 1.373(4) . ? C67 H67A 0.9300 . ? C68 C69 1.391(4) . ? C68 H68A 0.9300 . ? C69 C70 1.384(3) . ? C69 H69A 0.9300 . ? C70 C71 1.464(3) . ? C72 C73 1.467(3) . ? C73 C74 1.388(3) . ? C74 C75 1.377(3) . ? C74 H74A 0.9300 . ? C75 C76 1.387(4) . ? C75 H75A 0.9300 . ? C76 C77 1.370(4) . ? C76 H76A 0.9300 . ? C77 H77A 0.9300 . ? 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 N3 Fe11 N3 180.00(10) 3_765 . ? N3 Fe11 N2 89.74(8) 3_765 3_765 ? N3 Fe11 N2 90.26(8) . 3_765 ? N3 Fe11 N2 90.26(8) 3_765 . ? N3 Fe11 N2 89.74(8) . . ? N2 Fe11 N2 180.00(11) 3_765 . ? N3 Fe11 N1 92.84(7) 3_765 3_765 ? N3 Fe11 N1 87.16(7) . 3_765 ? N2 Fe11 N1 75.87(7) 3_765 3_765 ? N2 Fe11 N1 104.13(7) . 3_765 ? N3 Fe11 N1 87.16(7) 3_765 . ? N3 Fe11 N1 92.84(7) . . ? N2 Fe11 N1 104.13(7) 3_765 . ? N2 Fe11 N1 75.87(7) . . ? N1 Fe11 N1 180.00(12) 3_765 . ? C1 N1 C5 118.2(2) . . ? C1 N1 Fe11 125.77(17) . . ? C5 N1 Fe11 115.91(15) . . ? C6 N2 N4 108.64(19) . . ? C6 N2 Fe11 114.47(16) . . ? N4 N2 Fe11 136.59(15) . . ? C13 N3 Fe11 164.3(2) . . ? C7 N4 N2 106.79(19) . . ? C12 N5 C8 117.1(2) . . ? C6 N6 C7 105.68(18) . . ? C6 N6 N7 124.8(2) . . ? C7 N6 N7 129.3(2) . . ? N6 N7 H1N 101.3(16) . . ? N6 N7 H2N 101.3(17) . . ? H1N N7 H2N 106(2) . . ? N1 C1 C2 122.8(2) . . ? N1 C1 H1A 118.6 . . ? C2 C1 H1A 118.6 . . ? C3 C2 C1 118.5(2) . . ? C3 C2 H2A 120.7 . . ? C1 C2 H2A 120.7 . . ? C2 C3 C4 119.4(2) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C5 C4 C3 118.9(2) . . ? C5 C4 H4A 120.5 . . ? C3 C4 H4A 120.5 . . ? N1 C5 C4 122.2(2) . . ? N1 C5 C6 112.6(2) . . ? C4 C5 C6 125.2(2) . . ? N2 C6 N6 108.9(2) . . ? N2 C6 C5 120.8(2) . . ? N6 C6 C5 130.2(2) . . ? N4 C7 N6 109.9(2) . . ? N4 C7 C8 124.0(2) . . ? N6 C7 C8 126.0(2) . . ? N5 C8 C9 123.5(2) . . ? N5 C8 C7 116.6(2) . . ? C9 C8 C7 119.9(2) . . ? C10 C9 C8 118.3(2) . . ? C10 C9 H9A 120.9 . . ? C8 C9 H9A 120.9 . . ? C11 C10 C9 118.9(3) . . ? C11 C10 H10A 120.6 . . ? C9 C10 H10A 120.6 . . ? C10 C11 C12 119.1(2) . . ? C10 C11 H11A 120.5 . . ? C12 C11 H11A 120.5 . . ? N5 C12 C11 123.2(3) . . ? N5 C12 H12A 118.4 . . ? C11 C12 H12A 118.4 . . ? N3 C13 S1 178.5(3) . . ? N17 Fe12 N10 179.49(9) . . ? N17 Fe12 N9 90.60(8) . . ? N10 Fe12 N9 89.84(8) . . ? N17 Fe12 N16 89.27(8) . . ? N10 Fe12 N16 90.30(8) . . ? N9 Fe12 N16 179.52(8) . . ? N17 Fe12 N15 93.72(8) . . ? N10 Fe12 N15 86.44(8) . . ? N9 Fe12 N15 103.57(8) . . ? N16 Fe12 N15 75.98(7) . . ? N17 Fe12 N8 89.03(8) . . ? N10 Fe12 N8 90.83(8) . . ? N9 Fe12 N8 75.87(7) . . ? N16 Fe12 N8 104.59(7) . . ? N15 Fe12 N8 177.21(7) . . ? C14 N8 C18 118.3(2) . . ? C14 N8 Fe12 125.30(17) . . ? C18 N8 Fe12 116.42(15) . . ? C19 N9 N11 109.01(19) . . ? C19 N9 Fe12 114.44(16) . . ? N11 N9 Fe12 136.26(15) . . ? C26 N10 Fe12 165.0(2) . . ? C20 N11 N9 106.31(19) . . ? C25 N12 C21 117.1(2) . . ? C19 N13 C20 105.92(18) . . ? C19 N13 N14 124.7(2) . . ? C20 N13 N14 129.2(2) . . ? N13 N14 H4N 97.9(18) . . ? N13 N14 H3N 103.1(16) . . ? H4N N14 H3N 104(2) . . ? C27 N15 C31 117.8(2) . . ? C27 N15 Fe12 125.80(17) . . ? C31 N15 Fe12 116.09(16) . . ? C32 N16 N18 108.46(19) . . ? C32 N16 Fe12 114.54(16) . . ? N18 N16 Fe12 136.68(15) . . ? C39 N17 Fe12 168.2(2) . . ? C33 N18 N16 106.70(19) . . ? C38 N19 C34 116.9(2) . . ? C32 N20 C33 105.65(19) . . ? C32 N20 N21 124.7(2) . . ? C33 N20 N21 129.6(2) . . ? N20 N21 H6N 96.6(17) . . ? N20 N21 H5N 100.1(15) . . ? H6N N21 H5N 108(2) . . ? N8 C14 C15 122.4(2) . . ? N8 C14 H14A 118.8 . . ? C15 C14 H14A 118.8 . . ? C16 C15 C14 118.8(2) . . ? C16 C15 H15A 120.6 . . ? C14 C15 H15A 120.6 . . ? C15 C16 C17 119.3(2) . . ? C15 C16 H16A 120.3 . . ? C17 C16 H16A 120.3 . . ? C18 C17 C16 118.6(2) . . ? C18 C17 H17A 120.7 . . ? C16 C17 H17A 120.7 . . ? N8 C18 C17 122.6(2) . . ? N8 C18 C19 111.9(2) . . ? C17 C18 C19 125.5(2) . . ? N9 C19 N13 108.7(2) . . ? N9 C19 C18 121.1(2) . . ? N13 C19 C18 130.2(2) . . ? N11 C20 N13 110.1(2) . . ? N11 C20 C21 124.3(2) . . ? N13 C20 C21 125.7(2) . . ? N12 C21 C22 123.4(2) . . ? N12 C21 C20 116.6(2) . . ? C22 C21 C20 120.0(2) . . ? C23 C22 C21 118.0(2) . . ? C23 C22 H22A 121.0 . . ? C21 C22 H22A 121.0 . . ? C24 C23 C22 119.3(3) . . ? C24 C23 H23A 120.3 . . ? C22 C23 H23A 120.3 . . ? C23 C24 C25 119.1(3) . . ? C23 C24 H24A 120.5 . . ? C25 C24 H24A 120.5 . . ? N12 C25 C24 123.0(2) . . ? N12 C25 H25A 118.5 . . ? C24 C25 H25A 118.5 . . ? N10 C26 S2 178.9(3) . . ? N15 C27 C28 123.1(3) . . ? N15 C27 H27A 118.5 . . ? C28 C27 H27A 118.5 . . ? C29 C28 C27 118.4(3) . . ? C29 C28 H28A 120.8 . . ? C27 C28 H28A 120.8 . . ? C28 C29 C30 119.4(2) . . ? C28 C29 H29A 120.3 . . ? C30 C29 H29A 120.3 . . ? C31 C30 C29 118.8(2) . . ? C31 C30 H30A 120.6 . . ? C29 C30 H30A 120.6 . . ? N15 C31 C30 122.6(2) . . ? N15 C31 C32 112.5(2) . . ? C30 C31 C32 124.9(2) . . ? N16 C32 N20 109.2(2) . . ? N16 C32 C31 120.5(2) . . ? N20 C32 C31 130.3(2) . . ? N18 C33 N20 110.0(2) . . ? N18 C33 C34 124.2(2) . . ? N20 C33 C34 125.8(2) . . ? N19 C34 C35 123.8(2) . . ? N19 C34 C33 116.8(2) . . ? C35 C34 C33 119.4(2) . . ? C36 C35 C34 118.0(2) . . ? C36 C35 H35A 121.0 . . ? C34 C35 H35A 121.0 . . ? C37 C36 C35 119.0(3) . . ? C37 C36 H36A 120.5 . . ? C35 C36 H36A 120.5 . . ? C36 C37 C38 118.7(3) . . ? C36 C37 H37A 120.6 . . ? C38 C37 H37A 120.6 . . ? N19 C38 C37 123.6(3) . . ? N19 C38 H38A 118.2 . . ? C37 C38 H38A 118.2 . . ? N17 C39 S3 178.3(3) . . ? N24 Fe21 N24 180.00(4) 3_665 . ? N24 Fe21 N23 92.12(8) 3_665 . ? N24 Fe21 N23 87.88(8) . . ? N24 Fe21 N23 87.88(8) 3_665 3_665 ? N24 Fe21 N23 92.12(8) . 3_665 ? N23 Fe21 N23 180.00(9) . 3_665 ? N24 Fe21 N22 89.70(7) 3_665 3_665 ? N24 Fe21 N22 90.30(7) . 3_665 ? N23 Fe21 N22 104.48(7) . 3_665 ? N23 Fe21 N22 75.52(7) 3_665 3_665 ? N24 Fe21 N22 90.30(7) 3_665 . ? N24 Fe21 N22 89.70(7) . . ? N23 Fe21 N22 75.52(7) . . ? N23 Fe21 N22 104.48(7) 3_665 . ? N22 Fe21 N22 180.0 3_665 . ? C40 N22 C44 117.9(2) . . ? C40 N22 Fe21 126.14(18) . . ? C44 N22 Fe21 115.83(15) . . ? C45 N23 N25 108.75(19) . . ? C45 N23 Fe21 113.23(16) . . ? N25 N23 Fe21 133.57(16) . . ? C52 N24 Fe21 168.8(2) . . ? C46 N25 N23 106.4(2) . . ? C51 N26 C47 116.7(2) . . ? C45 N27 C46 105.8(2) . . ? C45 N27 N28 124.3(2) . . ? C46 N27 N28 129.7(2) . . ? N27 N28 H8N 99.3(17) . . ? N27 N28 H7N 104.8(17) . . ? H8N N28 H7N 103(2) . . ? N22 C40 C41 123.0(2) . . ? N22 C40 H40A 118.5 . . ? C41 C40 H40A 118.5 . . ? C42 C41 C40 118.6(2) . . ? C42 C41 H41A 120.7 . . ? C40 C41 H41A 120.7 . . ? C41 C42 C43 119.6(3) . . ? C41 C42 H42A 120.2 . . ? C43 C42 H42A 120.2 . . ? C44 C43 C42 118.4(3) . . ? C44 C43 H43A 120.8 . . ? C42 C43 H43A 120.8 . . ? N22 C44 C43 122.5(2) . . ? N22 C44 C45 111.7(2) . . ? C43 C44 C45 125.7(2) . . ? N23 C45 N27 109.0(2) . . ? N23 C45 C44 120.8(2) . . ? N27 C45 C44 130.3(2) . . ? N25 C46 N27 110.1(2) . . ? N25 C46 C47 123.2(2) . . ? N27 C46 C47 126.6(2) . . ? N26 C47 C48 123.0(2) . . ? N26 C47 C46 117.1(2) . . ? C48 C47 C46 119.9(2) . . ? C49 C48 C47 118.6(2) . . ? C49 C48 H48A 120.7 . . ? C47 C48 H48A 120.7 . . ? C48 C49 C50 119.1(3) . . ? C48 C49 H49A 120.5 . . ? C50 C49 H49A 120.5 . . ? C51 C50 C49 118.3(2) . . ? C51 C50 H50A 120.9 . . ? C49 C50 H50A 120.9 . . ? N26 C51 C50 124.3(3) . . ? N26 C51 H51A 117.8 . . ? C50 C51 H51A 117.8 . . ? N24 C52 S4 178.5(2) . . ? N38 Fe22 N31 179.83(9) . . ? N38 Fe22 N37 92.35(8) . . ? N31 Fe22 N37 87.65(8) . . ? N38 Fe22 N30 88.63(8) . . ? N31 Fe22 N30 91.37(8) . . ? N37 Fe22 N30 178.53(7) . . ? N38 Fe22 N29 89.18(8) . . ? N31 Fe22 N29 90.98(8) . . ? N37 Fe22 N29 103.33(8) . . ? N30 Fe22 N29 75.58(8) . . ? N38 Fe22 N36 90.17(8) . . ? N31 Fe22 N36 89.66(8) . . ? N37 Fe22 N36 75.01(8) . . ? N30 Fe22 N36 106.09(8) . . ? N29 Fe22 N36 178.19(7) . . ? C53 N29 C57 117.9(2) . . ? C53 N29 Fe22 126.36(18) . . ? C57 N29 Fe22 115.56(16) . . ? C58 N30 N32 108.81(19) . . ? C58 N30 Fe22 113.47(16) . . ? N32 N30 Fe22 134.71(16) . . ? C65 N31 Fe22 172.9(2) . . ? C59 N32 N30 