data_06jn59lm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H4 Fe N3 O2 S2' _chemical_formula_weight 282.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'N' 'N' 0.0061 0.0033 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3947(15) _cell_length_b 8.2739(16) _cell_length_c 9.1533(18) _cell_angle_alpha 69.300(2) _cell_angle_beta 68.851(2) _cell_angle_gamma 78.218(3) _cell_volume 486.70(17) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 2950 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description lamellar _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.925 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 282 _exptl_absorpt_coefficient_mu 1.956 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.73357 _exptl_absorpt_correction_T_max 0.95588 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5738 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 28.33 _reflns_number_total 2417 _reflns_number_gt 2113 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment contr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2417 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 0.36026(4) 1.73594(4) -1.01309(3) 0.01462(10) Uani 1 1 d . . . S1 S 0.27625(8) 1.40328(7) -0.52001(6) 0.01824(12) Uani 1 1 d . . . S2 S 0.53613(7) 1.61303(6) -0.83358(6) 0.01659(12) Uani 1 1 d . . . O2 O 0.2059(2) 2.07370(19) -0.99777(18) 0.0258(4) Uani 1 1 d . . . O1 O 0.0228(2) 1.5528(2) -0.8557(2) 0.0331(4) Uani 1 1 d . . . N3 N 0.4625(2) 1.2770(2) -0.75976(19) 0.0143(3) Uani 1 1 d . . . N2 N 0.2987(2) 1.9456(2) -1.0182(2) 0.0177(4) Uani 1 1 d . . . N1 N 0.1676(2) 1.6174(2) -0.9322(2) 0.0185(4) Uani 1 1 d . . . C1 C 0.4323(3) 1.4195(3) -0.7169(2) 0.0152(4) Uani 1 1 d . . . C2 C 0.2456(3) 1.1907(3) -0.4892(2) 0.0154(4) Uani 1 1 d . . . C3 C 0.3568(3) 1.1440(2) -0.6305(2) 0.0140(4) Uani 1 1 d . . . C4 C 0.3544(3) 0.9765(3) -0.6322(2) 0.0165(4) Uani 1 1 d . . . C5 C 0.2434(3) 0.8615(3) -0.4929(2) 0.0187(4) Uani 1 1 d . . . C6 C 0.1331(3) 0.9102(3) -0.3533(2) 0.0192(4) Uani 1 1 d . . . C7 C 0.1334(3) 1.0751(3) -0.3495(2) 0.0189(4) Uani 1 1 d . . . H6A H 0.0612 0.8303 -0.2603 0.080 Uiso 1 1 d . . . H4A H 0.4282 0.9475 -0.7195 0.080 Uiso 1 1 d . . . H5A H 0.2458 0.7547 -0.4985 0.080 Uiso 1 1 d . . . H7A H 0.0562 1.1086 -0.2506 0.080 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 0.01596(16) 0.01293(16) 0.01382(16) -0.00481(11) -0.00259(11) -0.00145(11) S1 0.0223(3) 0.0152(3) 0.0155(2) -0.0071(2) -0.0015(2) -0.0020(2) S2 0.0205(3) 0.0136(2) 0.0164(2) -0.00419(19) -0.0058(2) -0.00389(19) O2 0.0284(9) 0.0153(8) 0.0259(8) -0.0082(6) 0.0011(7) -0.0002(6) O1 0.0243(9) 0.0386(11) 0.0345(9) -0.0089(8) -0.0031(7) -0.0143(8) N3 0.0158(8) 0.0126(8) 0.0137(8) -0.0025(6) -0.0049(6) -0.0024(6) N2 0.0190(9) 0.0159(9) 0.0158(8) -0.0045(7) -0.0028(7) -0.0022(7) N1 0.0179(9) 0.0182(9) 0.0181(8) -0.0058(7) -0.0043(7) -0.0010(7) C1 0.0146(9) 0.0177(10) 0.0135(9) -0.0046(8) -0.0050(7) -0.0013(7) C2 0.0157(9) 0.0135(9) 0.0173(10) -0.0053(8) -0.0057(8) 0.0003(7) C3 0.0128(9) 0.0142(9) 0.0145(9) -0.0031(7) -0.0053(7) -0.0008(7) C4 0.0165(9) 0.0169(10) 0.0170(9) -0.0073(8) -0.0045(8) -0.0009(8) C5 0.0187(10) 0.0158(10) 0.0223(10) -0.0041(8) -0.0084(8) -0.0029(8) C6 0.0177(10) 0.0175(10) 0.0193(10) -0.0014(8) -0.0054(8) -0.0035(8) C7 0.0170(10) 0.0209(11) 0.0161(10) -0.0039(8) -0.0034(8) -0.0021(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.6840(18) . ? Fe1 N2 1.6897(18) . ? Fe1 N3 2.0459(17) 2_683 ? Fe1 S2 2.2904(6) . ? S1 C1 1.729(2) . ? S1 C2 1.729(2) . ? S2 C1 1.731(2) . ? O2 N2 1.174(2) . ? O1 N1 1.162(2) . ? N3 C1 1.324(3) . ? N3 C3 1.409(2) . ? N3 Fe1 2.0459(17) 2_683 ? C2 C7 1.390(3) . ? C2 C3 1.398(3) . ? C3 C4 1.395(3) . ? C4 C5 1.382(3) . ? C4 H4A 0.8730 . ? C5 C6 1.392(3) . ? C5 H5A 0.8990 . ? C6 C7 1.377(3) . ? C6 H6A 0.9290 . ? C7 H7A 0.9812 . ? 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 N1 Fe1 N2 113.35(8) . . ? N1 Fe1 N3 114.39(8) . 2_683 ? N2 Fe1 N3 109.67(7) . 2_683 ? N1 Fe1 S2 104.05(6) . . ? N2 Fe1 S2 107.22(6) . . ? N3 Fe1 S2 107.60(5) 2_683 . ? C1 S1 C2 90.53(10) . . ? C1 S2 Fe1 102.40(7) . . ? C1 N3 C3 110.78(16) . . ? C1 N3 Fe1 122.20(14) . 2_683 ? C3 N3 Fe1 127.02(13) . 2_683 ? O2 N2 Fe1 161.21(16) . . ? O1 N1 Fe1 167.37(17) . . ? N3 C1 S1 114.79(15) . . ? N3 C1 S2 127.08(15) . . ? S1 C1 S2 118.11(12) . . ? C7 C2 C3 122.09(19) . . ? C7 C2 S1 128.44(16) . . ? C3 C2 S1 109.47(15) . . ? C4 C3 C2 119.10(18) . . ? C4 C3 N3 126.47(18) . . ? C2 C3 N3 114.43(18) . . ? C5 C4 C3 118.74(18) . . ? C5 C4 H4A 122.9 . . ? C3 C4 H4A 118.3 . . ? C4 C5 C6 121.43(19) . . ? C4 C5 H5A 116.2 . . ? C6 C5 H5A 122.4 . . ? C7 C6 C5 120.63(19) . . ? C7 C6 H6A 119.3 . . ? C5 C6 H6A 120.1 . . ? C6 C7 C2 118.00(19) . . ? C6 C7 H7A 120.4 . . ? C2 C7 H7A 121.6 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.573 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.089