# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 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@gmail.com loop_ _publ_author_name 'Yu Wang' 'Chou-Fu Sheu' 'Che-Hsiu Shih' K.Sugimoto 'Bing-Ming Cheng' M.Takata data_gs _database_code_depnum_ccdc_archive 'CCDC 843267' #TrackingRef '843267.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Fe(abpt)2(NCS)2 _chemical_melting_point 'not measured' _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 0.0007 0.0007 '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 0.0018 0.0015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.0662 0.0602 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.2560 0.4380 '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 1 21/c 1' 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 10.79060(20) _cell_length_b 15.68846(20) _cell_length_c 16.9891(7) _cell_angle_alpha 90.00 _cell_angle_beta 107.5972(7) _cell_angle_gamma 90.00 _cell_volume 2741.47(13) _cell_formula_units_Z 4 _cell_measurement_temperature 20(2) _cell_measurement_reflns_used 17433 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 18.2 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.285 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.760 _exptl_absorpt_correction_T_max 0.825 _exptl_absorpt_process_details 'Multi-scan (2001 Higashi)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 20(2) _diffrn_radiation_wavelength 0.49812 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47941 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 24.53 _reflns_number_total 13154 _reflns_number_gt 12100 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID AUTO' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+1.1129P] 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 13154 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0814 _refine_ls_wR_factor_gt 0.0790 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.003 _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 0.00517(3) Uani 1 2 d S . . S1 S 1.434818(19) 0.049302(14) 0.167871(12) 0.01149(4) Uani 1 1 d . . . N1 N 0.99384(6) -0.10140(4) 0.06964(4) 0.00673(9) Uani 1 1 d . . . N2 N 0.92017(6) 0.05303(4) 0.07892(4) 0.00685(9) Uani 1 1 d . . . N3 N 1.17544(7) 0.02436(4) 0.07066(4) 0.00837(10) Uani 1 1 d . . . N4 N 0.87595(6) 0.13162(4) 0.09272(4) 0.00731(9) Uani 1 1 d . . . N5 N 0.70375(7) 0.17164(4) 0.24293(4) 0.00893(10) Uani 1 1 d . . . N6 N 0.83113(6) 0.03871(4) 0.17769(4) 0.00693(9) Uani 1 1 d . . . N7 N 0.79001(7) -0.00155(4) 0.23980(4) 0.00984(11) Uani 1 1 d . . . H1N H 0.7155(18) 0.0244(12) 0.2400(11) 0.031(4) Uiso 1 1 d . . . H2N H 0.8490(19) 0.0161(11) 0.2876(12) 0.031(4) Uiso 1 1 d . . . C1 C 1.04076(7) -0.17913(4) 0.06269(4) 0.00796(11) Uani 1 1 d . . . H1A H 1.0830 -0.1879 0.0231 0.010 Uiso 1 1 calc R . . C2 C 1.02895(8) -0.24741(4) 0.11229(5) 0.00869(11) Uani 1 1 d . . . H2A H 1.0622 -0.3007 0.1055 0.010 Uiso 1 1 calc R . . C3 C 0.96687(8) -0.23500(5) 0.17207(5) 0.00886(11) Uani 1 1 d . . . H3A H 0.9572 -0.2799 0.2054 0.011 Uiso 1 1 calc R . . C4 C 0.91945(7) -0.15433(5) 0.18122(5) 0.00854(11) Uani 1 1 d . . . H4B H 0.8784 -0.1440 0.2212 0.010 Uiso 1 1 calc R . . C5 C 0.93501(7) -0.08967(4) 0.12926(4) 0.00689(10) Uani 1 1 d . . . C6 C 0.89330(7) -0.00205(4) 0.13024(4) 0.00666(11) Uani 1 1 d . . . C7 C 0.82280(7) 0.12223(4) 0.15306(4) 0.00707(10) Uani 1 1 d . . . C8 C 0.76550(7) 0.19215(5) 0.18769(4) 0.00721(10) Uani 1 1 d . . . C9 C 0.77881(8) 0.27559(5) 0.16308(5) 0.00963(11) Uani 1 1 d . . . H9A H 0.8191 0.2868 0.1229 0.012 Uiso 1 1 calc R . . C10 C 0.73064(8) 0.34148(5) 0.19979(5) 0.01064(12) Uani 1 1 d . . . H10A H 0.7391 0.3979 0.1853 0.013 Uiso 1 1 calc R . . C11 C 0.66940(8) 0.32168(5) 0.25882(5) 0.01059(12) Uani 1 1 d . . . H11A H 0.6383 0.3645 0.2857 0.013 Uiso 1 1 calc R . . C12 C 0.65602(8) 0.23633(5) 0.27655(5) 0.01062(12) Uani 1 1 d . . . H12A H 0.6113 0.2233 0.3140 0.013 Uiso 1 1 calc R . . C13 C 1.28319(7) 0.03326(5) 0.11156(5) 0.00861(11) Uani 1 1 d . . . Fe2 Fe 1.0000 0.0000 0.5000 0.00533(3) Uani 1 2 d S . . S2 S 1.169617(19) 0.067055(12) 0.272469(11) 0.00860(4) Uani 1 1 d . . . N8 N 0.86921(6) -0.09918(4) 0.42718(4) 0.00711(9) Uani 1 1 d . . . N9 N 0.81161(6) 0.05897(4) 0.46085(4) 0.00750(10) Uani 1 1 d . . . N10 N 1.04456(7) 0.03973(4) 0.39286(4) 0.01051(11) Uani 1 1 d . . . N11 N 0.76109(6) 0.13378(4) 0.47896(4) 0.00813(10) Uani 1 1 d . . . N12 N 0.42166(7) 0.16490(5) 0.45626(4) 0.01024(11) Uani 1 1 d . . . N13 N 0.60037(6) 0.04707(4) 0.41640(4) 0.00750(10) Uani 1 1 d . . . N14 N 0.47521(7) 0.01260(5) 0.37927(4) 0.01026(11) Uani 1 1 d . . . H3N H 0.4221(15) 0.0427(10) 0.3993(10) 0.020(4) Uiso 1 1 d . . . H4N H 0.4536(16) 0.0224(10) 0.3246(10) 0.022(4) Uiso 1 1 d . . . C14 C 0.90670(7) -0.17607(5) 0.40901(5) 0.00863(11) Uani 1 1 d . . . H14A H 0.9948 -0.1894 0.4269 0.010 Uiso 1 1 calc R . . C15 C 0.81959(8) -0.23716(5) 0.36452(5) 0.01028(12) Uani 1 1 d . . . H15A H 0.8487 -0.2902 0.3531 0.012 Uiso 1 1 calc R . . C16 C 0.68843(8) -0.21682(5) 0.33771(5) 0.01130(12) Uani 1 1 d . . . H16A H 0.6280 -0.2564 0.3081 0.014 Uiso 1 1 calc R . . C17 C 0.64770(8) -0.13668(5) 0.35542(5) 0.01004(12) Uani 1 1 d . . . H17A H 0.5602 -0.1217 0.3375 0.012 Uiso 1 1 calc R . . C18 C 0.74089(7) -0.07980(4) 0.40048(4) 0.00715(10) Uani 1 1 d . . . C19 C 0.71481(7) 0.00673(4) 0.42432(4) 0.00700(11) Uani 1 1 d . . . C20 C 0.63329(7) 0.12592(5) 0.45170(4) 0.00757(11) Uani 1 1 d . . . C21 C 0.54161(7) 0.19171(5) 0.45994(4) 0.00851(11) Uani 1 1 d . . . C22 C 0.58176(8) 0.27644(5) 0.47231(5) 0.01157(12) Uani 1 1 d . . . H22A H 0.6652 0.2924 0.4732 0.014 Uiso 1 1 calc R . . C23 C 0.49349(9) 0.33634(6) 0.48318(6) 0.01458(14) Uani 1 1 d . . . H23A H 0.5171 0.3933 0.4924 0.017 Uiso 1 1 calc R . . C24 C 0.36932(8) 0.30964(6) 0.48007(5) 0.01411(14) Uani 1 1 d . . . H24A H 0.3086 0.3483 0.4876 0.017 Uiso 1 1 calc R . . C25 C 0.33767(8) 0.22391(6) 0.46544(5) 0.01252(13) Uani 1 1 d . . . H25A H 0.2536 0.2067 0.4618 0.015 Uiso 1 1 calc R . . C26 C 1.09877(7) 0.05118(5) 0.34317(5) 0.00845(11) 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 0.00606(6) 0.00435(6) 0.00501(6) 0.00003(4) 0.00152(5) -0.00021(4) S1 0.00710(7) 0.01527(8) 0.01099(8) 0.00226(6) 0.00106(6) -0.00093(6) N1 0.0076(2) 0.0058(2) 0.0065(2) -0.00024(17) 0.00181(18) -0.00003(18) N2 0.0081(2) 0.0052(2) 0.0072(2) 0.00031(17) 0.00216(19) 0.00034(18) N3 0.0097(2) 0.0073(2) 0.0081(2) -0.00006(18) 0.0027(2) -0.00052(19) N4 0.0088(2) 0.0057(2) 0.0079(2) -0.00028(17) 0.00314(19) 0.00071(18) N5 0.0098(2) 0.0090(2) 0.0089(2) 0.00001(19) 0.0041(2) 0.00116(19) N6 0.0084(2) 0.0062(2) 0.0070(2) 0.00079(17) 0.00344(19) 0.00025(18) N7 0.0118(3) 0.0105(3) 0.0091(2) 0.00327(19) 0.0060(2) 0.0012(2) C1 0.0096(3) 0.0055(2) 0.0087(3) 0.0001(2) 0.0027(2) 0.0004(2) C2 0.0102(3) 0.0061(3) 0.0094(3) 0.0007(2) 0.0024(2) -0.0001(2) C3 0.0106(3) 0.0063(2) 0.0094(3) 0.0013(2) 0.0027(2) -0.0006(2) C4 0.0102(3) 0.0070(3) 0.0088(3) 0.0014(2) 0.0035(2) -0.0002(2) C5 0.0073(3) 0.0060(2) 0.0070(2) 0.00038(19) 0.0017(2) -0.0002(2) C6 0.0076(3) 0.0059(2) 0.0066(2) 0.00036(18) 0.0023(2) 0.00047(19) C7 0.0076(3) 0.0062(2) 0.0073(2) 0.00046(19) 0.0022(2) 0.0004(2) C8 0.0075(3) 0.0067(2) 0.0072(2) -0.00043(19) 0.0018(2) 0.0007(2) C9 0.0107(3) 0.0073(3) 0.0114(3) 0.0013(2) 0.0041(2) 0.0009(2) C10 0.0108(3) 0.0075(3) 0.0132(3) -0.0002(2) 0.0030(2) 0.0012(2) C11 0.0109(3) 0.0094(3) 0.0109(3) -0.0011(2) 0.0025(2) 0.0029(2) C12 0.0122(3) 0.0106(3) 0.0098(3) 0.0001(2) 0.0045(2) 0.0027(2) C13 0.0097(3) 0.0077(3) 0.0086(3) 0.0006(2) 0.0029(2) -0.0001(2) Fe2 0.00541(6) 0.00513(6) 