# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1625 data_8 #----------------------------------------------------------------------- _audit_creation_date '1999-05-18' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #----------------------------------------------------------------------- _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Walker, N. & Stuart. D. (1983). Acta Cryst. A39, 158-166. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. ; #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #----------------------------------------------------------------------- _cell_length_a 11.776(3) _cell_length_b 12.172(2) _cell_length_c 9.949(1) _cell_angle_alpha 106.28(1) _cell_angle_beta 108.82(1) _cell_angle_gamma 80.96(2) _cell_volume 1292.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 30.5 _cell_measurement_theta_max 37.0 #----------------------------------------------------------------------- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #----------------------------------------------------------------------- # ENTER EXPERIMENTAL SECTION _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 614.28 _chemical_formula_analytical 'C23 H24 Fe2 N2 O P2 S3 ' _chemical_formula_sum 'C23 H24 Fe2 N2 O P2 S3 ' _chemical_formula_moiety 'C23 H24 Fe2 N2 O P2 S3 ' _chemical_formula_structural 'C23 H24 Fe2 N2 O P2 S3 ' _chemical_compound_source - _exptl_crystal_F_000 628.00 _exptl_absorpt_coefficient_mu 12.601 _exptl_absorpt_correction_type ; \DF (DIFABS; Walker & Stuart, 1983) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.793 _exptl_special_details ; The scan width was (0.79+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #----------------------------------------------------------------------- _diffrn_special_details ; - ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -2.24 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 4 2 1 5 1 -1 5 0 _diffrn_reflns_number 4066 _reflns_number_total 3847 _reflns_number_gt 2599 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.08910 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.80 _diffrn_reflns_theta_max 60.07 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.02053 _diffrn_orient_matrix_UB_12 0.06699 _diffrn_orient_matrix_UB_13 0.08667 _diffrn_orient_matrix_UB_21 0.00922 _diffrn_orient_matrix_UB_22 0.04624 _diffrn_orient_matrix_UB_23 -0.06407 _diffrn_orient_matrix_UB_31 -0.08709 _diffrn_orient_matrix_UB_32 0.02719 _diffrn_orient_matrix_UB_33 -0.01960 #----------------------------------------------------------------------- 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 46 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 48 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 4 0.029 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 4 0.283 0.434 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 6 0.319 0.557 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Fe 0 4 -1.179 3.204 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 2 0.047 0.032 ;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_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Fe(1) 0.86180(8) 0.19806(7) 0.5928(1) 0.0414(3) 1.000 . Uani d ? Fe(2) 0.25507(8) 0.21769(8) 0.1954(1) 0.0490(3) 1.000 . Uani d ? S(1) 0.7611(2) 0.1420(1) 0.1472(2) 0.0703(6) 1.000 . Uani d ? S(2) 0.4397(2) 0.5100(1) 0.2707(2) 0.0706(6) 1.000 . Uani d ? S(3) 0.4243(2) 0.1907(2) -0.2226(2) 0.120(1) 1.000 . Uani d ? P(1) 0.7604(1) 0.2901(1) 0.2814(2) 0.0406(4) 1.000 . Uani d ? P(2) 0.4966(1) 0.3522(1) 0.2394(2) 0.0420(4) 1.000 . Uani d ? O(1) 0.6343(3) 0.3314(3) 0.3224(4) 0.048(1) 1.000 . Uani d ? N(1) 0.7894(5) 0.3923(4) 0.2249(5) 0.057(2) 1.000 . Uani d ? N(2) 0.4919(5) 0.2917(5) 0.0659(5) 0.079(2) 1.000 . Uani d ? C(1) 0.7600(7) 0.3906(7) 0.0689(8) 0.091(3) 1.000 . Uani d ? C(2) 0.8037(7) 0.5076(6) 0.3211(8) 0.091(3) 1.000 . Uani d ? C(3) 0.4609(6) 0.2483(6) -0.0559(7) 0.060(2) 1.000 . Uani d ? C(4) 0.8574(5) 0.2994(4) 0.4610(6) 0.038(2) 1.000 . Uani d ? C(5) 0.8371(5) 0.3672(4) 0.5982(6) 0.047(2) 1.000 . Uani d ? C(6) 0.9415(6) 0.3460(5) 0.7101(6) 0.053(2) 1.000 . Uani d ? C(7) 1.0234(5) 0.2664(5) 0.6490(7) 0.052(2) 1.000 . Uani d ? C(8) 0.9724(5) 0.2395(5) 0.4964(7) 0.048(2) 1.000 . Uani d ? C(9) 0.7237(6) 0.0946(6) 0.4932(8) 0.069(3) 1.000 . Uani d ? C(10) 0.7160(7) 0.1575(6) 0.631(1) 0.077(3) 1.000 . Uani d ? C(11) 0.8236(7) 0.1324(6) 0.7385(8) 0.071(3) 1.000 . Uani d ? C(12) 0.8953(6) 0.0519(5) 0.6650(7) 0.057(2) 1.000 . Uani d ? C(13) 0.8350(6) 0.0281(5) 0.5141(7) 0.057(2) 1.000 . Uani d ? C(14) 0.4254(5) 0.2588(5) 0.2867(6) 0.048(2) 1.000 . Uani d ? C(15) 0.4222(6) 0.1403(6) 0.2322(9) 0.076(3) 1.000 . Uani d ? C(16) 0.3565(9) 0.1020(8) 0.305(1) 0.123(4) 1.000 . Uani d ? C(17) 0.3192(9) 0.195(1) 0.401(1) 0.122(5) 1.000 . Uani d ? C(18) 0.3632(6) 0.2926(7) 0.3953(7) 0.074(3) 1.000 . Uani d ? C(19) 0.1786(6) 0.2933(7) 0.0277(8) 0.070(2) 1.000 . Uani d ? C(20) 0.1744(7) 0.1777(7) -0.0219(7) 0.073(3) 1.000 . Uani d ? C(21) 0.1128(7) 0.1375(7) 0.0453(9) 0.077(3) 1.000 . Uani d ? C(22) 0.0738(6) 0.2274(9) 0.1392(9) 0.088(3) 1.000 . Uani d ? C(23) 0.1140(7) 0.3299(6) 0.1337(9) 0.092(3) 1.000 . Uani d ? H(1a) 0.6857 0.4338 0.0405 0.109 1.000 . Uiso c ? H(1b) 0.8219 0.4244 0.0554 0.109 1.000 . Uiso c ? H(1c) 0.7547 0.3141 0.0124 0.109 1.000 . Uiso c ? H(2a) 0.8240 0.5036 0.4201 0.109 1.000 . Uiso c ? H(2b) 0.8654 0.5410 0.3075 0.109 1.000 . Uiso c ? H(2c) 0.7300 0.5535 0.2980 0.109 1.000 . Uiso c ? H(5) 0.7682 0.4168 0.6118 0.056 1.000 . Uiso c ? H(6) 0.9561 0.3802 0.8113 0.065 1.000 . Uiso c ? H(7) 1.0988 0.2356 0.7018 0.061 1.000 . Uiso c ? H(8) 1.0097 0.1896 0.4276 0.059 1.000 . Uiso c ? H(9) 0.6654 0.0958 0.4021 0.081 1.000 . Uiso c ? H(10) 0.6483 0.2094 0.6456 0.096 1.000 . Uiso c ? H(11) 0.8426 0.1648 0.8410 0.090 1.000 . Uiso c ? H(12) 0.9718 0.0186 0.7099 0.068 1.000 . Uiso c ? H(13) 0.8635 -0.0236 0.4383 0.070 1.000 . Uiso c ? H(15) 0.4577 0.0946 0.1590 0.090 1.000 . Uiso c ? H(16) 0.3427 0.0233 0.2883 0.150 1.000 . Uiso c ? H(17) 0.2696 0.1908 0.4590 0.151 1.000 . Uiso c ? H(18) 0.3556 0.3683 0.4555 0.094 1.000 . Uiso c ? H(19) 0.2172 0.3413 -0.0033 0.083 1.000 . Uiso c ? H(20) 0.2096 0.1311 -0.0948 0.093 1.000 . Uiso c ? H(21) 0.0996 0.0586 0.0301 0.093 1.000 . Uiso c ? H(22) 0.0275 0.2228 0.2006 0.107 1.000 . Uiso c ? H(23) 0.1021 0.4061 0.1892 0.112 1.000 . Uiso c ? 