106.2(2) . . ? C64 N33 C60 116.6(2) . . ? C58 N34 C59 105.9(2) . . ? C58 N34 N35 123.4(2) . . ? C59 N34 N35 130.5(2) . . ? N34 N35 H10N 95.7(19) . . ? N34 N35 H9N 105(2) . . ? H10N N35 H9N 93(3) . . ? C66 N36 C70 117.6(2) . . ? C66 N36 Fe22 126.32(19) . . ? C70 N36 Fe22 116.05(16) . . ? C71 N37 N39 109.4(2) . . ? C71 N37 Fe22 114.69(16) . . ? N39 N37 Fe22 134.44(16) . . ? C78 N38 Fe22 171.4(2) . . ? C72 N39 N37 106.4(2) . . ? C77 N40 C73 116.4(3) . . ? C71 N41 C72 106.0(2) . . ? C71 N41 N42 124.8(2) . . ? C72 N41 N42 129.1(2) . . ? N41 N42 H11N 105.8(18) . . ? N41 N42 H12N 101.7(17) . . ? H11N N42 H12N 103(2) . . ? N29 C53 C54 122.9(3) . . ? N29 C53 H53A 118.5 . . ? C54 C53 H53A 118.5 . . ? C55 C54 C53 118.9(3) . . ? C55 C54 H54A 120.6 . . ? C53 C54 H54A 120.6 . . ? C54 C55 C56 119.4(3) . . ? C54 C55 H55A 120.3 . . ? C56 C55 H55A 120.3 . . ? C55 C56 C57 118.4(3) . . ? C55 C56 H56A 120.8 . . ? C57 C56 H56A 120.8 . . ? N29 C57 C56 122.4(2) . . ? N29 C57 C58 112.3(2) . . ? C56 C57 C58 125.2(2) . . ? N30 C58 N34 109.2(2) . . ? N30 C58 C57 120.7(2) . . ? N34 C58 C57 130.1(2) . . ? N32 C59 N34 109.9(2) . . ? N32 C59 C60 123.4(2) . . ? N34 C59 C60 126.5(2) . . ? N33 C60 C61 123.5(2) . . ? N33 C60 C59 117.5(2) . . ? C61 C60 C59 118.9(2) . . ? C62 C61 C60 118.6(2) . . ? C62 C61 H61A 120.7 . . ? C60 C61 H61A 120.7 . . ? C61 C62 C63 118.4(3) . . ? C61 C62 H62A 120.8 . . ? C63 C62 H62A 120.8 . . ? C64 C63 C62 118.8(3) . . ? C64 C63 H63A 120.6 . . ? C62 C63 H63A 120.6 . . ? N33 C64 C63 124.1(3) . . ? N33 C64 H64A 117.9 . . ? C63 C64 H64A 117.9 . . ? N31 C65 S5 177.7(2) . . ? N36 C66 C67 123.3(3) . . ? N36 C66 H66A 118.4 . . ? C67 C66 H66A 118.4 . . ? C68 C67 C66 118.9(3) . . ? C68 C67 H67A 120.6 . . ? C66 C67 H67A 120.6 . . ? C67 C68 C69 119.1(3) . . ? C67 C68 H68A 120.5 . . ? C69 C68 H68A 120.5 . . ? C70 C69 C68 119.0(3) . . ? C70 C69 H69A 120.5 . . ? C68 C69 H69A 120.5 . . ? N36 C70 C69 122.2(2) . . ? N36 C70 C71 111.9(2) . . ? C69 C70 C71 125.8(2) . . ? N37 C71 N41 108.6(2) . . ? N37 C71 C70 121.0(2) . . ? N41 C71 C70 130.4(2) . . ? N39 C72 N41 109.7(2) . . ? N39 C72 C73 124.0(2) . . ? N41 C72 C73 126.2(2) . . ? N40 C73 C74 123.5(2) . . ? N40 C73 C72 117.2(2) . . ? C74 C73 C72 119.1(2) . . ? C75 C74 C73 118.6(2) . . ? C75 C74 H74A 120.7 . . ? C73 C74 H74A 120.7 . . ? C74 C75 C76 118.5(3) . . ? C74 C75 H75A 120.8 . . ? C76 C75 H75A 120.8 . . ? C77 C76 C75 118.7(3) . . ? C77 C76 H76A 120.7 . . ? C75 C76 H76A 120.7 . . ? N40 C77 C76 124.2(3) . . ? N40 C77 H77A 117.9 . . ? C76 C77 H77A 117.9 . . ? N38 C78 S6 178.4(3) . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.349 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.063 # Attachment 'CCDC 732125_PhaseC_60K_F_v.cif' data_PhaseC-60K _database_code_depnum_ccdc_archive 'CCDC 732125' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H20 Fe N14 S2' _chemical_formula_sum 'C26 H20 Fe N14 S2' _chemical_formula_weight 648.53 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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.3266(2) _cell_length_b 17.4800(4) _cell_length_c 9.6827(4) _cell_angle_alpha 90.000 _cell_angle_beta 91.1120(10) _cell_angle_gamma 90.000 _cell_volume 2762.82(13) _cell_formula_units_Z 4 _cell_measurement_temperature 60(2) _cell_measurement_reflns_used 20112 _cell_measurement_theta_min 1.25 _cell_measurement_theta_max 27.5 _exptl_crystal_description Block _exptl_crystal_colour Red-Brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.744 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.805 _exptl_absorpt_correction_T_max 0.863 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 60(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 KappaCCD _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23421 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6155 _reflns_number_gt 5547 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD server software (Nonius, 1997)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL/PC & Mercury 1.4.1 (CCDC)' _computing_publication_material 'XIF in SHELXTL/PC' _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^)+(0.0239P)^2^+2.0393P] 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 6155 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0660 _refine_ls_wR_factor_gt 0.0634 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 0.5000 0.5000 0.00913(7) Uani 1 2 d S . . S1 S 0.07464(2) 0.73719(2) 0.70457(4) 0.01911(9) Uani 1 1 d . . . N1 N -0.09743(7) 0.53549(6) 0.38624(12) 0.0112(2) Uani 1 1 d . . . N2 N 0.05543(7) 0.52761(6) 0.32764(12) 0.0110(2) Uani 1 1 d . . . N3 N 0.02142(7) 0.60260(7) 0.57173(12) 0.0130(2) Uani 1 1 d . . . N4 N 0.13372(7) 0.52678(6) 0.27933(12) 0.0121(2) Uani 1 1 d . . . N5 N 0.18592(7) 0.59970(7) -0.05912(13) 0.0149(2) Uani 1 1 d . . . N6 N 0.05095(7) 0.57692(6) 0.12056(12) 0.0108(2) Uani 1 1 d . . . N7 N 0.01884(8) 0.61441(7) 0.00153(13) 0.0139(2) Uani 1 1 d . . . H1N H 0.0588(12) 0.6114(11) -0.056(2) 0.026(5) Uiso 1 1 d . . . H2N H 0.0197(12) 0.6642(13) 0.028(2) 0.032(5) Uiso 1 1 d . . . C1 C -0.17649(8) 0.53207(8) 0.42173(15) 0.0130(3) Uani 1 1 d . . . H1A H -0.1892 0.5142 0.5092 0.016 Uiso 1 1 calc R . . C2 C -0.24018(8) 0.55423(8) 0.33284(15) 0.0151(3) Uani 1 1 d . . . H2A H -0.2942 0.5508 0.3609 0.018 Uiso 1 1 calc R . . C3 C -0.22262(8) 0.58133(8) 0.20277(15) 0.0157(3) Uani 1 1 d . . . H3A H -0.2644 0.5969 0.1425 0.019 Uiso 1 1 calc R . . C4 C -0.14120(8) 0.58486(8) 0.16359(15) 0.0141(3) Uani 1 1 d . . . H4A H -0.1274 0.6027 0.0766 0.017 Uiso 1 1 calc R . . C5 C -0.08100(8) 0.56125(7) 0.25731(14) 0.0114(3) Uani 1 1 d . . . C6 C 0.00632(8) 0.55707(7) 0.23140(14) 0.0111(3) Uani 1 1 d . . . C7 C 0.12998(8) 0.55731(7) 0.15414(14) 0.0116(3) Uani 1 1 d . . . C8 C 0.20093(8) 0.56740(7) 0.06477(14) 0.0121(3) Uani 1 1 d . . . C9 C 0.27830(8) 0.54424(8) 0.11024(15) 0.0147(3) Uani 1 1 d . . . H9A H 0.2857 0.5203 0.1953 0.018 Uiso 1 1 calc R . . C10 C 0.34404(9) 0.55786(8) 0.02526(16) 0.0167(3) Uani 1 1 d . . . H10A H 0.3968 0.5437 0.0528 0.020 Uiso 1 1 calc R . . C11 C 0.32993(9) 0.59286(8) -0.10138(16) 0.0190(3) Uani 1 1 d . . . H11A H 0.3731 0.6035 -0.1596 0.023 Uiso 1 1 calc R . . C12 C 0.25023(9) 0.61178(8) -0.13963(16) 0.0182(3) Uani 1 1 d . . . H12A H 0.2410 0.6340 -0.2258 0.022 Uiso 1 1 calc R . . C13 C 0.04409(8) 0.65860(8) 0.62481(15) 0.0133(3) Uani 1 1 d . . . Fe2 Fe 0.5000 0.5000 0.5000 0.01081(7) Uani 1 2 d S . . S2 S 0.44093(2) 0.38686(2) 0.95131(4) 0.01633(8) Uani 1 1 d . . . N9 N 0.57041(7) 0.58970(7) 0.59696(12) 0.0129(2) Uani 1 1 d . . . N11 N 0.64711(7) 0.59445(6) 0.65623(12) 0.0132(2) Uani 1 1 d . . . N13 N 0.57237(7) 0.69106(6) 0.72841(12) 0.0125(2) Uani 1 1 d . . . N8 N 0.41228(7) 0.59660(7) 0.52188(12) 0.0133(2) Uani 1 1 d . . . N10 N 0.46873(7) 0.46199(7) 0.70045(13) 0.0156(2) Uani 1 1 d . . . N12 N 0.71003(7) 0.74372(7) 0.89691(13) 0.0152(2) Uani 1 1 d . . . N14 N 0.54422(8) 0.75605(7) 0.80116(14) 0.0177(3) Uani 1 1 d . . . H4N H 0.5498(12) 0.7953(12) 0.742(2) 0.030(5) Uiso 1 1 d . . . H3N H 0.5813(13) 0.7630(11) 0.870(2) 0.030(5) Uiso 1 1 d . . . C19 C 0.52589(8) 0.64789(8) 0.64094(14) 0.0126(3) Uani 1 1 d . . . C20 C 0.64757(8) 0.65633(8) 0.73463(14) 0.0125(3) Uani 1 1 d . . . C21 C 0.72059(8) 0.68525(8) 0.80891(14) 0.0131(3) Uani 1 1 d . . . C18 C 0.44042(8) 0.65823(8) 0.59313(15) 0.0133(3) Uani 1 1 d . . . C26 C 0.45681(8) 0.43215(8) 0.80610(15) 0.0132(3) Uani 1 1 d . . . C22 C 0.79716(9) 0.65442(8) 0.77908(15) 0.0153(3) Uani 1 1 d . . . H22A H 0.8016 0.6119 0.7219 0.018 Uiso 1 1 calc R . . C14 C 0.33581(9) 0.59888(8) 0.47011(15) 0.0158(3) Uani 1 1 d . . . H14A H 0.3163 0.5568 0.4206 0.019 Uiso 1 1 calc R . . C17 C 0.39282(9) 0.72303(8) 0.61410(16) 0.0173(3) Uani 1 1 d . . . H17A H 0.4137 0.7647 0.6629 0.021 Uiso 1 1 calc R . . C25 C 0.77790(9) 0.77424(8) 0.95432(15) 0.0179(3) Uani 1 1 d . . . H25A