0.00557(6) -0.00004(4) 0.00183(5) 0.00000(4) S2 0.00944(7) 0.00912(7) 0.00812(7) 0.00111(5) 0.00399(6) 0.00083(5) N8 0.0074(2) 0.0065(2) 0.0076(2) -0.00018(17) 0.00247(19) 0.00045(18) N9 0.0073(2) 0.0058(2) 0.0092(2) -0.00144(18) 0.00218(19) 0.00030(18) N10 0.0126(3) 0.0101(3) 0.0097(2) 0.0004(2) 0.0046(2) -0.0002(2) N11 0.0076(2) 0.0065(2) 0.0100(2) -0.00117(18) 0.00219(19) 0.00146(18) N12 0.0085(2) 0.0127(3) 0.0095(2) 0.0006(2) 0.0026(2) 0.0029(2) N13 0.0058(2) 0.0070(2) 0.0090(2) -0.00088(18) 0.00127(19) 0.00022(18) N14 0.0059(2) 0.0111(3) 0.0124(3) -0.0012(2) 0.0006(2) -0.0008(2) C14 0.0093(3) 0.0072(3) 0.0097(3) -0.0004(2) 0.0034(2) 0.0010(2) C15 0.0117(3) 0.0071(3) 0.0119(3) -0.0018(2) 0.0035(2) 0.0000(2) C16 0.0112(3) 0.0085(3) 0.0132(3) -0.0030(2) 0.0022(2) -0.0013(2) C17 0.0087(3) 0.0084(3) 0.0121(3) -0.0021(2) 0.0016(2) -0.0011(2) C18 0.0073(3) 0.0063(2) 0.0077(2) -0.0003(2) 0.0021(2) 0.0002(2) C19 0.0065(3) 0.0063(2) 0.0077(2) -0.00016(19) 0.0014(2) 0.00048(19) C20 0.0077(3) 0.0066(2) 0.0080(2) -0.0004(2) 0.0019(2) 0.0012(2) C21 0.0086(3) 0.0088(3) 0.0077(2) -0.0005(2) 0.0018(2) 0.0023(2) C22 0.0109(3) 0.0095(3) 0.0134(3) -0.0025(2) 0.0024(2) 0.0021(2) C23 0.0145(3) 0.0118(3) 0.0153(3) -0.0040(3) 0.0012(3) 0.0046(3) C24 0.0128(3) 0.0156(3) 0.0125(3) -0.0028(3) 0.0017(3) 0.0070(3) C25 0.0100(3) 0.0166(3) 0.0107(3) -0.0002(2) 0.0027(2) 0.0049(3) C26 0.0095(3) 0.0070(3) 0.0085(3) -0.0002(2) 0.0021(2) 0.0003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N3 1.9485(7) 3_755 ? Fe1 N3 1.9485(7) . ? Fe1 N2 1.9825(6) . ? Fe1 N2 1.9825(6) 3_755 ? Fe1 N1 1.9956(6) 3_755 ? Fe1 N1 1.9956(6) . ? S1 C13 1.6459(8) . ? N1 C1 1.3392(9) . ? N1 C5 1.3609(9) . ? N2 C6 1.3204(9) . ? N2 N4 1.3677(9) . ? N3 C13 1.1687(10) . ? N4 C7 1.3255(9) . ? N5 C12 1.3414(10) . ? N5 C8 1.3440(9) . ? N6 C6 1.3549(9) . ? N6 C7 1.3702(9) . ? N6 N7 1.4114(9) . ? N7 H1N 0.902(18) . ? N7 H2N 0.910(19) . ? C1 C2 1.3924(10) . ? C1 H1A 0.9300 . ? C2 C3 1.3890(11) . ? C2 H2A 0.9300 . ? C3 C4 1.3914(11) . ? C3 H3A 0.9300 . ? C4 C5 1.3877(10) . ? C4 H4B 0.9300 . ? C5 C6 1.4482(10) . ? C7 C8 1.4668(10) . ? C8 C9 1.3948(10) . ? C9 C10 1.3870(11) . ? C9 H9A 0.9300 . ? C10 C11 1.3927(11) . ? C10 H10A 0.9300 . ? C11 C12 1.3896(11) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? Fe2 N10 2.1124(7) . ? Fe2 N10 2.1124(7) 3_756 ? Fe2 N9 2.1478(6) . ? Fe2 N9 2.1478(6) 3_756 ? Fe2 N8 2.2108(6) 3_756 ? Fe2 N8 2.2108(6) . ? S2 C26 1.6261(8) . ? N8 C14 1.3378(9) . ? N8 C18 1.3549(10) . ? N9 C19 1.3251(10) . ? N9 N11 1.3678(9) . ? N10 C26 1.1771(10) . ? N11 C20 1.3211(10) . ? N12 C25 1.3372(10) . ? N12 C21 1.3443(10) . ? N13 C19 1.3576(10) . ? N13 C20 1.3738(10) . ? N13 N14 1.4139(9) . ? N14 H3N 0.886(16) . ? N14 H4N 0.900(16) . ? C14 C15 1.3942(11) . ? C14 H14A 0.9300 . ? C15 C16 1.3865(12) . ? C15 H15A 0.9300 . ? C16 C17 1.3944(11) . ? C16 H16A 0.9300 . ? C17 C18 1.3885(10) . ? C17 H17A 0.9300 . ? C18 C19 1.4680(10) . ? C20 C21 1.4654(10) . ? C21 C22 1.3942(11) . ? C22 C23 1.3896(11) . ? C22 H22A 0.9300 . ? C23 C24 1.3895(13) . ? C23 H23A 0.9300 . ? C24 C25 1.3914(13) . ? 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(5) 3_755 . ? N3 Fe1 N2 87.66(3) 3_755 . ? N3 Fe1 N2 92.34(3) . . ? N3 Fe1 N2 92.34(3) 3_755 3_755 ? N3 Fe1 N2 87.66(3) . 3_755 ? N2 Fe1 N2 180.00(4) . 3_755 ? N3 Fe1 N1 89.50(3) 3_755 3_755 ? N3 Fe1 N1 90.50(3) . 3_755 ? N2 Fe1 N1 99.53(3) . 3_755 ? N2 Fe1 N1 80.47(3) 3_755 3_755 ? N3 Fe1 N1 90.50(3) 3_755 . ? N3 Fe1 N1 89.50(3) . . ? N2 Fe1 N1 80.47(3) . . ? N2 Fe1 N1 99.53(3) 3_755 . ? N1 Fe1 N1 180.00(4) 3_755 . ? C1 N1 C5 117.55(6) . . ? C1 N1 Fe1 126.33(5) . . ? C5 N1 Fe1 116.12(5) . . ? C6 N2 N4 108.61(6) . . ? C6 N2 Fe1 113.52(5) . . ? N4 N2 Fe1 137.70(5) . . ? C13 N3 Fe1 175.14(6) . . ? C7 N4 N2 106.70(6) . . ? C12 N5 C8 116.83(7) . . ? C6 N6 C7 105.55(6) . . ? C6 N6 N7 123.90(6) . . ? C7 N6 N7 130.53(6) . . ? N6 N7 H1N 106.4(12) . . ? N6 N7 H2N 103.7(12) . . ? H1N N7 H2N 104.0(16) . . ? N1 C1 C2 122.76(7) . . ? N1 C1 H1A 118.6 . . ? C2 C1 H1A 118.6 . . ? C3 C2 C1 119.15(7) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C2 C3 C4 118.96(7) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C5 C4 C3 118.32(7) . . ? C5 C4 H4B 120.8 . . ? C3 C4 H4B 120.8 . . ? N1 C5 C4 123.23(7) . . ? N1 C5 C6 110.69(6) . . ? C4 C5 C6 126.07(7) . . ? N2 C6 N6 109.34(6) . . ? N2 C6 C5 118.85(6) . . ? N6 C6 C5 131.78(6) . . ? N4 C7 N6 109.79(6) . . ? N4 C7 C8 124.10(6) . . ? N6 C7 C8 126.11(6) . . ? N5 C8 C9 123.49(7) . . ? N5 C8 C7 117.33(6) . . ? C9 C8 C7 119.17(6) . . ? C10 C9 C8 118.56(7) . . ? C10 C9 H9A 120.7 . . ? C8 C9 H9A 120.7 . . ? C9 C10 C11 118.78(7) . . ? C9 C10 H10A 120.6 . . ? C11 C10 H10A 120.6 . . ? C12 C11 C10 118.30(7) . . ? C12 C11 H11A 120.8 . . ? C10 C11 H11A 120.8 . . ? N5 C12 C11 123.94(7) . . ? N5 C12 H12A 118.0 . . ? C11 C12 H12A 118.0 . . ? N3 C13 S1 177.95(7) . . ? N10 Fe2 N10 180.0 . 3_756 ? N10 Fe2 N9 92.68(3) . . ? N10 Fe2 N9 87.32(3) 3_756 . ? N10 Fe2 N9 87.32(3) . 3_756 ? N10 Fe2 N9 92.68(3) 3_756 3_756 ? N9 Fe2 N9 180.00(4) . 3_756 ? N10 Fe2 N8 90.08(3) . 3_756 ? N10 Fe2 N8 89.92(3) 3_756 3_756 ? N9 Fe2 N8 104.74(2) . 3_756 ? N9 Fe2 N8 75.26(2) 3_756 3_756 ? N10 Fe2 N8 89.92(3) . . ? N10 Fe2 N8 90.08(3) 3_756 . ? N9 Fe2 N8 75.26(2) . . ? N9 Fe2 N8 104.74(2) 3_756 . ? N8 Fe2 N8 180.00(2) 3_756 . ? C14 N8 C18 118.35(6) . . ? C14 N8 Fe2 125.26(5) . . ? C18 N8 Fe2 116.38(5) . . ? C19 N9 N11 108.95(6) . . ? C19 N9 Fe2 114.64(5) . . ? N11 N9 Fe2 134.77(5) . . ? C26 N10 Fe2 162.73(7) . . ? C20 N11 N9 106.60(6) . . ? C25 N12 C21 117.06(7) . . ? C19 N13 C20 105.61(6) . . ? C19 N13 N14 125.70(6) . . ? C20 N13 N14 128.69(6) . . ? N13 N14 H3N 105.4(10) . . ? N13 N14 H4N 108.1(11) . . ? H3N N14 H4N 108.0(14) . . ? N8 C14 C15 122.93(7) . . ? N8 C14 H14A 118.5 . . ? C15 C14 H14A 118.5 . . ? C16 C15 C14 118.29(7) . . ? C16 C15 H15A 120.9 . . ? C14 C15 H15A 120.9 . . ? C15 C16 C17 119.58(7) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C18 C17 C16 118.39(7) . . ? C18 C17 H17A 120.8 . . ? C16 C17 H17A 120.8 . . ? N8 C18 C17 122.47(7) . . ? N8 C18 C19 112.14(6) . . ? C17 C18 C19 125.39(7) . . ? N9 C19 N13 108.83(6) . . ? N9 C19 C18 120.76(7) . . ? N13 C19 C18 130.40(7) . . ? N11 C20 N13 109.99(6) . . ? N11 C20 C21 124.33(7) . . ? N13 C20 C21 125.66(7) . . ? N12 C21 C22 123.80(7) . . ? N12 C21 C20 116.33(7) . . ? C22 C21 C20 119.86(7) . . ? C23 C22 C21 118.07(8) . . ? C23 C22 H22A 121.0 . . ? C21 C22 H22A 121.0 . . ? C24 C23 C22 118.87(8) . . ? C24 C23 H23A 120.6 . . ? C22 C23 H23A 120.6 . . ? C23 C24 C25 118.69(7) . . ? C23 C24 H24A 120.7 . . ? C25 C24 H24A 120.7 . . ? N12 C25 C24 123.48(8) . . ? N12 C25 H25A 118.3 . . ? C24 C25 H25A 118.3 . . ? N10 C26 S2 178.35(7) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 24.53 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.687 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.078 # Attachment '843268.cif' data_pi1 _database_code_depnum_ccdc_archive 'CCDC 843268' #TrackingRef '843268.