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) 0.0515(6) 0.0334(5) 0.0465(6) 0.0022(4) 0.0193(4) 0.0179(4) Fe(2) 0.0493(6) 0.0577(6) 0.0450(6) -0.0098(5) 0.0079(5) 0.0238(5) S(1) 0.093(1) 0.049(1) 0.058(1) 0.0085(9) 0.026(1) -0.0017(8) S(2) 0.079(1) 0.049(1) 0.081(1) 0.0052(9) 0.010(1) 0.0303(9) S(3) 0.140(2) 0.157(2) 0.043(1) -0.004(2) 0.027(1) -0.004(1) P(1) 0.0473(9) 0.0378(8) 0.0423(9) 0.0043(7) 0.0190(7) 0.0158(7) P(2) 0.0461(9) 0.0492(9) 0.0357(8) -0.0003(7) 0.0145(7) 0.0168(7) O(1) 0.035(2) 0.072(3) 0.038(2) 0.003(2) 0.014(2) 0.015(2) N(1) 0.083(4) 0.049(3) 0.057(3) -0.001(3) 0.036(3) 0.028(3) N(2) 0.068(4) 0.131(6) 0.029(3) 0.000(4) 0.015(3) 0.008(3) C(1) 0.126(7) 0.110(6) 0.061(5) -0.004(5) 0.036(5) 0.050(5) C(2) 0.140(8) 0.063(5) 0.090(6) -0.031(5) 0.029(5) 0.041(4) C(3) 0.060(4) 0.075(5) 0.052(4) 0.004(3) 0.021(4) 0.026(4) C(4) 0.038(3) 0.030(3) 0.047(3) 0.005(2) 0.011(3) 0.015(3) C(5) 0.062(4) 0.034(3) 0.047(4) 0.009(3) 0.020(3) 0.016(3) C(6) 0.069(4) 0.048(4) 0.041(4) -0.009(3) 0.009(3) 0.014(3) C(7) 0.056(4) 0.046(4) 0.056(4) 0.003(3) 0.009(3) 0.027(3) C(8) 0.049(4) 0.046(4) 0.063(4) 0.006(3) 0.024(3) 0.029(3) C(9) 0.061(5) 0.057(5) 0.098(6) -0.013(4) 0.003(4) 0.048(4) C(10) 0.081(6) 0.050(4) 0.135(8) 0.011(4) 0.071(6) 0.037(5) C(11) 0.113(7) 0.053(4) 0.068(5) -0.005(4) 0.050(5) 0.018(4) C(12) 0.069(4) 0.044(4) 0.058(4) -0.001(3) 0.011(4) 0.025(3) C(13) 0.078(5) 0.036(3) 0.064(5) -0.007(3) 0.025(4) 0.016(3) C(14) 0.052(4) 0.045(4) 0.053(4) -0.003(3) 0.014(3) 0.024(3) C(15) 0.057(4) 0.055(5) 0.112(6) -0.006(3) 0.000(4) 0.042(4) C(16) 0.087(7) 0.111(8) 0.18(1) -0.046(6) -0.037(8) 0.115(8) C(17) 0.113(8) 0.20(1) 0.080(7) -0.090(9) -0.021(6) 0.095(7) C(18) 0.069(5) 0.120(6) 0.041(4) -0.042(4) 0.004(3) 0.025(4) C(19) 0.065(5) 0.078(5) 0.066(5) -0.017(4) -0.006(4) 0.041(4) C(20) 0.086(5) 0.073(5) 0.051(4) -0.001(4) 0.012(4) 0.012(4) C(21) 0.071(5) 0.077(5) 0.082(6) -0.021(4) 0.007(4) 0.027(5) C(22) 0.062(5) 0.136(8) 0.071(6) 0.002(5) 0.029(4) 0.024(6) C(23) 0.086(6) 0.059(5) 0.082(6) 0.022(4) -0.004(5) -0.013(4) #----------------------------------------------------------------------- _refine_special_details ; - ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.000011869 _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 2599 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.0393 _refine_ls_goodness_of_fit_ref 2.084 _refine_ls_shift/esd_max 0.2230 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -0.42 _refine_diff_density_max 0.32 #----------------------------------------------------------------------- _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) C(4) 2.022(5) . . yes Fe(1) C(5) 2.021(5) . . yes Fe(1) C(6) 2.032(6) . . yes Fe(1) C(7) 2.043(6) . . yes Fe(1) C(8) 2.038(6) . . yes Fe(1) C(9) 2.029(6) . . yes Fe(1) C(10) 2.030(7) . . yes Fe(1) C(11) 2.031(7) . . yes Fe(1) C(12) 2.037(6) . . yes Fe(1) C(13) 2.033(6) . . yes Fe(2) C(14) 1.996(6) . . yes Fe(2) C(15) 2.010(7) . . yes Fe(2) C(16) 2.021(8) . . yes Fe(2) C(17) 2.027(8) . . yes Fe(2) C(18) 2.030(6) . . yes Fe(2) C(19) 2.018(6) . . yes Fe(2) C(20) 2.011(7) . . yes Fe(2) C(21) 2.017(7) . . yes Fe(2) C(22) 2.018(7) . . yes Fe(2) C(23) 2.025(7) . . yes S(1) P(1) 1.919(2) . . yes S(2) P(2) 1.905(2) . . yes S(3) C(3) 1.552(7) . . yes P(1) O(1) 1.632(4) . . yes P(1) N(1) 1.623(5) . . yes P(1) C(4) 1.766(5) . . yes P(2) O(1) 1.581(4) . . yes P(2) N(2) 1.662(5) . . yes P(2) C(14) 1.753(6) . . yes N(1) C(1) 1.472(8) . . yes N(1) C(2) 1.459(8) . . yes N(2) C(3) 1.139(7) . . yes C(1) H(1a) 0.95 . . no C(1) H(1b) 0.95 . . no C(1) H(1c) 0.94 . . no C(2) H(2a) 0.95 . . no C(2) H(2b) 0.95 . . no C(2) H(2c) 0.95 . . no C(4) C(5) 1.456(7) . . yes C(4) C(8) 1.420(7) . . yes C(5) C(6) 1.413(7) . . yes C(5) H(5) 0.95 . . no C(6) C(7) 1.412(8) . . yes C(6) H(6) 0.94 . . no C(7) C(8) 1.402(7) . . yes C(7) H(7) 0.95 . . no C(8) H(8) 0.95 . . no C(9) C(10) 1.391(9) . . yes C(9) C(13) 1.415(8) . . yes C(9) H(9) 0.95 . . no C(10) C(11) 1.427(9) . . yes C(10) H(10) 0.96 . . no C(11) C(12) 1.394(8) . . yes C(11) H(11) 0.95 . . no C(12) C(13) 1.406(8) . . yes C(12) H(12) 0.95 . . no C(13) H(13) 0.95 . . no C(14) C(15) 1.393(8) . . yes C(14) C(18) 1.428(8) . . yes C(15) C(16) 1.41(1) . . yes C(15) H(15) 0.95 . . no C(16) C(17) 1.38(1) . . yes C(16) H(16) 0.96 . . no C(17) C(18) 1.40(1) . . yes C(17) H(17) 0.95 . . no C(18) H(18) 0.96 . . no C(19) C(20) 1.357(9) . . yes C(19) C(23) 1.43(1) . . yes C(19) H(19) 0.96 . . no C(20) C(21) 1.35(1) . . yes C(20) H(20) 0.95 . . no C(21) C(22) 1.35(1) . . yes C(21) H(21) 0.96 . . no C(22) C(23) 1.42(1) . . yes C(22) H(22) 0.96 . . no C(23) H(23) 0.95 . . no #----------------------------------------------------------------------- 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 C(4) Fe(1) C(5) 42.2(2) . . . yes C(4) Fe(1) C(6) 68.8(2) . . . yes C(4) Fe(1) C(7) 69.0(2) . . . yes C(4) Fe(1) C(8) 40.9(2) . . . yes C(4) Fe(1) C(9) 108.5(2) . . . yes C(4) Fe(1) C(10) 125.3(3) . . . yes C(4) Fe(1) C(11) 162.0(3) . . . yes C(4) Fe(1) C(12) 156.9(2) . . . yes C(4) Fe(1) C(13) 122.2(2) . . . yes C(5) Fe(1) C(6) 40.8(2) . . . yes C(5) Fe(1) C(7) 69.5(2) . . . yes C(5) Fe(1) C(8) 69.5(2) . . . yes C(5) Fe(1) C(9) 121.0(2) . . . yes C(5) Fe(1) C(10) 106.6(2) . . . yes C(5) Fe(1) C(11) 122.8(3) . . . yes C(5) Fe(1) C(12) 159.5(2) . . . yes C(5) Fe(1) C(13) 157.7(2) . . . yes C(6) Fe(1) C(7) 40.5(2) . . . yes C(6) Fe(1) C(8) 67.7(2) . . . yes C(6) Fe(1) C(9) 156.1(3) . . . yes C(6) Fe(1) C(10) 120.8(3) . . . yes C(6) Fe(1) C(11) 106.2(3) . . . yes C(6) Fe(1) C(12) 123.6(2) . . . yes C(6) Fe(1) C(13) 160.8(2) . . . yes C(7) Fe(1) C(8) 40.2(2) . . . yes C(7) Fe(1) C(9) 162.5(3) . . . yes C(7) Fe(1) C(10) 155.4(3) . . . yes C(7) Fe(1) C(11) 119.3(3) . . . yes C(7) Fe(1) C(12) 106.9(2) . . . yes C(7) Fe(1) C(13) 124.9(2) . . . yes C(8) Fe(1) C(9) 126.8(3) . . . yes C(8) Fe(1) C(10) 163.1(3) . . . yes C(8) Fe(1) C(11) 154.8(3) . . . yes C(8) Fe(1) C(12) 121.4(2) . . . yes C(8) Fe(1) C(13) 109.3(2) . . . yes C(9) Fe(1) C(10) 40.1(3) . . . yes C(9) Fe(1) C(11) 68.6(3) . . . yes C(9) Fe(1) C(12) 68.3(2) . . . yes C(9) Fe(1) C(13) 40.8(2) . . . yes C(10) Fe(1) C(11) 41.1(3) . . . yes C(10) Fe(1) C(12) 67.9(3) . . . yes C(10) Fe(1) C(13) 67.7(3) . . . yes C(11) Fe(1) C(12) 40.1(2) . . . yes C(11) Fe(1) C(13) 68.0(3) . . . yes C(12) Fe(1) C(13) 40.4(2) . . . yes C(14) Fe(2) C(15) 40.7(2) . . . yes C(14) Fe(2) C(16) 68.5(3) . . . yes C(14) Fe(2) C(17) 69.1(3) . . . yes C(14) Fe(2) C(18) 41.5(2) . . . yes C(14) Fe(2) C(19) 108.8(3) . . . yes C(14) Fe(2) C(20) 123.9(3) . . . yes C(14) Fe(2) C(21) 157.8(3) . . . yes C(14) Fe(2) C(22) 161.8(3) . . . yes C(14) Fe(2) C(23) 124.4(3) . . . yes C(15) Fe(2) C(16) 41.0(4) . . . yes C(15) Fe(2) C(17) 68.7(4) . . . yes C(15) Fe(2) C(18) 68.6(3) . . . yes C(15) Fe(2) C(19) 122.9(3) . . . yes C(15) Fe(2) C(20) 108.0(3) . . . yes C(15) Fe(2) C(21) 121.6(3) . . . yes C(15) Fe(2) C(22) 156.4(3) . . . yes C(15) Fe(2) C(23) 160.2(4) . . . yes C(16) Fe(2) C(17) 39.8(4) . . . yes C(16) Fe(2) C(18) 67.3(4) . . . yes C(16) Fe(2) C(19) 158.5(5) . . . yes C(16) Fe(2) C(20) 123.1(4) . . . yes C(16) Fe(2) C(21) 107.0(3) . . . yes C(16) Fe(2) C(22) 121.3(4) . . . yes C(16) Fe(2) C(23) 157.8(5) . . . yes C(17) Fe(2) C(18) 40.3(3) . . . yes C(17) Fe(2) C(19) 161.0(4) . . . yes C(17) Fe(2) C(20) 157.4(4) . . . yes C(17) Fe(2) C(21) 122.2(3) . . . yes C(17) Fe(2) C(22) 107.7(4) . . . yes C(17) Fe(2) C(23) 123.2(4) . . . yes C(18) Fe(2) C(19) 125.7(3) . . . yes C(18) Fe(2) C(20) 161.2(3) . . . yes C(18) Fe(2) C(21) 158.6(3) . . . yes C(18) Fe(2) C(22) 124.6(3) . . . yes C(18) Fe(2) C(23) 109.1(3) . . . yes C(19) Fe(2) C(20) 39.4(3) . . . yes C(19) Fe(2) C(21) 67.0(3) . . . yes C(19) Fe(2) C(22) 68.0(3) . . . yes C(19) Fe(2) C(23) 41.4(3) . . . yes C(20) Fe(2) C(21) 39.1(3) . . . yes C(20) Fe(2) C(22) 65.8(3) . . . yes C(20) Fe(2) C(23) 67.4(3) . . . yes C(21) Fe(2) C(22) 39.1(3) . . . yes C(21) Fe(2) C(23) 67.9(3) . . . yes C(22) Fe(2) C(23) 41.2(3) . . . yes S(1) P(1) O(1) 114.3(2) . . . yes S(1) P(1) N(1) 113.7(2) . . . yes S(1) P(1) C(4) 115.7(2) . . . yes O(1) P(1) N(1) 106.5(2) . . . yes O(1) P(1) C(4) 98.1(2) . . . yes N(1) P(1) C(4) 