# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1389 data_Feazpy2NCS2MeOH2 #------------------------------------------------------------------------------ _audit_creation_date 'Mon Oct 19 18:31:07 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 602.47 _chemical_formula_analytical ? _chemical_formula_sum 'C24 H22 Fe N10 O2 S2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 7.232(4) _cell_length_b 16.960(3) _cell_length_c 11.950(3) _cell_angle_alpha 90 _cell_angle_beta 94.65(3) _cell_angle_gamma 90 _cell_volume 1460.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 288.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 6.0 _cell_measurement_theta_max 51.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 620.00 _exptl_absorpt_coefficient_mu 0.698 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_ambient_temperature 288.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXISIV' _diffrn_reflns_number 2004 _reflns_number_total 2004 _reflns_number_observed 1168 _reflns_observed_criterion >2.5sigma(I) _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI 0.193 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 6.00 _diffrn_reflns_theta_max 51.4 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe 0 2 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 4 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 48 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 20 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 4 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 44 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Fe1 0.0000 0.5000 0.0000 0.0339(5) Uani d . 0.50 S S1 -0.3680(5) 0.7286(2) 0.0920(3) 0.095(1) Uani d . 1.00 . O1 0.1626(8) 0.5871(3) -0.0773(4) 0.042(2) Uani d . 1.00 . N1 0.1919(9) 0.5060(4) 0.1542(4) 0.038(2) Uani d . 1.00 . N2 0.508(1) 0.5278(4) 0.4678(4) 0.040(2) Uani d . 1.00 . N3 -0.082(1) 0.2416(5) 0.5753(8) 0.069(3) Uani d . 1.00 . N4 0.040(1) 0.4834(4) 0.5409(5) 0.048(3) Uani d . 1.00 . N5 -0.156(1) 0.5963(4) 0.0552(5) 0.049(3) Uani d . 1.00 . C1 0.278(1) 0.5721(5) 0.1909(6) 0.039(3) Uani d . 1.00 . C2 0.386(1) 0.5808(5) 0.2915(6) 0.044(3) Uani d . 1.00 . C3 0.405(1) 0.5155(5) 0.3609(6) 0.036(3) Uani d . 1.00 . C4 0.319(1) 0.4451(5) 0.3262(6) 0.035(2) Uani d . 1.00 . C5 0.218(1) 0.4436(5) 0.2240(6) 0.038(3) Uani d . 1.00 . C6 -0.149(2) 0.2802(6) 0.4836(9) 0.078(4) Uani d . 1.00 . C7 -0.113(1) 0.3599(6) 0.4653(8) 0.067(4) Uani d . 1.00 . C8 -0.004(1) 0.3992(5) 0.5466(7) 0.048(3) Uani d . 1.00 . C9 0.071(1) 0.3596(6) 0.6405(7) 0.065(4) Uani d . 1.00 . C10 0.027(2) 0.2800(6) 0.6510(8) 0.072(4) Uani d . 1.00 . C11 -0.246(1) 0.6515(5) 0.0685(7) 0.045(3) Uani d . 1.00 . C12 0.329(2) 0.5778(6) -0.1274(9) 0.084(4) Uani d . 1.00 . H1 0.2639 0.6187 0.1432 0.0476 Uiso calc . 1.00 . H2 0.4472 0.6304 0.3130 0.0509 Uiso calc . 1.00 . H3 0.3308 0.3982 0.3725 0.0413 Uiso calc . 1.00 . H4 0.1616 0.3937 0.1989 0.0439 Uiso calc . 1.00 . H5 -0.2263 0.2527 0.4236 0.0829 Uiso calc . 1.00 . H6 -0.1611 0.3876 0.3955 0.0744 Uiso calc . 1.00 . H7 0.1548 0.3857 0.6987 0.0765 Uiso calc . 1.00 . H8 0.0710 0.2500 0.7206 0.0877 Uiso calc . 1.00 . H9 0.3748 0.6268 -0.1555 0.0871 Uiso calc . 1.00 . H10 0.4268 0.5562 -0.0765 0.0871 Uiso calc . 1.00 . H11 0.3152 0.5420 -0.1911 0.0871 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe(1) 0.040(1) 0.0289(9) 0.0315(8) 0.008(1) -0.0038(7) -0.0035(9) S(1) 0.070(2) 0.040(2) 0.177(3) 0.019(2) 0.024(2) -0.012(2) O(1) 0.041(4) 0.035(4) 0.053(3) 0.006(3) 0.015(3) -0.001(3) N(1) 0.048(4) 0.031(4) 0.033(3) 0.000(4) -0.006(3) -0.005(4) N(2) 0.043(5) 0.040(5) 0.038(4) -0.007(4) -0.001(4) -0.002(3) N(3) 0.068(7) 0.038(5) 0.103(6) 0.010(5) 0.016(5) -0.002(5) N(4) 0.051(5) 0.038(6) 0.054(5) -0.010(4) -0.002(4) -0.007(3) N(5) 0.060(6) 0.043(5) 0.044(4) 0.017(4) 0.009(4) 0.000(4) C(1) 0.056(6) 0.034(5) 0.023(4) -0.002(5) -0.018(4) 0.004(4) C(2) 0.051(6) 0.044(6) 0.032(4) -0.006(5) -0.023(4) 0.002(4) C(3) 0.036(5) 0.043(6) 0.028(4) 0.005(4) -0.003(3) -0.001(4) C(4) 0.039(5) 0.038(5) 0.024(4) 0.007(4) -0.020(4) 0.008(4) C(5) 0.045(6) 0.035(5) 0.032(4) 0.000(4) -0.016(4) -0.011(4) C(6) 0.082(9) 0.036(6) 0.113(9) -0.011(6) -0.004(7) -0.035(6) C(7) 0.068(8) 0.049(7) 0.082(7) 0.004(6) -0.013(6) 0.003(6) C(8) 0.038(6) 0.045(6) 0.060(6) -0.015(5) 0.002(5) -0.018(5) C(9) 0.072(9) 0.056(7) 0.065(7) 0.004(6) -0.008(6) -0.007(6) C(10) 0.083(9) 0.045(7) 