H 0.7718 0.8140 1.0172 0.021 Uiso 1 1 calc R . . C16 C 0.31314(9) 0.72385(8) 0.56017(17) 0.0190(3) Uani 1 1 d . . . H16A H 0.2797 0.7662 0.5733 0.023 Uiso 1 1 calc R . . C15 C 0.28398(9) 0.66129(9) 0.48690(16) 0.0185(3) Uani 1 1 d . . . H15A H 0.2310 0.6609 0.4497 0.022 Uiso 1 1 calc R . . C24 C 0.85656(9) 0.75020(8) 0.92569(16) 0.0187(3) Uani 1 1 d . . . H24A H 0.9019 0.7747 0.9651 0.022 Uiso 1 1 calc R . . C23 C 0.86624(9) 0.68858(8) 0.83665(15) 0.0179(3) Uani 1 1 d . . . H23A H 0.9182 0.6706 0.8161 0.021 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01062(12) 0.00822(12) 0.00858(14) 0.00134(10) 0.00039(10) 0.00046(9) S1 0.02512(18) 0.01165(16) 0.0203(2) -0.00128(14) -0.00546(14) -0.00226(13) N1 0.0125(5) 0.0090(5) 0.0120(6) -0.0007(4) -0.0003(4) -0.0002(4) N2 0.0115(5) 0.0100(5) 0.0116(6) 0.0006(4) 0.0012(4) 0.0003(4) N3 0.0139(5) 0.0133(6) 0.0117(6) 0.0016(4) 0.0002(4) 0.0014(4) N4 0.0125(5) 0.0119(5) 0.0118(6) 0.0012(4) 0.0023(4) 0.0009(4) N5 0.0188(6) 0.0147(6) 0.0115(6) 0.0014(5) 0.0031(5) 0.0024(4) N6 0.0128(5) 0.0101(5) 0.0095(6) 0.0021(4) -0.0007(4) 0.0004(4) N7 0.0168(6) 0.0155(6) 0.0094(6) 0.0045(5) -0.0009(5) 0.0013(5) C1 0.0139(6) 0.0120(6) 0.0131(7) 0.0004(5) 0.0011(5) -0.0010(5) C2 0.0112(6) 0.0157(6) 0.0184(8) -0.0010(5) -0.0008(5) -0.0016(5) C3 0.0143(6) 0.0161(6) 0.0165(8) 0.0010(5) -0.0039(5) -0.0007(5) C4 0.0159(6) 0.0143(6) 0.0120(7) 0.0015(5) -0.0016(5) -0.0012(5) C5 0.0143(6) 0.0089(6) 0.0109(7) -0.0002(5) 0.0007(5) -0.0012(5) C6 0.0140(6) 0.0086(6) 0.0105(7) -0.0006(5) -0.0006(5) -0.0006(5) C7 0.0135(6) 0.0096(6) 0.0118(7) 0.0000(5) -0.0010(5) 0.0008(5) C8 0.0152(6) 0.0100(6) 0.0112(7) -0.0012(5) 0.0020(5) 0.0003(5) C9 0.0171(6) 0.0143(6) 0.0128(7) -0.0009(5) 0.0004(5) 0.0007(5) C10 0.0152(6) 0.0163(7) 0.0186(8) -0.0026(6) 0.0027(5) 0.0010(5) C11 0.0203(7) 0.0185(7) 0.0185(8) -0.0008(6) 0.0095(6) -0.0004(6) C12 0.0244(7) 0.0178(7) 0.0127(7) 0.0026(6) 0.0053(6) 0.0024(6) C13 0.0134(6) 0.0139(6) 0.0125(7) 0.0043(5) 0.0000(5) 0.0022(5) Fe2 0.01283(13) 0.00988(13) 0.00976(15) 0.00045(10) 0.00164(10) -0.00056(10) S2 0.01878(17) 0.01717(17) 0.01317(19) 0.00423(13) 0.00351(13) -0.00023(13) N9 0.0130(5) 0.0120(5) 0.0138(6) 0.0000(4) 0.0007(4) -0.0006(4) N11 0.0141(5) 0.0123(5) 0.0132(6) -0.0004(5) 0.0001(4) -0.0008(4) N13 0.0157(5) 0.0099(5) 0.0119(6) 0.0000(4) 0.0023(4) 0.0003(4) N8 0.0151(5) 0.0140(5) 0.0108(6) 0.0027(4) 0.0025(4) -0.0007(4) N10 0.0176(6) 0.0144(6) 0.0148(7) 0.0007(5) 0.0013(5) -0.0002(5) N12 0.0212(6) 0.0132(5) 0.0113(6) -0.0002(5) 0.0016(5) -0.0023(5) N14 0.0247(7) 0.0112(6) 0.0171(7) -0.0038(5) 0.0012(5) 0.0048(5) C19 0.0164(6) 0.0097(6) 0.0120(7) 0.0019(5) 0.0028(5) -0.0004(5) C20 0.0159(6) 0.0106(6) 0.0110(7) 0.0015(5) 0.0028(5) -0.0002(5) C21 0.0189(7) 0.0105(6) 0.0098(7) 0.0028(5) -0.0008(5) -0.0015(5) C18 0.0148(6) 0.0134(6) 0.0118(7) 0.0041(5) 0.0037(5) -0.0009(5) C26 0.0123(6) 0.0119(6) 0.0155(7) -0.0020(5) 0.0007(5) 0.0006(5) C22 0.0211(7) 0.0144(6) 0.0104(7) 0.0007(5) -0.0023(5) 0.0027(5) C14 0.0160(6) 0.0191(7) 0.0123(7) 0.0027(5) 0.0020(5) -0.0020(5) C17 0.0188(7) 0.0120(6) 0.0211(8) 0.0019(6) 0.0029(6) 0.0006(5) C25 0.0282(8) 0.0140(6) 0.0114(7) -0.0009(5) -0.0012(6) -0.0033(6) C16 0.0166(7) 0.0156(7) 0.0249(8) 0.0062(6) 0.0057(6) 0.0042(5) C15 0.0148(6) 0.0231(7) 0.0175(8) 0.0071(6) 0.0014(5) 0.0017(6) C24 0.0225(7) 0.0184(7) 0.0148(8) 0.0034(6) -0.0066(6) -0.0039(6) C23 0.0188(7) 0.0199(7) 0.0147(8) 0.0038(6) -0.0045(6) 0.0025(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N3 1.9524(12) 3_566 ? Fe1 N3 1.9524(12) . ? Fe1 N2 1.9738(12) 3_566 ? Fe1 N2 1.9738(12) . ? Fe1 N1 2.0151(11) . ? Fe1 N1 2.0151(11) 3_566 ? S1 C13 1.6484(14) . ? N1 C1 1.3435(17) . ? N1 C5 1.3588(18) . ? N2 C6 1.3219(17) . ? N2 N4 1.3698(15) . ? N3 C13 1.1627(18) . ? N4 C7 1.3248(18) . ? N5 C12 1.3366(19) . ? N5 C8 1.3441(18) . ? N6 C6 1.3541(18) . ? N6 C7 1.3682(17) . ? N6 N7 1.4176(16) . ? N7 H1N 0.87(2) . ? N7 H2N 0.91(2) . ? C1 C2 1.3919(19) . ? C1 H1A 0.9300 . ? C2 C3 1.381(2) . ? C2 H2A 0.9300 . ? C3 C4 1.391(2) . ? C3 H3A 0.9300 . ? C4 C5 1.3876(19) . ? C4 H4A 0.9300 . ? C5 C6 1.4543(18) . ? C7 C8 1.4700(19) . ? C8 C9 1.3900(19) . ? C9 C10 1.386(2) . ? C9 H9A 0.9300 . ? C10 C11 1.386(2) . ? C10 H10A 0.9300 . ? C11 C12 1.386(2) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? Fe2 N10 2.1232(12) . ? Fe2 N10 2.1232(12) 3_666 ? Fe2 N9 2.1494(12) 3_666 ? Fe2 N9 2.1494(12) . ? Fe2 N8 2.2270(12) 3_666 ? Fe2 N8 2.2270(12) . ? S2 C26 1.6386(15) . ? N9 C19 1.3253(18) . ? N9 N11 1.3699(16) . ? N11 C20 1.3214(18) . ? N13 C19 1.3557(18) . ? N13 C20 1.3699(17) . ? N13 N14 1.4179(16) . ? N8 C14 1.3369(18) . ? N8 C18 1.3547(18) . ? N10 C26 1.1679(19) . ? N12 C25 1.3407(19) . ? N12 C21 1.3440(18) . ? N14 H4N 0.90(2) . ? N14 H3N 0.90(2) . ? C19 C18 1.4728(19) . ? C20 C21 1.4699(19) . ? C21 C22 1.397(2) . ? C18 C17 1.3907(19) . ? C22 C23 1.384(2) . ? C22 H22A 0.9300 . ? C14 C15 1.392(2) . ? C14 H14A 0.9300 . ? C17 C16 1.393(2) . ? C17 H17A 0.9300 . ? C25 C24 1.384(2) . ? C25 H25A 0.9300 . ? C16 C15 1.383(2) . ? C16 H16A 0.9300 . ? C15 H15A 0.9300 . ? C24 C23 1.391(2) . ? C24 H24A 0.9300 . ? C23 H23A 0.9300 . ? 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 N3 Fe1 N3 180.00(3) 3_566 . ? N3 Fe1 N2 89.67(5) 3_566 3_566 ? N3 Fe1 N2 90.33(5) . 3_566 ? N3 Fe1 N2 90.33(5) 3_566 . ? N3 Fe1 N2 89.67(5) . . ? N2 Fe1 N2 180.000(1) 3_566 . ? N3 Fe1 N1 87.38(5) 3_566 . ? N3 Fe1 N1 92.62(5) . . ? N2 Fe1 N1 99.64(5) 3_566 . ? N2 Fe1 N1 80.36(5) . . ? N3 Fe1 N1 92.62(5) 3_566 3_566 ? N3 Fe1 N1 87.38(5) . 3_566 ? N2 Fe1 N1 80.36(5) 3_566 3_566 ? N2 Fe1 N1 99.64(5) . 3_566 ? N1 Fe1 N1 180.0 . 3_566 ? C1 N1 C5 117.22(12) . . ? C1 N1 Fe1 126.78(10) . . ? C5 N1 Fe1 115.88(9) . . ? C6 N2 N4 108.70(11) . . ? C6 N2 Fe1 114.18(9) . . ? N4 N2 Fe1 137.09(9) . . ? C13 N3 Fe1 169.70(11) . . ? C7 N4 N2 106.34(11) . . ? C12 N5 C8 117.08(12) . . ? C6 N6 C7 105.48(11) . . ? C6 N6 N7 124.52(11) . . ? C7 N6 N7 129.89(11) . . ? N6 N7 H1N 102.9(13) . . ? N6 N7 H2N 102.2(13) . . ? H1N N7 H2N 103.3(18) . . ? N1 C1 C2 122.65(13) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C3 C2 C1 119.58(13) . . ? C3 C2 H2A 120.2 . . ? C1 C2 H2A 120.2 . . ? C2 C3 C4 118.72(13) . . ? C2 C3 H3A 120.6 . . ? C4 C3 H3A 120.6 . . ? C5 C4 C3 118.49(13) . . ? C5 C4 H4A 120.8 . . ? C3 C4 H4A 120.8 . . ? N1 C5 C4 123.34(12) . . ? N1 C5 C6 110.70(12) . . ? C4 C5 C6 125.91(13) . . ? N2 C6 N6 109.28(12) . . ? N2 C6 C5 118.76(12) . . ? N6 C6 C5 131.94(12) . . ? N4 C7 N6 110.18(12) . . ? N4 C7 C8 124.34(12) . . ? N6 C7 C8 125.47(12) . . ? N5 C8 C9 123.63(13) . . ? N5 C8 C7 116.35(12) . . ? C9 C8 C7 120.02(13) . . ? C10 C9 C8 118.13(13) . . ? C10 C9 H9A 120.9 . . ? C8 C9 H9A 120.9 . . ? C11 C10 C9 118.95(13) . . ? C11 C10 H10A 120.5 . . ? C9 C10 H10A 120.5 . . ? C10 C11 C12 118.75(13) . . ? C10 C11 H11A 120.6 . . ? C12 C11 H11A 120.6 . . ? N5 C12 C11 123.40(14) . . ? N5 C12 H12A 118.3 . . ? C11 C12 H12A 118.3 . . ? N3 C13 S1 178.15(14) . . ? N10 Fe2 N10 180.0 . 3_666 ? N10 Fe2 N9 92.00(5) . 3_666 ? N10 Fe2 N9 88.00(5) 3_666 3_666 ? N10 Fe2 N9 88.00(5) . . ? N10 Fe2 N9 92.00(5) 3_666 . ? N9 Fe2 N9 180.00(4) 3_666 . ? N10 Fe2 N8 90.93(4) . 3_666 ? N10 Fe2 N8 89.07(4) 3_666 3_666 ? N9 Fe2 N8 75.22(4) 3_666 3_666 ? N9 Fe2 N8 104.78(4) . 