107.0(3) . . . yes S(2) P(2) O(1) 113.6(2) . . . yes S(2) P(2) N(2) 112.9(2) . . . yes S(2) P(2) C(14) 118.2(2) . . . yes O(1) P(2) N(2) 102.1(2) . . . yes O(1) P(2) C(14) 103.9(2) . . . yes N(2) P(2) C(14) 104.5(3) . . . yes P(1) O(1) P(2) 137.9(2) . . . yes P(1) N(1) C(1) 123.2(5) . . . yes P(1) N(1) C(2) 120.0(4) . . . yes C(1) N(1) C(2) 113.1(5) . . . yes P(2) N(2) C(3) 163.7(6) . . . yes N(1) C(1) H(1a) 109.3 . . . no N(1) C(1) H(1b) 108.8 . . . no N(1) C(1) H(1c) 109.4 . . . no H(1a) C(1) H(1b) 109.3 . . . no H(1a) C(1) H(1c) 110.1 . . . no H(1b) C(1) H(1c) 109.8 . . . no N(1) C(2) H(2a) 109.7 . . . no N(1) C(2) H(2b) 109.5 . . . no N(1) C(2) H(2c) 109.4 . . . no H(2a) C(2) H(2b) 109.7 . . . no H(2a) C(2) H(2c) 109.3 . . . no H(2b) C(2) H(2c) 109.3 . . . no S(3) C(3) N(2) 177.2(6) . . . yes Fe(1) C(4) P(1) 126.1(3) . . . yes Fe(1) C(4) C(5) 68.9(3) . . . yes Fe(1) C(4) C(8) 70.1(3) . . . yes P(1) C(4) C(5) 127.9(4) . . . yes P(1) C(4) C(8) 124.8(4) . . . yes C(5) C(4) C(8) 107.2(5) . . . yes Fe(1) C(5) C(4) 68.9(3) . . . yes Fe(1) C(5) C(6) 70.0(3) . . . yes Fe(1) C(5) H(5) 126.1 . . . no C(4) C(5) C(6) 106.0(5) . . . yes C(4) C(5) H(5) 127.9 . . . no C(6) C(5) H(5) 126.1 . . . no Fe(1) C(6) C(5) 69.2(3) . . . yes Fe(1) C(6) C(7) 70.2(3) . . . yes Fe(1) C(6) H(6) 128.1 . . . no C(5) C(6) C(7) 110.1(5) . . . yes C(5) C(6) H(6) 125.8 . . . no C(7) C(6) H(6) 124.1 . . . no Fe(1) C(7) C(6) 69.3(3) . . . yes Fe(1) C(7) C(8) 69.7(3) . . . yes Fe(1) C(7) H(7) 125.4 . . . no C(6) C(7) C(8) 107.3(5) . . . yes C(6) C(7) H(7) 126.3 . . . no C(8) C(7) H(7) 126.4 . . . no Fe(1) C(8) C(4) 68.9(3) . . . yes Fe(1) C(8) C(7) 70.1(3) . . . yes Fe(1) C(8) H(8) 127.8 . . . no C(4) C(8) C(7) 109.3(5) . . . yes C(4) C(8) H(8) 125.5 . . . no C(7) C(8) H(8) 125.2 . . . no Fe(1) C(9) C(10) 70.0(4) . . . yes Fe(1) C(9) C(13) 69.7(3) . . . yes Fe(1) C(9) H(9) 125.5 . . . no C(10) C(9) C(13) 107.5(6) . . . yes C(10) C(9) H(9) 126.5 . . . no C(13) C(9) H(9) 126.0 . . . no Fe(1) C(10) C(9) 69.9(4) . . . yes Fe(1) C(10) C(11) 69.4(4) . . . yes Fe(1) C(10) H(10) 125.7 . . . no C(9) C(10) C(11) 108.6(6) . . . yes C(9) C(10) H(10) 123.5 . . . no C(11) C(10) H(10) 127.9 . . . no Fe(1) C(11) C(10) 69.4(4) . . . yes Fe(1) C(11) C(12) 70.2(4) . . . yes Fe(1) C(11) H(11) 125.4 . . . no C(10) C(11) C(12) 107.3(6) . . . yes C(10) C(11) H(11) 126.1 . . . no C(12) C(11) H(11) 126.6 . . . no Fe(1) C(12) C(11) 69.7(4) . . . yes Fe(1) C(12) C(13) 69.6(3) . . . yes Fe(1) C(12) H(12) 126.8 . . . no C(11) C(12) C(13) 108.5(6) . . . yes C(11) C(12) H(12) 125.5 . . . no C(13) C(12) H(12) 126.0 . . . no Fe(1) C(13) C(9) 69.5(3) . . . yes Fe(1) C(13) C(12) 70.0(3) . . . yes Fe(1) C(13) H(13) 126.1 . . . no C(9) C(13) C(12) 108.1(6) . . . yes C(9) C(13) H(13) 125.4 . . . no C(12) C(13) H(13) 126.4 . . . no Fe(2) C(14) P(2) 126.5(3) . . . yes Fe(2) C(14) C(15) 70.2(4) . . . yes Fe(2) C(14) C(18) 70.5(3) . . . yes P(2) C(14) C(15) 127.6(5) . . . yes P(2) C(14) C(18) 124.7(5) . . . yes C(15) C(14) C(18) 107.7(6) . . . yes Fe(2) C(15) C(14) 69.1(4) . . . yes Fe(2) C(15) C(16) 69.9(5) . . . yes Fe(2) C(15) H(15) 125.9 . . . no C(14) C(15) C(16) 107.3(8) . . . yes C(14) C(15) H(15) 125.6 . . . no C(16) C(15) H(15) 127.1 . . . no Fe(2) C(16) C(15) 69.1(4) . . . yes Fe(2) C(16) C(17) 70.4(6) . . . yes Fe(2) C(16) H(16) 127.7 . . . no C(15) C(16) C(17) 109.3(8) . . . yes C(15) C(16) H(16) 123.9 . . . no C(17) C(16) H(16) 126.8 . . . no Fe(2) C(17) C(16) 69.8(6) . . . yes Fe(2) C(17) C(18) 70.0(4) . . . yes Fe(2) C(17) H(17) 124.1 . . . no C(16) C(17) C(18) 108.0(9) . . . yes C(16) C(17) H(17) 124.8 . . . no C(18) C(17) H(17) 127.2 . . . no Fe(2) C(18) C(14) 67.9(3) . . . yes Fe(2) C(18) C(17) 69.7(4) . . . yes Fe(2) C(18) H(18) 129.4 . . . no C(14) C(18) C(17) 107.7(7) . . . yes C(14) C(18) H(18) 126.2 . . . no C(17) C(18) H(18) 126.1 . . . no Fe(2) C(19) C(20) 70.0(4) . . . yes Fe(2) C(19) C(23) 69.6(4) . . . yes Fe(2) C(19) H(19) 125.9 . . . no C(20) C(19) C(23) 107.1(7) . . . yes C(20) C(19) H(19) 126.4 . . . no C(23) C(19) H(19) 126.6 . . . no Fe(2) C(20) C(19) 70.6(4) . . . yes Fe(2) C(20) C(21) 70.7(4) . . . yes Fe(2) C(20) H(20) 126.0 . . . no C(19) C(20) C(21) 110.8(7) . . . yes C(19) C(20) H(20) 124.8 . . . no C(21) C(20) H(20) 124.4 . . . no Fe(2) C(21) C(20) 70.2(4) . . . yes Fe(2) C(21) C(22) 70.4(4) . . . yes Fe(2) C(21) H(21) 124.6 . . . no C(20) C(21) C(22) 108.3(7) . . . yes C(20) C(21) H(21) 126.0 . . . no C(22) C(21) H(21) 125.6 . . . no Fe(2) C(22) C(21) 70.4(4) . . . yes Fe(2) C(22) C(23) 69.7(4) . . . yes Fe(2) C(22) H(22) 125.3 . . . no C(21) C(22) C(23) 109.0(7) . . . yes C(21) C(22) H(22) 125.5 . . . no C(23) C(22) H(22) 125.5 . . . no Fe(2) C(23) C(19) 69.1(4) . . . yes Fe(2) C(23) C(22) 69.1(4) . . . yes Fe(2) C(23) H(23) 124.9 . . . no C(19) C(23) C(22) 104.7(6) . . . yes C(19) C(23) H(23) 127.1 . . . no C(22) C(23) H(23) 128.1 . . . 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(3) C(17) 3.552(8) . 1_554 no C(2) C(7) 3.567(9) . 2_766 no C(7) C(20) 3.559(9) . 1_656 no C(7) C(19) 3.563(9) . 1_656 no #===END data_10 #----------------------------------------------------------------------- _audit_creation_date '1998-11-25' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #----------------------------------------------------------------------- _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Walker, N. & Stuart. D. (1983). Acta Cryst. A39, 158-166. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. ; #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #----------------------------------------------------------------------- _cell_length_a 7.347(2) _cell_length_b 14.262(3) _cell_length_c 25.660(2) _cell_angle_alpha 90.00(1) _cell_angle_beta 95.75(1) _cell_angle_gamma 90.00(2) _cell_volume 2675.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 17 _cell_measurement_theta_min 25.1 _cell_measurement_theta_max 32.4 #----------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 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 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 633.32 _chemical_formula_analytical 'C27 H25 Fe2 N P2 S3 ' _chemical_formula_sum 'C27 H25 Fe2 N P2 S3 ' _chemical_formula_moiety 'C27 H25 Fe2 N P2 S3 ' _chemical_formula_structural 'C27 H25 Fe2 N P2 S3 ' _chemical_compound_source - _exptl_crystal_F_000 1296.00 _exptl_absorpt_coefficient_mu 12.154 _exptl_absorpt_correction_type ; \DF (DIFABS; Walker & Stuart, 1983) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.252 _exptl_special_details ; The scan width was (0.73+0.35tan\q)\% with an \w scan speed of 16\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #----------------------------------------------------------------------- _diffrn_special_details ; - ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.12 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 2 -9 2 1 -8 0 3 -7 _diffrn_reflns_number 4535 _reflns_number_total 4194 _reflns_number_gt 2100 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.34831 _diffrn_reflns_av_sigmaI/netI 0.120 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 60.10 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.01997 _diffrn_orient_matrix_UB_12 0.06776 _diffrn_orient_matrix_UB_13 -0.00767 _diffrn_orient_matrix_UB_21 0.00774 _diffrn_orient_matrix_UB_22 0.01439 _diffrn_orient_matrix_UB_23 0.03830 _diffrn_orient_matrix_UB_31 0.13511 _diffrn_orient_matrix_UB_32 -0.01084 _diffrn_orient_matrix_UB_33 0.00291 #----------------------------------------------------------------------- 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 0 108 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 100 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 4 0.029 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 8 0.283 0.434 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 12 0.319 0.557 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Fe 0 8 -1.179 3.204 ;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_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Fe(1) 0.3028(2) 0.1275(1) 0.42119(5) 0.0462(5) 1.000 . Uani d ? Fe(2) 0.0871(2) 0.2336(1) 0.12150(6) 0.0481(5) 1.000 . Uani d ? S(1) 0.6399(4) 0.1224(2) 0.2935(1) 0.070(1) 1.000 . Uani d ? S(2) 0.1775(4) 0.1779(2) 0.27260(9) 0.0585(9) 1.000 . Uani d ? S(3) 0.0667(4) 0.4150(2) 0.2535(1) 0.067(1) 1.000 . Uani d ? P(1) 0.4439(4) 0.2039(2) 0.30836(9) 0.0495(9) 1.000 . Uani d ? P(2) 0.2268(3) 0.3117(2) 0.24216(9) 0.0474(8) 1.000 . Uani d ? N(1) 0.430(1) 0.3074(6) 0.2785(3) 0.047(3) 1.000 . Uani d ? C(1) 0.570(1) 0.3814(8) 0.2828(4) 0.058(4) 1.000 . Uani d ? C(2) 0.616(1) 0.4147(9) 0.3390(4) 0.057(4) 1.000 . Uani d ? C(3) 0.493(2) 0.4685(9) 0.3626(5) 0.068(4) 1.000 . Uani d ? C(4) 0.524(2) 0.493(1) 0.4145(6) 0.093(6) 1.000 . Uani d ? C(5) 0.678(2) 0.462(1) 0.4437(5) 0.095(6) 1.000 . Uani d ? C(6) 0.799(2) 0.405(1) 0.4204(5) 0.083(5) 1.000 . Uani d ? C(7) 0.769(1) 0.3812(9) 0.3676(4) 0.068(4) 1.000 . Uani d ? C(11) 0.424(1) 0.2200(7) 0.3767(3) 0.048(3) 1.000 . Uani d ? C(12) 0.279(1) 0.2608(9) 0.3987(4) 0.064(4) 1.000 . Uani d ? C(13) 0.313(1) 0.2562(9) 0.4544(4) 0.061(4) 1.000 . Uani d ? C(14) 0.478(2) 0.2123(8) 0.4660(3) 0.056(4) 1.000 . Uani d ? C(15) 0.552(1) 0.1870(9) 0.4188(4) 0.061(4) 1.000 . Uani d ? C(16) 0.220(2) 0.0180(9) 0.3752(4) 0.070(5) 1.000 . Uani d ? C(17) 0.071(2) 0.063(1) 0.3946(5) 0.078(5) 1.000 . Uani d ? C(18) 0.091(2) 0.057(1) 0.4489(4) 0.077(5) 1.000 . Uani d ? C(19) 0.255(2) 0.0142(9) 0.4648(4) 0.062(4) 1.000 . Uani d ? C(20) 0.334(2) -0.0135(9) 0.4193(5) 0.075(5) 1.000 . Uani d ? C(21) 0.267(1) 0.2965(7) 0.1754(3) 0.041(3) 1.000 . Uani d ? C(22) 0.211(1) 0.3607(8) 0.1347(4) 0.052(4) 1.000 . Uani d ? C(23) 0.265(2) 0.3187(9) 0.0878(3) 0.063(4) 1.000 . Uani d ? C(24) 0.346(1) 0.2336(8) 0.0991(4) 0.053(4) 1.000 . Uani d ? C(25) 0.349(1) 0.2174(8) 0.1539(4) 0.051(4) 1.000 . Uani d ? C(26) -0.135(2) 0.186(1) 0.1558(4) 0.076(5) 1.000 . Uani d ? C(27) -0.190(1) 0.253(1) 0.1159(6) 0.080(5) 1.000 . Uani d ? C(28) -0.136(2) 0.217(1) 0.0690(6) 0.093(6) 1.000 . Uani d ? C(29) -0.048(2) 0.135(1) 0.0785(6) 0.093(6) 1.000 . Uani d ? C(30) -0.052(2) 0.112(1) 0.1311(7) 0.088(6) 1.000 . Uani d ? H(1a) 0.6780 0.3574 0.2701 0.070 1.000 . Uiso c ? H(1b) 0.5260 0.4330 0.2619 0.070 1.000 . Uiso c ? H(3) 0.3860 0.4905 0.3426 0.082 1.000 . Uiso c ? H(4) 0.4381 0.5318 0.4300 0.113 1.000 . Uiso c ? H(5) 0.7015 0.4793 0.4795 0.116 1.000 . Uiso c ? H(6) 0.9048 0.3817 0.4408 0.100 1.000 . Uiso c ? H(7) 0.8530 0.3417 0.3518 0.083 1.000 . Uiso c ? H(12) 0.1731 0.2871 0.3798 0.076 1.000 . Uiso c ? H(13) 0.2354 0.2790 0.4789 0.073 1.000 . Uiso c ? H(14) 0.5345 0.2009 0.5002 0.066 1.000 . Uiso c ? H(15) 0.6638 0.1552 0.4158 0.073 1.000 . Uiso c ? H(16) 0.2407 0.0093 0.3395 0.085 1.000 . Uiso c ? H(17) -0.0273 0.0919 0.3740 0.094 1.000 . Uiso c ? H(18) 0.0060 0.0783 0.4715 0.093 1.000 . Uiso c ? H(19) 0.3063 0.0052 0.4999 0.074 1.000 . Uiso c ? H(20) 0.4450 -0.0480 0.4185 0.090 1.000 . Uiso c ? H(22) 0.1505 0.4196 0.1379 0.063 1.000 . Uiso c ? H(23) 0.2468 0.3466 0.0540 0.077 1.000 . Uiso c ? H(24) 0.3931 0.1925 0.0745 0.065 1.000 . Uiso c ? H(25) 0.3957 0.1634 0.1725 0.061 1.000 . Uiso c ? H(26) -0.1501 0.1901 0.1919 0.092 1.000 . Uiso c ? H(27) -0.2514 0.3103 0.1201 0.097 1.000 . Uiso c ? H(28) -0.1575 0.2447 0.0355 0.111 1.000 . Uiso c ? H(29) 0.0095 0.0974 0.0539 0.110 1.000 . Uiso c ? H(30) -0.0066 0.0549 0.1473 0.105 1.000 . Uiso c ? 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) 0.0370(9) 0.072(1) 0.0334(9) -0.0074(9) 0.0206(7) 0.0062(8) Fe(2) 0.0350(9) 0.074(1) 0.0377(9) 0.0012(9) 0.0170(7) 0.0059(8) S(1) 0.064(2) 0.099(3) 0.053(2) 0.016(2) 0.028(1) 0.002(2) S(2) 0.050(2) 0.086(2) 0.041(1) -0.019(2) 0.013(1) 0.014(1) S(3) 0.049(2) 0.097(3) 0.060(2) 0.012(2) 0.032(1) -0.004(2) P(1) 0.038(2) 0.080(2) 0.034(1) -0.006(2) 0.023(1) 0.006(1) P(2) 0.033(1) 0.078(2) 0.036(1) -0.004(2) 0.025(1) 0.004(1) N(1) 0.031(5) 0.077(7) 0.035(5) -0.010(5) 0.015(3) 0.009(4) C(1) 0.036(6) 0.081(9) 0.061(7) -0.004(6) 0.025(5) 0.016(6) C(2) 0.038(7) 0.08(1) 0.052(7) -0.016(7) 0.019(5) -0.009(6) C(3) 0.056(8) 0.08(1) 0.070(8) 0.000(7) 0.017(6) 0.003(7) C(4) 0.08(1) 0.11(1) 0.10(1) -0.02(1) 0.048(9) -0.019(9) C(5) 0.10(1) 0.13(2) 0.055(9) -0.03(1) 0.027(8) -0.022(8) C(6) 0.072(9) 0.11(1) 0.063(9) -0.016(9) 0.004(7) 0.015(8) C(7) 0.048(7) 0.11(1) 0.054(8) -0.016(7) 0.018(6) 0.005(7) C(11) 0.050(6) 0.062(8) 0.036(6) -0.008(6) 0.027(5) -0.005(5) C(12) 0.044(7) 0.11(1) 0.036(6) 0.003(7) 0.018(5) -0.001(6) C(13) 0.055(7) 0.10(1) 0.037(6) 0.001(7) 0.025(5) 0.015(6) C(14) 0.063(8) 0.077(9) 0.029(6) -0.021(7) 0.019(5) -0.010(5) C(15) 0.040(7) 0.09(1) 0.050(7) -0.010(7) 0.010(5) -0.004(6) C(16) 0.078(9) 0.09(1) 0.045(7) -0.016(8) 0.013(7) 0.008(6) C(17) 0.056(8) 0.09(1) 0.09(1) -0.022(8) 0.009(7) 0.027(8) C(18) 0.075(9) 0.11(1) 0.048(7) -0.021(9) 0.029(6) 0.031(7) C(19) 0.053(8) 0.09(1) 0.041(7) -0.007(7) 0.003(6) 0.004(6) C(20) 0.063(9) 0.08(1) 0.080(9) -0.001(7) 0.013(7) 0.000(7) C(21) 0.036(6) 0.054(7) 0.037(5) -0.001(5) 0.025(4) -0.002(5) C(22) 0.042(6) 0.064(9) 0.054(7) 0.005(6) 0.019(5) 0.013(6) C(23) 0.069(8) 0.10(1) 0.027(6) -0.003(8) 0.027(5) 0.020(6) C(24) 0.064(7) 0.063(8) 0.037(6) 0.003(6) 0.035(5) 0.004(5) C(25) 0.035(6) 0.075(9) 0.045(6) 0.008(6) 0.022(5) 0.012(5) C(26) 0.048(8) 0.13(1) 0.057(8) -0.017(9) 0.018(6) 0.003(8) C(27) 0.021(6) 0.09(1) 0.13(1) -0.003(7) 0.013(7) -0.01(1) C(28) 0.043(8) 0.14(2) 0.10(1) -0.007(9) 0.005(8) 0.04(1) C(29) 0.07(1) 0.13(2) 0.08(1) -0.01(1) 0.013(8) -0.03(1) C(30) 0.066(9) 0.07(1) 0.13(1) -0.009(8) 0.012(9) 0.026(9) #----------------------------------------------------------------------- _refine_special_details ; - ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.0000030(2) _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 2100 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_all 0.0582 _refine_ls_wR_factor_ref 0.0582 _refine_ls_goodness_of_fit_all 2.316 _refine_ls_goodness_of_fit_ref 2.316 _refine_ls_shift/esd_max 0.0280 _refine_ls_shift/esd_mean 0.0520 _refine_diff_density_min -0.77 _refine_diff_density_max 0.56 #----------------------------------------------------------------------- _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) C(11) 2.010(9) . . yes Fe(1) C(12) 1.99(1) . . yes Fe(1) C(13) 2.02(1) . . yes Fe(1) C(14) 2.04(1) . . yes Fe(1) C(15) 2.03(1) . . yes Fe(1) C(16) 2.01(1) . . yes Fe(1) C(17) 2.00(1) . . yes Fe(1) C(18) 2.04(1) . . yes Fe(1) C(19) 2.02(1) . . yes Fe(1) C(20) 2.02(1) . . yes Fe(2) C(21) 2.022(9) . . yes Fe(2) C(22) 2.04(1) . . yes Fe(2) C(23) 