0.084(8) -0.001(6) -0.012(7) -0.001(6) C(11) 0.048(6) 0.027(5) 0.061(5) 0.008(5) 0.011(5) -0.009(4) C(12) 0.087(10) 0.039(7) 0.135(10) 0.002(6) 0.054(8) 0.004(7) #------------------------------------------------------------------------------ _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian' _refine_ls_extinction_coef 0.0044(9) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1168 _refine_ls_number_parameters 179 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0634 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0638 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.423 _refine_ls_shift/esd_max 0.0430 _refine_ls_shift/esd_mean 0.0040 _refine_diff_density_min -0.38 _refine_diff_density_max 0.35 #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe(1) O(1) 2.143(6) 1_555 1_555 yes Fe(1) O(1) 2.143(6) 1_555 3_565 yes Fe(1) N(1) 2.217(5) 1_555 1_555 yes Fe(1) N(1) 2.217(5) 1_555 3_565 yes Fe(1) N(5) 2.121(7) 1_555 1_555 yes Fe(1) N(5) 2.121(7) 1_555 3_565 yes S(1) C(11) 1.616(9) 1_555 1_555 yes O(1) C(12) 1.39(1) 1_555 1_555 yes N(1) C(1) 1.338(9) 1_555 1_555 yes N(1) C(2) 2.430(9) 1_555 1_555 yes N(1) C(4) 2.414(9) 1_555 1_555 yes N(1) C(5) 1.352(9) 1_555 1_555 yes N(2) N(2) 1.23(1) 1_555 3_666 yes N(2) C(2) 2.392(9) 1_555 1_555 yes N(2) C(3) 1.441(9) 1_555 1_555 yes N(2) C(3) 2.218(9) 1_555 3_666 yes N(3) C(6) 1.33(1) 1_555 1_555 yes N(3) C(7) 2.40(1) 1_555 1_555 yes N(3) C(9) 2.39(1) 1_555 1_555 yes N(3) C(10) 1.32(1) 1_555 1_555 yes N(4) N(4) 1.23(1) 1_555 3_566 yes N(4) C(8) 1.47(1) 1_555 1_555 yes N(4) C(8) 2.25(1) 1_555 3_566 yes N(4) C(9) 2.41(1) 1_555 1_555 yes N(5) C(11) 1.156(10) 1_555 1_555 yes C(1) C(2) 1.389(9) 1_555 1_555 yes C(1) C(3) 2.365(9) 1_555 1_555 yes C(1) C(5) 2.26(1) 1_555 1_555 yes C(2) C(3) 1.38(1) 1_555 1_555 yes C(2) C(4) 2.40(1) 1_555 1_555 yes C(3) C(4) 1.39(1) 1_555 1_555 yes C(3) C(5) 2.37(1) 1_555 1_555 yes C(4) C(5) 1.369(9) 1_555 1_555 yes C(6) C(7) 1.40(1) 1_555 1_555 yes C(6) C(8) 2.37(1) 1_555 1_555 yes C(6) C(10) 2.28(1) 1_555 1_555 yes C(7) C(8) 1.37(1) 1_555 1_555 yes C(7) C(9) 2.39(1) 1_555 1_555 yes C(8) C(9) 1.38(1) 1_555 1_555 yes C(8) C(10) 2.38(1) 1_555 1_555 yes C(9) C(10) 1.40(1) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Fe(1) O(1) 180.0 1_555 1_555 3_565 yes O(1) Fe(1) N(1) 89.9(2) 1_555 1_555 1_555 yes O(1) Fe(1) N(1) 90.1(2) 1_555 1_555 3_565 yes O(1) Fe(1) N(5) 85.9(2) 1_555 1_555 1_555 yes O(1) Fe(1) N(5) 94.1(2) 1_555 1_555 3_565 yes O(1) Fe(1) N(1) 90.1(2) 3_565 1_555 1_555 yes O(1) Fe(1) N(1) 89.9(2) 3_565 1_555 3_565 yes O(1) Fe(1) N(5) 94.1(2) 3_565 1_555 1_555 yes O(1) Fe(1) N(5) 85.9(2) 3_565 1_555 3_565 yes N(1) Fe(1) N(1) 180.0 1_555 1_555 3_565 yes N(1) Fe(1) N(5) 91.1(3) 1_555 1_555 1_555 yes N(1) Fe(1) N(5) 88.9(3) 1_555 1_555 3_565 yes N(1) Fe(1) N(5) 88.9(3) 3_565 1_555 1_555 yes N(1) Fe(1) N(5) 91.1(3) 3_565 1_555 3_565 yes N(5) Fe(1) N(5) 180.0 1_555 1_555 3_565 yes Fe(1) O(1) C(12) 129.0(5) 1_555 1_555 1_555 yes Fe(1) O(1) H(9) 155.7(3) 1_555 1_555 1_555 no Fe(1) O(1) H(10) 112.2(2) 1_555 1_555 1_555 no Fe(1) O(1) H(11) 112.8(2) 1_555 1_555 1_555 no C(12) O(1) H(9) 26.7(4) 1_555 1_555 1_555 no C(12) O(1) H(10) 26.8(5) 1_555 1_555 1_555 no C(12) O(1) H(11) 27.2(5) 1_555 1_555 1_555 no H(9) O(1) H(10) 46.1(1) 1_555 1_555 1_555 no H(9) O(1) H(11) 46.2(1) 1_555 1_555 1_555 no H(10) O(1) H(11) 46.2(1) 1_555 1_555 1_555 no Fe(1) N(1) C(1) 123.6(5) 1_555 1_555 1_555 yes Fe(1) N(1) C(2) 150.9(4) 1_555 1_555 1_555 yes Fe(1) N(1) C(4) 149.0(4) 1_555 1_555 1_555 yes Fe(1) N(1) C(5) 121.6(5) 1_555 1_555 1_555 yes Fe(1) N(1) H(1) 98.0(3) 1_555 1_555 1_555 no Fe(1) N(1) H(4) 95.9(3) 1_555 1_555 1_555 no C(1) N(1) C(2) 27.6(4) 1_555 1_555 1_555 yes C(1) N(1) C(4) 86.8(4) 1_555 1_555 1_555 yes C(1) N(1) C(5) 114.5(6) 1_555 1_555 1_555 yes C(1) N(1) H(1) 25.7(3) 1_555 1_555 1_555 no C(1) N(1) H(4) 140.4(5) 1_555 1_555 1_555 no C(2) N(1) C(4) 59.3(3) 1_555 1_555 1_555 yes C(2) N(1) C(5) 87.0(4) 1_555 1_555 1_555 yes C(2) N(1) H(1) 53.3(2) 1_555 1_555 1_555 no C(2) N(1) H(4) 112.8(3) 1_555 1_555 1_555 no C(4) N(1) C(5) 27.7(4) 1_555 1_555 1_555 yes C(4) N(1) H(1) 112.6(3) 1_555 1_555 1_555 no C(4) N(1) H(4) 53.6(2) 1_555 1_555 1_555 no C(5) N(1) H(1) 140.3(5) 1_555 1_555 1_555 no C(5) N(1) H(4) 25.9(3) 1_555 1_555 1_555 no H(1) N(1) H(4) 166.1(3) 1_555 1_555 1_555 no N(2) N(2) C(2) 142.7(7) 3_666 1_555 1_555 yes N(2) N(2) C(3) 112.2(8) 3_666 1_555 1_555 yes