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Fe(abpt)2(NCS)2 _chemical_melting_point 'not measured' _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 0.0007 0.0007 '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 0.0018 0.0015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.0662 0.0602 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.2560 0.4380 '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 1 21/c 1' 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 10.72100(19) _cell_length_b 15.89090(19) _cell_length_c 17.18610(70) _cell_angle_alpha 90.0000(10) _cell_angle_beta 106.0191(7) _cell_angle_gamma 90.0000(10) _cell_volume 2814.24(13) _cell_formula_units_Z 4 _cell_measurement_temperature 20(2) _cell_measurement_reflns_used 11736 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 18.2 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.279 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.844 _exptl_absorpt_correction_T_max 0.910 _exptl_absorpt_process_details 'Multi-scan (2001 Higashi)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 20(2) _diffrn_radiation_wavelength 0.49812 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31788 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 24.48 _reflns_number_total 13095 _reflns_number_gt 11126 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID AUTO' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0606P)^2^+0.1177P] 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 13095 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0944 _refine_ls_wR_factor_gt 0.0912 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 1.0000 0.0000 0.0000 0.00656(4) Uani 1 2 d S . . S1 S 1.44924(3) 0.048508(18) 0.166126(17) 0.01860(5) Uani 1 1 d . . . N1 N 0.98773(8) -0.09983(4) 0.08496(5) 0.00852(11) Uani 1 1 d . . . N2 N 0.91094(8) 0.06005(4) 0.08351(5) 0.00815(11) Uani 1 1 d . . . N3 N 1.19042(8) 0.03114(5) 0.07253(5) 0.01132(12) Uani 1 1 d . . . N4 N 0.86635(8) 0.13866(4) 0.09486(5) 0.00854(11) Uani 1 1 d . . . N5 N 0.70068(8) 0.18700(5) 0.24786(5) 0.01013(12) Uani 1 1 d . . . N6 N 0.82777(8) 0.05175(4) 0.18587(5) 0.00801(11) Uani 1 1 d . . . N7 N 0.79032(8) 0.01809(5) 0.25225(5) 0.01108(13) Uani 1 1 d . . . C1 C 1.02980(9) -0.17868(5) 0.08173(6) 0.01003(13) Uani 1 1 d . . . H1A H 1.0730 -0.1918 0.0433 0.012 Uiso 1 1 calc R . . C2 C 1.01143(10) -0.24185(5) 0.13369(6) 0.01137(14) Uani 1 1 d . . . H2A H 1.0409 -0.2963 0.1297 0.014 Uiso 1 1 calc R . . C3 C 0.94803(10) -0.22167(5) 0.19166(6) 0.01189(14) Uani 1 1 d . . . H3A H 0.9345 -0.2627 0.2271 0.014 Uiso 1 1 calc R . . C4 C 0.90485(9) -0.13952(5) 0.19642(6) 0.01090(14) Uani 1 1 d . . . H4B H 0.8626 -0.1247 0.2349 0.013 Uiso 1 1 calc R . . C5 C 0.92679(9) -0.08041(5) 0.14194(5) 0.00835(13) Uani 1 1 d . . . C6 C 0.88694(9) 0.00824(5) 0.13808(5) 0.00787(12) Uani 1 1 d . . . C7 C 0.81696(8) 0.13299(5) 0.15738(5) 0.00807(12) Uani 1 1 d . . . C8 C 0.76111(8) 0.20414(5) 0.19067(5) 0.00827(12) Uani 1 1 d . . . C9 C 0.77491(9) 0.28519(5) 0.16298(6) 0.01032(13) Uani 1 1 d . . . H9A H 0.8142 0.2940 0.1217 0.012 Uiso 1 1 calc R . . C10 C 0.72874(9) 0.35241(5) 0.19847(6) 0.01224(14) Uani 1 1 d . . . H10A H 0.7374 0.4073 0.1819 0.015 Uiso 1 1 calc R . . C11 C 0.66901(10) 0.33618(5) 0.25964(6) 0.01226(14) Uani 1 1 d . . . H11A H 0.6393 0.3800 0.2857 0.015 Uiso 1 1 calc R . . C12 C 0.65504(10) 0.25307(5) 0.28061(6) 0.01231(15) Uani 1 1 d . . . H12A H 0.6116 0.2424 0.3196 0.015 Uiso 1 1 calc R . . C13 C 1.29821(9) 0.03734(5) 0.11194(6) 0.01035(14) Uani 1 1 d . . . Fe2 Fe 1.0000 0.0000 0.5000 0.00574(4) Uani 1 2 d S . . S2 S 1.17048(2) 0.072196(13) 0.271039(13) 0.00924(4) Uani 1 1 d . . . N8 N 0.87213(7) -0.09987(4) 0.43020(4) 0.00732(11) Uani 1 1 d . . . N9 N 0.81249(7) 0.05802(4) 0.45821(5) 0.00782(11) Uani 1 1 d . . . N10 N 1.05439(8) 0.03782(5) 0.39536(5) 0.01076(12) Uani 1 1 d . . . N11 N 0.76041(8) 0.13210(4) 0.47544(5) 0.00848(11) Uani 1 1 d . . . N12 N 0.41780(8) 0.16144(4) 0.45048(5) 0.00964(12) Uani 1 1 d . . . N13 N 0.60177(7) 0.04617(4) 0.41353(5) 0.00759(11) Uani 1 1 d . . . N14 N 0.47744(8) 0.01232(5) 0.37564(5) 0.01069(12) Uani 1 1 d . . . H1N H 0.7314(19) 0.0526(11) 0.2575(12) 0.025(4) Uiso 1 1 d . . . H2N H 0.8617(18) 0.0298(10) 0.2972(11) 0.021(4) Uiso 1 1 d . . . C14 C 0.91050(9) -0.17757(5) 0.41644(5) 0.00884(13) Uani 1 1 d . . . H14A H 0.9980 -0.1911 0.4356 0.011 Uiso 1 1 calc R . . C15 C 0.82477(9) -0.23889(5) 0.37460(6) 0.00996(13) Uani 1 1 d . . . H15A H 0.8544 -0.2923 0.3665 0.012 Uiso 1 1 calc R . . C16 C 0.69413(9) -0.21836(5) 0.34522(6) 0.01120(14) Uani 1 1 d . . . H16A H 0.6349 -0.2580 0.3170 0.013 Uiso 1 1 calc R . . C17 C 0.65259(9) -0.13761(5) 0.35849(6) 0.00999(13) Uani 1 1 d . . . H17A H 0.5658 -0.1224 0.3390 0.012 Uiso 1 1 calc R . . C18 C 0.74450(8) -0.08049(5) 0.40168(5) 0.00721(12) Uani 1 1 d . . . C19 C 0.71672(8) 0.00620(4) 0.42248(5) 0.00727(12) Uani 1 1 d . . . C20 C 0.63294(8) 0.12428(5) 0.44823(5) 0.00774(12) Uani 1 1 d . . . C21 C 0.53929(8) 0.18840(5) 0.45763(5) 0.00821(12) Uani 1 1 d . . . C22 C 0.57958(9) 0.27179(5) 0.47458(6) 0.01047(14) Uani 1 1 d . . . H22A H 0.6647 0.2878 0.4790 0.013 Uiso 1 1 calc R . . C23 C 0.48817(10) 0.32999(5) 0.48463(6) 0.01237(15) Uani 1 1 d . . . H23A H 0.5112 0.3860 0.4962 0.015 Uiso 1 1 calc R . . C24 C 0.36189(10) 0.30316(5) 0.47711(6) 0.01229(14) Uani 1 1 d . . . H24A H 0.2991 0.3408 0.4836 0.015 Uiso 1 1 calc R . . C25 C 0.33117(9) 0.21870(5) 0.45961(6) 0.01135(14) Uani 1 1 d . . . H25A H 0.2463 0.2013 0.4540 0.014 Uiso 1 1 calc R . . C26 C 1.10480(9) 0.05266(5) 0.34408(5) 0.00869(13) Uani 1 1 d . . . H3N H 0.4209(18) 0.0445(10) 0.3981(11) 0.025(4) Uiso 1 1 d . . . H4N H 0.463(2) 0.0232(11) 0.3183(13) 0.031(5) Uiso 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 0.00757(8) 0.00631(6) 0.00566(7) 0.00017(5) 0.00160(6) -0.00025(5) S1 0.00925(10) 0.03101(12) 0.01342(11) 0.00837(9) -0.00040(8) -0.00574(8) N1 0.0092(3) 0.0071(2) 0.0087(3) 0.0002(2) 0.0016(2) -0.0006(2) N2 0.0110(3) 0.0062(2) 0.0075(3) 0.0003(2) 0.0029(2) 0.0000(2) N3 0.0112(3) 0.0124(3) 0.0098(3) -0.0003(2) 0.0020(3) -0.0012(2) N4 0.0102(3) 0.0075(2) 0.0085(3) 0.0001(2) 0.0035(2) 0.0005(2) N5 0.0108(3) 0.0116(3) 0.0086(3) -0.0003(2) 0.0038(3) 0.0007(2) N6 0.0090(3) 0.0083(2) 0.0071(3) 0.0016(2) 0.0029(2) -0.0003(2) N7 0.0112(3) 0.0150(3) 0.0082(3) 0.0048(2) 0.0045(3) 0.0008(2) C1 0.0111(4) 0.0073(3) 0.0109(3) 0.0000(2) 0.0016(3) 0.0003(2) C2 0.0122(4) 0.0071(3) 0.0130(4) 0.0009(2) 0.0006(3) -0.0005(2) C3 0.0133(4) 0.0087(3) 0.0121(4) 0.0026(2) 0.0009(3) -0.0014(2) C4 0.0133(4) 0.0087(3) 0.0104(3) 0.0025(2) 0.0027(3) -0.0010(2) C5 0.0095(3) 0.0070(3) 0.0078(3) 0.0013(2) 0.0010(3) -0.0004(2) C6 0.0089(3) 0.0075(3) 0.0071(3) 0.0008(2) 0.0020(3) -0.0004(2) C7 0.0088(3) 0.0074(3) 0.0081(3) 0.0004(2) 0.0023(3) -0.0001(2) C8 0.0082(3) 0.0088(3) 0.0077(3) -0.0005(2) 0.0020(3) 0.0003(2) C9 0.0102(4) 0.0093(3) 0.0118(3) 0.0012(2) 0.0037(3) 0.0012(2) C10 0.0119(4) 0.0097(3) 0.0147(4) 0.0001(3) 0.0030(3) 0.0021(3) C11 0.0124(4) 0.0126(3) 0.0113(4) -0.0009(3) 0.0025(3) 0.0035(3) C12 0.0127(4) 0.0150(3) 0.0098(3) -0.0001(3) 0.0040(3) 0.0029(3) C13 0.0110(4) 0.0103(3) 0.0098(3) 0.0015(2) 0.0031(3) -0.0010(2) Fe2 0.00570(7) 0.00607(6) 0.00566(7) -0.00022(4) 0.00195(6) 0.00018(5) S2 0.01003(9) 0.01046(8) 0.00809(9) 0.00125(6) 0.00395(7) 0.00039(6) N8 0.0080(3) 0.0071(2) 0.0070(3) -0.0001(2) 0.0024(2) 0.0008(2) N9 0.0077(3) 0.0066(2) 0.0090(3) -0.0018(2) 0.0019(2) 0.0006(2) N10 0.0120(3) 0.0117(3) 0.0092(3) 0.0000(2) 0.0041(3) -0.0005(2) N11 0.0078(3) 0.0074(2) 0.0100(3) -0.0014(2) 0.0021(2) 0.0016(2) N12 0.0082(3) 0.0112(3) 0.0096(3) 0.0002(2) 0.0028(3) 0.0021(2) N13 0.0066(3) 0.0071(2) 0.0086(3) -0.0011(2) 0.0012(2) 0.00035(19) N14 0.0059(3) 0.0108(3) 0.0137(3) -0.0023(2) -0.0001(3) -0.0008(2) C14 0.0096(3) 0.0078(3) 0.0095(3) -0.0004(2) 0.0035(3) 0.0012(2) C15 0.0121(4) 0.0076(3) 0.0105(3) -0.0019(2) 0.0037(3) 0.0001(2) C16 0.0120(4) 0.0085(3) 0.0123(4) -0.0033(2) 0.0021(3) -0.0014(2) C17 0.0087(3) 0.0084(3) 0.0120(3) -0.0021(2) 0.0013(3) -0.0003(2) C18 0.0079(3) 0.0067(3) 0.0071(3) -0.0003(2) 0.0021(3) 0.0004(2) C19 0.0070(3) 0.0070(3) 0.0075(3) -0.0002(2) 0.0015(3) 