3_666 ? N10 Fe2 N8 89.07(4) . . ? N10 Fe2 N8 90.93(4) 3_666 . ? N9 Fe2 N8 104.78(4) 3_666 . ? N9 Fe2 N8 75.22(4) . . ? N8 Fe2 N8 180.0 3_666 . ? C19 N9 N11 108.76(11) . . ? C19 N9 Fe2 114.09(9) . . ? N11 N9 Fe2 134.75(9) . . ? C20 N11 N9 106.57(11) . . ? C19 N13 C20 105.74(11) . . ? C19 N13 N14 124.99(12) . . ? C20 N13 N14 129.20(12) . . ? C14 N8 C18 118.19(12) . . ? C14 N8 Fe2 125.77(10) . . ? C18 N8 Fe2 116.04(9) . . ? C26 N10 Fe2 170.95(11) . . ? C25 N12 C21 116.76(13) . . ? N13 N14 H4N 104.7(13) . . ? N13 N14 H3N 105.0(13) . . ? H4N N14 H3N 107.4(18) . . ? N9 C19 N13 108.91(12) . . ? N9 C19 C18 121.02(12) . . ? N13 C19 C18 130.07(12) . . ? N11 C20 N13 110.02(12) . . ? N11 C20 C21 123.92(12) . . ? N13 C20 C21 125.93(12) . . ? N12 C21 C22 123.43(13) . . ? N12 C21 C20 117.31(12) . . ? C22 C21 C20 119.14(13) . . ? N8 C18 C17 122.48(13) . . ? N8 C18 C19 111.87(12) . . ? C17 C18 C19 125.64(13) . . ? N10 C26 S2 177.61(13) . . ? C23 C22 C21 118.43(13) . . ? C23 C22 H22A 120.8 . . ? C21 C22 H22A 120.8 . . ? N8 C14 C15 123.01(14) . . ? N8 C14 H14A 118.5 . . ? C15 C14 H14A 118.5 . . ? C18 C17 C16 118.31(14) . . ? C18 C17 H17A 120.8 . . ? C16 C17 H17A 120.8 . . ? N12 C25 C24 123.97(14) . . ? N12 C25 H25A 118.0 . . ? C24 C25 H25A 118.0 . . ? C15 C16 C17 119.60(13) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C16 C15 C14 118.40(13) . . ? C16 C15 H15A 120.8 . . ? C14 C15 H15A 120.8 . . ? C25 C24 C23 118.44(13) . . ? C25 C24 H24A 120.8 . . ? C23 C24 H24A 120.8 . . ? C22 C23 C24 118.84(14) . . ? C22 C23 H23A 120.6 . . ? C24 C23 H23A 120.6 . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.369 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.051 # Attachment 'CCDC 732126_PhaseC_25K_F_v.cif' data_PhaseC-25K _database_code_depnum_ccdc_archive 'CCDC 732126' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H20 Fe N14 S2' _chemical_formula_sum 'C26 H20 Fe N14 S2' _chemical_formula_weight 648.53 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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.2391(4) _cell_length_b 17.3845(4) _cell_length_c 29.6127(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.6600(11) _cell_angle_gamma 90.000 _cell_volume 8359.6(3) _cell_formula_units_Z 12 _cell_measurement_temperature 25(2) _cell_measurement_reflns_used 22142 _cell_measurement_theta_min 1.25 _cell_measurement_theta_max 27.47 _exptl_crystal_description Block _exptl_crystal_colour Red-Brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3984 _exptl_absorpt_coefficient_mu 0.738 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_correction_T_max 0.864 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 25(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 KappaCCD _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49898 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0735 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 27.47 _reflns_number_total 18518 _reflns_number_gt 12242 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD server software (Nonius, 1997)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL/PC & Mercury 1.4.1 (CCDC)' _computing_publication_material 'XIF in SHELXTL/PC' _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^)+(0.0395P)^2^+1.2220P] 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 18518 _refine_ls_number_parameters 1201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0866 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1030 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Fe11 Fe 1.0000 0.5000 0.0000 0.00744(11) Uani 1 2 d S . . S1 S 0.92092(4) 0.25878(4) -0.07284(2) 0.01583(15) Uani 1 1 d . . . N1 N 1.09928(12) 0.46242(12) 0.04567(7) 0.0105(5) Uani 1 1 d . . . N2 N 0.93813(12) 0.47297(11) 0.06109(6) 0.0090(4) Uani 1 1 d . . . N3 N 0.97740(13) 0.38710(12) -0.02404(7) 0.0134(5) Uani 1 1 d . . . N4 N 0.85815(12) 0.47115(12) 0.07572(7) 0.0103(5) Uani 1 1 d . . . N5 N 0.79828(12) 0.39564(12) 0.18465(6) 0.0108(5) Uani 1 1 d . . . N6 N 0.93961(12) 0.42428(11) 0.12907(6) 0.0089(4) Uani 1 1 d . . . N7 N 0.96967(14) 0.38616(13) 0.16845(7) 0.0113(5) Uani 1 1 d . . . H1N H 0.9288(16) 0.3896(15) 0.1881(8) 0.014 Uiso 1 1 d . . . H2N H 0.9687(16) 0.3376(15) 0.1591(8) 0.014 Uiso 1 1 d . . . C1 C 1.17941(15) 0.46385(14) 0.03672(8) 0.0121(6) Uani 1 1 d . . . H1A H 1.1958 0.4791 0.0081 0.015 Uiso 1 1 calc R . . C2 C 1.24000(15) 0.44339(14) 0.06848(8) 0.0139(6) Uani 1 1 d . . . H2A H 1.2955 0.4447 0.0611 0.017 Uiso 1 1 calc R . . C3 C 1.21542(15) 0.42122(15) 0.11092(8) 0.0149(6) Uani 1 1 d . . . H3A H 1.2544 0.4070 0.1326 0.018 Uiso 1 1 calc R . . C4 C 1.13209(15) 0.42030(14) 0.12110(8) 0.0134(6) Uani 1 1 d . . . H4A H 1.1144 0.4061 0.1497 0.016 Uiso 1 1 calc R . . C5 C 1.07611(15) 0.44098(14) 0.08762(8) 0.0096(5) Uani 1 1 d . . . C6 C 0.98635(15) 0.44490(14) 0.09356(8) 0.0087(5) Uani 1 1 d . . . C7 C 0.85995(15) 0.44126(14) 0.11686(8) 0.0093(5) Uani 1 1 d . . . C8 C 0.78690(15) 0.43161(14) 0.14478(8) 0.0093(5) Uani 1 1 d . . . C9 C 0.71130(15) 0.46060(14) 0.13023(8) 0.0117(6) Uani 1 1 d . . . H9A H 0.7063 0.4859 0.1027 0.014 Uiso 1 1 calc R . . C10 C 0.64382(15) 0.45098(14) 0.15757(8) 0.0130(6) Uani 1 1 d . . . H10A H 0.5926 0.4701 0.1489 0.016 Uiso 1 1 calc R . . C11 C 0.65377(16) 0.41232(15) 0.19813(8) 0.0139(6) Uani 1 1 d . . . H11A H 0.6091 0.4038 0.2168 0.017 Uiso 1 1 calc R . . C12 C 0.73191(16) 0.38651(15) 0.21037(8) 0.0142(6) Uani 1 1 d . . . H12A H 0.7383 0.3615 0.2380 0.017 Uiso 1 1 calc R . . C13 C 0.95299(15) 0.33431(15) -0.04408(8) 0.0115(6) Uani 1 1 d . . . Fe12 Fe -0.02106(2) 1.00305(2) 0.165634(10) 0.00761(9) Uani 1 1 d . . . S2 S 0.06661(4) 0.76461(4) 0.23850(2) 0.01509(15) Uani 1 1 d . . . S3 S -0.09591(4) 1.24758(4) 0.09488(2) 0.01606(15) Uani 1 1 d . . . N8 N -0.11876(12) 0.95803(12) 0.12264(7) 0.0118(5) Uani 1 1 d . . . N9 N 0.03932(12) 0.97655(12) 0.10457(7) 0.0107(5) Uani 1 1 d . . . N10 N 0.00499(13) 0.89184(12) 0.19029(6) 0.0121(5) Uani 1 1 d . . . N11 N 0.11870(12) 0.98047(12) 0.08879(7) 0.0102(5) Uani 1 1 d . . . N12 N 0.17575(13) 0.91049(12) -0.02216(6) 0.0117(5) Uani 1 1 d . . . N13 N 0.03910(12) 0.92398(12) 0.03789(6) 0.0091(5) Uani 1 1 d . . . N14 N 0.01017(14) 0.88180(13) -0.00029(7) 0.0121(5) Uani 1 1 d . . . H4N H 0.0140(16) 0.8331(15) 0.0106(8) 0.015 Uiso 1 1 d . . . H3N H 0.0558(16) 0.8860(15) -0.0222(8) 0.015 Uiso 1 1 d . . . N15 N 0.07924(12) 1.04127(12) 0.20953(7) 0.0113(5) Uani 1 1 d . . . N16 N -0.08070(12) 1.03057(12) 0.22705(7) 0.0109(5) Uani 1 1 d . . . N17 N -0.04816(13) 1.11410(13) 0.14166(7) 0.0150(5) Uani 1 1 d . . . N18 N -0.16012(12) 1.03372(12) 0.24246(7) 0.0106(5) Uani 1 1 d . . . N19 N -0.21409(13) 1.10452(12) 0.35346(6) 0.0116(5) Uani 1 1 d . . . N20 N -0.07616(12) 1.07907(11) 0.29506(6) 0.0089(5) Uani 1 1 d . . . N21 N -0.04395(14) 1.11514(13) 0.33455(7) 0.0121(5) Uani 1 1 d . . . H6N H -0.0395(16) 1.1632(15) 0.3250(8) 0.015 Uiso 1 1 d . . . H5N H -0.0852(16) 1.1117(15) 0.3544(8) 0.015 Uiso 1 1 d . . . C14 C -0.19879(15) 0.95475(15) 0.13304(9) 0.0143(6) Uani 1 1 d . . . H14A H -0.2150 0.9721 0.1613 0.017 Uiso 1 1 calc R . . C15 C -0.25861(16) 0.92661(15) 0.10345(9) 0.0175(6) Uani 1 1 d . . . H15A H -0.3137 0.9258 0.1117 0.021 Uiso 1 1 calc R . . C16 C -0.23498(16) 0.89983(15) 0.06161(9) 0.0163(6) Uani 1 1 d . . . H16A H -0.2739 0.8802 0.0414 0.020 Uiso 1 1 calc R . . C17 C -0.15235(15) 0.90261(15) 0.05008(9) 0.0146(6) Uani 1 1 d . . . H17A H -0.1350 0.8850 0.0221 0.018 Uiso 1 1 calc R . . C18 C -0.09613(15) 0.93226(14) 0.08127(8) 0.0104(5) Uani 1 1 d . . . C19 C -0.00787(15) 0.94278(14) 0.07376(8) 0.0099(5) Uani 1 1 d . . . C20 C 0.11723(15) 0.94784(14) 0.04837(8) 0.0095(5) Uani 1 1 d . . . C21 C 0.18903(15) 0.93977(14) 0.01932(8) 0.0100(5) Uani 1 1 d . . . C22 C 0.26648(15) 0.96236(14) 0.03509(8) 0.0115(6) Uani 1 1 d . . . H22A H 0.2730 0.9842 0.0636 0.014 Uiso 1 1 calc R . . C23 C 0.33324(15) 0.95152(14) 0.00741(8) 0.0123(6) Uani 1 1 d . . . H23A H 0.3859 0.9654 0.0171 0.015 Uiso 1 1 calc R . . C24 C 0.32079(16) 0.91977(14) -0.03488(8) 0.0145(6) Uani 1 1 d . . . H24A H 0.3649 0.9115 -0.0540 0.017 Uiso 1 1 calc R . . C25 C 0.24099(16) 0.90041(15) -0.04831(8) 0.0142(6) Uani 1 1 d . . . H25A H 0.2329 0.8794 -0.0769 0.017 Uiso 1 1 calc R . . C26 C 0.03134(15) 0.83895(15) 0.20997(8) 0.0120(6) Uani 1 1 d . . . C27 C 0.15946(15) 1.03824(15) 0.19989(9) 0.0143(6) Uani 1 1 d . . . H27A H 0.1748 1.0241 