N(2) N(2) C(3) 37.0(5) 3_666 1_555 3_666 yes N(2) N(2) H(3) 88.1(5) 3_666 1_555 3_666 no C(2) N(2) C(3) 31.5(4) 1_555 1_555 1_555 yes C(2) N(2) C(3) 173.9(5) 1_555 1_555 3_666 yes C(2) N(2) H(3) 126.9(3) 1_555 1_555 3_666 no C(3) N(2) C(3) 149.2(4) 1_555 1_555 3_666 yes C(3) N(2) H(3) 158.1(5) 1_555 1_555 3_666 no C(3) N(2) H(3) 51.6(2) 3_666 1_555 3_666 no C(6) N(3) C(7) 29.2(5) 1_555 1_555 1_555 yes C(6) N(3) C(9) 89.1(6) 1_555 1_555 1_555 yes C(6) N(3) C(10) 118.5(9) 1_555 1_555 1_555 yes C(6) N(3) H(5) 24.9(4) 1_555 1_555 1_555 no C(6) N(3) H(8) 145.3(7) 1_555 1_555 1_555 no C(7) N(3) C(9) 59.9(4) 1_555 1_555 1_555 yes C(7) N(3) C(10) 89.3(6) 1_555 1_555 1_555 yes C(7) N(3) H(5) 54.0(3) 1_555 1_555 1_555 no C(7) N(3) H(8) 116.1(4) 1_555 1_555 1_555 no C(9) N(3) C(10) 29.4(5) 1_555 1_555 1_555 yes C(9) N(3) H(5) 113.9(4) 1_555 1_555 1_555 no C(9) N(3) H(8) 56.2(3) 1_555 1_555 1_555 no C(10) N(3) H(5) 143.3(7) 1_555 1_555 1_555 no C(10) N(3) H(8) 26.8(5) 1_555 1_555 1_555 no H(5) N(3) H(8) 170.1(5) 1_555 1_555 1_555 no N(4) N(4) C(8) 113.2(8) 3_566 1_555 1_555 yes N(4) N(4) C(8) 36.7(5) 3_566 1_555 3_566 yes N(4) N(4) C(9) 143.9(8) 3_566 1_555 1_555 yes N(4) N(4) H(6) 88.4(7) 3_566 1_555 3_566 no C(8) N(4) C(8) 149.9(4) 1_555 1_555 3_566 yes C(8) N(4) C(9) 30.9(4) 1_555 1_555 1_555 yes C(8) N(4) H(6) 158.0(5) 1_555 1_555 3_566 no C(8) N(4) C(9) 177.7(5) 3_566 1_555 1_555 yes C(8) N(4) H(6) 51.8(3) 3_566 1_555 3_566 no C(9) N(4) H(6) 127.3(3) 1_555 1_555 3_566 no Fe(1) N(5) C(11) 169.8(7) 1_555 1_555 1_555 yes N(1) C(1) C(2) 126.0(7) 1_555 1_555 1_555 yes N(1) C(1) C(3) 94.5(5) 1_555 1_555 1_555 yes N(1) C(1) C(5) 32.9(3) 1_555 1_555 1_555 yes N(1) C(1) H(1) 117.7(6) 1_555 1_555 1_555 no N(1) C(1) H(2) 149.4(5) 1_555 1_555 1_555 no C(2) C(1) C(3) 31.5(4) 1_555 1_555 1_555 yes C(2) C(1) C(5) 93.1(5) 1_555 1_555 1_555 yes C(2) C(1) H(1) 116.3(7) 1_555 1_555 1_555 no C(2) C(1) H(2) 23.4(4) 1_555 1_555 1_555 no C(3) C(1) C(5) 61.6(3) 1_555 1_555 1_555 yes C(3) C(1) H(1) 147.8(6) 1_555 1_555 1_555 no C(3) C(1) H(2) 54.8(2) 1_555 1_555 1_555 no C(5) C(1) H(1) 150.6(6) 1_555 1_555 1_555 no C(5) C(1) H(2) 116.4(4) 1_555 1_555 1_555 no H(1) C(1) H(2) 92.9(5) 1_555 1_555 1_555 no N(1) C(2) N(2) 123.3(4) 1_555 1_555 1_555 yes N(1) C(2) C(1) 26.5(4) 1_555 1_555 1_555 yes N(1) C(2) C(3) 90.5(5) 1_555 1_555 1_555 yes N(1) C(2) C(4) 60.0(3) 1_555 1_555 1_555 yes N(1) C(2) H(1) 52.1(2) 1_555 1_555 1_555 no N(1) C(2) H(2) 148.6(6) 1_555 1_555 1_555 no N(2) C(2) C(1) 149.7(6) 1_555 1_555 1_555 yes N(2) C(2) C(3) 32.9(4) 1_555 1_555 1_555 yes N(2) C(2) C(4) 63.3(3) 1_555 1_555 1_555 yes N(2) C(2) H(1) 174.8(5) 1_555 1_555 1_555 no N(2) C(2) H(2) 88.0(4) 1_555 1_555 1_555 no C(1) C(2) C(3) 117.0(7) 1_555 1_555 1_555 yes C(1) C(2) C(4) 86.5(5) 1_555 1_555 1_555 yes C(1) C(2) H(1) 25.6(4) 1_555 1_555 1_555 no C(1) C(2) H(2) 122.2(8) 1_555 1_555 1_555 no C(3) C(2) C(4) 30.5(4) 1_555 1_555 1_555 yes C(3) C(2) H(1) 142.6(6) 1_555 1_555 1_555 no C(3) C(2) H(2) 120.8(7) 1_555 1_555 1_555 no C(4) C(2) H(1) 112.1(4) 1_555 1_555 1_555 no C(4) C(2) H(2) 151.3(6) 1_555 1_555 1_555 no H(1) C(2) H(2) 96.5(5) 1_555 1_555 1_555 no N(2) C(3) N(2) 30.8(4) 1_555 1_555 3_666 yes N(2) C(3) C(1) 147.1(6) 1_555 1_555 1_555 yes N(2) C(3) C(2) 115.7(7) 1_555 1_555 1_555 yes N(2) C(3) C(4) 125.1(7) 1_555 1_555 1_555 yes N(2) C(3) C(5) 155.5(6) 1_555 1_555 1_555 yes N(2) C(3) H(2) 91.8(5) 1_555 1_555 1_555 no N(2) C(3) H(3) 101.4(5) 1_555 1_555 1_555 no N(2) C(3) C(1) 171.6(5) 3_666 1_555 1_555 yes N(2) C(3) C(2) 145.5(6) 3_666 1_555 1_555 yes N(2) C(3) C(4) 94.5(5) 3_666 1_555 1_555 yes N(2) C(3) C(5) 124.8(4) 3_666 1_555 1_555 yes N(2) C(3) H(2) 122.1(4) 3_666 1_555 1_555 no N(2) C(3) H(3) 71.1(3) 3_666 1_555 1_555 no C(1) C(3) C(2) 31.6(4) 1_555 1_555 1_555 yes C(1) C(3) C(4) 87.7(5) 1_555 1_555 1_555 yes C(1) C(3) C(5) 57.1(3) 1_555 1_555 1_555 yes C(1) C(3) H(2) 55.5(3) 1_555 1_555 1_555 no C(1) C(3) H(3) 111.3(4) 1_555 1_555 1_555 no C(2) C(3) C(4) 119.2(6) 1_555 1_555 1_555 yes C(2) C(3) C(5) 88.6(5) 1_555 1_555 1_555 yes C(2) C(3) H(2) 23.9(3) 1_555 1_555 1_555 no C(2) C(3) H(3) 142.9(6) 1_555 1_555 1_555 no C(4) C(3) C(5) 30.6(4) 1_555 1_555 1_555 yes C(4) C(3) H(2) 143.1(5) 1_555 1_555 1_555 no C(4) C(3) H(3) 23.7(3) 1_555 1_555 1_555 no C(5) C(3) H(2) 112.6(4) 1_555 1_555 1_555 no C(5) C(3) H(3) 54.3(3) 1_555 1_555 1_555 no H(2) C(3) H(3) 166.8(4) 1_555 1_555 1_555 