0.0007(2) C20 0.0076(3) 0.0071(3) 0.0084(3) -0.0008(2) 0.0020(3) 0.0009(2) C21 0.0083(3) 0.0087(3) 0.0074(3) -0.0004(2) 0.0019(3) 0.0022(2) C22 0.0100(3) 0.0091(3) 0.0122(4) -0.0021(2) 0.0028(3) 0.0009(2) C23 0.0135(4) 0.0103(3) 0.0132(4) -0.0024(3) 0.0034(3) 0.0031(3) C24 0.0125(4) 0.0131(3) 0.0114(4) -0.0013(3) 0.0034(3) 0.0050(3) C25 0.0093(3) 0.0139(3) 0.0110(3) 0.0004(3) 0.0029(3) 0.0036(3) C26 0.0091(3) 0.0079(3) 0.0086(3) -0.0002(2) 0.0015(3) 0.0002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N3 2.1359(9) 3_755 ? Fe1 N3 2.1359(9) . ? Fe1 N2 2.1536(7) 3_755 ? Fe1 N2 2.1536(7) . ? Fe1 N1 2.1844(7) . ? Fe1 N1 2.1844(7) 3_755 ? S1 C13 1.6396(10) . ? N1 C1 1.3381(10) . ? N1 C5 1.3543(11) . ? N2 C6 1.3255(10) . ? N2 N4 1.3706(9) . ? N3 C13 1.1713(13) . ? N4 C7 1.3256(10) . ? N5 C12 1.3455(11) . ? N5 C8 1.3458(10) . ? N5 N7 2.8449(11) . ? N6 C6 1.3574(11) . ? N6 C7 1.3742(10) . ? N6 N7 1.4148(10) . ? N7 H1N 0.860(17) . ? N7 H2N 0.944(19) . ? C1 C2 1.3931(12) . ? C1 H1A 0.9300 . ? C2 C3 1.3897(13) . ? C2 H2A 0.9300 . ? C3 C4 1.3951(12) . ? C3 H3A 0.9300 . ? C4 C5 1.3914(11) . ? C4 H4B 0.9300 . ? C5 C6 1.4681(11) . ? C7 C8 1.4673(11) . ? C8 C9 1.3951(11) . ? C9 C10 1.3873(12) . ? C9 H9A 0.9300 . ? C10 C11 1.3975(13) . ? C10 H10A 0.9300 . ? C11 C12 1.3879(12) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? Fe2 N10 2.1246(8) . ? Fe2 N10 2.1246(8) 3_756 ? Fe2 N9 2.1471(8) 3_756 ? Fe2 N9 2.1471(8) . ? Fe2 N8 2.2202(7) . ? Fe2 N8 2.2202(7) 3_756 ? S2 C26 1.6297(9) . ? N8 C14 1.3429(10) . ? N8 C18 1.3555(11) . ? N9 C19 1.3272(11) . ? N9 N11 1.3699(9) . ? N10 C26 1.1778(11) . ? N11 C20 1.3225(12) . ? N12 C25 1.3400(11) . ? N12 C21 1.3442(12) . ? N12 N14 2.8517(10) . ? N13 C19 1.3568(11) . ? N13 C20 1.3777(10) . ? N13 N14 1.4181(11) . ? N14 H3N 0.952(17) . ? N14 H4N 0.97(2) . ? C14 C15 1.3952(12) . ? C14 H14A 0.9300 . ? C15 C16 1.3903(14) . ? C15 H15A 0.9300 . ? C16 C17 1.3974(11) . ? C16 H16A 0.9300 . ? C17 C18 1.3937(12) . ? C17 H17A 0.9300 . ? C18 C19 1.4741(10) . ? C20 C21 1.4704(11) . ? C21 C22 1.3992(11) . ? C22 C23 1.3924(12) . ? C22 H22A 0.9300 . ? C23 C24 1.3910(14) . ? C23 H23A 0.9300 . ? C24 C25 1.3950(12) . ? 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(6) 3_755 . ? N3 Fe1 N2 92.10(3) 3_755 3_755 ? N3 Fe1 N2 87.90(3) . 3_755 ? N3 Fe1 N2 87.90(3) 3_755 . ? N3 Fe1 N2 92.10(3) . . ? N2 Fe1 N2 180.00(5) 3_755 . ? N3 Fe1 N1 89.87(3) 3_755 . ? N3 Fe1 N1 90.13(3) . . ? N2 Fe1 N1 104.08(3) 3_755 . ? N2 Fe1 N1 75.92(3) . . ? N3 Fe1 N1 90.13(3) 3_755 3_755 ? N3 Fe1 N1 89.87(3) . 3_755 ? N2 Fe1 N1 75.92(3) 3_755 3_755 ? N2 Fe1 N1 104.08(3) . 3_755 ? N1 Fe1 N1 180.00(4) . 3_755 ? C1 N1 C5 118.61(7) . . ? C1 N1 Fe1 124.69(6) . . ? C5 N1 Fe1 116.60(5) . . ? C6 N2 N4 108.78(7) . . ? C6 N2 Fe1 113.87(5) . . ? N4 N2 Fe1 137.29(5) . . ? C13 N3 Fe1 171.34(7) . . ? C7 N4 N2 106.65(6) . . ? C12 N5 C8 116.85(7) . . ? C12 N5 N7 152.15(6) . . ? C8 N5 N7 89.03(5) . . ? C6 N6 C7 105.70(7) . . ? C6 N6 N7 125.40(7) . . ? C7 N6 N7 128.87(7) . . ? N6 N7 N5 77.93(4) . . ? N6 N7 H1N 102.9(12) . . ? N5 N7 H1N 31.6(11) . . ? N6 N7 H2N 103.8(10) . . ? N5 N7 H2N 91.5(10) . . ? H1N N7 H2N 103.9(16) . . ? N1 C1 C2 122.63(8) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C3 C2 C1 118.48(7) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? C2 C3 C4 119.59(8) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 118.15(8) . . ? C5 C4 H4B 120.9 . . ? C3 C4 H4B 120.9 . . ? N1 C5 C4 122.52(7) . . ? N1 C5 C6 112.24(7) . . ? C4 C5 C6 125.24(8) . . ? N2 C6 N6 109.03(7) . . ? N2 C6 C5 121.13(7) . . ? N6 C6 C5 129.81(7) . . ? N4 C7 N6 109.83(7) . . ? N4 C7 C8 124.13(7) . . ? N6 C7 C8 126.04(7) . . ? N5 C8 C9 123.62(7) . . ? N5 C8 C7 117.35(7) . . ? C9 C8 C7 119.03(7) . . ? C10 C9 C8 118.46(8) . . ? C10 C9 H9A 120.8 . . ? C8 C9 H9A 120.8 . . ? C9 C10 C11 118.80(8) . . ? C9 C10 H10A 120.6 . . ? C11 C10 H10A 120.6 . . ? C12 C11 C10 118.40(8) . . ? C12 C11 H11A 120.8 . . ? C10 C11 H11A 120.8 . . ? N5 C12 C11 123.78(8) . . ? N5 C12 H12A 118.1 . . ? C11 C12 H12A 118.1 . . ? N3 C13 S1 178.50(8) . . ? N10 Fe2 N10 180.0 . 3_756 ? N10 Fe2 N9 87.38(3) . 3_756 ? N10 Fe2 N9 92.62(3) 3_756 3_756 ? N10 Fe2 N9 92.62(3) . . ? N10 Fe2 N9 87.38(3) 3_756 . ? N9 Fe2 N9 180.0 3_756 . ? N10 Fe2 N8 91.01(3) . . ? N10 Fe2 N8 88.99(3) 3_756 . ? N9 Fe2 N8 104.79(3) 3_756 . ? N9 Fe2 N8 75.21(3) . . ? N10 Fe2 N8 88.99(3) . 3_756 ? N10 Fe2 N8 91.01(3) 3_756 3_756 ? N9 Fe2 N8 75.21(3) 3_756 3_756 ? N9 Fe2 N8 104.79(3) . 3_756 ? N8 Fe2 N8 180.0 . 3_756 ? C14 N8 C18 118.23(7) . . ? C14 N8 Fe2 125.37(6) . . ? C18 N8 Fe2 116.37(5) . . ? C19 N9 N11 108.89(7) . . ? C19 N9 Fe2 114.95(5) . . ? N11 N9 Fe2 134.15(6) . . ? C26 N10 Fe2 168.45(8) . . ? C20 N11 N9 106.61(7) . . ? C25 N12 C21 117.28(7) . . ? C25 N12 N14 149.99(7) . . ? C21 N12 N14 88.51(5) . . ? C19 N13 C20 105.57(7) . . ? C19 N13 N14 125.72(7) . . ? C20 N13 N14 128.71(7) . . ? N13 N14 N12 77.12(4) . . ? N13 N14 H3N 103.5(11) . . ? N12 N14 H3N 28.9(10) . . ? N13 N14 H4N 105.3(12) . . ? N12 N14 H4N 108.5(10) . . ? H3N N14 H4N 112.1(15) . . ? N8 C14 C15 122.87(8) . . ? N8 C14 H14A 118.6 . . ? C15 C14 H14A 118.6 . . ? C16 C15 C14 118.53(7) . . ? C16 C15 H15A 120.7 . . ? C14 C15 H15A 120.7 . . ? C15 C16 C17 119.39(8) . . ? C15 C16 H16A 120.3 . . ? C17 C16 H16A 120.3 . . ? C18 C17 C16 118.34(8) . . ? C18 C17 H17A 120.8 . . ? C16 C17 H17A 120.8 . . ? N8 C18 C17 122.64(7) . . ? N8 C18 C19 112.09(7) . . ? C17 C18 C19 125.27(8) . . ? N9 C19 N13 108.94(7) . . ? N9 C19 C18 120.64(7) . . ? N13 C19 C18 130.38(8) . . ? N11 C20 N13 109.95(7) . . ? N11 C20 C21 124.49(7) . . ? N13 C20 C21 125.49(8) . . ? N12 C21 C22 123.82(7) . . ? N12 C21 C20 116.28(7) . . ? C22 C21 C20 119.88(8) . . ? C23 C22 C21 117.86(8) . . ? C23 C22 H22A 121.1 . . ? C21 C22 H22A 121.1 . . ? C24 C23 C22 119.03(8) . . ? C24 C23 H23A 120.5 . . ? C22 C23 H23A 120.5 . . ? C23 C24 C25 118.73(8) . . ? C23 C24 H24A 120.6 . . ? C25 C24 H24A 120.6 . . ? N12 C25 C24 123.27(9) . . ? N12 C25 H25A 118.4 . . ? C24 C25 H25A 118.4 . . ? N10 C26 S2 178.22(9) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 24.48 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.777 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.083 data_pi2 _database_code_depnum_ccdc_archive 'CCDC 843269' #TrackingRef '843269.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Fe(abpt)2(NCS)2 _chemical_melting_point 'not measured' _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 0.0007 0.0007 '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 0.0018 0.0015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.0656 0.0596 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.2546 0.4343 '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 1 21/c 1' 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 10.6323(3) _cell_length_b 15.8857(4) _cell_length_c 17.2296(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.9133(7) _cell_angle_gamma 90.00 _cell_volume 2798.59(16) _cell_formula_units_Z 4 _cell_measurement_temperature 20(2) _cell_measurement_reflns_used 17563 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 18.2 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.277 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.852 _exptl_absorpt_correction_T_max 0.879 _exptl_absorpt_process_details 'Multi-scan (2001 Higashi)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 20(2) _diffrn_radiation_wavelength 0.4959 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40592 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 24.62 _reflns_number_total 13701 _reflns_number_gt 11041 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID AUTO' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0606P)^2^+0.8710P] 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 13701 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1133 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 1.0000 0.0000 0.0000 0.0084(3) Uiso 0.1997(17) 2 d SP . 