0.1709 0.017 Uiso 1 1 calc R . . C28 C 0.22110(16) 1.05534(15) 0.23148(9) 0.0169(6) Uani 1 1 d . . . H28A H 0.2763 1.0535 0.2235 0.020 Uiso 1 1 calc R . . C29 C 0.19900(16) 1.07501(15) 0.27456(9) 0.0160(6) Uani 1 1 d . . . H29A H 0.2391 1.0867 0.2962 0.019 Uiso 1 1 calc R . . C30 C 0.11598(15) 1.07725(14) 0.28552(9) 0.0140(6) Uani 1 1 d . . . H30A H 0.0996 1.0899 0.3146 0.017 Uiso 1 1 calc R . . C31 C 0.05847(15) 1.06039(14) 0.25242(8) 0.0104(5) Uani 1 1 d . . . C32 C -0.03096(15) 1.05748(14) 0.25911(8) 0.0098(5) Uani 1 1 d . . . C33 C -0.15641(15) 1.06329(14) 0.28351(8) 0.0102(5) Uani 1 1 d . . . C34 C -0.22870(15) 1.07612(14) 0.31196(8) 0.0107(5) Uani 1 1 d . . . C35 C -0.30700(15) 1.05921(15) 0.29529(8) 0.0136(6) Uani 1 1 d . . . H35A H -0.3144 1.0385 0.2666 0.016 Uiso 1 1 calc R . . C36 C -0.37345(15) 1.07398(14) 0.32251(8) 0.0144(6) Uani 1 1 d . . . H36A H -0.4267 1.0630 0.3125 0.017 Uiso 1 1 calc R . . C37 C -0.35994(16) 1.10529(15) 0.36485(8) 0.0153(6) Uani 1 1 d . . . H37A H -0.4039 1.1173 0.3834 0.018 Uiso 1 1 calc R . . C38 C -0.27945(16) 1.11838(15) 0.37910(8) 0.0145(6) Uani 1 1 d . . . H38A H -0.2706 1.1378 0.4080 0.017 Uiso 1 1 calc R . . C39 C -0.06900(15) 1.16935(15) 0.12266(8) 0.0133(6) Uani 1 1 d . . . Fe21 Fe 0.5000 0.5000 0.0000 0.00767(11) Uani 1 2 d S . . S4 S 0.42884(4) 0.38967(4) 0.14666(2) 0.01280(15) Uani 1 1 d . . . N22 N 0.40966(12) 0.59501(12) 0.00628(6) 0.0094(5) Uani 1 1 d . . . N23 N 0.57106(12) 0.59410(12) 0.02691(6) 0.0095(5) Uani 1 1 d . . . N24 N 0.47655(12) 0.46645(12) 0.06770(7) 0.0113(5) Uani 1 1 d . . . N25 N 0.64713(12) 0.59832(12) 0.04730(6) 0.0107(5) Uani 1 1 d . . . N26 N 0.70328(12) 0.74076(11) 0.13182(6) 0.0098(5) Uani 1 1 d . . . N27 N 0.56867(12) 0.69185(12) 0.07308(6) 0.0092(4) Uani 1 1 d . . . N28 N 0.53656(13) 0.75270(13) 0.09911(7) 0.0123(5) Uani 1 1 d . . . H8N H 0.5442(16) 0.7942(15) 0.0822(8) 0.015 Uiso 1 1 d . . . H7N H 0.5693(16) 0.7574(15) 0.1216(8) 0.015 Uiso 1 1 d . . . C40 C 0.33268(15) 0.59583(15) -0.01075(8) 0.0114(6) Uani 1 1 d . . . H40A H 0.3128 0.5519 -0.0250 0.014 Uiso 1 1 calc R . . C41 C 0.28175(15) 0.65948(15) -0.00790(8) 0.0136(6) Uani 1 1 d . . . H41A H 0.2287 0.6583 -0.0201 0.016 Uiso 1 1 calc R . . C42 C 0.31120(15) 0.72462(15) 0.01341(8) 0.0135(6) Uani 1 1 d . . . H42A H 0.2778 0.7678 0.0160 0.016 Uiso 1 1 calc R . . C43 C 0.39105(15) 0.72548(15) 0.03106(8) 0.0126(6) Uani 1 1 d . . . H43A H 0.4121 0.7691 0.0452 0.015 Uiso 1 1 calc R . . C44 C 0.43821(15) 0.65964(14) 0.02701(8) 0.0092(5) Uani 1 1 d . . . C45 C 0.52413(15) 0.65038(14) 0.04262(8) 0.0081(5) Uani 1 1 d . . . C46 C 0.64511(15) 0.65809(14) 0.07489(8) 0.0079(5) Uani 1 1 d . . . C47 C 0.71635(15) 0.68459(14) 0.10166(8) 0.0086(5) Uani 1 1 d . . . C48 C 0.79401(15) 0.65301(14) 0.09360(8) 0.0104(5) Uani 1 1 d . . . H48A H 0.8002 0.6122 0.0736 0.012 Uiso 1 1 calc R . . C49 C 0.86123(15) 0.68403(14) 0.11609(8) 0.0127(6) Uani 1 1 d . . . H49A H 0.9140 0.6658 0.1105 0.015 Uiso 1 1 calc R . . C50 C 0.84914(15) 0.74280(15) 0.14712(8) 0.0127(6) Uani 1 1 d . . . H50A H 0.8933 0.7647 0.1627 0.015 Uiso 1 1 calc R . . C51 C 0.76947(16) 0.76774(15) 0.15419(8) 0.0125(6) Uani 1 1 d . . . H51A H 0.7613 0.8056 0.1758 0.015 Uiso 1 1 calc R . . C52 C 0.45714(15) 0.43531(14) 0.10106(8) 0.0111(5) Uani 1 1 d . . . Fe22 Fe 0.49007(2) 0.00535(2) 0.161544(11) 0.00810(9) Uani 1 1 d . . . S5 S 0.54605(4) -0.11577(4) 0.01487(2) 0.01174(14) Uani 1 1 d . . . S6 S 0.40985(4) 0.13310(4) 0.30187(2) 0.01267(14) Uani 1 1 d . . . N29 N 0.39699(12) -0.08588(12) 0.17140(6) 0.0097(5) Uani 1 1 d . . . N30 N 0.55767(12) -0.08691(12) 0.19406(6) 0.0095(5) Uani 1 1 d . . . N31 N 0.51957(13) -0.03775(12) 0.09660(7) 0.0122(5) Uani 1 1 d . . . N32 N 0.63404(12) -0.09373(12) 0.21398(6) 0.0103(5) Uani 1 1 d . . . N33 N 0.68911(12) -0.24361(12) 0.29415(6) 0.0101(5) Uani 1 1 d . . . N34 N 0.55084(12) -0.18110(12) 0.24254(6) 0.0089(4) Uani 1 1 d . . . N35 N 0.51352(13) -0.23719(13) 0.27035(7) 0.0118(5) Uani 1 1 d . . . H10N H 0.5488(16) -0.2805(15) 0.2664(8) 0.014 Uiso 1 1 d . . . H9N H 0.5195(16) -0.2200(15) 0.2980(8) 0.014 Uiso 1 1 d . . . N36 N 0.57925(12) 0.10149(12) 0.15174(6) 0.0105(5) Uani 1 1 d . . . N37 N 0.42099(12) 0.09308(12) 0.12788(6) 0.0095(4) Uani 1 1 d . . . N38 N 0.46199(13) 0.04977(12) 0.22605(7) 0.0126(5) Uani 1 1 d . . . N39 N 0.34245(12) 0.09851(12) 0.11053(6) 0.0106(5) Uani 1 1 d . . . N40 N 0.27475(13) 0.24651(12) 0.03231(6) 0.0114(5) Uani 1 1 d . . . N41 N 0.41625(12) 0.19524(12) 0.08520(6) 0.0094(5) Uani 1 1 d . . . N42 N 0.44263(14) 0.26115(13) 0.06133(7) 0.0128(5) Uani 1 1 d . . . H11N H 0.4073(16) 0.2664(15) 0.0393(8) 0.015 Uiso 1 1 d . . . H12N H 0.4370(16) 0.3013(15) 0.0794(8) 0.015 Uiso 1 1 d . . . C53 C 0.32039(15) -0.08702(15) 0.15427(8) 0.0113(6) Uani 1 1 d . . . H53A H 0.3018 -0.0441 0.1384 0.014 Uiso 1 1 calc R . . C54 C 0.26728(15) -0.14875(15) 0.15891(8) 0.0130(6) Uani 1 1 d . . . H54A H 0.2144 -0.1472 0.1466 0.016 Uiso 1 1 calc R . . C55 C 0.29503(15) -0.21297(15) 0.18236(8) 0.0132(6) Uani 1 1 d . . . H55A H 0.2609 -0.2555 0.1858 0.016 Uiso 1 1 calc R . . C56 C 0.37432(15) -0.21318(15) 0.20063(8) 0.0120(6) Uani 1 1 d . . . H56A H 0.3941 -0.2556 0.2165 0.014 Uiso 1 1 calc R . . C57 C 0.42315(15) -0.14867(14) 0.19468(7) 0.0095(5) Uani 1 1 d . . . C58 C 0.50865(15) -0.14018(14) 0.21083(8) 0.0086(5) Uani 1 1 d . . . C59 C 0.62951(15) -0.15102(14) 0.24310(8) 0.0091(5) Uani 1 1 d . . . C60 C 0.70099(15) -0.18165(14) 0.26811(8) 0.0089(5) Uani 1 1 d . . . C61 C 0.77816(15) -0.14823(14) 0.26101(8) 0.0108(5) Uani 1 1 d . . . H61A H 0.7833 -0.1037 0.2439 0.013 Uiso 1 1 calc R . . C62 C 0.84641(15) -0.18334(14) 0.28015(8) 0.0118(6) Uani 1 1 d . . . H62A H 0.8988 -0.1637 0.2753 0.014 Uiso 1 1 calc R . . C63 C 0.83602(15) -0.24791(15) 0.30662(8) 0.0130(6) Uani 1 1 d . . . H63A H 0.8811 -0.2728 0.3196 0.016 Uiso 1 1 calc R . . C64 C 0.75642(15) -0.27485(15) 0.31335(8) 0.0114(6) Uani 1 1 d . . . H64A H 0.7495 -0.3170 0.3323 0.014 Uiso 1 1 calc R . . C65 C 0.53078(15) -0.06897(14) 0.06187(8) 0.0105(5) Uani 1 1 d . . . C66 C 0.65610(15) 0.10559(15) 0.16847(8) 0.0134(6) Uani 1 1 d . . . H66A H 0.6759 0.0644 0.1854 0.016 Uiso 1 1 calc R . . C67 C 0.70757(16) 0.16787(15) 0.16182(8) 0.0145(6) Uani 1 1 d . . . H67A H 0.7604 0.1687 0.1743 0.017 Uiso 1 1 calc R . . C68 C 0.67882(15) 0.22889(15) 0.13621(8) 0.0143(6) Uani 1 1 d . . . H68A H 0.7124 0.2712 0.1308 0.017 Uiso 1 1 calc R . . C69 C 0.59913(15) 0.22624(15) 0.11866(8) 0.0133(6) Uani 1 1 d . . . H69A H 0.5785 0.2670 0.1016 0.016 Uiso 1 1 calc R . . C70 C 0.55098(15) 0.16226(15) 0.12684(8) 0.0100(5) Uani 1 1 d . . . C71 C 0.46467(15) 0.15140(14) 0.11269(8) 0.0086(5) Uani 1 1 d . . . C72 C 0.34066(15) 0.16056(14) 0.08508(8) 0.0099(5) Uani 1 1 d . . . C73 C 0.26533(15) 0.19135(14) 0.06371(8) 0.0097(5) Uani 1 1 d . . . C74 C 0.18897(15) 0.16563(14) 0.07857(8) 0.0110(5) Uani 1 1 d . . . H74A H 0.1852 0.1253 0.0991 0.013 Uiso 1 1 calc R . . C75 C 0.11905(16) 0.20165(14) 0.06201(8) 0.0126(6) Uani 1 1 d . . . H75A H 0.0672 0.1867 0.0717 0.015 Uiso 1 1 calc R . . C76 C 0.12729(16) 0.26037(15) 0.03068(8) 0.0142(6) Uani 1 1 d . . . H76A H 0.0813 0.2865 0.0196 0.017 Uiso 1 1 calc R . . C77 C 0.20540(16) 0.27911(15) 0.01631(8) 0.0138(6) Uani 1 1 d . . . H77A H 0.2102 0.3167 -0.0058 0.017 Uiso 1 1 calc R . . C78 C 0.43998(15) 0.08370(14) 0.25807(8) 0.0104(5) 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 Fe11 0.0082(2) 0.0068(3) 0.0073(3) 0.0010(2) 0.00058(19) 0.0004(2) S1 0.0200(4) 0.0105(4) 0.0170(4) 0.0000(3) -0.0031(3) -0.0018(3) N1 0.0099(11) 0.0071(11) 0.0144(12) -0.0002(9) 0.0017(9) -0.0005(9) N2 0.0092(10) 0.0062(11) 0.0115(11) 0.0004(9) 0.0006(8) 0.0010(9) N3 0.0143(12) 0.0137(12) 0.0122(12) 0.0011(10) 0.0003(9) 0.0022(10) N4 0.0078(10) 0.0105(12) 0.0128(12) -0.0019(9) 0.0016(8) 0.0003(9) N5 0.0134(11) 