no N(1) C(4) C(2) 60.7(3) 1_555 1_555 1_555 yes N(1) C(4) C(3) 91.0(5) 1_555 1_555 1_555 yes N(1) C(4) C(5) 27.3(4) 1_555 1_555 1_555 yes N(1) C(4) H(3) 147.9(6) 1_555 1_555 1_555 no N(1) C(4) H(4) 52.6(2) 1_555 1_555 1_555 no C(2) C(4) C(3) 30.3(4) 1_555 1_555 1_555 yes C(2) C(4) C(5) 88.0(5) 1_555 1_555 1_555 yes C(2) C(4) H(3) 151.4(6) 1_555 1_555 1_555 no C(2) C(4) H(4) 113.2(3) 1_555 1_555 1_555 no C(3) C(4) C(5) 118.3(7) 1_555 1_555 1_555 yes C(3) C(4) H(3) 121.1(6) 1_555 1_555 1_555 no C(3) C(4) H(4) 143.5(5) 1_555 1_555 1_555 no C(5) C(4) H(3) 120.6(8) 1_555 1_555 1_555 no C(5) C(4) H(4) 25.3(4) 1_555 1_555 1_555 no H(3) C(4) H(4) 95.4(5) 1_555 1_555 1_555 no N(1) C(5) C(1) 32.5(3) 1_555 1_555 1_555 yes N(1) C(5) C(3) 93.8(5) 1_555 1_555 1_555 yes N(1) C(5) C(4) 125.0(7) 1_555 1_555 1_555 yes N(1) C(5) H(3) 149.1(6) 1_555 1_555 1_555 no N(1) C(5) H(4) 117.0(7) 1_555 1_555 1_555 no C(1) C(5) C(3) 61.3(3) 1_555 1_555 1_555 yes C(1) C(5) C(4) 92.5(5) 1_555 1_555 1_555 yes C(1) C(5) H(3) 116.6(4) 1_555 1_555 1_555 no C(1) C(5) H(4) 149.5(6) 1_555 1_555 1_555 no C(3) C(5) C(4) 31.1(4) 1_555 1_555 1_555 yes C(3) C(5) H(3) 55.3(3) 1_555 1_555 1_555 no C(3) C(5) H(4) 149.1(6) 1_555 1_555 1_555 no C(4) C(5) H(3) 24.1(4) 1_555 1_555 1_555 no C(4) C(5) H(4) 118.0(8) 1_555 1_555 1_555 no H(3) C(5) H(4) 93.9(5) 1_555 1_555 1_555 no N(3) C(6) C(7) 123.1(9) 1_555 1_555 1_555 yes N(3) C(6) C(8) 92.1(6) 1_555 1_555 1_555 yes N(3) C(6) C(10) 30.6(5) 1_555 1_555 1_555 yes N(3) C(6) H(5) 120.7(10) 1_555 1_555 1_555 no N(3) C(6) H(6) 146.6(7) 1_555 1_555 1_555 no C(7) C(6) C(8) 31.0(5) 1_555 1_555 1_555 yes C(7) C(6) C(10) 92.4(6) 1_555 1_555 1_555 yes C(7) C(6) H(5) 116(1) 1_555 1_555 1_555 no C(7) C(6) H(6) 23.6(5) 1_555 1_555 1_555 no C(8) C(6) C(10) 61.4(4) 1_555 1_555 1_555 yes C(8) C(6) H(5) 147.2(9) 1_555 1_555 1_555 no C(8) C(6) H(6) 54.6(3) 1_555 1_555 1_555 no C(10) C(6) H(5) 151.3(9) 1_555 1_555 1_555 no C(10) C(6) H(6) 116.0(5) 1_555 1_555 1_555 no H(5) C(6) H(6) 92.7(8) 1_555 1_555 1_555 no N(3) C(7) C(6) 27.7(5) 1_555 1_555 1_555 yes N(3) C(7) C(8) 89.7(6) 1_555 1_555 1_555 yes N(3) C(7) C(9) 59.8(4) 1_555 1_555 1_555 yes N(3) C(7) H(5) 53.6(3) 1_555 1_555 1_555 no N(3) C(7) H(6) 150.0(8) 1_555 1_555 1_555 no C(6) C(7) C(8) 117.4(9) 1_555 1_555 1_555 yes C(6) C(7) C(9) 87.6(7) 1_555 1_555 1_555 yes C(6) C(7) H(5) 25.8(5) 1_555 1_555 1_555 no C(6) C(7) H(6) 122.3(10) 1_555 1_555 1_555 no C(8) C(7) C(9) 29.9(5) 1_555 1_555 1_555 yes C(8) C(7) H(5) 143.3(7) 1_555 1_555 1_555 no C(8) C(7) H(6) 120.3(10) 1_555 1_555 1_555 no C(9) C(7) H(5) 113.4(5) 1_555 1_555 1_555 no C(9) C(7) H(6) 150.1(8) 1_555 1_555 1_555 no H(5) C(7) H(6) 96.4(6) 1_555 1_555 1_555 no N(4) C(8) N(4) 30.1(4) 1_555 1_555 3_566 yes N(4) C(8) C(6) 155.1(6) 1_555 1_555 1_555 yes N(4) C(8) C(7) 123.6(8) 1_555 1_555 1_555 yes N(4) C(8) C(9) 116.1(7) 1_555 1_555 1_555 yes N(4) C(8) C(10) 147.3(6) 1_555 1_555 1_555 yes N(4) C(8) H(6) 99.1(5) 1_555 1_555 1_555 no N(4) C(8) H(7) 92.4(5) 1_555 1_555 1_555 no N(4) C(8) C(6) 125.0(5) 3_566 1_555 1_555 yes N(4) C(8) C(7) 93.6(6) 3_566 1_555 1_555 yes N(4) C(8) C(9) 146.0(7) 3_566 1_555 1_555 yes N(4) C(8) C(10) 175.7(5) 3_566 1_555 1_555 yes N(4) C(8) H(6) 69.1(3) 3_566 1_555 1_555 no N(4) C(8) H(7) 122.4(4) 3_566 1_555 1_555 no C(6) C(8) C(7) 31.5(5) 1_555 1_555 1_555 yes C(6) C(8) C(9) 88.8(7) 1_555 1_555 1_555 yes C(6) C(8) C(10) 57.5(4) 1_555 1_555 1_555 yes C(6) C(8) H(6) 56.1(3) 1_555 1_555 1_555 no C(6) C(8) H(7) 112.5(5) 1_555 1_555 1_555 no C(7) C(8) C(9) 120.3(9) 1_555 1_555 1_555 yes C(7) C(8) C(10) 89.0(6) 1_555 1_555 1_555 yes C(7) C(8) H(6) 24.6(4) 1_555 1_555 1_555 no C(7) C(8) H(7) 144.0(7) 1_555 1_555 1_555 no C(9) C(8) C(10) 31.3(5) 1_555 1_555 1_555 yes C(9) C(8) H(6) 144.9(7) 1_555 1_555 1_555 no C(9) C(8) H(7) 23.7(4) 1_555 1_555 1_555 no C(10) C(8) H(6) 113.6(4) 1_555 1_555 1_555 no C(10) C(8) H(7) 55.0(3) 1_555 1_555 1_555 no H(6) C(8) H(7) 168.3(5) 1_555 1_555 1_555 no N(3) C(9) N(4) 123.1(5) 1_555 1_555 1_555 yes N(3) C(9) C(7) 60.3(4) 1_555 1_555 1_555 yes N(3) C(9) C(8) 90.0(6) 1_555 1_555 1_555 yes N(3) C(9) C(10) 27.8(5) 1_555 1_555 1_555 yes N(3) C(9) H(7) 147.8(8) 1_555 1_555 1_555 no N(3) C(9) H(8) 52.2(3) 1_555 1_555 1_555 no N(4) C(9) C(7) 62.8(4) 1_555 1_555 1_555 yes N(4) C(9) C(8) 33.1(5) 1_555 1_555 1_555 yes N(4) C(9) C(10) 150.8(7) 1_555 1_555 1_555 yes N(4) C(9) H(7) 89.1(7) 1_555 