2.04(1) . . yes Fe(2) C(24) 2.04(1) . . yes Fe(2) C(25) 2.029(9) . . yes Fe(2) C(26) 2.04(1) . . yes Fe(2) C(27) 2.05(1) . . yes Fe(2) C(28) 2.03(1) . . yes Fe(2) C(29) 1.99(1) . . yes Fe(2) C(30) 2.04(1) . . yes S(1) P(1) 1.918(4) . . yes S(2) P(1) 2.110(4) . . yes S(2) P(2) 2.108(4) . . yes S(3) P(2) 1.925(4) . . yes P(1) N(1) 1.661(8) . . yes P(1) C(11) 1.790(9) . . yes P(2) N(1) 1.680(7) . . yes P(2) C(21) 1.781(9) . . yes N(1) C(1) 1.47(1) . . yes C(1) C(2) 1.52(1) . . yes C(1) H(1a) 0.95 . . no C(1) H(1b) 0.95 . . no C(2) C(3) 1.37(1) . . yes C(2) C(7) 1.37(1) . . yes C(3) C(4) 1.37(1) . . yes C(3) H(3) 0.95 . . no C(4) C(5) 1.37(2) . . yes C(4) H(4) 0.96 . . no C(5) C(6) 1.38(2) . . yes C(5) H(5) 0.95 . . no C(6) C(7) 1.39(1) . . yes C(6) H(6) 0.95 . . no C(7) H(7) 0.95 . . no C(11) C(12) 1.38(1) . . yes C(11) C(15) 1.44(1) . . yes C(12) C(13) 1.43(1) . . yes C(12) H(12) 0.95 . . no C(13) C(14) 1.37(1) . . yes C(13) H(13) 0.95 . . no C(14) C(15) 1.42(1) . . yes C(14) H(14) 0.95 . . no C(15) H(15) 0.95 . . no C(16) C(17) 1.40(2) . . yes C(16) C(20) 1.41(1) . . yes C(16) H(16) 0.95 . . no C(17) C(18) 1.39(1) . . yes C(17) H(17) 0.94 . . no C(18) C(19) 1.37(1) . . yes C(18) H(18) 0.95 . . no C(19) C(20) 1.41(1) . . yes C(19) H(19) 0.95 . . no C(20) H(20) 0.95 . . no C(21) C(22) 1.42(1) . . yes C(21) C(25) 1.42(1) . . yes C(22) C(23) 1.43(1) . . yes C(22) H(22) 0.96 . . no C(23) C(24) 1.37(1) . . yes C(23) H(23) 0.95 . . no C(24) C(25) 1.42(1) . . yes C(24) H(24) 0.95 . . no C(25) H(25) 0.95 . . no C(26) C(27) 1.43(2) . . yes C(26) C(30) 1.40(2) . . yes C(26) H(26) 0.95 . . no C(27) C(28) 1.40(2) . . yes C(27) H(27) 0.95 . . no C(28) C(29) 1.35(2) . . yes C(28) H(28) 0.94 . . no C(29) C(30) 1.39(2) . . yes C(29) H(29) 0.96 . . no C(30) H(30) 0.96 . . no #----------------------------------------------------------------------- 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 C(11) Fe(1) C(12) 40.5(4) . . . yes C(11) Fe(1) C(13) 69.0(4) . . . yes C(11) Fe(1) C(14) 68.8(4) . . . yes C(11) Fe(1) C(15) 41.8(4) . . . yes C(11) Fe(1) C(16) 107.5(4) . . . yes C(11) Fe(1) C(17) 121.4(4) . . . yes C(11) Fe(1) C(18) 156.8(5) . . . yes C(11) Fe(1) C(19) 162.3(5) . . . yes C(11) Fe(1) C(20) 125.5(5) . . . yes C(12) Fe(1) C(13) 41.7(4) . . . yes C(12) Fe(1) C(14) 68.2(4) . . . yes C(12) Fe(1) C(15) 69.3(5) . . . yes C(12) Fe(1) C(16) 123.9(4) . . . yes C(12) Fe(1) C(17) 107.1(5) . . . yes C(12) Fe(1) C(18) 121.7(5) . . . yes C(12) Fe(1) C(19) 155.7(5) . . . yes C(12) Fe(1) C(20) 161.6(5) . . . yes C(13) Fe(1) C(14) 39.4(4) . . . yes C(13) Fe(1) C(15) 68.6(4) . . . yes C(13) Fe(1) C(16) 161.3(5) . . . yes C(13) Fe(1) C(17) 124.0(5) . . . yes C(13) Fe(1) C(18) 107.5(5) . . . yes C(13) Fe(1) C(19) 119.7(4) . . . yes C(13) Fe(1) C(20) 155.8(4) . . . yes C(14) Fe(1) C(15) 40.9(4) . . . yes C(14) Fe(1) C(16) 158.1(5) . . . yes C(14) Fe(1) C(17) 159.6(5) . . . yes C(14) Fe(1) C(18) 124.0(4) . . . yes C(14) Fe(1) C(19) 107.4(4) . . . yes C(14) Fe(1) C(20) 122.4(5) . . . yes C(15) Fe(1) C(16) 121.8(5) . . . yes C(15) Fe(1) C(17) 157.9(5) . . . yes C(15) Fe(1) C(18) 160.2(4) . . . yes C(15) Fe(1) C(19) 124.1(5) . . . yes C(15) Fe(1) C(20) 108.0(5) . . . yes C(16) Fe(1) C(17) 41.0(5) . . . yes C(16) Fe(1) C(18) 68.0(5) . . . yes C(16) Fe(1) C(19) 69.2(4) . . . yes C(16) Fe(1) C(20) 40.9(4) . . . yes C(17) Fe(1) C(18) 40.2(4) . . . yes C(17) Fe(1) C(19) 68.3(4) . . . yes C(17) Fe(1) C(20) 68.2(5) . . . yes C(18) Fe(1) C(19) 39.6(4) . . . yes C(18) Fe(1) C(20) 67.1(5) . . . yes C(19) Fe(1) C(20) 40.9(4) . . . yes C(21) Fe(2) C(22) 40.9(4) . . . yes C(21) Fe(2) C(23) 67.9(4) . . . yes C(21) Fe(2) C(24) 68.3(4) . . . yes C(21) Fe(2) C(25) 41.0(4) . . . yes C(21) Fe(2) C(26) 110.3(4) . . . yes C(21) Fe(2) C(27) 124.4(5) . . . yes C(21) Fe(2) C(28) 159.0(6) . . . yes C(21) Fe(2) C(29) 161.3(6) . . . yes C(21) Fe(2) C(30) 126.5(5) . . . yes C(22) Fe(2) C(23) 41.2(4) . . . yes C(22) Fe(2) C(24) 68.6(4) . . . yes C(22) Fe(2) C(25) 69.2(4) . . . yes C(22) Fe(2) C(26) 125.8(5) . . . yes C(22) Fe(2) C(27) 108.5(5) . . . yes C(22) Fe(2) C(28) 122.0(6) . . . yes C(22) Fe(2) C(29) 155.3(6) . . . yes C(22) Fe(2) C(30) 162.8(6) . . . yes C(23) Fe(2) C(24) 39.3(4) . . . yes C(23) Fe(2) C(25) 67.7(4) . . . yes C(23) Fe(2) C(26) 162.3(6) . . . yes C(23) Fe(2) C(27) 124.5(6) . . . yes C(23) Fe(2) C(28) 107.3(5) . . . yes C(23) Fe(2) C(29) 119.4(5) . . . yes C(23) Fe(2) C(30) 155.1(6) . . . yes C(24) Fe(2) C(25) 40.9(3) . . . yes C(24) Fe(2) C(26) 157.9(6) . . . yes C(24) Fe(2) C(27) 158.4(5) . . . yes C(24) Fe(2) C(28) 121.9(5) . . . yes C(24) Fe(2) C(29) 105.7(5) . . . yes C(24) Fe(2) C(30) 121.7(6) . . . yes C(25) Fe(2) C(26) 123.3(5) . . . yes C(25) Fe(2) C(27) 159.9(5) . . . yes C(25) Fe(2) C(28) 158.1(6) . . . yes C(25) Fe(2) C(29) 123.0(6) . . . yes C(25) Fe(2) C(30) 108.6(5) . . . yes C(26) Fe(2) C(27) 40.8(5) . . . yes C(26) Fe(2) C(28) 67.7(5) . . . yes C(26) Fe(2) C(29) 68.3(5) . . . yes C(26) Fe(2) C(30) 40.2(5) . . . yes C(27) Fe(2) C(28) 40.2(5) . . . yes C(27) Fe(2) C(29) 67.6(5) . . . yes C(27) Fe(2) C(30) 67.4(6) . . . yes C(28) Fe(2) C(29) 39.3(6) . . . yes C(28) Fe(2) C(30) 66.4(5) . . . yes C(29) Fe(2) C(30) 40.3(5) . . . yes P(1) S(2) P(2) 79.3(1) . . . yes S(1) P(1) S(2) 119.3(2) . . . yes S(1) P(1) N(1) 117.3(3) . . . yes S(1) P(1) C(11) 114.2(4) . . . yes S(2) P(1) N(1) 86.8(3) . . . yes S(2) P(1) C(11) 106.6(3) . . . yes N(1) P(1) C(11) 109.3(5) . . . yes S(2) P(2) S(3) 120.4(2) . . . yes S(2) P(2) N(1) 86.4(3) . . . yes S(2) P(2) C(21) 107.3(4) . . . yes S(3) P(2) N(1) 117.8(3) . . . yes S(3) P(2) C(21) 113.6(4) . . . yes N(1) P(2) C(21) 107.9(4) . . . yes P(1) N(1) P(2) 107.4(5) . . . yes P(1) N(1) C(1) 126.3(6) . . . yes P(2) N(1) C(1) 126.3(7) . . . yes N(1) C(1) C(2) 112.5(8) . . . yes N(1) C(1) H(1a) 108.5 . . . no N(1) C(1) H(1b) 108.5 . . . no C(2) C(1) H(1a) 108.8 . . . no C(2) C(1) H(1b) 109.0 . . . no H(1a) C(1) H(1b) 109.5 . . . no C(1) C(2) C(3) 120(1) . . . yes C(1) C(2) C(7) 119(1) . . . yes C(3) C(2) C(7) 120(1) . . . yes C(2) C(3) C(4) 121(1) . . . yes C(2) C(3) H(3) 119.6 . . . no C(4) C(3) H(3) 119.1 . . . no C(3) C(4) C(5) 120(1) . . . yes C(3) C(4) H(4) 120.0 . . . no C(5) C(4) H(4) 120.3 . . . no C(4) C(5) C(6) 119(1) . . . yes C(4) C(5) H(5) 120.1 . . . no C(6) C(5) H(5) 120.9 . . . no C(5) C(6) C(7) 121(1) . . . yes C(5) C(6) H(6) 119.2 . . . no C(7) C(6) H(6) 119.7 . . . no C(2) C(7) C(6) 119(1) . . . yes C(2) C(7) H(7) 120.7 . . . no C(6) C(7) H(7) 120.6 . . . no Fe(1) C(11) P(1) 123.8(5) . . . yes Fe(1) C(11) C(12) 69.0(6) . . . yes Fe(1) C(11) C(15) 69.7(6) . . . yes P(1) C(11) C(12) 126.5(8) . . . yes P(1) C(11) C(15) 125.6(8) . . . yes C(12) C(11) C(15) 107.8(8) . . . yes Fe(1) C(12) C(11) 70.5(7) . . . yes Fe(1) C(12) C(13) 70.4(7) . . . yes Fe(1) C(12) H(12) 124.7 . . . no C(11) C(12) C(13) 108.7(9) . . . yes C(11) C(12) H(12) 125.7 . . . no C(13) C(12) H(12) 125.6 . . . no Fe(1) C(13) C(12) 67.9(7) . . . yes Fe(1) C(13) C(14) 70.9(7) . . . yes Fe(1) C(13) H(13) 126.1 . . . no C(12) C(13) C(14) 107.6(9) . . . yes C(12) C(13) H(13) 126.1 . . . no C(14) C(13) H(13) 126.3 . . . no Fe(1) C(14) C(13) 69.7(7) . . . yes Fe(1) C(14) C(15) 69.1(6) . . . yes Fe(1) C(14) H(14) 127.9 . . . no C(13) C(14) C(15) 109.7(9) . . . yes