0.0094(12) 0.0097(11) 0.0001(9) 0.0002(9) -0.0018(9) N6 0.0102(11) 0.0085(11) 0.0081(11) 0.0006(9) -0.0009(8) -0.0008(9) N7 0.0154(12) 0.0113(12) 0.0073(12) 0.0037(10) -0.0006(9) 0.0010(10) C1 0.0132(13) 0.0077(13) 0.0155(14) -0.0009(11) 0.0044(11) -0.0021(11) C2 0.0087(13) 0.0100(14) 0.0232(16) -0.0028(12) 0.0011(11) -0.0017(11) C3 0.0124(13) 0.0126(15) 0.0195(15) 0.0003(12) -0.0063(11) -0.0013(11) C4 0.0148(14) 0.0125(14) 0.0130(14) -0.0001(11) -0.0004(11) 0.0009(11) C5 0.0075(12) 0.0061(13) 0.0151(14) -0.0005(11) -0.0001(10) 0.0005(10) C6 0.0092(12) 0.0055(13) 0.0113(14) 0.0000(10) -0.0006(10) -0.0013(10) C7 0.0113(13) 0.0065(13) 0.0101(13) -0.0009(10) -0.0014(10) 0.0012(10) C8 0.0105(13) 0.0069(13) 0.0104(13) -0.0033(10) 0.0003(10) -0.0020(10) C9 0.0131(13) 0.0106(14) 0.0113(14) 0.0002(11) -0.0006(10) -0.0020(11) C10 0.0104(13) 0.0121(14) 0.0165(14) -0.0034(11) -0.0021(11) 0.0003(11) C11 0.0133(13) 0.0151(15) 0.0134(14) -0.0028(11) 0.0034(11) -0.0035(11) C12 0.0195(14) 0.0133(15) 0.0098(14) 0.0016(11) 0.0024(11) -0.0016(12) C13 0.0099(13) 0.0159(15) 0.0088(13) 0.0064(11) 0.0015(10) 0.0036(11) Fe12 0.00850(17) 0.0070(2) 0.00738(19) -0.00066(15) 0.00062(14) -0.00035(15) S2 0.0193(4) 0.0110(4) 0.0149(4) 0.0004(3) -0.0013(3) 0.0014(3) S3 0.0160(3) 0.0107(4) 0.0215(4) -0.0014(3) 0.0006(3) -0.0005(3) N8 0.0086(11) 0.0089(12) 0.0178(12) 0.0050(9) 0.0028(9) 0.0020(9) N9 0.0088(10) 0.0104(12) 0.0127(11) -0.0017(9) 0.0013(9) -0.0007(9) N10 0.0109(11) 0.0147(12) 0.0105(11) -0.0017(10) 0.0000(9) -0.0015(10) N11 0.0095(10) 0.0087(11) 0.0124(11) 0.0012(9) 0.0000(8) -0.0001(9) N12 0.0151(11) 0.0105(12) 0.0096(11) -0.0009(9) -0.0005(9) -0.0008(9) N13 0.0084(10) 0.0104(12) 0.0083(11) -0.0012(9) -0.0027(8) 0.0000(9) N14 0.0163(12) 0.0107(12) 0.0094(12) -0.0043(10) -0.0026(9) -0.0026(10) N15 0.0110(11) 0.0079(11) 0.0152(12) 0.0046(9) 0.0019(9) 0.0015(9) N16 0.0102(11) 0.0098(12) 0.0128(11) 0.0012(9) -0.0008(9) 0.0001(9) N17 0.0169(12) 0.0163(13) 0.0118(12) -0.0017(10) 0.0027(9) -0.0017(10) N18 0.0088(11) 0.0103(12) 0.0125(12) 0.0010(9) 0.0008(9) 0.0001(9) N19 0.0147(11) 0.0089(12) 0.0114(12) 0.0015(9) 0.0005(9) -0.0008(9) N20 0.0087(10) 0.0081(11) 0.0100(11) -0.0010(9) -0.0022(8) -0.0006(9) N21 0.0151(12) 0.0108(12) 0.0104(12) -0.0022(10) -0.0021(9) -0.0020(10) C14 0.0122(13) 0.0119(14) 0.0190(15) 0.0066(12) 0.0039(11) 0.0036(11) C15 0.0089(13) 0.0147(15) 0.0288(17) 0.0079(12) 0.0011(11) 0.0026(11) C16 0.0124(13) 0.0143(15) 0.0221(16) 0.0039(12) -0.0055(11) -0.0035(11) C17 0.0122(13) 0.0106(14) 0.0210(15) -0.0004(12) -0.0019(11) 0.0021(11) C18 0.0129(13) 0.0050(13) 0.0134(14) 0.0006(11) 0.0018(10) 0.0007(10) C19 0.0128(13) 0.0065(13) 0.0103(13) -0.0011(11) 0.0010(10) 0.0020(11) C20 0.0110(13) 0.0053(13) 0.0123(14) 0.0014(11) -0.0006(10) -0.0007(10) C21 0.0119(13) 0.0072(13) 0.0108(13) 0.0019(11) -0.0004(10) 0.0008(10) C22 0.0152(13) 0.0096(14) 0.0096(13) -0.0004(11) -0.0016(10) -0.0030(11) C23 0.0118(13) 0.0101(14) 0.0151(14) 0.0025(11) -0.0007(11) 0.0001(11) C24 0.0149(14) 0.0098(14) 0.0189(15) 0.0017(11) 0.0053(11) -0.0016(11) C25 0.0195(14) 0.0127(14) 0.0106(14) -0.0015(11) 0.0014(11) -0.0016(12) C26 0.0113(13) 0.0138(15) 0.0110(14) -0.0037(11) 0.0029(10) -0.0034(11) C27 0.0132(14) 0.0106(14) 0.0192(15) 0.0025(11) 0.0030(11) 0.0018(11) C28 0.0083(13) 0.0131(15) 0.0291(17) 0.0041(12) -0.0005(11) 0.0002(11) C29 0.0140(14) 0.0113(14) 0.0224(16) -0.0015(12) -0.0050(12) 0.0023(12) C30 0.0140(14) 0.0113(14) 0.0166(14) -0.0022(11) -0.0011(11) 0.0001(11) C31 0.0115(13) 0.0048(13) 0.0148(14) 0.0000(11) -0.0003(10) -0.0007(10) C32 0.0123(13) 0.0069(13) 0.0102(13) -0.0006(10) -0.0023(10) -0.0001(10) C33 0.0127(13) 0.0066(13) 0.0114(14) 0.0012(11) -0.0007(10) -0.0004(11) C34 0.0131(13) 0.0049(13) 0.0141(14) 0.0028(11) -0.0007(11) -0.0002(11) C35 0.0151(14) 0.0145(15) 0.0111(14) 0.0036(11) -0.0020(11) 0.0007(11) C36 0.0109(13) 0.0127(15) 0.0194(15) 0.0046(12) -0.0018(11) -0.0030(11) C37 0.0171(14) 0.0149(15) 0.0140(14) 0.0044(12) 0.0048(11) 0.0018(12) C38 0.0178(14) 0.0141(15) 0.0116(14) 0.0017(11) 0.0005(11) -0.0008(12) C39 0.0098(13) 0.0172(15) 0.0131(14) -0.0054(12) 0.0026(10) -0.0030(11) Fe21 0.0079(2) 0.0080(3) 0.0072(3) 0.0006(2) 0.00009(19) -0.0008(2) S4 0.0114(3) 0.0153(4) 0.0117(3) 0.0043(3) 0.0016(3) 0.0005(3) N22 0.0090(10) 0.0111(12) 0.0081(11) 0.0023(9) 0.0003(8) -0.0017(9) N23 0.0084(10) 0.0096(11) 0.0106(11) 0.0018(9) -0.0016(8) -0.0013(9) N24 0.0104(11) 0.0109(12) 0.0127(12) -0.0005(9) -0.0003(9) -0.0003(9) N25 0.0101(11) 0.0106(12) 0.0114(11) 0.0010(9) -0.0014(9) -0.0008(9) N26 0.0139(11) 0.0080(11) 0.0075(11) 0.0010(9) 0.0007(9) -0.0018(9) N27 0.0110(11) 0.0071(11) 0.0093(11) -0.0014(9) 0.0001(8) 0.0014(9) N28 0.0152(12) 0.0105(12) 0.0111(12) -0.0026(9) -0.0031(9) 0.0030(10) C40 0.0120(13) 0.0151(14) 0.0071(13) 0.0014(11) 0.0013(10) -0.0043(11) C41 0.0084(13) 0.0208(16) 0.0116(14) 0.0051(12) -0.0013(10) -0.0009(11) C42 0.0126(13) 0.0099(14) 0.0178(14) 0.0046(11) 0.0016(11) 0.0023(11) C43 0.0133(13) 0.0100(14) 0.0146(14) 0.0019(11) 0.0005(11) -0.0014(11) C44 0.0099(12) 0.0112(14) 0.0064(13) 0.0042(10) 0.0019(10) -0.0008(10) C45 0.0120(13) 0.0044(13) 0.0079(13) 0.0022(10) 0.0024(10) -0.0011(10) C46 0.0099(12) 0.0050(13) 0.0088(13) 0.0039(10) 0.0004(10) 0.0007(10) C47 0.0110(12) 0.0094(13) 0.0054(13) 0.0021(10) 0.0002(10) -0.0013(10) C48 0.0134(13) 0.0112(14) 0.0065(13) 0.0007(11) 0.0008(10) 0.0007(11) C49 0.0106(13) 0.0128(14) 0.0147(14) 0.0055(11) -0.0008(10) 0.0002(11) C50 0.0137(13) 0.0144(15) 0.0100(13) 0.0020(11) -0.0037(10) -0.0038(11) C51 0.0205(14) 0.0106(14) 0.0063(13) -0.0005(11) 0.0010(10) -0.0036(12) C52 0.0110(13) 0.0086(14) 0.0136(14) -0.0031(11) -0.0017(11) 0.0005(11) Fe22 0.00855(18) 0.0088(2) 0.00701(19) -0.00060(15) 0.00093(14) 0.00015(16) S5 0.0127(3) 0.0122(3) 0.0104(3) -0.0025(3) 0.0012(3) -0.0001(3) S6 0.0133(3) 0.0134(4) 0.0114(3) -0.0030(3) 0.0028(3) -0.0008(3) N29 0.0095(11) 0.0135(12) 0.0062(11) -0.0007(9) -0.0002(8) 0.0002(9) N30 0.0072(10) 0.0108(12) 0.0105(11) -0.0007(9) 0.0004(8) 0.0001(9) N31 0.0117(11) 0.0106(12) 0.0144(12) 0.0021(10) -0.0017(9) 0.0004(9) N32 0.0093(11) 0.0106(12) 0.0108(11) -0.0003(9) -0.0027(8) 0.0004(9) N33 0.0127(11) 0.0096(12) 0.0081(11) -0.0007(9) 0.0016(8) 0.0004(9) N34 0.0111(11) 0.0090(11) 0.0067(11) -0.0008(9) 0.0010(8) 0.0000(9) N35 0.0160(12) 0.0098(12) 0.0097(12) 0.0029(10) 0.0028(9) -0.0009(10) N36 0.0126(11) 0.0130(12) 0.0060(11) -0.0025(9) 0.0026(8) 0.0010(9) N37 0.0072(10) 0.0120(12) 0.0092(11) 0.0004(9) 0.0013(8) 0.0012(9) N38 0.0125(11) 0.0127(12) 0.0124(12) 0.0005(10) 0.0006(9) -0.0004(9) N39 0.0101(11) 0.0097(12) 0.0120(11) -0.0010(9) -0.0005(9) 0.0011(9) N40 0.0153(11) 0.0097(12) 0.0093(11) -0.0012(9) 0.0007(9) 0.0020(9) N41 0.0108(11) 0.0088(11) 0.0087(11) -0.0005(9) 0.0015(8) -0.0003(9) N42 0.0166(12) 0.0080(12) 0.0137(13) 0.0018(10) -0.0009(9) -0.0026(10) C53 0.0134(13) 0.0149(14) 0.0055(13) 0.0002(11) 0.0010(10) 0.0014(11) C54 0.0108(13) 0.0186(15) 0.0096(13) -0.0027(11) -0.0006(10) 0.0006(11) C55 0.0126(13) 0.0135(15) 0.0137(14) -0.0039(11) 0.0011(11) -0.0020(11) C56 0.0157(14) 0.0108(14) 0.0096(13) -0.0027(11) 0.0024(10) -0.0009(11) C57 0.0118(13) 0.0120(14) 0.0046(12) -0.0023(10) 0.0027(10) 0.0012(11) C58 0.0131(13) 0.0058(13) 0.0068(13) -0.0030(10) 0.0012(10) 0.0014(11) C59 0.0117(13) 0.0088(14) 0.0070(13) -0.0032(10) 0.0017(10) -0.0019(10) C60 0.0120(13) 0.0079(13) 0.0067(13) -0.0022(10) 0.0002(10) 0.0013(10) C61 0.0162(13) 0.0086(13) 0.0076(13) -0.0011(11) 0.0002(10) -0.0016(11) C62 0.0125(13) 0.0128(14) 0.0102(13) -0.0031(11) 0.0008(10) -0.0036(11) C63 0.0133(13) 0.0150(15) 0.0106(13) -0.0004(11) -0.0025(10) 0.0045(11) C64 0.0189(14) 0.0100(14) 0.0052(13) -0.0004(11) -0.0002(10) 0.0023(11) C65 0.0088(12) 0.0101(14) 0.0127(14) 0.0013(11) -0.0032(10) 0.0010(11) C66 0.0125(13) 0.0182(15) 