1_555 1_555 no N(4) C(9) H(8) 174.3(5) 1_555 1_555 1_555 no C(7) C(9) C(8) 29.8(5) 1_555 1_555 1_555 yes C(7) C(9) C(10) 88.0(7) 1_555 1_555 1_555 yes C(7) C(9) H(7) 151.9(8) 1_555 1_555 1_555 no C(7) C(9) H(8) 112.4(5) 1_555 1_555 1_555 no C(8) C(9) C(10) 117.8(9) 1_555 1_555 1_555 yes C(8) C(9) H(7) 122.2(10) 1_555 1_555 1_555 no C(8) C(9) H(8) 142.1(7) 1_555 1_555 1_555 no C(10) C(9) H(7) 120.0(9) 1_555 1_555 1_555 no C(10) C(9) H(8) 24.5(5) 1_555 1_555 1_555 no H(7) C(9) H(8) 95.7(6) 1_555 1_555 1_555 no N(3) C(10) C(6) 30.9(5) 1_555 1_555 1_555 yes N(3) C(10) C(8) 91.9(6) 1_555 1_555 1_555 yes N(3) C(10) C(9) 122.8(9) 1_555 1_555 1_555 yes N(3) C(10) H(7) 147.2(8) 1_555 1_555 1_555 no N(3) C(10) H(8) 116(1) 1_555 1_555 1_555 no C(6) C(10) C(8) 61.1(4) 1_555 1_555 1_555 yes C(6) C(10) C(9) 92.0(7) 1_555 1_555 1_555 yes C(6) C(10) H(7) 116.3(5) 1_555 1_555 1_555 no C(6) C(10) H(8) 147.5(9) 1_555 1_555 1_555 no C(8) C(10) C(9) 30.9(5) 1_555 1_555 1_555 yes C(8) C(10) H(7) 55.3(3) 1_555 1_555 1_555 no C(8) C(10) H(8) 151.1(8) 1_555 1_555 1_555 no C(9) C(10) H(7) 24.4(4) 1_555 1_555 1_555 no C(9) C(10) H(8) 120.3(10) 1_555 1_555 1_555 no H(7) C(10) H(8) 96.1(7) 1_555 1_555 1_555 no S(1) C(11) N(5) 177.9(8) 1_555 1_555 1_555 yes O(1) C(12) H(9) 112.7(9) 1_555 1_555 1_555 no O(1) C(12) H(10) 112.7(9) 1_555 1_555 1_555 no O(1) C(12) H(11) 111(1) 1_555 1_555 1_555 no H(9) C(12) H(10) 106(1) 1_555 1_555 1_555 no H(9) C(12) H(11) 106(1) 1_555 1_555 1_555 no H(10) C(12) H(11) 106.1(10) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) N(3) 2.685(9) 1_555 2_555 ? O(1) C(6) 3.47(1) 1_555 2_555 ? N(2) N(4) 3.29(1) 1_555 3_666 ? N(2) C(7) 3.58(1) 1_555 3_566 ? N(3) C(12) 3.39(1) 1_555 2_545 ? N(3) C(11) 3.40(1) 1_555 2_545 ? N(3) N(5) 3.45(1) 1_555 2_545 ? N(4) C(4) 3.38(1) 1_555 3_566 ? N(4) C(4) 3.45(1) 1_555 1_555 ? N(4) C(3) 3.51(1) 1_555 3_566 ? N(4) C(3) 3.58(1) 1_555 1_555 ? C(1) C(9) 3.55(1) 1_555 3_566 ? C(2) C(8) 3.52(1) 1_555 3_566 ? C(3) C(8) 3.50(1) 1_555 3_566 ? C(5) C(12) 3.58(1) 1_555 3_665 ? #------------------------------------------------------------------------------ data_Febpy #------------------------------------------------------------------------------ _audit_creation_date 'Tue Dec 16 16:03:18 1997' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 520.41 _chemical_formula_analytical ? _chemical_formula_sum 'C22 H20 Fe N6 O2 S2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 9.017(1) _cell_length_b 10.222(1) _cell_length_c 7.489(1) _cell_angle_alpha 104.318(9) _cell_angle_beta 96.65(1) _cell_angle_gamma 107.454(10) _cell_volume 624.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 288.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 6.0 _cell_measurement_theta_max 51.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.250 _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 268.00 _exptl_absorpt_coefficient_mu 0.800 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_ambient_temperature 288.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXISIV' _diffrn_reflns_number 1962 _reflns_number_total 1962 _reflns_number_observed 1580 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI 0.084 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 6.00 _diffrn_reflns_theta_max 50.5 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 22 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 20 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 6 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 2 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Fe 0 1 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 2 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Fe1 0.0000 0.0000 0.0000 0.0359(2) Uani d . 0.50 S S1 0.1189(2) -0.2617(1) 0.4319(2) 0.0901(5) Uani d . 1.00 . O1 0.1768(3) -0.0582(2) -0.1348(3) 0.0471(7) Uani d . 1.00 . N1 0.1879(4) 0.1889(3) 0.2038(4) 0.0386(8) Uani d . 1.00 . N2 0.0247(4) -0.1245(3) 0.1849(4) 0.0488(9) Uani d . 1.00 . N3 0.6905(5) 0.2478(4) 0.0492(5) 0.066(1) Uani d . 1.00 . C1 0.1805(5) 0.3198(3) 0.2277(5) 0.0405(10) Uani d . 1.00 . C2 0.2978(5) 0.4433(3) 0.3445(5) 0.0412(10) Uani d . 1.00 . C3 0.4339(4) 0.4344(3) 0.4396(4) 0.0322(9) Uani d . 1.00 . C4 0.4408(5) 0.2968(3) 0.4155(5) 0.044(1) Uani d . 1.00 . C5 0.3166(5) 0.1790(3) 0.2987(5) 0.046(1) Uani d . 1.00 . C6 0.0656(5) -0.1789(4) 0.2881(5) 0.044(1) Uani d . 1.00 . C7 0.5469(6) 0.2073(4) -0.0562(7) 0.067(1) Uani d . 