1 N3 N 1.1970(3) 0.0271(3) 0.0760(3) 0.0126(9) Uiso 0.1997(17) 1 d PG . 1 C13 C 1.3031(2) 0.03987(18) 0.11706(17) 0.0117(11) Uiso 0.1997(17) 1 d PG . 1 S1 S 1.45075(19) 0.06163(13) 0.17523(13) 0.01911(16) Uiso 0.1997(17) 1 d PG . 1 Fe3 Fe 0.95902(5) -0.00333(2) -0.01447(3) 0.01045(8) Uiso 0.4001(8) 1 d P . 2 S3 S 1.28264(6) -0.00412(4) 0.05988(4) 0.01294(12) Uiso 0.4001(8) 1 d P . 2 C27 C 1.3975(3) 0.02036(18) 0.14369(17) 0.0156(4) Uiso 0.4001(8) 1 d P . 2 N15 N 1.4799(3) 0.03361(18) 0.20354(18) 0.01911(16) Uiso 0.4001(8) 1 d P . 2 S4 S 0.53409(12) -0.07400(8) -0.18768(8) 0.01911(16) Uiso 0.3201(7) 1 d P . 2 S4' S 0.5173(4) -0.0249(3) -0.1689(3) 0.0191(6) Uiso 0.0800(2) 1 d P . 2 C28 C 0.6692(5) -0.0410(2) -0.1261(2) 0.0221(6) Uiso 0.4001(8) 1 d P . 2 N16 N 0.7717(3) -0.02483(19) -0.08178(18) 0.0171(5) Uiso 0.4001(8) 1 d P . 2 N1 N 0.98490(10) -0.10094(6) 0.07710(5) 0.01420(15) Uani 1 1 d . . . N2 N 0.92090(11) 0.05906(6) 0.08516(6) 0.01637(16) Uani 1 1 d . . . N4 N 0.87837(11) 0.13759(6) 0.09872(6) 0.01690(17) Uani 1 1 d . . . N5 N 0.71905(11) 0.18485(7) 0.25474(6) 0.01721(17) Uani 1 1 d . . . N6 N 0.82854(9) 0.04756(6) 0.18265(5) 0.01336(14) Uani 1 1 d . . . N7 N 0.78185(13) 0.00928(8) 0.24322(8) 0.0225(2) Uani 1 1 d . . . C1 C 1.02579(11) -0.17936(7) 0.07067(7) 0.01526(17) Uani 1 1 d . . . H1A H 1.0660 -0.1914 0.0303 0.018 Uiso 1 1 calc R . . C2 C 1.01062(11) -0.24377(7) 0.12194(7) 0.01635(18) Uani 1 1 d . . . H2A H 1.0392 -0.2981 0.1158 0.020 Uiso 1 1 calc R . . C3 C 0.95187(12) -0.22514(7) 0.18252(7) 0.01784(19) Uani 1 1 d . . . H3A H 0.9403 -0.2671 0.2176 0.021 Uiso 1 1 calc R . . C4 C 0.91037(11) -0.14339(7) 0.19060(7) 0.01653(18) Uani 1 1 d . . . H4B H 0.8717 -0.1296 0.2312 0.020 Uiso 1 1 calc R . . C5 C 0.92819(10) -0.08310(7) 0.13644(6) 0.01294(16) Uani 1 1 d . . . C6 C 0.89120(11) 0.00564(6) 0.13614(6) 0.01279(16) Uani 1 1 d . . . C7 C 0.82308(10) 0.12994(7) 0.15827(6) 0.01273(16) Uani 1 1 d . . . C8 C 0.76886(10) 0.20086(7) 0.19275(6) 0.01296(16) Uani 1 1 d . . . C9 C 0.77439(11) 0.28102(7) 0.16133(7) 0.01644(18) Uani 1 1 d . . . H9A H 0.8079 0.2892 0.1174 0.020 Uiso 1 1 calc R . . C10 C 0.72905(12) 0.34832(8) 0.19682(8) 0.0190(2) Uani 1 1 d . . . H10A H 0.7324 0.4028 0.1776 0.023 Uiso 1 1 calc R . . C11 C 0.67829(12) 0.33302(8) 0.26172(7) 0.01805(19) Uani 1 1 d . . . H11A H 0.6480 0.3770 0.2873 0.022 Uiso 1 1 calc R . . C12 C 0.67395(13) 0.25100(8) 0.28728(7) 0.0192(2) Uani 1 1 d . . . H12A H 0.6375 0.2410 0.3297 0.023 Uiso 1 1 calc R . . Fe2 Fe 1.0000 0.0000 0.5000 0.00961(4) Uani 1 2 d S . . S2 S 1.16889(3) 0.069297(18) 0.270916(16) 0.01513(5) Uani 1 1 d . . . N8 N 0.87005(9) -0.09814(5) 0.42842(5) 0.01116(13) Uani 1 1 d . . . N9 N 0.81179(9) 0.05900(5) 0.46035(5) 0.01189(14) Uani 1 1 d . . . N10 N 1.05171(10) 0.03954(6) 0.39541(6) 0.01568(16) Uani 1 1 d . . . N11 N 0.75970(9) 0.13246(5) 0.47880(5) 0.01218(14) Uani 1 1 d . . . N12 N 0.41597(9) 0.16080(6) 0.45621(6) 0.01352(14) Uani 1 1 d . . . N13 N 0.59982(9) 0.04744(5) 0.41669(5) 0.01154(13) Uani 1 1 d . . . N14 N 0.47499(9) 0.01361(6) 0.37929(7) 0.01618(16) Uani 1 1 d . . . H1N H 0.418(2) 0.0433(13) 0.3985(12) 0.026(5) Uiso 1 1 d . . . H2N H 0.457(2) 0.0225(16) 0.3271(15) 0.044(7) Uiso 1 1 d . . . C14 C 0.90812(11) -0.17457(6) 0.41110(6) 0.01317(16) Uani 1 1 d . . . H14A H 0.9961 -0.1887 0.4299 0.016 Uiso 1 1 calc R . . C15 C 0.82172(11) -0.23371(7) 0.36617(7) 0.01501(17) Uani 1 1 d . . . H15A H 0.8510 -0.2866 0.3558 0.018 Uiso 1 1 calc R . . C16 C 0.69100(12) -0.21186(7) 0.33724(7) 0.01620(18) Uani 1 1 d . . . H16A H 0.6312 -0.2500 0.3067 0.019 Uiso 1 1 calc R . . C17 C 0.64993(11) -0.13252(7) 0.35419(7) 0.01486(17) Uani 1 1 d . . . H17A H 0.5627 -0.1166 0.3351 0.018 Uiso 1 1 calc R . . C18 C 0.74237(10) -0.07769(6) 0.40039(6) 0.01133(15) Uani 1 1 d . . . C19 C 0.71492(10) 0.00779(6) 0.42393(6) 0.01127(15) Uani 1 1 d . . . C20 C 0.63131(10) 0.12463(6) 0.45200(6) 0.01134(15) Uani 1 1 d . . . C21 C 0.53720(10) 0.18846(6) 0.46172(6) 0.01169(15) Uani 1 1 d . . . C22 C 0.57590(11) 0.27211(7) 0.47715(7) 0.01524(17) Uani 1 1 d . . . H22A H 0.6608 0.2889 0.4800 0.018 Uiso 1 1 calc R . . C23 C 0.48408(11) 0.32961(7) 0.48819(7) 0.01739(19) Uani 1 1 d . . . H23A H 0.5065 0.3858 0.4992 0.021 Uiso 1 1 calc R . . C24 C 0.35804(11) 0.30176(7) 0.48247(7) 0.01627(18) Uani 1 1 d . . . H24A H 0.2945 0.3389 0.4896 0.020 Uiso 1 1 calc R . . C25 C 0.32875(11) 0.21741(7) 0.46599(7) 0.01531(17) Uani 1 1 d . . . H25A H 0.2439 0.1993 0.4615 0.018 Uiso 1 1 calc R . . C26 C 1.10169(10) 0.05207(6) 0.34367(6) 0.01316(16) Uani 1 1 d . . . H4N H 0.823(2) 0.0346(15) 0.2853(14) 0.035(6) Uiso 1 1 d . . . H3N H 0.703(4) 0.023(2) 0.235(2) 0.085(11) Uiso 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 N1 0.0191(4) 0.0110(3) 0.0118(3) -0.0001(3) 0.0031(3) -0.0033(3) N2 0.0277(5) 0.0103(3) 0.0131(4) 0.0000(3) 0.0091(3) -0.0032(3) N4 0.0285(5) 0.0111(3) 0.0140(4) -0.0011(3) 0.0105(3) -0.0029(3) N5 0.0226(4) 0.0174(4) 0.0133(4) -0.0009(3) 0.0077(3) -0.0033(3) N6 0.0148(3) 0.0143(3) 0.0113(3) 0.0032(3) 0.0040(3) -0.0014(3) N7 0.0272(5) 0.0230(5) 0.0222(5) 0.0105(4) 0.0148(4) 0.0026(4) C1 0.0179(4) 0.0118(4) 0.0147(4) 0.0001(3) 0.0023(3) -0.0027(3) C2 0.0164(4) 0.0127(4) 0.0173(4) 0.0033(3) 0.0002(3) -0.0015(3) C3 0.0183(4) 0.0156(4) 0.0181(4) 0.0071(4) 0.0025(4) -0.0003(3) C4 0.0184(4) 0.0158(4) 0.0149(4) 0.0057(3) 0.0038(3) -0.0005(3) C5 0.0145(4) 0.0121(4) 0.0105(4) 0.0014(3) 0.0005(3) -0.0028(3) C6 0.0157(4) 0.0122(4) 0.0098(4) 0.0008(3) 0.0024(3) -0.0033(3) C7 0.0147(4) 0.0128(4) 0.0102(4) 0.0004(3) 0.0026(3) -0.0026(3) C8 0.0125(4) 0.0145(4) 0.0112(4) 0.0002(3) 0.0021(3) -0.0013(3) C9 0.0166(4) 0.0162(4) 0.0180(4) 0.0051(4) 0.0072(4) 0.0041(3) C10 0.0192(5) 0.0177(5) 0.0215(5) 0.0051(4) 0.0077(4) 0.0064(4) C11 0.0181(4) 0.0198(5) 0.0157(4) 0.0006(4) 0.0038(4) 0.0054(4) C12 0.0236(5) 0.0213(5) 0.0139(4) -0.0003(4) 0.0073(4) 0.0009(4) Fe2 0.01100(8) 0.00877(8) 0.00902(8) -0.00022(6) 0.00269(6) 0.00066(6) S2 0.01478(11) 0.01796(11) 0.01292(10) 0.00313(8) 0.00423(8) -0.00088(8) N8 0.0132(3) 0.0093(3) 0.0112(3) -0.0001(3) 0.0038(3) 0.0009(3) N9 0.0122(3) 0.0094(3) 0.0134(3) -0.0018(3) 0.0024(3) 0.0008(3) N10 0.0199(4) 0.0141(4) 0.0136(4) 0.0001(3) 0.0055(3) -0.0005(3) N11 0.0123(3) 0.0099(3) 0.0139(3) -0.0019(3) 0.0030(3) 0.0016(3) N12 0.0120(3) 0.0141(3) 0.0140(4) 0.0014(3) 0.0027(3) 0.0018(3) N13 0.0112(3) 0.0098(3) 0.0123(3) -0.0013(3) 0.0010(3) 0.0003(3) N14 0.0113(3) 0.0149(4) 0.0195(4) -0.0037(3) -0.0005(3) -0.0011(3) C14 0.0166(4) 0.0107(4) 0.0129(4) -0.0001(3) 0.0053(3) 0.0017(3) C15 0.0200(4) 0.0108(4) 0.0150(4) -0.0023(3) 0.0061(3) 0.0004(3) C16 0.0196(5) 0.0126(4) 0.0153(4) -0.0037(3) 0.0031(3) -0.0011(3) C17 0.0156(4) 0.0125(4) 0.0148(4) -0.0024(3) 0.0014(3) -0.0003(3) C18 0.0138(4) 0.0100(3) 0.0098(3) -0.0003(3) 0.0026(3) 0.0006(3) C19 0.0122(4) 0.0101(3) 0.0105(3) -0.0003(3) 0.0013(3) 0.0013(3) C20 0.0121(4) 0.0101(3) 0.0113(4) -0.0012(3) 0.0024(3) 0.0007(3) C21 0.0129(4) 0.0114(4) 0.0106(4) 0.0004(3) 0.0028(3) 0.0023(3) C22 0.0145(4) 0.0127(4) 0.0190(4) -0.0031(3) 0.0055(3) 0.0007(3) C23 0.0184(5) 0.0136(4) 0.0202(5) -0.0036(3) 0.0054(4) 0.0030(3) C24 0.0167(4) 0.0162(4) 0.0161(4) -0.0008(3) 0.0049(3) 0.0055(3) C25 0.0129(4) 0.0174(4) 0.0157(4) 0.0019(3) 0.0040(3) 0.0034(3) C26 0.0148(4) 0.0113(4) 0.0121(4) -0.0003(3) 0.0017(3) -0.0009(3) _geom_special_details ; Irrational bond distances and bond angles are due to the fact that atoms Fe3, S3, S4, C27, C28, N15 and N16 are corresponding to a NCS linkage isomer which is disordered over the inversion center site. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.1017(10) . ? Fe1 N2 2.1017(10) 3_755 ? Fe1 N1 2.1163(9) . ? Fe1 N1 2.1163(9) 3_755 ? Fe1 N3 2.187(2) 3_755 ? Fe1 N3 2.187(2) . ? N3 C13 1.1726 . ? C13 S1 1.6514 . ? Fe3 N16 2.040(3) . ? Fe3 N2 2.1154(10) . ? Fe3 N1 2.1486(10) 3_755 ? Fe3 N1 2.1751(10) . ? Fe3 N2 2.1795(11) 3_755 ? Fe3 S3 3.3262(8) . ? S3 C27 1.661(3) . ? C27 N15 1.175(4) . ? S4 C28 1.621(5) . ? C28 N16 1.175(5) . ? N1 C1 1.3340(14) . ? N1 C5 1.3517(14) . ? N2 C6 1.3204(14) . ? N2 N4 1.3687(14) . ? N4 C7 1.3205(14) . ? N5 C12 1.3401(16) . ? N5 C8 1.3403(14) . ? N5 N7 2.8874(16) . ? N6 C6 1.3499(14) . ? N6 C7 1.3708(14) . ? N6 N7 1.4105(14) . ? N7 H4N 0.84(2) . ? N7 H3N 0.84(4) . ? C1 C2 1.3897(15) . ? C1 H1A 0.9300 . ? C2 C3 1.3873(18) . ? C2 H2A 0.9300 . ? C3 C4 1.3908(17) . ? C3 H3A 0.9300 . ? C4 C5 1.3860(15) . ? C4 H4B 0.9300 . ? C5 C6 1.4631(15) . ? C7 C8 1.4636(15) . ? C8 C9 1.3911(15) . ? C9 C10 1.3823(16) . ? C9 H9A 0.9300 . ? C10 C11 1.3899(17) . ? C10 H10A 0.9300 . ? C11 C12 1.3801(18) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? Fe2 N10 2.1184(10) 3_756 ? Fe2 N10 2.1184(10) . ? Fe2 N9 2.1447(9) . ? Fe2 N9 2.1447(9) 3_756 ? Fe2 N8 2.2194(9) 3_756 ? Fe2 N8 2.2194(9) . ? S2 C26 1.6271(11) . ? N8 C14 1.3391(13) . ? N8 C18 1.3498(13) . ? N9 C19 1.3273(13) . ? N9 N11 1.3662(12) . ? N10 C26 1.1733(14) . ? N11 C20 1.3215(13) . ? N12 C25 1.3352(14) . ? N12 C21 1.3403(14) . ? N12 N14 2.8415(14) . ? N13 C19 1.3514(13) . ? N13 C20 1.3690(13) . ? N13 N14 1.4130(13) . ? N14 H1N 0.90(2) . ? N14 H2N 0.88(3) . ? C14 C15 1.3914(15) . ? C14 H14A 0.9300 . ? C15 C16 1.3859(17) . ? C15 H15A 0.9300 . ? C16 C17 1.3908(15) . ? C16 H16A 0.9300 . ? C17 C18 1.3890(15) . ? C17 H17A 0.9300 . ? C18 C19 1.4691(14) . ? C20 C21 1.4661(14) . ? C21 C22 1.3949(15) . ? C22 C23 1.3876(15) . ? C22 H22A 0.9300 . ? C23 C24 1.3889(17) . ? C23 H23A 0.9300 . ? C24 C25 1.3873(17) . ? 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 N2 Fe1 N2 180.00(7) . 3_755 ? N2 Fe1 N1 77.66(4) . . ? N2 Fe1 N1 102.34(4) 3_755 . ? N2 Fe1 N1 102.34(4) . 3_755 ? N2 Fe1 N1 77.66(4) 3_755 3_755 ? N1 Fe1 N1 180.00(6) . 3_755 ? N2 Fe1 N3 90.27(14) . 3_755 ? N2 Fe1 N3 89.73(14) 3_755 3_755 ? N1 Fe1 N3 90.10(13) . 3_755 ? N1 Fe1 N3 89.90(13) 3_755 3_755 ? N2 Fe1 N3 89.73(14) . . ? N2 Fe1 N3 90.27(14) 3_755 . ? N1 Fe1 N3 89.90(13) . . ? N1 Fe1 N3 90.10(13) 3_755 . ? N3 Fe1 N3 180.0(2) 3_755 . ? C13 N3 Fe1 178.6(2) . . ? N3 C13 S1 177.8 . . ? N16 Fe3 N2 99.52(9) . . ? N16 Fe3 N1 101.87(9) . 3_755 ? N2 Fe3 N1 100.82(4) . 3_755 ? N16 Fe3 N1 101.69(9) . . ? N2 Fe3 N1 76.09(4) . . ? N1 Fe3 N1 156.42(3) 3_755 . ? N16 Fe3 N2 104.15(9) . 3_755 ? N2 Fe3 N2 156.31(3) . 3_755 ? N1 Fe3 N2 75.33(4) 3_755 3_755 ? N1 Fe3 N2 97.98(4) . 3_755 ? N16 Fe3 S3 164.56(9) . . ? N2 Fe3 S3 95.59(4) . . ? N1 Fe3 S3 78.23(3) 3_755 . ? N1 Fe3 S3 78.82(3) . . ? N2 Fe3 S3 60.73(3) 3_755 . ? C27 S3 Fe3 140.34(10) . . ? N15 C27 S3 176.8(3) . . ? N16 C28 S4 173.6(3) . . ? C28 N16 Fe3 173.2(3) . . ? C1 N1 C5 118.79(9) . . ? C1 N1 Fe1 124.96(8) . . ? C5 N1 Fe1 116.25(7) . . ? C1 N1 Fe3 125.79(8) . . ? C5 N1 Fe3 113.90(7) . . ? Fe1 N1 Fe3 11.716(14) . . ? C6 N2 N4 108.78(9) . . ? C6 N2 Fe1 113.08(7) . . ? N4 N2 Fe1 137.75(7) . . ? C6 N2 Fe3 111.88(7) . . ? N4 N2 Fe3 135.34(7) . . ? Fe1 N2 Fe3 12.024(15) . . ? C7 N4 N2 106.68(9) . . ? C12 N5 C8 116.72(10) . . ? C12 N5 N7 154.45(8) . . ? C8 N5 N7 88.80(7) . . ? C6 N6 C7 105.99(8) . . ? C6 N6 N7 123.89(10) . . ? C7 N6 N7 130.12(10) . . ? N6 N7 N5 76.67(6) . . ? N6 N7 H4N 103.3(16) . . ? N5 N7 H4N 63.3(16) . . ? N6 N7 H3N 107(2) . . ? N5 N7 H3N 61(2) . . ? H4N N7 H3N 106(3) . . ? N1 C1 C2 122.52(11) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C3 C2 C1 118.41(11) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? C2 C3 C4 119.68(10) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 118.17(11) . . ? C5 C4 H4B 120.9 . . ? C3 C4 H4B 120.9 . . ? N1 C5 C4 122.41(10) . . ? N1 C5 C6 112.00(9) . . ? C4 C5 C6 125.58(10) . . ? N2 C6 N6 108.95(9) . . ? N2 C6 C5 120.56(10) . . ? N6 C6 C5 130.48(9) . . ? N4 C7 N6 109.60(9) . . ? N4 C7 C8 123.59(9) . . ? N6 C7 C8 126.78(9) . . ? N5 C8 C9 123.49(10) . . ? N5 C8 C7 117.59(10) . . ? C9 C8 C7 118.90(9) . . ? C10 C9 C8 118.61(10) . . ? C10 C9 H9A 120.7 . . ? C8 C9 H9A 120.7 . . ? C9 C10 C11 118.69(11) . . ? C9 C10 H10A 120.7 . . ? C11 C10 H10A 120.7 . . ? C12 C11 C10 118.43(11) . . ? C12 C11 H11A 120.8 . . ? C10 C11 H11A 120.8 . . ? N5 C12 C11 124.03(11) . . ? N5 C12 H12A 118.0 . . ? C11 C12 H12A 118.0 . . ? N10 Fe2 N10 180.0 3_756 . ? N10 Fe2 N9 87.90(4) 3_756 . ? N10 Fe2 N9 92.10(4) . . ? N10 Fe2 N9 92.10(4) 3_756 3_756 ? N10 Fe2 N9 87.90(4) . 3_756 ? N9 Fe2 N9 180.0 . 3_756 ? N10 Fe2 N8 90.16(3) 3_756 3_756 ? N10 Fe2 N8 89.84(3) . 3_756 ? N9 Fe2 N8 104.74(3) . 3_756 ? N9 Fe2 N8 75.26(3) 3_756 3_756 ? N10 Fe2 N8 89.84(3) 3_756 . ? N10 Fe2 N8 90.16(3) . . ? N9 Fe2 N8 75.26(3) . . ? N9 Fe2 N8 104.74(3) 3_756 . ? N8 Fe2 N8 180.00(3) 3_756 . ? C14 N8 C18 118.31(9) . . ? C14 N8 Fe2 125.49(7) . . ? C18 N8 Fe2 116.20(7) . . ? C19 N9 N11 108.79(8) . . ? C19 N9 Fe2 114.71(7) . . ? N11 N9 Fe2 134.55(7) . . ? C26 N10 Fe2 166.89(9) . . ? C20 N11 N9 106.50(8) . . ? C25 N12 C21 117.26(10) . . ? C25 N12 N14 149.66(8) . . ? C21 N12 N14 88.38(6) . . ? C19 N13 C20 105.75(8) . . ? C19 N13 N14 125.34(9) . . ? C20 N13 N14 128.91(9) . . ? N13 N14 N12 76.96(6) . . ? N13 N14 H1N 106.1(13) . . ? N12 N14 H1N 30.8(13) . . ? N13 N14 H2N 108.7(17) . . ? N12 N14 H2N 109.4(17) . . ? H1N N14 H2N 108(2) . . ? N8 C14 C15 122.85(10) . . ? N8 C14 H14A 118.6 . . ? C15 C14 H14A 118.6 . . ? C16 C15 C14 118.36(10) . . ? C16 C15 H15A 120.8 . . ? C14 C15 H15A 120.8 . . ? C15 C16 C17 119.54(10) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C18 C17 C16 118.36(10) . . ? C18 C17 H17A 120.8 . . ? C16 C17 H17A 120.8 . . ? N8 C18 C17 122.57(9) . . ? N8 C18 C19 112.34(9) . . ? C17 C18 C19 125.09(9) . . ? N9 C19 N13 108.88(8) . . ? N9 C19 C18 120.65(9) . . ? N13 C19 C18 130.44(9) . . ? N11 C20 N13 110.06(9) . . ? N11 C20 C21 124.53(9) . . ? N13 C20 C21 125.37(9) . . ? N12 C21 C22 123.60(9) . . ? N12 C21 C20 116.00(9) . . ? C22 C21 C20 120.38(9) . . ? C23 C22 C21 118.12(10) . . ? C23 C22 H22A 120.9 . . ? C21 C22 H22A 120.9 . . ? C22 C23 C24 118.82(11) . . ? C22 C23 H23A 120.6 . . ? C24 C23 H23A 120.6 . . ? C25 C24 C23 118.70(10) . . ? C25 C24 H24A 120.7 . . ? C23 C24 H24A 120.7 . . ? N12 C25 C24 123.49(10) . . ? N12 C25 H25A 118.3 . . ? C24 C25 H25A 118.3 . . ? N10 C26 S2 179.14(10) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 24.62 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.498 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.094 # Attachment '843270.cif' data_is _database_code_depnum_ccdc_archive 'CCDC 843270' #TrackingRef '843270.