0.0094(13) -0.0029(11) 0.0011(10) 0.0012(11) C67 0.0106(13) 0.0207(16) 0.0121(14) -0.0065(12) 0.0020(10) -0.0006(12) C68 0.0112(13) 0.0122(14) 0.0197(15) -0.0061(12) 0.0042(11) -0.0053(11) C69 0.0148(14) 0.0101(14) 0.0151(14) -0.0031(11) 0.0017(11) 0.0026(11) C70 0.0101(12) 0.0141(14) 0.0060(13) -0.0053(11) 0.0030(10) -0.0001(11) C71 0.0127(13) 0.0064(13) 0.0068(13) -0.0029(10) 0.0005(10) 0.0017(10) C72 0.0098(12) 0.0094(14) 0.0107(13) -0.0022(11) 0.0016(10) -0.0009(10) C73 0.0131(13) 0.0079(13) 0.0080(13) -0.0003(10) -0.0008(10) 0.0001(11) C74 0.0162(13) 0.0074(13) 0.0092(13) -0.0011(10) -0.0015(10) 0.0007(11) C75 0.0131(13) 0.0129(14) 0.0119(14) -0.0036(11) -0.0024(10) -0.0008(11) C76 0.0170(14) 0.0131(14) 0.0124(14) -0.0027(11) -0.0045(11) 0.0028(12) C77 0.0209(14) 0.0108(14) 0.0097(14) 0.0009(11) -0.0027(11) 0.0038(12) C78 0.0079(12) 0.0097(14) 0.0135(14) 0.0028(11) -0.0006(10) -0.0010(10) _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 N3 2.119(2) . ? Fe11 N3 2.119(2) 3_765 ? Fe11 N2 2.1318(19) 3_765 ? Fe11 N2 2.1318(19) . ? Fe11 N1 2.1919(19) 3_765 ? Fe11 N1 2.1919(19) . ? S1 C13 1.646(3) . ? N1 C1 1.331(3) . ? N1 C5 1.355(3) . ? N2 C6 1.326(3) . ? N2 N4 1.374(3) . ? N3 C13 1.160(3) . ? N4 C7 1.324(3) . ? N5 C12 1.336(3) . ? N5 C8 1.347(3) . ? N6 C6 1.352(3) . ? N6 C7 1.371(3) . ? N6 N7 1.423(3) . ? N7 H1N 0.89(3) . ? N7 H2N 0.89(3) . ? C1 C2 1.399(3) . ? C1 H1A 0.9300 . ? C2 C3 1.378(3) . ? C2 H2A 0.9300 . ? C3 C4 1.390(3) . ? C3 H3A 0.9300 . ? C4 C5 1.385(3) . ? C4 H4A 0.9300 . ? C5 C6 1.472(3) . ? C7 C8 1.463(3) . ? C8 C9 1.391(3) . ? C9 C10 1.380(3) . ? C9 H9A 0.9300 . ? C10 C11 1.384(3) . ? C10 H10A 0.9300 . ? C11 C12 1.390(3) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? Fe12 N17 2.102(2) . ? Fe12 N10 2.108(2) . ? Fe12 N9 2.117(2) . ? Fe12 N16 2.125(2) . ? Fe12 N8 2.169(2) . ? Fe12 N15 2.176(2) . ? S2 C26 1.644(3) . ? S3 C39 1.646(3) . ? N8 C14 1.340(3) . ? N8 C18 1.359(3) . ? N9 C19 1.322(3) . ? N9 N11 1.378(3) . ? N10 C26 1.167(3) . ? N11 C20 1.325(3) . ? N12 C25 1.331(3) . ? N12 C21 1.345(3) . ? N13 C19 1.355(3) . ? N13 C20 1.367(3) . ? N13 N14 1.423(3) . ? N14 H4N 0.91(3) . ? N14 H3N 0.99(3) . ? N15 C27 1.338(3) . ? N15 C31 1.359(3) . ? N16 C32 1.325(3) . ? N16 N18 1.374(3) . ? N17 C39 1.162(3) . ? N18 C33 1.320(3) . ? N19 C38 1.334(3) . ? N19 C34 1.343(3) . ? N20 C32 1.353(3) . ? N20 C33 1.371(3) . ? N20 N21 1.421(3) . ? N21 H6N 0.89(3) . ? N21 H5N 0.90(3) . ? C14 C15 1.390(3) . ? C14 H14A 0.9300 . ? C15 C16 1.382(4) . ? C15 H15A 0.9300 . ? C16 C17 1.389(3) . ? C16 H16A 0.9300 . ? C17 C18 1.390(3) . ? C17 H17A 0.9300 . ? C18 C19 1.464(3) . ? C20 C21 1.464(3) . ? C21 C22 1.393(3) . ? C22 C23 1.380(3) . ? C22 H22A 0.9300 . ? C23 C24 1.381(3) . ? C23 H23A 0.9300 . ? C24 C25 1.392(3) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C27 C28 1.394(3) . ? C27 H27A 0.9300 . ? C28 C29 1.372(3) . ? C28 H28A 0.9300 . ? C29 C30 1.391(3) . ? C29 H29A 0.9300 . ? C30 C31 1.378(3) . ? C30 H30A 0.9300 . ? C31 C32 1.469(3) . ? C33 C34 1.470(3) . ? C34 C35 1.390(3) . ? C35 C36 1.378(3) . ? C35 H35A 0.9300 . ? C36 C37 1.382(3) . ? C36 H36A 0.9300 . ? C37 C38 1.388(3) . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? Fe21 N24 2.126(2) 3_665 ? Fe21 N24 2.126(2) . ? Fe21 N23 2.150(2) 3_665 ? Fe21 N23 2.150(2) . ? Fe21 N22 2.218(2) 3_665 ? Fe21 N22 2.218(2) . ? S4 C52 1.637(3) . ? N22 C40 1.343(3) . ? N22 C44 1.360(3) . ? N23 C45 1.328(3) . ? N23 N25 1.371(3) . ? N24 C52 1.173(3) . ? N25 C46 1.322(3) . ? N26 C51 1.341(3) . ? N26 C47 1.342(3) . ? N27 C45 1.357(3) . ? N27 C46 1.374(3) . ? N27 N28 1.412(3) . ? N28 H8N 0.89(3) . ? N28 H7N 0.85(2) . ? C40 C41 1.385(3) . ? C40 H40A 0.9300 . ? C41 C42 1.379(3) . ? C41 H41A 0.9300 . ? C42 C43 1.393(3) . ? C42 H42A 0.9300 . ? C43 C44 1.383(3) . ? C43 H43A 0.9300 . ? C44 C45 1.474(3) . ? C46 C47 1.469(3) . ? C47 C48 1.398(3) . ? C48 C49 1.382(3) . ? C48 H48A 0.9300 . ? C49 C50 1.390(3) . ? C49 H49A 0.9300 . ? C50 C51 1.383(3) . ? C50 H50A 0.9300 . ? C51 H51A 0.9300 . ? Fe22 N38 2.115(2) . ? Fe22 N31 2.124(2) . ? Fe22 N37 2.134(2) . ? Fe22 N30 2.163(2) . ? Fe22 N29 2.213(2) . ? Fe22 N36 2.233(2) . ? S5 C65 1.634(3) . ? S6 C78 1.635(3) . ? N29 C53 1.338(3) . ? N29 C57 1.357(3) . ? N30 C58 1.322(3) . ? N30 N32 1.372(3) . ? N31 C65 1.179(3) . ? N32 C59 1.320(3) . ? N33 C60 1.340(3) . ? N33 C64 1.341(3) . ? N34 C58 1.357(3) . ? N34 C59 1.380(3) . ? N34 N35 1.417(3) . ? N35 H10N 0.95(3) . ? N35 H9N 0.87(2) . ? N36 C66 1.339(3) . ? N36 C70 1.365(3) . ? N37 C71 1.319(3) . ? N37 N39 1.373(3) . ? N38 C78 1.176(3) . ? N39 C72 1.316(3) . ? N40 C77 1.342(3) . ? N40 C73 1.346(3) . ? N41 C71 1.359(3) . ? N41 C72 1.368(3) . ? N41 N42 1.415(3) . ? N42 H11N 0.87(2) . ? N42 H12N 0.88(3) . ? C53 C54 1.385(3) . ? C53 H53A 0.9300 . ? C54 C55 1.387(3) . ? C54 H54A 0.9300 . ? C55 C56 1.391(3) . ? C55 H55A 0.9300 . ? C56 C57 1.386(3) . ? C56 H56A 0.9300 . ? C57 C58 1.471(3) . ? C59 C60 1.469(3) . ? C60 C61 1.399(3) . ? C61 C62 1.381(3) . ? C61 H61A 0.9300 . ? C62 C63 1.381(3) . ? C62 H62A 0.9300 . ? C63 C64 1.391(3) . ? C63 H63A 0.9300 . ? C64 H64A 0.9300 . ? C66 C67 1.383(3) . ? C66 H66A 0.9300 . ? C67 C68 1.382(3) . ? C67 H67A 0.9300 . ? C68 C69 1.390(3) . ? C68 H68A 0.9300 . ? C69 C70 1.383(3) . ? C69 H69A 0.9300 . ? C70 C71 1.470(3) . ? C72 C73 1.472(3) . ? C73 C74 1.394(3) . ? C74 C75 1.382(3) . ? C74 H74A 0.9300 . ? C75 C76 1.387(3) . ? C75 H75A 0.9300 . ? C76 C77 1.382(3) . ? C76 H76A 0.9300 . ? C77 H77A 0.9300 . ? 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 N3 Fe11 N3 180.00(11) . 3_765 ? N3 Fe11 N2 90.04(8) . 3_765 ? N3 Fe11 N2 89.96(8) 3_765 3_765 ? N3 Fe11 N2 89.96(8) . . ? N3 Fe11 N2 90.04(8) 3_765 . ? N2 Fe11 N2 180.00(10) 3_765 . ? N3 Fe11 N1 86.87(8) . 3_765 ? N3 Fe11 N1 93.13(8) 3_765 3_765 ? N2 Fe11 N1 76.18(7) 3_765 3_765 ? N2 Fe11 N1 103.82(7) . 3_765 ? N3 Fe11 N1 93.13(8) . . ? N3 Fe11 N1 86.87(8) 3_765 . ? N2 Fe11 N1 103.82(7) 3_765 . ? N2 Fe11 N1 76.18(7) . . ? N1 Fe11 N1 180.00(8) 3_765 . ? C1 N1 C5 118.0(2) . . ? C1 N1 Fe11 125.83(17) . . ? C5 N1 Fe11 115.96(16) . . ? C6 N2 N4 108.37(19) . . ? C6 N2 Fe11 114.61(16) . . ? N4 N2 Fe11 136.80(15) . . ? C13 N3 Fe11 164.1(2) . . ? C7 N4 N2 106.75(19) . . ? C12 N5 C8 116.8(2) . . ? C6 N6 C7 105.91(19) . . ? C6 N6 N7 124.8(2) . . ? C7 N6 N7 129.1(2) . . ? N6 N7 H1N 104.7(16) . . ? N6 N7 H2N 100.6(16) . . ? H1N N7 H2N 105(2) . . ? N1 C1 C2 122.9(2) . . ? N1 C1 H1A 118.6 . . ? C2 C1 H1A 118.6 . . ? C3 C2 C1 118.4(2) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? C2 C3 C4 119.6(2) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 118.3(2) . . ? C5 C4 H4A 120.8 . . ? C3 C4 H4A 120.8 . . ? N1 C5 C4 122.8(2) . . ? N1 C5 C6 112.5(2) . . ? C4 C5 C6 124.7(2) . . ? N2 C6 N6 109.2(2) . . ? N2 C6 C5 120.5(2) . . ? N6 C6 C5 130.3(2) . . ? N4 C7 N6 109.7(2) . . ? N4 C7 C8 123.7(2) . . ? N6 C7 C8 126.5(2) . . ? N5 C8 C9 123.5(2) . . ? N5 C8 C7 116.4(2) . . ? C9 C8 C7 120.1(2) . . ? C10 C9 C8 118.6(2) . . ? C10 C9 H9A 120.7 . . ? C8 C9 H9A 120.7 . . ? C9 C10 C11 118.8(2) . . ? C9 C10 H10A 120.6 . . ? C11 C10 H10A 120.6 . . ? C10 C11 C12 118.7(2) . . ? C10 C11 H11A 120.7 . . ? C12 C11 H11A 120.7 . . ? N5 C12 C11 123.5(2) . . ? N5 C12 H12A 118.2 . . ? C11 C12 H12A 118.2 . . ? N3 C13 S1 178.5(2) . . ? N17 Fe12 N10 179.29(8) . . ? N17 Fe12 N9 90.50(8) . . ? N10 Fe12 N9 90.18(8) . . ? N17 Fe12 N16 89.24(8) . . ? N10 Fe12 N16 90.09(8) . . ? N9 Fe12 N16 179.40(8) . . ? N17 Fe12 N8 89.10(8) . . ? N10 Fe12 N8 90.85(8) . . ? N9 Fe12 N8 76.29(8) . . ? N16 Fe12 N8 104.25(8) . . ? N17 Fe12 N15 94.23(8) . . ? N10 Fe12 N15 85.83(8) . . ? N9 Fe12 N15 103.05(8) . . ? N16 Fe12 N15 76.43(8) . . ? N8 Fe12 N15 176.62(7) . . ? C14 N8 C18 117.8(2) . . ? C14 N8 Fe12 125.82(18) . . ? C18 N8 Fe12 116.40(16) . . ? C19 N9 N11 108.96(19) . . ? C19 N9 Fe12 114.55(16) . . ? N11 N9 Fe12 