1.00 . C8 0.4668(6) 0.3005(4) -0.0788(6) 0.058(1) Uani d . 1.00 . C9 0.5402(5) 0.4471(4) 0.0090(5) 0.046(1) Uani d . 1.00 . C10 0.6921(6) 0.4912(4) 0.1208(6) 0.059(1) Uani d . 1.00 . C11 0.7604(6) 0.3887(5) 0.1354(7) 0.072(2) Uani d . 1.00 . H1 0.0856 0.3290 0.1597 0.0456 Uiso calc . 1.00 . H2 0.2857 0.5370 0.3576 0.0459 Uiso calc . 1.00 . H3 0.5327 0.2836 0.4825 0.0494 Uiso calc . 1.00 . H4 0.3218 0.0836 0.2848 0.0507 Uiso calc . 1.00 . H5 0.4918 0.1039 -0.1217 0.0748 Uiso calc . 1.00 . H6 0.3570 0.2611 -0.1588 0.0663 Uiso calc . 1.00 . H7 0.7495 0.5934 0.1871 0.0719 Uiso calc . 1.00 . H8 0.8699 0.4227 0.2115 0.0845 Uiso calc . 1.00 . H9 0.2254 -0.1199 -0.1009 0.0709 Uiso calc . 1.00 . H10 0.1388 -0.0924 -0.2669 0.0709 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe(1) 0.0368(5) 0.0254(3) 0.0381(4) 0.0079(3) -0.0068(3) 0.0064(3) S(1) 0.154(1) 0.1008(7) 0.0554(7) 0.0907(7) 0.0184(7) 0.0365(5) O(1) 0.049(2) 0.045(1) 0.048(1) 0.023(1) 0.002(1) 0.010(1) N(1) 0.036(2) 0.032(1) 0.040(2) 0.008(1) -0.004(1) 0.006(1) N(2) 0.053(2) 0.041(2) 0.049(2) 0.014(2) -0.006(2) 0.016(1) N(3) 0.077(3) 0.078(2) 0.074(2) 0.054(2) 0.027(2) 0.037(2) C(1) 0.032(2) 0.030(2) 0.049(2) 0.009(2) -0.007(2) 0.004(1) C(2) 0.039(2) 0.030(2) 0.046(2) 0.011(2) 0.001(2) 0.003(1) C(3) 0.032(2) 0.029(1) 0.029(2) 0.006(1) 0.000(2) 0.004(1) C(4) 0.043(2) 0.036(2) 0.045(2) 0.012(2) -0.011(2) 0.009(2) C(5) 0.044(3) 0.026(2) 0.054(2) 0.006(2) -0.011(2) 0.006(1) C(6) 0.051(3) 0.040(2) 0.041(2) 0.019(2) 0.005(2) 0.010(2) C(7) 0.074(4) 0.062(2) 0.076(3) 0.035(2) 0.016(3) 0.025(2) C(8) 0.058(3) 0.058(2) 0.064(3) 0.030(2) 0.006(2) 0.021(2) C(9) 0.049(3) 0.059(2) 0.049(2) 0.033(2) 0.022(2) 0.031(2) C(10) 0.047(3) 0.065(2) 0.075(3) 0.029(2) 0.012(2) 0.028(2) C(11) 0.059(3) 0.084(3) 0.091(3) 0.039(2) 0.011(3) 0.040(2) #------------------------------------------------------------------------------ _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian' _refine_ls_extinction_coef 0.132(3) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1580 _refine_ls_number_parameters 152 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0467 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0541 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.036 _refine_ls_shift/esd_max 0.0040 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -0.55 _refine_diff_density_max 0.59 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe(1) O(1) 2.135(3) 1_555 1_555 yes Fe(1) O(1) 2.135(3) 1_555 2_555 yes Fe(1) N(1) 2.216(2) 1_555 1_555 yes Fe(1) N(1) 2.216(2) 1_555 2_555 yes Fe(1) N(2) 2.134(3) 1_555 1_555 yes Fe(1) N(2) 2.134(3) 1_555 2_555 yes S(1) C(6) 1.638(4) 1_555 1_555 yes N(1) C(1) 1.328(4) 1_555 1_555 yes N(1) C(2) 2.390(4) 1_555 1_555 yes N(1) C(4) 2.392(4) 1_555 1_555 yes N(1) C(5) 1.333(5) 1_555 1_555 yes N(2) C(6) 1.146(5) 1_555 1_555 yes N(3) C(7) 1.324(6) 1_555 1_555 yes N(3) C(8) 2.395(6) 1_555 1_555 yes N(3) C(11) 1.337(5) 1_555 1_555 yes C(1) C(2) 1.385(4) 1_555 1_555 yes C(1) C(3) 2.398(4) 1_555 1_555 yes C(1) C(5) 2.269(6) 1_555 1_555 yes C(2) C(3) 1.385(5) 1_555 1_555 yes C(2) C(4) 2.363(6) 1_555 1_555 yes C(3) C(3) 1.492(6) 1_555 2_666 yes C(3) C(4) 1.395(5) 1_555 1_555 yes C(4) C(5) 1.383(4) 1_555 1_555 yes C(7) C(8) 1.386(7) 1_555 1_555 yes C(7) C(9) 2.398(6) 1_555 1_555 yes C(7) C(11) 2.260(6) 1_555 1_555 yes C(8) C(9) 1.390(5) 1_555 1_555 yes C(8) C(10) 2.375(5) 1_555 1_555 yes C(9) C(9) 1.496(8) 1_555 2_665 yes C(9) C(10) 1.399(6) 1_555 1_555 yes C(9) C(11) 2.397(7) 1_555 1_555 yes C(10) C(11) 1.385(7) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Fe(1) O(1) 180.0 1_555 1_555 2_555 yes O(1) Fe(1) N(1) 89.9(1) 1_555 1_555 1_555 yes O(1) Fe(1) N(1) 90.1(1) 1_555 1_555 2_555 yes O(1) Fe(1) N(2) 89.8(1) 1_555 1_555 1_555 yes O(1) Fe(1) N(2) 90.2(1) 1_555 1_555 2_555 yes O(1) Fe(1) N(1) 90.1(1) 2_555 1_555 1_555 yes O(1) Fe(1) N(1) 89.9(1) 2_555 1_555 2_555 yes O(1) Fe(1) N(2) 90.2(1) 2_555 1_555 1_555 yes O(1) Fe(1) N(2) 89.8(1) 2_555 1_555 2_555 yes N(1) Fe(1) N(1) 180.0 1_555 1_555 2_555 yes N(1) Fe(1) N(2) 89.3(1) 1_555 1_555 1_555 yes N(1) Fe(1) N(2) 90.7(1) 1_555 1_555 2_555 yes N(1) Fe(1) N(2) 90.7(1) 2_555 1_555 1_555 yes N(1) Fe(1) N(2) 89.3(1) 2_555 1_555 2_555 yes N(2) Fe(1) N(2) 180.0 1_555 1_555 2_555 yes Fe(1) O(1) H(9) 122.9(2) 1_555 1_555 1_555 no Fe(1) O(1) H(10) 109.5(2) 1_555 1_555 1_555 no H(9) O(1) H(10) 107.9(3) 1_555 1_555 