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Fe(abpt)2(NCS)2 _chemical_melting_point 'not measured' _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 0.0007 0.0007 '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 0.0018 0.0015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.0656 0.0596 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.2546 0.4343 '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 1 21/c 1' 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 10.6715(6) _cell_length_b 15.8611(2) _cell_length_c 17.1977(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.252(4) _cell_angle_gamma 90.00 _cell_volume 2794.58(18) _cell_formula_units_Z 4 _cell_measurement_temperature 20(2) _cell_measurement_reflns_used 17563 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 18.2 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.278 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.858 _exptl_absorpt_correction_T_max 0.873 _exptl_absorpt_process_details 'Multi-scan (2001 Higashi)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 20(2) _diffrn_radiation_wavelength 0.4959 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42088 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 24.41 _reflns_number_total 13411 _reflns_number_gt 11113 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID AUTO' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+2.1144P] 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 13411 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1345 _refine_ls_wR_factor_gt 0.1278 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _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 0.0046(2) Uiso 0.1886(12) 2 d SP . 1 N3 N 1.1759(3) 0.0245(3) 0.0695(3) 0.0140(9) Uiso 0.1886(12) 1 d PG . 1 C13 C 1.2834(2) 0.0354(2) 0.10916(18) 0.0146(10) Uiso 0.1886(12) 1 d PG . 1 S1 S 1.4334(2) 0.05449(14) 0.16543(13) 0.01783(15) Uiso 0.1886(12) 1 d PG . 1 Fe3 Fe 0.95931(5) -0.00332(3) -0.01394(3) 0.01203(9) Uiso 0.4057(6) 1 d P . 2 S3 S 1.28426(8) -0.00468(5) 0.06070(5) 0.01557(14) Uiso 0.4057(6) 1 d P . 2 C27 C 1.3984(3) 0.0195(2) 0.1438(2) 0.0168(5) Uiso 0.4057(6) 1 d P . 2 N15 N 1.4814(3) 0.0332(2) 0.2038(2) 0.01783(15) Uiso 0.4057(6) 1 d P . 2 S4 S 0.53343(12) -0.07221(8) -0.18655(8) 0.01783(15) Uiso 0.3246(5) 1 d P . 2 S4' S 0.5144(5) -0.0284(3) -0.1702(3) 0.0222(8) Uiso 0.0811(1) 1 d P . 2 C28 C 0.6719(3) -0.0409(2) -0.1251(2) 0.0185(5) Uiso 0.4057(6) 1 d P . 2 N16 N 0.7745(3) -0.02591(18) -0.08124(17) 0.0149(4) Uiso 0.4057(6) 1 d P . 2 N1 N 0.98619(11) -0.10076(7) 0.07543(7) 0.01519(17) Uani 1 1 d . . . N2 N 0.92163(12) 0.05815(7) 0.08392(7) 0.01718(19) Uani 1 1 d . . . N4 N 0.87903(12) 0.13669(7) 0.09758(7) 0.01784(19) Uani 1 1 d . . . N5 N 0.71933(12) 0.18338(8) 0.25365(7) 0.0187(2) Uani 1 1 d . . . N6 N 0.82875(11) 0.04634(7) 0.18135(7) 0.01535(18) Uani 1 1 d . . . N7 N 0.78288(16) 0.00774(9) 0.24227(10) 0.0251(3) Uani 1 1 d . . . C1 C 1.02741(13) -0.17909(8) 0.06861(8) 0.0168(2) Uani 1 1 d . . . H1A H 1.0675 -0.1907 0.0283 0.020 Uiso 1 1 calc R . . C2 C 1.01257(13) -0.24409(8) 0.11973(9) 0.0183(2) Uani 1 1 d . . . H2A H 1.0417 -0.2982 0.1135 0.022 Uiso 1 1 calc R . . C3 C 0.95346(14) -0.22645(9) 0.18009(9) 0.0199(2) Uani 1 1 d . . . H3A H 0.9419 -0.2690 0.2147 0.024 Uiso 1 1 calc R . . C4 C 0.91153(13) -0.14493(9) 0.18871(9) 0.0183(2) Uani 1 1 d . . . H4B H 0.8729 -0.1316 0.2294 0.022 Uiso 1 1 calc R . . C5 C 0.92903(12) -0.08394(8) 0.13476(8) 0.01428(19) Uani 1 1 d . . . C6 C 0.89164(12) 0.00450(8) 0.13477(8) 0.01395(19) Uani 1 1 d . . . C7 C 0.82356(12) 0.12881(8) 0.15710(8) 0.01407(18) Uani 1 1 d . . . C8 C 0.76933(12) 0.19977(8) 0.19184(8) 0.01475(19) Uani 1 1 d . . . C9 C 0.77477(13) 0.28022(9) 0.16054(9) 0.0188(2) Uani 1 1 d . . . H9A H 0.8082 0.2887 0.1167 0.023 Uiso 1 1 calc R . . C10 C 0.72913(14) 0.34737(9) 0.19632(10) 0.0208(2) Uani 1 1 d . . . H10A H 0.7325 0.4020 0.1773 0.025 Uiso 1 1 calc R . . C11 C 0.67815(14) 0.33185(10) 0.26111(9) 0.0199(2) Uani 1 1 d . . . H11A H 0.6477 0.3758 0.2867 0.024 Uiso 1 1 calc R . . C12 C 0.67396(15) 0.24937(10) 0.28642(9) 0.0210(2) Uani 1 1 d . . . H12A H 0.6375 0.2390 0.3287 0.025 Uiso 1 1 calc R . . Fe2 Fe 1.0000 0.0000 0.5000 0.01041(5) Uani 1 2 d S . . S2 S 1.16882(3) 0.06892(2) 0.270568(19) 0.01554(6) Uani 1 1 d . . . N8 N 0.87050(10) -0.09814(7) 0.42801(6) 0.01225(16) Uani 1 1 d . . . N9 N 0.81192(10) 0.05910(7) 0.46015(7) 0.01321(16) Uani 1 1 d . . . N10 N 1.05248(12) 0.03962(7) 0.39575(7) 0.01650(18) Uani 1 1 d . . . N11 N 0.75968(10) 0.13260(7) 0.47859(7) 0.01331(16) Uani 1 1 d . . . N12 N 0.41577(10) 0.16065(7) 0.45627(7) 0.01480(17) Uani 1 1 d . . . N13 N 0.59985(10) 0.04745(7) 0.41631(7) 0.01292(16) Uani 1 1 d . . . N14 N 0.47482(11) 0.01356(8) 0.37872(8) 0.01778(19) Uani 1 1 d . . . H1N H 0.711(4) 0.020(3) 0.238(3) 0.081(13) Uiso 1 1 d . . . H2N H 0.828(3) 0.036(2) 0.2874(19) 0.042(7) Uiso 1 1 d . . . C14 C 0.90857(12) -0.17454(8) 0.41065(7) 0.01399(18) Uani 1 1 d . . . H14A H 0.9965 -0.1886 0.4296 0.017 Uiso 1 1 calc R . . C15 C 0.82230(13) -0.23392(8) 0.36542(8) 0.0166(2) Uani 1 1 d . . . H15A H 0.8515 -0.2868 0.3548 0.020 Uiso 1 1 calc R . . C16 C 0.69121(13) -0.21210(9) 0.33657(8) 0.0179(2) Uani 1 1 d . . . H16A H 0.6313 -0.2504 0.3061 0.021 Uiso 1 1 calc R . . C17 C 0.65009(12) -0.13274(8) 0.35354(8) 0.0162(2) Uani 1 1 d . . . H17A H 0.5630 -0.1169 0.3344 0.019 Uiso 1 1 calc R . . C18 C 0.74246(12) -0.07776(7) 0.39986(7) 0.01278(18) Uani 1 1 d . . . C19 C 0.71533(12) 0.00763(7) 0.42368(8) 0.01250(18) Uani 1 1 d . . . C20 C 0.63115(11) 0.12470(7) 0.45161(7) 0.01262(18) Uani 1 1 d . . . C21 C 0.53712(11) 0.18864(8) 0.46139(7) 0.01316(18) Uani 1 1 d . . . C22 C 0.57560(13) 0.27241(8) 0.47654(9) 0.0172(2) Uani 1 1 d . . . H22A H 0.6600 0.2894 0.4790 0.021 Uiso 1 1 calc R . . C23 C 0.48371(13) 0.32987(9) 0.48788(9) 0.0190(2) Uani 1 1 d . . . H23A H 0.5060 0.3862 0.4988 0.023 Uiso 1 1 calc R . . C24 C 0.35774(13) 0.30186(9) 0.48268(8) 0.0182(2) Uani 1 1 d . . . H24A H 0.2947 0.3390 0.4901 0.022 Uiso 1 1 calc R . . C25 C 0.32853(12) 0.21737(9) 0.46627(8) 0.0167(2) Uani 1 1 d . . . H25A H 0.2440 0.1991 0.4620 0.020 Uiso 1 1 calc R . . C26 C 1.10193(12) 0.05214(8) 0.34380(8) 0.01388(18) Uani 1 1 d . . . H3N H 0.417(2) 0.0426(17) 0.3988(16) 0.030(6) Uiso 1 1 d . . . H4N H 0.463(3) 0.0171(19) 0.3291(19) 0.042(8) Uiso 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 N1 0.0188(4) 0.0114(4) 0.0147(4) -0.0006(3) 0.0036(3) -0.0028(3) N2 0.0267(5) 0.0113(4) 0.0154(4) 0.0014(3) 0.0091(4) -0.0023(4) N4 0.0269(5) 0.0119(4) 0.0173(5) 0.0010(4) 0.0105(4) -0.0016(4) N5 0.0230(5) 0.0185(5) 0.0168(5) 0.0015(4) 0.0091(4) -0.0006(4) N6 0.0169(4) 0.0144(4) 0.0164(4) 0.0037(3) 0.0073(3) -0.0008(3) N7 0.0307(6) 0.0237(6) 0.0276(6) 0.0116(5) 0.0188(5) 0.0042(5) C1 0.0188(5) 0.0126(5) 0.0179(5) -0.0009(4) 0.0031(4) -0.0012(4) C2 0.0176(5) 0.0133(5) 0.0217(6) 0.0032(4) 0.0016(4) -0.0009(4) C3 0.0196(5) 0.0161(5) 0.0233(6) 0.0075(5) 0.0048(4) -0.0004(4) C4 0.0188(5) 0.0164(5) 0.0199(5) 0.0067(4) 0.0060(4) -0.0001(4) C5 0.0149(4) 0.0122(4) 0.0149(5) 0.0024(4) 0.0028(4) -0.0021(4) C6 0.0159(4) 0.0124(4) 0.0133(5) 0.0023(3) 0.0036(4) -0.0023(3) C7 0.0148(4) 0.0135(4) 0.0135(5) 0.0017(4) 0.0033(4) -0.0014(4) C8 0.0138(4) 0.0149(5) 0.0154(5) 0.0020(4) 0.0038(4) -0.0006(4) C9 0.0191(5) 0.0165(5) 0.0229(6) 0.0069(4) 0.0094(4) 0.0045(4) C10 0.0216(5) 0.0167(5) 0.0260(6) 0.0054(5) 0.0099(5) 0.0058(4) C11 0.0201(5) 0.0202(6) 0.0191(5) 0.0017(4) 0.0051(4) 0.0062(4) C12 0.0252(6) 0.0214(6) 0.0181(5) 0.0019(5) 0.0090(5) 0.0026(5) Fe2 0.01237(9) 0.00905(9) 0.01045(10) -0.00014(7) 0.00426(7) 0.00059(7) S2 0.01653(12) 0.01739(13) 0.01356(12) 0.00194(10) 0.00562(9) -0.00115(10) N8 0.0150(4) 0.0101(4) 0.0122(4) -0.0003(3) 0.0049(3) 0.0012(3) N9 0.0144(4) 0.0102(4) 0.0152(4) -0.0017(3) 0.0044(3) 0.0010(3) N10 0.0212(4) 0.0146(4) 0.0146(4) 0.0002(3) 0.0066(4) -0.0003(4) N11 0.0137(4) 0.0106(4) 0.0157(4) -0.0014(3) 0.0043(3) 0.0016(3) N12 0.0140(4) 0.0150(4) 0.0155(4) 0.0012(3) 0.0043(3) 0.0018(3) N13 