C(13) C(14) H(14) 125.0 . . . no C(15) C(14) H(14) 125.3 . . . no Fe(1) C(15) C(11) 68.5(5) . . . yes Fe(1) C(15) C(14) 69.9(6) . . . yes Fe(1) C(15) H(15) 126.5 . . . no C(11) C(15) C(14) 106(1) . . . yes C(11) C(15) H(15) 127.0 . . . no C(14) C(15) H(15) 126.9 . . . no Fe(1) C(16) C(17) 68.9(8) . . . yes Fe(1) C(16) C(20) 69.9(7) . . . yes Fe(1) C(16) H(16) 126.7 . . . no C(17) C(16) C(20) 106(1) . . . yes C(17) C(16) H(16) 127.2 . . . no C(20) C(16) H(16) 126.3 . . . no Fe(1) C(17) C(16) 70.1(7) . . . yes Fe(1) C(17) C(18) 71.5(7) . . . yes Fe(1) C(17) H(17) 124.3 . . . no C(16) C(17) C(18) 108(1) . . . yes C(16) C(17) H(17) 125.6 . . . no C(18) C(17) H(17) 125.9 . . . no Fe(1) C(18) C(17) 68.3(6) . . . yes Fe(1) C(18) C(19) 69.3(7) . . . yes Fe(1) C(18) H(18) 128.9 . . . no C(17) C(18) C(19) 109(1) . . . yes C(17) C(18) H(18) 125.6 . . . no C(19) C(18) H(18) 125.2 . . . no Fe(1) C(19) C(18) 71.2(7) . . . yes Fe(1) C(19) C(20) 69.9(7) . . . yes Fe(1) C(19) H(19) 124.1 . . . no C(18) C(19) C(20) 107.4(9) . . . yes C(18) C(19) H(19) 126.4 . . . no C(20) C(19) H(19) 126.2 . . . no Fe(1) C(20) C(16) 69.1(7) . . . yes Fe(1) C(20) C(19) 69.2(8) . . . yes Fe(1) C(20) H(20) 127.9 . . . no C(16) C(20) C(19) 108(1) . . . yes C(16) C(20) H(20) 125.9 . . . no C(19) C(20) H(20) 125.8 . . . no Fe(2) C(21) P(2) 123.6(5) . . . yes Fe(2) C(21) C(22) 70.3(6) . . . yes Fe(2) C(21) C(25) 69.8(6) . . . yes P(2) C(21) C(22) 124.5(8) . . . yes P(2) C(21) C(25) 126.1(8) . . . yes C(22) C(21) C(25) 109.3(8) . . . yes Fe(2) C(22) C(21) 68.9(6) . . . yes Fe(2) C(22) C(23) 69.2(6) . . . yes Fe(2) C(22) H(22) 126.2 . . . no C(21) C(22) C(23) 105(1) . . . yes C(21) C(22) H(22) 127.2 . . . no C(23) C(22) H(22) 127.5 . . . no Fe(2) C(23) C(22) 69.6(6) . . . yes Fe(2) C(23) C(24) 70.7(6) . . . yes Fe(2) C(23) H(23) 126.9 . . . no C(22) C(23) C(24) 110.2(8) . . . yes C(22) C(23) H(23) 124.4 . . . no C(24) C(23) H(23) 125.5 . . . no Fe(2) C(24) C(23) 70.1(6) . . . yes Fe(2) C(24) C(25) 69.0(5) . . . yes Fe(2) C(24) H(24) 126.5 . . . no C(23) C(24) C(25) 108.3(9) . . . yes C(23) C(24) H(24) 125.8 . . . no C(25) C(24) H(24) 125.9 . . . no Fe(2) C(25) C(21) 69.3(5) . . . yes Fe(2) C(25) C(24) 70.1(6) . . . yes Fe(2) C(25) H(25) 125.3 . . . no C(21) C(25) C(24) 107.0(9) . . . yes C(21) C(25) H(25) 126.5 . . . no C(24) C(25) H(25) 126.5 . . . no Fe(2) C(26) C(27) 69.7(7) . . . yes Fe(2) C(26) C(30) 69.8(7) . . . yes Fe(2) C(26) H(26) 125.5 . . . no C(27) C(26) C(30) 107(1) . . . yes C(27) C(26) H(26) 127.4 . . . no C(30) C(26) H(26) 126.0 . . . no Fe(2) C(27) C(26) 69.5(7) . . . yes Fe(2) C(27) C(28) 69.3(7) . . . yes Fe(2) C(27) H(27) 126.1 . . . no C(26) C(27) C(28) 107(1) . . . yes C(26) C(27) H(27) 126.9 . . . no C(28) C(27) H(27) 126.2 . . . no Fe(2) C(28) C(27) 70.5(7) . . . yes Fe(2) C(28) C(29) 68.8(8) . . . yes Fe(2) C(28) H(28) 127.3 . . . no C(27) C(28) C(29) 109(1) . . . yes C(27) C(28) H(28) 126.6 . . . no C(29) C(28) H(28) 123.9 . . . no Fe(2) C(29) C(28) 71.9(9) . . . yes Fe(2) C(29) C(30) 71.8(8) . . . yes Fe(2) C(29) H(29) 122.2 . . . no C(28) C(29) C(30) 109(1) . . . yes C(28) C(29) H(29) 127.1 . . . no C(30) C(29) H(29) 124.1 . . . no Fe(2) C(30) C(26) 70.0(8) . . . yes Fe(2) C(30) C(29) 67.8(8) . . . yes Fe(2) C(30) H(30) 128.2 . . . no C(26) C(30) C(29) 108(1) . . . yes C(26) C(30) H(30) 126.1 . . . no C(29) C(30) H(30) 125.7 . . . 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 C(4) C(24) 3.59(2) . 2_655 no C(17) C(22) 3.58(2) . 2_545 no C(18) C(18) 3.46(2) . 3_556 no C(20) C(27) 3.59(2) . 2_545 no C(24) C(27) 3.40(2) . 1_655 no #----------------------------------------------------------------------- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Fe(1) C(11) P(1) S(1) . . . . -80.2(6) no Fe(1) C(11) P(1) S(2) . . . . 53.6(7) no Fe(1) C(11) P(1) N(1) . . . . 146.0(6) no Fe(1) C(11) C(12) C(13) . . . . 60.3(8) no Fe(1) C(11) C(15) C(14) . . . . -60.2(8) no Fe(1) C(12) C(11) P(1) . . . . 117.2(9) no Fe(1) C(12) C(11) C(15) . . . . -59.1(8) no Fe(1) C(12) C(13) C(14) . . . . 60.0(8) no Fe(1) C(13) C(12) C(11) . . . . -60.4(9) no Fe(1) C(13) C(14) C(15) . . . . 57.6(8) no Fe(1) C(14) C(13) C(12) . . . . -58.2(8) no Fe(1) C(14) C(15) C(11) . . . . 59.2(7) no Fe(1) C(15) C(11) P(1) . . . . -117.7(8) no Fe(1) C(15) C(11) C(12) . . . . 58.6(8) no Fe(1) C(15) C(14) C(13) . . . . -57.9(9) no Fe(1) C(16) C(17) C(18) . . . . -61.5(9) no Fe(1) C(16) C(20) C(19) . . . . 58.3(9) no Fe(1) C(17) C(16) C(20) . . . . 60.2(9) no Fe(1) C(17) C(18) C(19) . . . . -57.2(9) no Fe(1) C(18) C(17) C(16) . . . . 60.6(9) no Fe(1) C(18) C(19) C(20) . . . . -60.8(9) no Fe(1) C(19) C(18) C(17) . . . . 56.6(9) no Fe(1) C(19) C(20) C(16) . . . . -58.2(9) no Fe(1) C(20) C(16) C(17) . . . . -59.5(9) no Fe(1) C(20) C(19) C(18) . . . . 61.6(9) no Fe(2) C(21) P(2) S(2) . . . . 56.6(6) no Fe(2) C(21) P(2) S(3) . . . . -79.0(6) no Fe(2) C(21) P(2) N(1) . . . . 148.4(6) no Fe(2) C(21) C(22) C(23) . . . . -60.0(7) no Fe(2) C(21) C(25) C(24) . . . . 60.3(7) no Fe(2) C(22) C(21) P(2) . . . . -117.8(8) no Fe(2) C(22) C(21) C(25) . . . . 59.1(7) no Fe(2) C(22) C(23) C(24) . . . . -59.1(9) no Fe(2) C(23) C(22) C(21) . . . . 59.8(7) no Fe(2) C(23) C(24) C(25) . . . . -58.5(8) no Fe(2) C(24) C(23) C(22) . . . . 58.5(8) no Fe(2) C(24) C(25) C(21) . . . . -59.8(7) no Fe(2) C(25) C(21) P(2) . . . . 117.5(8) no Fe(2) C(25) C(21) C(22) . . . . -59.4(7) no Fe(2) C(25) C(24) C(23) . . . . 59.2(8) no Fe(2) C(26) C(27) C(28) . . . . 59.5(9) no Fe(2) C(26) C(30) C(29) . . . . -57(1) no Fe(2) C(27) C(26) C(30) . . . . -60.4(9) no Fe(2) C(27) C(28) C(29) . . . . 58(1) no Fe(2) C(28) C(27) C(26) . . . . -59.7(8) no Fe(2) C(28) C(29) C(30) . . . . 63(1) no Fe(2) C(29) C(28) C(27) . . . . -59(1) no Fe(2) C(29) C(30) C(26) . . . . 58(1) no Fe(2) C(30) C(26) C(27) . . . . 60.3(9) no Fe(2) C(30) C(29) C(28) . . . . -63(1) no S(1) P(1) S(2) P(2) . . . . -118.2(2) no S(1) P(1) N(1) P(2) . . . . 119.5(3) no S(1) P(1) N(1) C(1) . . . . -60.2(8) no S(1) P(1) C(11) C(12) . . . . -168(1) no S(1) P(1) C(11) C(15) . . . . 8(1) no S(2) P(1) N(1) P(2) . . . . -2.0(4) no S(2) P(1) N(1) C(1) . . . . 178.3(7) no S(2) P(1) C(11) C(12) . . . . -34(1) no S(2) P(1) C(11) C(15) . . . . 141.7(9) no S(2) P(2) N(1) P(1) . . . . 2.0(4) no S(2) P(2) N(1) C(1) . . . . -178.3(7) no S(2) P(2) C(21) C(22) . . . . 144.7(8) no S(2) P(2) C(21) C(25) . . . . -31.7(9) no S(3) P(2) S(2) P(1) . . . . -121.9(2) no S(3) P(2) N(1) P(1) . . . . 124.7(4) no S(3) P(2) N(1) C(1) . . . . -55.6(8) no S(3) P(2) C(21) C(22) . . . . 9(1) no S(3) P(2) C(21) C(25) . . . . -167.4(8) no P(1) S(2) P(2) N(1) . . . . -1.5(3) no P(1) S(2) P(2) C(21) . . . . 106.1(3) no P(1) N(1) P(2) C(21) . . . . -105.0(5) no P(1) N(1) C(1) C(2) . . . . -59(1) no P(1) C(11) Fe(1) C(12) . . . . -121(1) no P(1) C(11) Fe(1) C(13) . . . . -159.1(8) no P(1) C(11) Fe(1) C(14) . . . . 158.5(8) no P(1) C(11) Fe(1) C(15) . . . . 120(1) no P(1) C(11) Fe(1) C(16) . . . . 1.5(8) no P(1) C(11) Fe(1) C(17) . . . . -41.2(9) no P(1) C(11) Fe(1) C(18) . . . . -73(1) no P(1) C(11) Fe(1) C(19) . . . . 78(2) no P(1) C(11) Fe(1) C(20) . . . . 43.1(9) no P(1) C(11) C(12) C(13) . . . . 177.5(8) no P(1) C(11) C(15) C(14) . . . . -177.9(8) no P(2) S(2) P(1) N(1) . . . . 1.5(3) no P(2) S(2) P(1) C(11) . . . . 