1_555 no Fe(1) N(1) C(1) 120.4(2) 1_555 1_555 1_555 yes Fe(1) N(1) C(2) 149.2(2) 1_555 1_555 1_555 yes Fe(1) N(1) C(4) 151.2(2) 1_555 1_555 1_555 yes Fe(1) N(1) C(5) 122.5(2) 1_555 1_555 1_555 yes Fe(1) N(1) H(1) 94.6(1) 1_555 1_555 1_555 no Fe(1) N(1) H(4) 96.9(1) 1_555 1_555 1_555 no C(1) N(1) C(2) 28.9(2) 1_555 1_555 1_555 yes C(1) N(1) C(4) 88.1(2) 1_555 1_555 1_555 yes C(1) N(1) C(5) 116.9(3) 1_555 1_555 1_555 yes C(1) N(1) H(1) 25.9(2) 1_555 1_555 1_555 no C(1) N(1) H(4) 142.7(2) 1_555 1_555 1_555 no C(2) N(1) C(4) 59.2(1) 1_555 1_555 1_555 yes C(2) N(1) C(5) 88.1(2) 1_555 1_555 1_555 yes C(2) N(1) H(1) 54.8(1) 1_555 1_555 1_555 no C(2) N(1) H(4) 113.8(2) 1_555 1_555 1_555 no C(4) N(1) C(5) 28.9(2) 1_555 1_555 1_555 yes C(4) N(1) H(1) 114.0(1) 1_555 1_555 1_555 no C(4) N(1) H(4) 54.6(1) 1_555 1_555 1_555 no C(5) N(1) H(1) 142.8(2) 1_555 1_555 1_555 no C(5) N(1) H(4) 25.8(2) 1_555 1_555 1_555 no H(1) N(1) H(4) 168.6(1) 1_555 1_555 1_555 no Fe(1) N(2) C(6) 168.0(3) 1_555 1_555 1_555 yes C(7) N(3) C(8) 28.6(2) 1_555 1_555 1_555 yes C(7) N(3) C(11) 116.2(4) 1_555 1_555 1_555 yes C(7) N(3) H(5) 25.9(2) 1_555 1_555 1_555 no C(7) N(3) H(8) 142.1(3) 1_555 1_555 1_555 no C(7) N(3) H(9) 121.7(3) 1_555 1_555 2_655 no C(8) N(3) C(11) 87.7(3) 1_555 1_555 1_555 yes C(8) N(3) H(5) 54.5(1) 1_555 1_555 1_555 no C(8) N(3) H(8) 113.6(2) 1_555 1_555 1_555 no C(8) N(3) H(9) 149.7(2) 1_555 1_555 2_655 no C(11) N(3) H(5) 142.1(4) 1_555 1_555 1_555 no C(11) N(3) H(8) 25.9(2) 1_555 1_555 1_555 no C(11) N(3) H(9) 121.4(3) 1_555 1_555 2_655 no H(5) N(3) H(8) 168.0(2) 1_555 1_555 1_555 no H(5) N(3) H(9) 96.1(2) 1_555 1_555 2_655 no H(8) N(3) H(9) 95.9(2) 1_555 1_555 2_655 no N(1) C(1) C(2) 123.5(4) 1_555 1_555 1_555 yes N(1) C(1) C(3) 93.5(2) 1_555 1_555 1_555 yes N(1) C(1) C(5) 31.6(2) 1_555 1_555 1_555 yes N(1) C(1) H(1) 118.0(3) 1_555 1_555 1_555 no N(1) C(1) H(2) 147.8(3) 1_555 1_555 1_555 no C(2) C(1) C(3) 30.1(2) 1_555 1_555 1_555 yes C(2) C(1) C(5) 91.9(3) 1_555 1_555 1_555 yes C(2) C(1) H(1) 118.4(4) 1_555 1_555 1_555 no C(2) C(1) H(2) 24.3(2) 1_555 1_555 1_555 no C(3) C(1) C(5) 61.9(1) 1_555 1_555 1_555 yes C(3) C(1) H(1) 148.5(3) 1_555 1_555 1_555 no C(3) C(1) H(2) 54.3(1) 1_555 1_555 1_555 no C(5) C(1) H(1) 149.6(3) 1_555 1_555 1_555 no C(5) C(1) H(2) 116.2(2) 1_555 1_555 1_555 no H(1) C(1) H(2) 94.1(2) 1_555 1_555 1_555 no N(1) C(2) C(1) 27.6(2) 1_555 1_555 1_555 yes N(1) C(2) C(3) 92.3(2) 1_555 1_555 1_555 yes N(1) C(2) C(4) 60.4(1) 1_555 1_555 1_555 yes N(1) C(2) H(1) 52.6(1) 1_555 1_555 1_555 no N(1) C(2) H(2) 147.7(3) 1_555 1_555 1_555 no C(1) C(2) C(3) 119.9(3) 1_555 1_555 1_555 yes C(1) C(2) C(4) 88.0(3) 1_555 1_555 1_555 yes C(1) C(2) H(1) 25.1(2) 1_555 1_555 1_555 no C(1) C(2) H(2) 120.1(4) 1_555 1_555 1_555 no C(3) C(2) C(4) 31.9(2) 1_555 1_555 1_555 yes C(3) C(2) H(1) 144.9(3) 1_555 1_555 1_555 no C(3) C(2) H(2) 120.0(3) 1_555 1_555 1_555 no C(4) C(2) H(1) 113.1(2) 1_555 1_555 1_555 no C(4) C(2) H(2) 151.9(3) 1_555 1_555 1_555 no H(1) C(2) H(2) 95.0(3) 1_555 1_555 1_555 no C(1) C(3) C(2) 30.0(2) 1_555 1_555 1_555 yes C(1) C(3) C(3) 151.5(4) 1_555 1_555 2_666 yes C(1) C(3) C(4) 86.4(2) 1_555 1_555 1_555 yes C(1) C(3) H(2) 54.4(1) 1_555 1_555 1_555 no C(1) C(3) H(3) 110.6(1) 1_555 1_555 1_555 no C(2) C(3) C(3) 121.6(4) 1_555 1_555 2_666 yes C(2) C(3) C(4) 116.4(3) 1_555 1_555 1_555 yes C(2) C(3) H(2) 24.3(2) 1_555 1_555 1_555 no C(2) C(3) H(3) 140.6(2) 1_555 1_555 1_555 no C(3) C(3) C(4) 122.0(4) 2_666 1_555 1_555 yes C(3) C(3) H(2) 97.2(3) 2_666 1_555 1_555 no C(3) C(3) H(3) 97.8(3) 2_666 1_555 1_555 no C(4) C(3) H(2) 140.7(2) 1_555 1_555 1_555 no C(4) C(3) H(3) 24.2(2) 1_555 1_555 1_555 no H(2) C(3) H(3) 164.9(2) 1_555 1_555 1_555 no N(1) C(4) C(2) 60.4(1) 1_555 1_555 1_555 yes N(1) C(4) C(3) 92.0(2) 1_555 1_555 1_555 yes N(1) C(4) C(5) 27.7(2) 1_555 1_555 1_555 yes N(1) C(4) H(3) 147.9(3) 1_555 1_555 1_555 no N(1) C(4) H(4) 52.3(1) 1_555 1_555 1_555 no C(2) C(4) C(3) 31.7(2) 1_555 1_555 1_555 yes C(2) C(4) C(5) 88.1(3) 1_555 1_555 1_555 yes C(2) C(4) H(3) 151.7(3) 1_555 1_555 1_555 no C(2) C(4) H(4) 112.7(2) 1_555 1_555 1_555 no C(3) C(4) C(5) 119.7(4) 1_555 1_555 1_555 yes C(3) C(4) H(3) 120.1(3) 1_555 1_555 1_555 no C(3) C(4) H(4) 144.3(3) 1_555 1_555 1_555 no C(5) C(4) H(3) 120.2(4) 1_555 1_555 1_555 no C(5) C(4) H(4) 24.6(2) 1_555 1_555 1_555 no H(3) C(4) H(4) 95.6(2) 1_555 1_555 1_555 no N(1) C(5) C(1) 31.5(2) 1_555 