136.30(15) . . ? C26 N10 Fe12 165.1(2) . . ? C20 N11 N9 106.14(19) . . ? C25 N12 C21 117.5(2) . . ? C19 N13 C20 106.14(19) . . ? C19 N13 N14 124.3(2) . . ? C20 N13 N14 129.3(2) . . ? N13 N14 H4N 100.3(16) . . ? N13 N14 H3N 103.8(14) . . ? H4N N14 H3N 105(2) . . ? C27 N15 C31 117.5(2) . . ? C27 N15 Fe12 125.77(17) . . ? C31 N15 Fe12 116.15(16) . . ? C32 N16 N18 108.3(2) . . ? C32 N16 Fe12 114.38(17) . . ? N18 N16 Fe12 137.05(15) . . ? C39 N17 Fe12 169.1(2) . . ? C33 N18 N16 106.75(19) . . ? C38 N19 C34 117.0(2) . . ? C32 N20 C33 105.71(19) . . ? C32 N20 N21 124.9(2) . . ? C33 N20 N21 129.3(2) . . ? N20 N21 H6N 100.7(16) . . ? N20 N21 H5N 103.8(16) . . ? H6N N21 H5N 110(2) . . ? N8 C14 C15 122.9(2) . . ? N8 C14 H14A 118.6 . . ? C15 C14 H14A 118.6 . . ? C16 C15 C14 119.0(2) . . ? C16 C15 H15A 120.5 . . ? C14 C15 H15A 120.5 . . ? C15 C16 C17 119.2(2) . . ? C15 C16 H16A 120.4 . . ? C17 C16 H16A 120.4 . . ? C16 C17 C18 118.6(2) . . ? C16 C17 H17A 120.7 . . ? C18 C17 H17A 120.7 . . ? N8 C18 C17 122.6(2) . . ? N8 C18 C19 111.8(2) . . ? C17 C18 C19 125.6(2) . . ? N9 C19 N13 108.7(2) . . ? N9 C19 C18 120.7(2) . . ? N13 C19 C18 130.5(2) . . ? N11 C20 N13 110.0(2) . . ? N11 C20 C21 124.5(2) . . ? N13 C20 C21 125.5(2) . . ? N12 C21 C22 123.2(2) . . ? N12 C21 C20 116.9(2) . . ? C22 C21 C20 119.9(2) . . ? C23 C22 C21 118.4(2) . . ? C23 C22 H22A 120.8 . . ? C21 C22 H22A 120.8 . . ? C22 C23 C24 119.0(2) . . ? C22 C23 H23A 120.5 . . ? C24 C23 H23A 120.5 . . ? C23 C24 C25 118.8(2) . . ? C23 C24 H24A 120.6 . . ? C25 C24 H24A 120.6 . . ? N12 C25 C24 123.1(2) . . ? N12 C25 H25A 118.4 . . ? C24 C25 H25A 118.4 . . ? N10 C26 S2 178.6(2) . . ? N15 C27 C28 122.8(2) . . ? N15 C27 H27A 118.6 . . ? C28 C27 H27A 118.6 . . ? C29 C28 C27 118.9(2) . . ? C29 C28 H28A 120.5 . . ? C27 C28 H28A 120.5 . . ? C28 C29 C30 119.2(2) . . ? C28 C29 H29A 120.4 . . ? C30 C29 H29A 120.4 . . ? C31 C30 C29 118.6(2) . . ? C31 C30 H30A 120.7 . . ? C29 C30 H30A 120.7 . . ? N15 C31 C30 122.9(2) . . ? N15 C31 C32 112.0(2) . . ? C30 C31 C32 125.1(2) . . ? N16 C32 N20 109.3(2) . . ? N16 C32 C31 120.7(2) . . ? N20 C32 C31 130.0(2) . . ? N18 C33 N20 109.9(2) . . ? N18 C33 C34 123.9(2) . . ? N20 C33 C34 126.1(2) . . ? N19 C34 C35 123.6(2) . . ? N19 C34 C33 116.5(2) . . ? C35 C34 C33 119.9(2) . . ? C36 C35 C34 118.2(2) . . ? C36 C35 H35A 120.9 . . ? C34 C35 H35A 120.9 . . ? C35 C36 C37 119.1(2) . . ? C35 C36 H36A 120.4 . . ? C37 C36 H36A 120.4 . . ? C36 C37 C38 118.7(2) . . ? C36 C37 H37A 120.7 . . ? C38 C37 H37A 120.7 . . ? N19 C38 C37 123.4(2) . . ? N19 C38 H38A 118.3 . . ? C37 C38 H38A 118.3 . . ? N17 C39 S3 178.3(3) . . ? N24 Fe21 N24 180.00(11) 3_665 . ? N24 Fe21 N23 87.73(7) 3_665 3_665 ? N24 Fe21 N23 92.27(7) . 3_665 ? N24 Fe21 N23 92.27(7) 3_665 . ? N24 Fe21 N23 87.73(7) . . ? N23 Fe21 N23 180.00(12) 3_665 . ? N24 Fe21 N22 89.97(7) 3_665 3_665 ? N24 Fe21 N22 90.03(7) . 3_665 ? N23 Fe21 N22 75.82(7) 3_665 3_665 ? N23 Fe21 N22 104.18(7) . 3_665 ? N24 Fe21 N22 90.03(7) 3_665 . ? N24 Fe21 N22 89.97(7) . . ? N23 Fe21 N22 104.18(7) 3_665 . ? N23 Fe21 N22 75.82(7) . . ? N22 Fe21 N22 180.00(12) 3_665 . ? C40 N22 C44 118.2(2) . . ? C40 N22 Fe21 126.17(17) . . ? C44 N22 Fe21 115.52(15) . . ? C45 N23 N25 108.92(19) . . ? C45 N23 Fe21 112.51(16) . . ? N25 N23 Fe21 132.93(16) . . ? C52 N24 Fe21 166.8(2) . . ? C46 N25 N23 106.6(2) . . ? C51 N26 C47 116.8(2) . . ? C45 N27 C46 105.9(2) . . ? C45 N27 N28 124.3(2) . . ? C46 N27 N28 129.6(2) . . ? N27 N28 H8N 104.2(17) . . ? N27 N28 H7N 105.5(18) . . ? H8N N28 H7N 106(2) . . ? N22 C40 C41 122.7(2) . . ? N22 C40 H40A 118.7 . . ? C41 C40 H40A 118.7 . . ? C42 C41 C40 118.7(2) . . ? C42 C41 H41A 120.7 . . ? C40 C41 H41A 120.7 . . ? C41 C42 C43 119.8(2) . . ? C41 C42 H42A 120.1 . . ? C43 C42 H42A 120.1 . . ? C44 C43 C42 118.2(2) . . ? C44 C43 H43A 120.9 . . ? C42 C43 H43A 120.9 . . ? N22 C44 C43 122.5(2) . . ? N22 C44 C45 111.6(2) . . ? C43 C44 C45 125.9(2) . . ? N23 C45 N27 108.7(2) . . ? N23 C45 C44 121.1(2) . . ? N27 C45 C44 130.2(2) . . ? N25 C46 N27 109.9(2) . . ? N25 C46 C47 123.7(2) . . ? N27 C46 C47 126.3(2) . . ? N26 C47 C48 123.3(2) . . ? N26 C47 C46 117.2(2) . . ? C48 C47 C46 119.4(2) . . ? C49 C48 C47 118.3(2) . . ? C49 C48 H48A 120.9 . . ? C47 C48 H48A 120.9 . . ? C48 C49 C50 119.3(2) . . ? C48 C49 H49A 120.4 . . ? C50 C49 H49A 120.4 . . ? C51 C50 C49 118.0(2) . . ? C51 C50 H50A 121.0 . . ? C49 C50 H50A 121.0 . . ? N26 C51 C50 124.2(2) . . ? N26 C51 H51A 117.9 . . ? C50 C51 H51A 117.9 . . ? N24 C52 S4 178.2(2) . . ? N38 Fe22 N31 179.08(8) . . ? N38 Fe22 N37 92.49(8) . . ? N31 Fe22 N37 87.25(8) . . ? N38 Fe22 N30 88.99(8) . . ? N31 Fe22 N30 91.31(8) . . ? N37 Fe22 N30 177.76(7) . . ? N38 Fe22 N29 89.31(8) . . ? N31 Fe22 N29 91.61(7) . . ? N37 Fe22 N29 102.58(8) . . ? N30 Fe22 N29 75.74(7) . . ? N38 Fe22 N36 89.49(8) . . ? N31 Fe22 N36 89.60(7) . . ? N37 Fe22 N36 75.07(8) . . ? N30 Fe22 N36 106.64(8) . . ? N29 Fe22 N36 177.31(7) . . ? C53 N29 C57 117.7(2) . . ? C53 N29 Fe22 126.45(17) . . ? C57 N29 Fe22 115.68(16) . . ? C58 N30 N32 108.85(19) . . ? C58 N30 Fe22 112.46(16) . . ? N32 N30 Fe22 134.97(16) . . ? C65 N31 Fe22 172.4(2) . . ? C59 N32 N30 106.8(2) . . ? C60 N33 C64 116.6(2) . . ? C58 N34 C59 105.6(2) . . ? C58 N34 N35 123.2(2) . . ? C59 N34 N35 131.0(2) . . ? N34 N35 H10N 102.1(15) . . ? N34 N35 H9N 105.4(17) . . ? H10N N35 H9N 109(2) . . ? C66 N36 C70 117.7(2) . . ? C66 N36 Fe22 126.50(17) . . ? C70 N36 Fe22 115.79(16) . . ? C71 N37 N39 108.69(19) . . ? C71 N37 Fe22 115.27(16) . . ? N39 N37 Fe22 134.85(16) . . ? C78 N38 Fe22 169.2(2) . . ? C72 N39 N37 106.6(2) . . ? C77 N40 C73 116.3(2) . . ? C71 N41 C72 105.5(2) . . ? C71 N41 N42 125.2(2) . . ? C72 N41 N42 129.2(2) . . ? N41 N42 H11N 105.0(17) . . ? N41 N42 H12N 107.7(17) . . ? H11N N42 H12N 107(2) . . ? N29 C53 C54 123.5(2) . . ? N29 C53 H53A 118.3 . . ? C54 C53 H53A 118.3 . . ? C53 C54 C55 118.3(2) . . ? C53 C54 H54A 120.8 . . ? C55 C54 H54A 120.8 . . ? C54 C55 C56 119.4(2) . . ? C54 C55 H55A 120.3 . . ? C56 C55 H55A 120.3 . . ? C57 C56 C55 118.5(2) . . ? C57 C56 H56A 120.8 . . ? C55 C56 H56A 120.8 . . ? N29 C57 C56 122.6(2) . . ? N29 C57 C58 111.9(2) . . ? C56 C57 C58 125.4(2) . . ? N30 C58 N34 109.0(2) . . ? N30 C58 C57 121.2(2) . . ? N34 C58 C57 129.7(2) . . ? N32 C59 N34 109.7(2) . . ? N32 C59 C60 123.6(2) . . ? N34 C59 C60 126.5(2) . . ? N33 C60 C61 123.7(2) . . ? N33 C60 C59 117.6(2) . . ? C61 C60 C59 118.5(2) . . ? C62 C61 C60 118.1(2) . . ? C62 C61 H61A 121.0 . . ? C60 C61 H61A 121.0 . . ? C63 C62 C61 119.3(2) . . ? C63 C62 H62A 120.3 . . ? C61 C62 H62A 120.3 . . ? C62 C63 C64 118.3(2) . . ? C62 C63 H63A 120.8 . . ? C64 C63 H63A 120.8 . . ? N33 C64 C63 123.9(2) . . ? N33 C64 H64A 118.1 . . ? C63 C64 H64A 118.1 . . ? N31 C65 S5 177.5(2) . . ? N36 C66 C67 123.4(2) . . ? N36 C66 H66A 118.3 . . ? C67 C66 H66A 118.3 . . ? C68 C67 C66 118.5(2) . . ? C68 C67 H67A 120.7 . . ? C66 C67 H67A 120.7 . . ? C67 C68 C69 119.1(2) . . ? C67 C68 H68A 120.4 . . ? C69 C68 H68A 120.4 . . ? C70 C69 C68 119.2(2) . . ? C70 C69 H69A 120.4 . . ? C68 C69 H69A 120.4 . . ? N36 C70 C69 122.0(2) . . ? N36 C70 C71 111.6(2) . . ? C69 C70 C71 126.3(2) . . ? N37 C71 N41 109.0(2) . . ? N37 C71 C70 121.1(2) . . ? N41 C71 C70 129.9(2) . . ? N39 C72 N41 110.2(2) . . ? N39 C72 C73 123.9(2) . . ? N41 C72 C73 125.6(2) . . ? N40 C73 C74 123.7(2) . . ? N40 C73 C72 117.1(2) . . ? C74 C73 C72 119.1(2) . . ? C75 C74 C73 118.2(2) . . ? C75 C74 H74A 120.9 . . ? C73 C74 H74A 120.9 . . ? C74 C75 C76 119.1(2) . . ? C74 C75 H75A 120.5 . . ? C76 C75 H75A 120.5 . . ? C77 C76 C75 118.4(2) . . ? C77 C76 H76A 120.8 . . ? C75 C76 H76A 120.8 . . ? N40 C77 C76 124.1(2) . . ? N40 C77 H77A 117.9 . . ? C76 C77 H77A 117.9 . . ? N38 C78 S6 178.4(2) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.433 _refine_diff_density_min -0.441 _refine_diff_density_rms 0.085