110.8(4) no P(2) N(1) P(1) C(11) . . . . -108.4(5) no P(2) N(1) C(1) C(2) . . . . 121.4(8) no P(2) C(21) Fe(2) C(22) . . . . 119.0(9) no P(2) C(21) Fe(2) C(23) . . . . 158.4(8) no P(2) C(21) Fe(2) C(24) . . . . -159.1(8) no P(2) C(21) Fe(2) C(25) . . . . -120.6(9) no P(2) C(21) Fe(2) C(26) . . . . -2.7(9) no P(2) C(21) Fe(2) C(27) . . . . 40.8(9) no P(2) C(21) Fe(2) C(28) . . . . 78(2) no P(2) C(21) Fe(2) C(29) . . . . -85(2) no P(2) C(21) Fe(2) C(30) . . . . -45.0(9) no P(2) C(21) C(22) C(23) . . . . -177.9(7) no P(2) C(21) C(25) C(24) . . . . 177.8(7) no N(1) P(1) C(11) C(12) . . . . 58(1) no N(1) P(1) C(11) C(15) . . . . -125.9(9) no N(1) P(2) C(21) C(22) . . . . -123.6(9) no N(1) P(2) C(21) C(25) . . . . 60(1) no N(1) C(1) C(2) C(3) . . . . -72(1) no N(1) C(1) C(2) C(7) . . . . 100(1) no C(1) N(1) P(1) C(11) . . . . 71.8(8) no C(1) N(1) P(2) C(21) . . . . 74.7(9) no C(1) C(2) C(3) C(4) . . . . 174(1) no C(1) C(2) C(7) C(6) . . . . -174(1) no C(2) C(3) C(4) C(5) . . . . -1(2) no C(2) C(7) C(6) C(5) . . . . -1(2) no C(3) C(2) C(7) C(6) . . . . -2(2) no C(3) C(4) C(5) C(6) . . . . -1(2) no C(4) C(3) C(2) C(7) . . . . 2(2) no C(4) C(5) C(6) C(7) . . . . 2(2) no C(11) Fe(1) C(12) C(13) . . . . -119.1(8) no C(11) Fe(1) C(13) C(12) . . . . 37.4(6) no C(11) Fe(1) C(13) C(14) . . . . -81.7(6) no C(11) Fe(1) C(14) C(13) . . . . 82.4(6) no C(11) Fe(1) C(14) C(15) . . . . -39.4(7) no C(11) Fe(1) C(15) C(14) . . . . 117(1) no C(11) Fe(1) C(16) C(17) . . . . -118.0(7) no C(11) Fe(1) C(16) C(20) . . . . 124.4(7) no C(11) Fe(1) C(17) C(16) . . . . 80.5(8) no C(11) Fe(1) C(17) C(18) . . . . -161.0(7) no C(11) Fe(1) C(18) C(17) . . . . 45(2) no C(11) Fe(1) C(18) C(19) . . . . 167(1) no C(11) Fe(1) C(19) C(18) . . . . -163(1) no C(11) Fe(1) C(19) C(20) . . . . -45(2) no C(11) Fe(1) C(20) C(16) . . . . -75.1(8) no C(11) Fe(1) C(20) C(19) . . . . 164.6(6) no C(11) C(12) Fe(1) C(13) . . . . 119.1(8) no C(11) C(12) Fe(1) C(14) . . . . 82.4(7) no C(11) C(12) Fe(1) C(15) . . . . 38.4(6) no C(11) C(12) Fe(1) C(16) . . . . -76.8(8) no C(11) C(12) Fe(1) C(17) . . . . -118.6(7) no C(11) C(12) Fe(1) C(18) . . . . -160.2(6) no C(11) C(12) Fe(1) C(19) . . . . 166.4(9) no C(11) C(12) Fe(1) C(20) . . . . -46(2) no C(11) C(12) C(13) C(14) . . . . 0(1) no C(11) C(15) Fe(1) C(12) . . . . -37.2(6) no C(11) C(15) Fe(1) C(13) . . . . -82.0(6) no C(11) C(15) Fe(1) C(14) . . . . -117(1) no C(11) C(15) Fe(1) C(16) . . . . 80.6(8) no C(11) C(15) Fe(1) C(17) . . . . 47(2) no C(11) C(15) Fe(1) C(18) . . . . -164(1) no C(11) C(15) Fe(1) C(19) . . . . 165.8(6) no C(11) C(15) Fe(1) C(20) . . . . 123.5(7) no C(11) C(15) C(14) C(13) . . . . 1(1) no C(12) Fe(1) C(11) C(15) . . . . 119.4(9) no C(12) Fe(1) C(13) C(14) . . . . -119.1(8) no C(12) Fe(1) C(14) C(13) . . . . 38.7(6) no C(12) Fe(1) C(14) C(15) . . . . -83.0(7) no C(12) Fe(1) C(15) C(14) . . . . 80.3(7) no C(12) Fe(1) C(16) C(17) . . . . -76.5(8) no C(12) Fe(1) C(16) C(20) . . . . 165.9(7) no C(12) Fe(1) C(17) C(16) . . . . 122.4(7) no C(12) Fe(1) C(17) C(18) . . . . -119.1(8) no C(12) Fe(1) C(18) C(17) . . . . 78.8(9) no C(12) Fe(1) C(18) C(19) . . . . -159.2(7) no C(12) Fe(1) C(19) C(18) . . . . 47(1) no C(12) Fe(1) C(19) C(20) . . . . 164.9(9) no C(12) Fe(1) C(20) C(16) . . . . -40(2) no C(12) Fe(1) C(20) C(19) . . . . -160(1) no C(12) C(11) Fe(1) C(13) . . . . -38.5(6) no C(12) C(11) Fe(1) C(14) . . . . -80.9(7) no C(12) C(11) Fe(1) C(15) . . . . -119.4(9) no C(12) C(11) Fe(1) C(16) . . . . 122.1(7) no C(12) C(11) Fe(1) C(17) . . . . 79.4(8) no C(12) C(11) Fe(1) C(18) . . . . 47(1) no C(12) C(11) Fe(1) C(19) . . . . -161(1) no C(12) C(11) Fe(1) C(20) . . . . 163.7(6) no C(12) C(11) C(15) C(14) . . . . -2(1) no C(12) C(13) Fe(1) C(14) . . . . 119.1(8) no C(12) C(13) Fe(1) C(15) . . . . 82.4(6) no C(12) C(13) Fe(1) C(16) . . . . -45(2) no C(12) C(13) Fe(1) C(17) . . . . -77.1(7) no C(12) C(13) Fe(1) C(18) . . . . -118.3(6) no C(12) C(13) Fe(1) C(19) . . . . -159.6(6) no C(12) C(13) Fe(1) C(20) . . . . 169(1) no C(12) C(13) C(14) C(15) . . . . -1(1) no C(13) Fe(1) C(11) C(15) . . . . 81.0(7) no C(13) Fe(1) C(14) C(15) . . . . -121.7(9) no C(13) Fe(1) C(15) C(14) . . . . 35.5(6) no C(13) Fe(1) C(16) C(17) . . . . -42(2) no C(13) Fe(1) C(16) C(20) . . . . -159(1) no C(13) Fe(1) C(17) C(16) . . . . 165.1(6) no C(13) Fe(1) C(17) C(18) . . . . -76.4(9) no C(13) Fe(1) C(18) C(17) . . . . 122.3(8) no C(13) Fe(1) C(18) C(19) . . . . -115.7(7) no C(13) Fe(1) C(19) C(18) . . . . 81.6(8) no C(13) Fe(1) C(19) C(20) . . . . -160.9(6) no C(13) Fe(1) C(20) C(16) . . . . 164(1) no C(13) Fe(1) C(20) C(19) . . . . 44(1) no C(13) C(12) Fe(1) C(14) . . . . -36.7(5) no C(13) C(12) Fe(1) C(15) . . . . -80.8(6) no C(13) C(12) Fe(1) C(16) . . . . 164.1(6) no C(13) C(12) Fe(1) C(17) . . . . 122.2(7) no C(13) C(12) Fe(1) C(18) . . . . 80.7(7) no C(13) C(12) Fe(1) C(19) . . . . 47(1) no C(13) C(12) Fe(1) C(20) . . . . -166(1) no C(13) C(12) C(11) C(15) . . . . 1(1) no C(13) C(14) Fe(1) C(15) . . . . 121.7(9) no C(13) C(14) Fe(1) C(16) . . . . 167(1) no C(13) C(14) Fe(1) C(17) . . . . -42(2) no C(13) C(14) Fe(1) C(18) . . . . -75.6(8) no C(13) C(14) Fe(1) C(19) . . . . -115.9(6) no C(13) C(14) Fe(1) C(20) . . . . -158.2(6) no C(14) Fe(1) C(11) C(15) . . . . 38.6(7) no C(14) Fe(1) C(16) C(17) . . . . 165(1) no C(14) Fe(1) C(16) C(20) . . . . 48(1) no C(14) Fe(1) C(17) C(16) . . . . -164(1) no C(14) Fe(1) C(17) C(18) . . . . -46(2) no C(14) Fe(1) C(18) C(17) . . . . 162.5(8) no C(14) Fe(1) C(18) C(19) . . . . -75.5(9) no C(14) Fe(1) C(19) C(18) . . . . 122.7(8) no C(14) Fe(1) C(19) C(20) . . . . -119.8(7) no C(14) Fe(1) C(20) C(16) . . . . -160.9(7) no C(14) Fe(1) C(20) C(19) . . . . 78.9(8) no C(14) C(13) Fe(1) C(15) . . . . -36.7(6) no C(14) C(13) Fe(1) C(16) . . . . -164(1) no C(14) C(13) Fe(1) C(17) . . . . 163.8(6) no C(14) C(13) Fe(1) C(18) . . . . 122.6(6) no C(14) C(13) Fe(1) C(19) . . . . 81.2(7) no C(14) C(13) Fe(1) C(20) . . . . 50(1) no C(14) C(15) Fe(1) C(16) . . . . -161.9(7) no C(14) C(15) Fe(1) C(17) . . . . 165(1) no C(14) C(15) Fe(1) C(18) . . . . -47(2) no C(14) C(15) Fe(1) C(19) . . . . -76.7(9) no C(14) C(15) Fe(1) C(20) . . . . -119.0(7) no C(15) Fe(1) C(16) C(17) . . . . -161.6(7) no C(15) Fe(1) C(16) C(20) . . . . 80.8(8) no C(15) Fe(1) C(17) C(16) . . . . 46(2) no C(15) Fe(1) C(17) C(18) . . . . 164(1) no C(15) Fe(1) C(18) C(17) . . . . -162(1) no C(15) Fe(1) C(18) C(19) . . . . -40(2) no C(15) Fe(1) C(19) C(18) . . . . 164.6(7) no C(15) Fe(1) C(19) C(20) . . . . -77.9(8) no C(15) Fe(1) C(20) C(16) . . . . -118.1(7) no C(15) Fe(1) C(20) C(19) . . . . 121.6(7) no C(15) C(11) Fe(1) C(16) . . . . -118.5(7) no C(15) C(11) Fe(1) C(17) . . . . -161.2(7) no C(15) C(11) Fe(1) C(18) . . . . 167(1) no C(15) C(11) Fe(1) C(19) . . . . -42(2) no C(15) C(11) Fe(1) C(20) . . . . -76.9(8) no C(15) C(14) Fe(1) C(16) . . . . 45(1) no C(15) C(14) Fe(1) C(17) . . . . -163(1) no C(15) C(14) Fe(1) C(18) . . . . 162.6(7) no C(15) C(14) Fe(1) C(19) . . . . 122.3(7) no C(15) C(14) Fe(1) C(20) . . . . 80.0(8) no C(16) Fe(1) C(17) C(18) . . . . 118(1) no C(16) Fe(1) C(18) C(17) . . . . -38.4(8) no C(16) Fe(1) C(18) C(19) . . . . 83.6(8) no C(16) Fe(1) C(19) C(18) . . . . -80.3(8) no C(16) Fe(1) C(19) C(20) . . . . 