1_555 1_555 yes N(1) C(5) C(4) 123.4(3) 1_555 1_555 1_555 yes N(1) C(5) H(3) 147.7(3) 1_555 1_555 1_555 no N(1) C(5) H(4) 117.6(3) 1_555 1_555 1_555 no C(1) C(5) C(4) 92.0(3) 1_555 1_555 1_555 yes C(1) C(5) H(3) 116.3(2) 1_555 1_555 1_555 no C(1) C(5) H(4) 149.0(3) 1_555 1_555 1_555 no C(4) C(5) H(3) 24.3(2) 1_555 1_555 1_555 no C(4) C(5) H(4) 119.0(4) 1_555 1_555 1_555 no H(3) C(5) H(4) 94.7(3) 1_555 1_555 1_555 no S(1) C(6) N(2) 178.0(3) 1_555 1_555 1_555 yes N(3) C(7) C(8) 124.2(4) 1_555 1_555 1_555 yes N(3) C(7) C(9) 93.9(3) 1_555 1_555 1_555 yes N(3) C(7) C(11) 32.1(2) 1_555 1_555 1_555 yes N(3) C(7) H(5) 118.3(5) 1_555 1_555 1_555 no N(3) C(7) H(6) 149.1(3) 1_555 1_555 1_555 no C(8) C(7) C(9) 30.3(2) 1_555 1_555 1_555 yes C(8) C(7) C(11) 92.2(3) 1_555 1_555 1_555 yes C(8) C(7) H(5) 117.4(5) 1_555 1_555 1_555 no C(8) C(7) H(6) 24.9(2) 1_555 1_555 1_555 no C(9) C(7) C(11) 61.9(2) 1_555 1_555 1_555 yes C(9) C(7) H(5) 147.7(4) 1_555 1_555 1_555 no C(9) C(7) H(6) 55.2(2) 1_555 1_555 1_555 no C(11) C(7) H(5) 150.4(5) 1_555 1_555 1_555 no C(11) C(7) H(6) 117.1(2) 1_555 1_555 1_555 no H(5) C(7) H(6) 92.5(3) 1_555 1_555 1_555 no N(3) C(8) C(7) 27.2(2) 1_555 1_555 1_555 yes N(3) C(8) C(9) 92.3(3) 1_555 1_555 1_555 yes N(3) C(8) C(10) 60.6(2) 1_555 1_555 1_555 yes N(3) C(8) H(5) 52.7(1) 1_555 1_555 1_555 no N(3) C(8) H(6) 146.7(3) 1_555 1_555 1_555 no C(7) C(8) C(9) 119.5(4) 1_555 1_555 1_555 yes C(7) C(8) C(10) 87.8(3) 1_555 1_555 1_555 yes C(7) C(8) H(5) 25.5(2) 1_555 1_555 1_555 no C(7) C(8) H(6) 119.5(4) 1_555 1_555 1_555 no C(9) C(8) C(10) 31.7(2) 1_555 1_555 1_555 yes C(9) C(8) H(5) 145.0(4) 1_555 1_555 1_555 no C(9) C(8) H(6) 121.0(4) 1_555 1_555 1_555 no C(10) C(8) H(5) 113.3(2) 1_555 1_555 1_555 no C(10) C(8) H(6) 152.7(4) 1_555 1_555 1_555 no H(5) C(8) H(6) 94.0(2) 1_555 1_555 1_555 no C(7) C(9) C(8) 30.2(2) 1_555 1_555 1_555 yes C(7) C(9) C(9) 152.2(4) 1_555 1_555 2_665 yes C(7) C(9) C(10) 86.6(3) 1_555 1_555 1_555 yes C(7) C(9) C(11) 56.2(2) 1_555 1_555 1_555 yes C(7) C(9) H(6) 54.4(1) 1_555 1_555 1_555 no C(7) C(9) H(7) 110.7(2) 1_555 1_555 1_555 no C(8) C(9) C(9) 122.1(5) 1_555 1_555 2_665 yes C(8) C(9) C(10) 116.8(4) 1_555 1_555 1_555 yes C(8) C(9) C(11) 86.4(3) 1_555 1_555 1_555 yes C(8) C(9) H(6) 24.3(2) 1_555 1_555 1_555 no C(8) C(9) H(7) 140.8(3) 1_555 1_555 1_555 no C(9) C(9) C(10) 121.2(4) 2_665 1_555 1_555 yes C(9) C(9) C(11) 151.5(4) 2_665 1_555 1_555 yes C(9) C(9) H(6) 97.8(3) 2_665 1_555 1_555 no C(9) C(9) H(7) 97.1(3) 2_665 1_555 1_555 no C(10) C(9) C(11) 30.4(2) 1_555 1_555 1_555 yes C(10) C(9) H(6) 141.0(3) 1_555 1_555 1_555 no C(10) C(9) H(7) 24.1(2) 1_555 1_555 1_555 no C(11) C(9) H(6) 110.7(2) 1_555 1_555 1_555 no C(11) C(9) H(7) 54.4(1) 1_555 1_555 1_555 no H(6) C(9) H(7) 165.1(2) 1_555 1_555 1_555 no C(8) C(10) C(9) 31.5(2) 1_555 1_555 1_555 yes C(8) C(10) C(11) 87.4(3) 1_555 1_555 1_555 yes C(8) C(10) H(7) 151.9(4) 1_555 1_555 1_555 no C(8) C(10) H(8) 112.9(2) 1_555 1_555 1_555 no C(9) C(10) C(11) 118.9(4) 1_555 1_555 1_555 yes C(9) C(10) H(7) 120.4(4) 1_555 1_555 1_555 no C(9) C(10) H(8) 144.4(3) 1_555 1_555 1_555 no C(11) C(10) H(7) 120.6(4) 1_555 1_555 1_555 no C(11) C(10) H(8) 25.5(2) 1_555 1_555 1_555 no H(7) C(10) H(8) 95.1(3) 1_555 1_555 1_555 no N(3) C(11) C(7) 31.7(2) 1_555 1_555 1_555 yes N(3) C(11) C(9) 93.6(3) 1_555 1_555 1_555 yes N(3) C(11) C(10) 124.3(4) 1_555 1_555 1_555 yes N(3) C(11) H(7) 148.5(4) 1_555 1_555 1_555 no N(3) C(11) H(8) 118.0(5) 1_555 1_555 1_555 no C(7) C(11) C(9) 61.9(2) 1_555 1_555 1_555 yes C(7) C(11) C(10) 92.6(3) 1_555 1_555 1_555 yes C(7) C(11) H(7) 116.8(3) 1_555 1_555 1_555 no C(7) C(11) H(8) 149.7(4) 1_555 1_555 1_555 no C(9) C(11) C(10) 30.7(2) 1_555 1_555 1_555 yes C(9) C(11) H(7) 54.9(2) 1_555 1_555 1_555 no C(9) C(11) H(8) 148.3(4) 1_555 1_555 1_555 no C(10) C(11) H(7) 24.2(2) 1_555 1_555 1_555 no C(10) C(11) H(8) 117.6(4) 1_555 1_555 1_555 no H(7) C(11) H(8) 93.4(3) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S(1) O(1) 3.278(3) 1_555 1_556 ? O(1) N(3) 2.725(5) 1_555 2_655 ? O(1) C(7) 3.489(5) 1_555 1_555 ? O(1) C(11) 3.588(6) 1_555 2_655 ? N(1) C(8) 3.580(6) 1_555 1_555 ? C(2) C(9) 3.432(6) 1_555 2_665 ? C(2) C(9) 3.516(6) 1_555 1_555 ? C(3) C(9) 3.490(5) 1_555 1_555 ? C(3) C(10) 3.553(6) 1_555 1_555 ? C(3) C(10) 3.585(6) 1_555 2_666 ? C(5) C(7) 3.572(7) 1_555 1_555 ? #------------------------------------------------------------------------------