0.0131(4) 0.0108(4) 0.0142(4) -0.0017(3) 0.0028(3) 0.0004(3) N14 0.0133(4) 0.0160(5) 0.0216(5) -0.0040(4) 0.0010(4) -0.0005(3) C14 0.0184(5) 0.0102(4) 0.0148(5) -0.0007(4) 0.0070(4) 0.0014(4) C15 0.0225(5) 0.0117(4) 0.0171(5) -0.0023(4) 0.0079(4) 0.0003(4) C16 0.0211(5) 0.0139(5) 0.0179(5) -0.0043(4) 0.0044(4) -0.0010(4) C17 0.0171(5) 0.0137(5) 0.0166(5) -0.0027(4) 0.0026(4) 0.0004(4) C18 0.0159(4) 0.0105(4) 0.0122(4) -0.0006(3) 0.0043(3) 0.0011(3) C19 0.0141(4) 0.0098(4) 0.0133(4) -0.0006(3) 0.0034(3) 0.0010(3) C20 0.0139(4) 0.0104(4) 0.0137(4) -0.0010(3) 0.0041(3) 0.0009(3) C21 0.0144(4) 0.0126(4) 0.0130(4) 0.0000(4) 0.0047(3) 0.0024(3) C22 0.0172(5) 0.0132(5) 0.0228(6) -0.0035(4) 0.0081(4) 0.0010(4) C23 0.0202(5) 0.0145(5) 0.0232(6) -0.0031(4) 0.0075(4) 0.0035(4) C24 0.0183(5) 0.0176(5) 0.0194(5) -0.0014(4) 0.0066(4) 0.0056(4) C25 0.0150(4) 0.0183(5) 0.0172(5) 0.0018(4) 0.0054(4) 0.0038(4) C26 0.0167(4) 0.0108(4) 0.0135(5) -0.0006(3) 0.0032(4) -0.0013(3) _geom_special_details ; Irrational bond distances and bond angles are due to the fact that atoms Fe3, S3, S4, C27, C28, N15 and N16 are corresponding to a NCS linkage isomer which is disordered over the inversion center site. ; 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 1.962(2) 3_755 ? Fe1 N3 1.962(2) . ? Fe1 N2 2.0758(12) 3_755 ? Fe1 N2 2.0758(12) . ? Fe1 N1 2.0893(11) 3_755 ? Fe1 N1 2.0893(11) . ? N3 C13 1.1717 . ? C13 S1 1.6502 . ? Fe3 N16 2.020(3) . ? Fe3 N2 2.0793(12) . ? Fe3 N1 2.1274(12) 3_755 ? Fe3 N1 2.1414(12) . ? Fe3 N2 2.1622(13) 3_755 ? Fe3 S3 3.3438(10) . ? S3 C27 1.643(4) . ? C27 N15 1.177(5) . ? S4 C28 1.635(4) . ? C28 N16 1.167(4) . ? N1 C1 1.3341(17) . ? N1 C5 1.3538(17) . ? N2 C6 1.3220(16) . ? N2 N4 1.3687(16) . ? N4 C7 1.3241(16) . ? N5 C8 1.3417(17) . ? N5 C12 1.3418(19) . ? N6 C6 1.3540(17) . ? N6 C7 1.3694(17) . ? N6 N7 1.4139(16) . ? N7 H1N 0.78(4) . ? N7 H2N 0.91(3) . ? C1 C2 1.3922(19) . ? C1 H1A 0.9300 . ? C2 C3 1.386(2) . ? C2 H2A 0.9300 . ? C3 C4 1.390(2) . ? C3 H3A 0.9300 . ? C4 C5 1.3887(18) . ? C4 H4B 0.9300 . ? C5 C6 1.4585(18) . ? C7 C8 1.4670(18) . ? C8 C9 1.3924(18) . ? C9 C10 1.385(2) . ? C9 H9A 0.9300 . ? C10 C11 1.392(2) . ? C10 H10A 0.9300 . ? C11 C12 1.383(2) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? Fe2 N10 2.1177(11) . ? Fe2 N10 2.1177(11) 3_756 ? Fe2 N9 2.1464(10) 3_756 ? Fe2 N9 2.1464(10) . ? Fe2 N8 2.2154(11) . ? Fe2 N8 2.2154(11) 3_756 ? S2 C26 1.6339(13) . ? N8 C14 1.3381(15) . ? N8 C18 1.3548(16) . ? N9 C19 1.3268(16) . ? N9 N11 1.3673(14) . ? N10 C26 1.1748(16) . ? N11 C20 1.3252(15) . ? N12 C25 1.3398(16) . ? N12 C21 1.3482(16) . ? N13 C19 1.3588(15) . ? N13 C20 1.3666(16) . ? N13 N14 1.4157(15) . ? N14 H3N 0.91(3) . ? N14 H4N 0.83(3) . ? C14 C15 1.3924(18) . ? C14 H14A 0.9300 . ? C15 C16 1.3908(19) . ? C15 H15A 0.9300 . ? C16 C17 1.3906(19) . ? C16 H16A 0.9300 . ? C17 C18 1.3882(18) . ? C17 H17A 0.9300 . ? C18 C19 1.4671(17) . ? C20 C21 1.4692(16) . ? C21 C22 1.3935(18) . ? C22 C23 1.3918(18) . ? C22 H22A 0.9300 . ? C23 C24 1.395(2) . ? C23 H23A 0.9300 . ? C24 C25 1.387(2) . ? 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(3) 3_755 . ? N3 Fe1 N2 89.52(16) 3_755 3_755 ? N3 Fe1 N2 90.48(16) . 3_755 ? N3 Fe1 N2 90.48(16) 3_755 . ? N3 Fe1 N2 89.52(16) . . ? N2 Fe1 N2 180.00(8) 3_755 . ? N3 Fe1 N1 89.73(16) 3_755 3_755 ? N3 Fe1 N1 90.27(16) . 3_755 ? N2 Fe1 N1 78.23(4) 3_755 3_755 ? N2 Fe1 N1 101.77(4) . 3_755 ? N3 Fe1 N1 90.27(16) 3_755 . ? N3 Fe1 N1 89.73(16) . . ? N2 Fe1 N1 101.77(4) 3_755 . ? N2 Fe1 N1 78.23(4) . . ? N1 Fe1 N1 180.00(6) 3_755 . ? C13 N3 Fe1 176.3(3) . . ? N3 C13 S1 177.8 . . ? N16 Fe3 N2 99.67(9) . . ? N16 Fe3 N1 102.22(9) . 3_755 ? N2 Fe3 N1 100.38(5) . 3_755 ? N16 Fe3 N1 101.33(9) . . ? N2 Fe3 N1 76.99(5) . . ? N1 Fe3 N1 156.40(3) 3_755 . ? N16 Fe3 N2 103.97(9) . 3_755 ? N2 Fe3 N2 156.35(3) . 3_755 ? N1 Fe3 N2 75.55(4) 3_755 3_755 ? N1 Fe3 N2 97.34(5) . 3_755 ? N16 Fe3 S3 163.78(8) . . ? N2 Fe3 S3 96.14(4) . . ? N1 Fe3 S3 78.31(4) 3_755 . ? N1 Fe3 S3 78.68(4) . . ? N2 Fe3 S3 60.22(4) 3_755 . ? C27 S3 Fe3 140.30(12) . . ? N15 C27 S3 177.2(3) . . ? N16 C28 S4 174.0(3) . . ? C28 N16 Fe3 174.5(3) . . ? C1 N1 C5 118.61(11) . . ? C1 N1 Fe1 125.14(9) . . ? C5 N1 Fe1 116.24(9) . . ? C1 N1 Fe3 126.18(9) . . ? C5 N1 Fe3 113.62(9) . . ? Fe1 N1 Fe3 11.759(16) . . ? C6 N2 N4 108.59(11) . . ? C6 N2 Fe1 113.15(9) . . ? N4 N2 Fe1 137.86(9) . . ? C6 N2 Fe3 111.78(9) . . ? N4 N2 Fe3 135.59(9) . . ? Fe1 N2 Fe3 12.059(16) . . ? C7 N4 N2 106.77(10) . . ? C8 N5 C12 116.86(12) . . ? C6 N6 C7 105.81(10) . . ? C6 N6 N7 123.91(11) . . ? C7 N6 N7 130.27(12) . . ? N6 N7 H1N 111(3) . . ? N6 N7 H2N 102.0(19) . . ? H1N N7 H2N 103(4) . . ? N1 C1 C2 122.38(13) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C3 C2 C1 118.66(13) . . ? C3 C2 H2A 120.7 . . ? C1 C2 H2A 120.7 . . ? C2 C3 C4 119.70(12) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 117.98(13) . . ? C5 C4 H4B 121.0 . . ? C3 C4 H4B 121.0 . . ? N1 C5 C4 122.66(12) . . ? N1 C5 C6 111.75(11) . . ? C4 C5 C6 125.58(12) . . ? N2 C6 N6 109.14(11) . . ? N2 C6 C5 120.14(12) . . ? N6 C6 C5 130.72(11) . . ? N4 C7 N6 109.68(11) . . ? N4 C7 C8 123.72(11) . . ? N6 C7 C8 126.57(11) . . ? N5 C8 C9 123.56(12) . . ? N5 C8 C7 117.63(11) . . ? C9 C8 C7 118.80(11) . . ? C10 C9 C8 118.37(12) . . ? C10 C9 H9A 120.8 . . ? C8 C9 H9A 120.8 . . ? C9 C10 C11 118.98(13) . . ? C9 C10 H10A 120.5 . . ? C11 C10 H10A 120.5 . . ? C12 C11 C10 118.26(13) . . ? C12 C11 H11A 120.9 . . ? C10 C11 H11A 120.9 . . ? N5 C12 C11 123.94(13) . . ? N5 C12 H12A 118.0 . . ? C11 C12 H12A 118.0 . . ? N10 Fe2 N10 180.0 . 3_756 ? N10 Fe2 N9 87.40(4) . 3_756 ? N10 Fe2 N9 92.60(4) 3_756 3_756 ? N10 Fe2 N9 92.60(4) . . ? N10 Fe2 N9 87.40(4) 3_756 . ? N9 Fe2 N9 180.0 3_756 . ? N10 Fe2 N8 90.39(4) . . ? N10 Fe2 N8 89.61(4) 3_756 . ? N9 Fe2 N8 104.65(4) 3_756 . ? N9 Fe2 N8 75.35(4) . . ? N10 Fe2 N8 89.61(4) . 3_756 ? N10 Fe2 N8 90.39(4) 3_756 3_756 ? N9 Fe2 N8 75.35(4) 3_756 3_756 ? N9 Fe2 N8 104.65(4) . 3_756 ? N8 Fe2 N8 180.00(5) . 3_756 ? C14 N8 C18 118.37(11) . . ? C14 N8 Fe2 125.46(8) . . ? C18 N8 Fe2 116.17(8) . . ? C19 N9 N11 108.73(10) . . ? C19 N9 Fe2 114.55(8) . . ? N11 N9 Fe2 134.74(8) . . ? C26 N10 Fe2 167.30(11) . . ? C20 N11 N9 106.70(10) . . ? C25 N12 C21 117.37(11) . . ? C19 N13 C20 105.83(10) . . ? C19 N13 N14 125.47(10) . . ? C20 N13 N14 128.70(10) . . ? N13 N14 H3N 106.5(16) . . ? N13 N14 H4N 107(2) . . ? H3N N14 H4N 116(3) . . ? N8 C14 C15 122.86(12) . . ? N8 C14 H14A 118.6 . . ? C15 C14 H14A 118.6 . . ? C16 C15 C14 118.21(12) . . ? C16 C15 H15A 120.9 . . ? C14 C15 H15A 120.9 . . ? C15 C16 C17 119.69(12) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C18 C17 C16 118.29(12) . . ? C18 C17 H17A 120.9 . . ? C16 C17 H17A 120.9 . . ? N8 C18 C17 122.57(11) . . ? N8 C18 C19 112.24(10) . . ? C17 C18 C19 125.18(11) . . ? N9 C19 N13 108.80(10) . . ? N9 C19 C18 120.81(10) . . ? N13 C19 C18 130.38(11) . . ? N11 C20 N13 109.92(10) . . ? N11 C20 C21 124.60(11) . . ? N13 C20 C21 125.44(11) . . ? N12 C21 C22 123.61(11) . . ? N12 C21 C20 116.07(11) . . ? C22 C21 C20 120.31(11) . . ? C23 C22 C21 117.92(12) . . ? C23 C22 H22A 121.0 . . ? C21 C22 H22A 121.0 . . ? C22 C23 C24 119.12(13) . . ? C22 C23 H23A 120.4 . . ? C24 C23 H23A 120.4 . . ? C25 C24 C23 118.59(12) . . ? C25 C24 H24A 120.7 . . ? C23 C24 H24A 120.7 . . ? N12 C25 C24 123.38(12) . . ? N12 C25 H25A 118.3 . . ? C24 C25 H25A 118.3 . . ? N10 C26 S2 179.14(13) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 24.41 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.490 _refine_diff_density_min -0.754 _refine_diff_density_rms 0.100