37.3(7) no C(16) Fe(1) C(20) C(19) . . . . -120(1) no C(16) C(17) Fe(1) C(18) . . . . -118(1) no C(16) C(17) Fe(1) C(19) . . . . -82.9(8) no C(16) C(17) Fe(1) C(20) . . . . -38.7(7) no C(16) C(17) C(18) C(19) . . . . 3(2) no C(16) C(20) Fe(1) C(17) . . . . 38.7(7) no C(16) C(20) Fe(1) C(18) . . . . 82.4(7) no C(16) C(20) Fe(1) C(19) . . . . 120(1) no C(16) C(20) C(19) C(18) . . . . 3(2) no C(17) Fe(1) C(16) C(20) . . . . -118(1) no C(17) Fe(1) C(18) C(19) . . . . 122(1) no C(17) Fe(1) C(19) C(18) . . . . -36.2(8) no C(17) Fe(1) C(19) C(20) . . . . 81.4(7) no C(17) Fe(1) C(20) C(19) . . . . -81.5(7) no C(17) C(16) Fe(1) C(18) . . . . 37.8(7) no C(17) C(16) Fe(1) C(19) . . . . 80.4(7) no C(17) C(16) Fe(1) C(20) . . . . 118(1) no C(17) C(16) C(20) C(19) . . . . -1(2) no C(17) C(18) Fe(1) C(19) . . . . -122(1) no C(17) C(18) Fe(1) C(20) . . . . -82.9(8) no C(17) C(18) C(19) C(20) . . . . -4(2) no C(18) Fe(1) C(16) C(20) . . . . -79.9(7) no C(18) Fe(1) C(19) C(20) . . . . 118(1) no C(18) Fe(1) C(20) C(19) . . . . -37.9(6) no C(18) C(17) Fe(1) C(19) . . . . 35.6(8) no C(18) C(17) Fe(1) C(20) . . . . 79.8(8) no C(18) C(17) C(16) C(20) . . . . -1(2) no C(18) C(19) Fe(1) C(20) . . . . -118(1) no C(19) Fe(1) C(16) C(20) . . . . -37.2(7) no C(19) C(18) Fe(1) C(20) . . . . 39.1(7) no C(21) Fe(2) C(22) C(23) . . . . 116.7(9) no C(21) Fe(2) C(23) C(22) . . . . -39.1(6) no C(21) Fe(2) C(23) C(24) . . . . 82.3(6) no C(21) Fe(2) C(24) C(23) . . . . -81.3(7) no C(21) Fe(2) C(24) C(25) . . . . 38.6(6) no C(21) Fe(2) C(25) C(24) . . . . -117.9(9) no C(21) Fe(2) C(26) C(27) . . . . 119.6(8) no C(21) Fe(2) C(26) C(30) . . . . -123.1(8) no C(21) Fe(2) C(27) C(26) . . . . -81(1) no C(21) Fe(2) C(27) C(28) . . . . 160.5(9) no C(21) Fe(2) C(28) C(27) . . . . -50(2) no C(21) Fe(2) C(28) C(29) . . . . -171(1) no C(21) Fe(2) C(29) C(28) . . . . 170(1) no C(21) Fe(2) C(29) C(30) . . . . 52(2) no C(21) Fe(2) C(30) C(26) . . . . 78.0(9) no C(21) Fe(2) C(30) C(29) . . . . -161.6(8) no C(21) C(22) Fe(2) C(23) . . . . -116.7(9) no C(21) C(22) Fe(2) C(24) . . . . -81.2(6) no C(21) C(22) Fe(2) C(25) . . . . -37.2(5) no C(21) C(22) Fe(2) C(26) . . . . 79.6(7) no C(21) C(22) Fe(2) C(27) . . . . 121.6(7) no C(21) C(22) Fe(2) C(28) . . . . 163.8(7) no C(21) C(22) Fe(2) C(29) . . . . -162(1) no C(21) C(22) Fe(2) C(30) . . . . 49(2) no C(21) C(22) C(23) C(24) . . . . 1(1) no C(21) C(25) Fe(2) C(22) . . . . 37.1(5) no C(21) C(25) Fe(2) C(23) . . . . 81.5(6) no C(21) C(25) Fe(2) C(24) . . . . 117.9(9) no C(21) C(25) Fe(2) C(26) . . . . -82.8(8) no C(21) C(25) Fe(2) C(27) . . . . -50(2) no C(21) C(25) Fe(2) C(28) . . . . 162(1) no C(21) C(25) Fe(2) C(29) . . . . -167.0(7) no C(21) C(25) Fe(2) C(30) . . . . -124.8(7) no C(21) C(25) C(24) C(23) . . . . -1(1) no C(22) Fe(2) C(21) C(25) . . . . -120.4(8) no C(22) Fe(2) C(23) C(24) . . . . 121.4(9) no C(22) Fe(2) C(24) C(23) . . . . -37.2(6) no C(22) Fe(2) C(24) C(25) . . . . 82.6(7) no C(22) Fe(2) C(25) C(24) . . . . -80.8(7) no C(22) Fe(2) C(26) C(27) . . . . 76.3(9) no C(22) Fe(2) C(26) C(30) . . . . -166.4(8) no C(22) Fe(2) C(27) C(26) . . . . -123.8(8) no C(22) Fe(2) C(27) C(28) . . . . 118(1) no C(22) Fe(2) C(28) C(27) . . . . -81(1) no C(22) Fe(2) C(28) C(29) . . . . 158.2(8) no C(22) Fe(2) C(29) C(28) . . . . -49(2) no C(22) Fe(2) C(29) C(30) . . . . -167(1) no C(22) Fe(2) C(30) C(26) . . . . 40(2) no C(22) Fe(2) C(30) C(29) . . . . 161(2) no C(22) C(21) Fe(2) C(23) . . . . 39.4(6) no C(22) C(21) Fe(2) C(24) . . . . 81.9(6) no C(22) C(21) Fe(2) C(25) . . . . 120.4(8) no C(22) C(21) Fe(2) C(26) . . . . -121.7(7) no C(22) C(21) Fe(2) C(27) . . . . -78.2(8) no C(22) C(21) Fe(2) C(28) . . . . -41(2) no C(22) C(21) Fe(2) C(29) . . . . 156(1) no C(22) C(21) Fe(2) C(30) . . . . -164.0(7) no C(22) C(21) C(25) C(24) . . . . 1(1) no C(22) C(23) Fe(2) C(24) . . . . -121.4(9) no C(22) C(23) Fe(2) C(25) . . . . -83.5(6) no C(22) C(23) Fe(2) C(26) . . . . 48(2) no C(22) C(23) Fe(2) C(27) . . . . 78.3(8) no C(22) C(23) Fe(2) C(28) . . . . 119.1(8) no C(22) C(23) Fe(2) C(29) . . . . 160.1(7) no C(22) C(23) Fe(2) C(30) . . . . -170(1) no C(22) C(23) C(24) C(25) . . . . 0(1) no C(23) Fe(2) C(21) C(25) . . . . -81.0(6) no C(23) Fe(2) C(24) C(25) . . . . 119.8(9) no C(23) Fe(2) C(25) C(24) . . . . -36.4(6) no C(23) Fe(2) C(26) C(27) . . . . 39(2) no C(23) Fe(2) C(26) C(30) . . . . 156(1) no C(23) Fe(2) C(27) C(26) . . . . -166.6(8) no C(23) Fe(2) C(27) C(28) . . . . 75(1) no C(23) Fe(2) C(28) C(27) . . . . -123.5(9) no C(23) Fe(2) C(28) C(29) . . . . 115.5(9) no C(23) Fe(2) C(29) C(28) . . . . -81(1) no C(23) Fe(2) C(29) C(30) . . . . 160.9(8) no C(23) Fe(2) C(30) C(26) . . . . -163(1) no C(23) Fe(2) C(30) C(29) . . . . -43(2) no C(23) C(22) Fe(2) C(24) . . . . 35.5(6) no C(23) C(22) Fe(2) C(25) . . . . 79.5(7) no C(23) C(22) Fe(2) C(26) . . . . -163.7(7) no C(23) C(22) Fe(2) C(27) . . . . -121.7(8) no C(23) C(22) Fe(2) C(28) . . . . -79.5(9) no C(23) C(22) Fe(2) C(29) . . . . -45(2) no C(23) C(22) Fe(2) C(30) . . . . 165(2) no C(23) C(22) C(21) C(25) . . . . -1(1) no C(23) C(24) Fe(2) C(25) . . . . -119.8(9) no C(23) C(24) Fe(2) C(26) . . . . -172(1) no C(23) C(24) Fe(2) C(27) . . . . 49(2) no C(23) C(24) Fe(2) C(28) . . . . 78.0(9) no C(23) C(24) Fe(2) C(29) . . . . 117.5(8) no C(23) C(24) Fe(2) C(30) . . . . 158.3(7) no C(24) Fe(2) C(21) C(25) . . . . -38.5(6) no C(24) Fe(2) C(26) C(27) . . . . -158(1) no C(24) Fe(2) C(26) C(30) . . . . -41(2) no C(24) Fe(2) C(27) C(26) . . . . 158(1) no C(24) Fe(2) C(27) C(28) . . . . 40(2) no C(24) Fe(2) C(28) C(27) . . . . -163.9(9) no C(24) Fe(2) C(28) C(29) . . . . 75(1) no C(24) Fe(2) C(29) C(28) . . . . -121.5(9) no C(24) Fe(2) C(29) C(30) . . . . 120.8(9) no C(24) Fe(2) C(30) C(26) . . . . 163.1(7) no C(24) Fe(2) C(30) C(29) . . . . -76(1) no C(24) C(23) Fe(2) C(25) . . . . 37.9(6) no C(24) C(23) Fe(2) C(26) . . . . 170(1) no C(24) C(23) Fe(2) C(27) . . . . -160.3(7) no C(24) C(23) Fe(2) C(28) . . . . -119.5(8) no C(24) C(23) Fe(2) C(29) . . . . -78.6(9) no C(24) C(23) Fe(2) C(30) . . . . -48(1) no C(24) C(25) Fe(2) C(26) . . . . 159.3(8) no C(24) C(25) Fe(2) C(27) . . . . -168(1) no C(24) C(25) Fe(2) C(28) . . . . 44(2) no C(24) C(25) Fe(2) C(29) . . . . 75.1(9) no C(24) C(25) Fe(2) C(30) . . . . 117.3(8) no C(25) Fe(2) C(26) C(27) . . . . 163.5(8) no C(25) Fe(2) C(26) C(30) . . . . -79.2(9) no C(25) Fe(2) C(27) C(26) . . . . -44(2) no C(25) Fe(2) C(27) C(28) . . . . -162(1) no C(25) Fe(2) C(28) C(27) . . . . 163(1) no C(25) Fe(2) C(28) C(29) . . . . 42(2) no C(25) Fe(2) C(29) C(28) . . . . -162.6(8) no C(25) Fe(2) C(29) C(30) . . . . 79.7(9) no C(25) Fe(2) C(30) C(26) . . . . 120.0(8) no C(25) Fe(2) C(30) C(29) . . . . -119.5(9) no C(25) C(21) Fe(2) C(26) . . . . 117.9(7) no C(25) C(21) Fe(2) C(27) . . . . 161.4(7) no C(25) C(21) Fe(2) C(28) . . . . -162(1) no C(25) C(21) Fe(2) C(29) . . . . 36(2) no C(25) C(21) Fe(2) C(30) . . . . 75.6(8) no C(25) C(24) Fe(2) C(26) . . . . -52(1) no C(25) C(24) Fe(2) C(27) . . . . 169(1) no C(25) C(24) Fe(2) C(28) . . . . -162.1(8) no C(25) C(24) Fe(2) C(29) . . . . -122.7(8) no C(25) C(24) Fe(2) C(30) . . . . -81.9(8) no C(26) Fe(2) C(27) C(28) . . . . -118(1) no C(26) Fe(2) C(28) C(27) . . . . 38.5(9) no C(26) Fe(2) C(28) C(29) . . . . -82(1) no C(26) Fe(2) C(29) C(28) . . . . 80.9(9) no C(26) Fe(2) C(29) C(30) . . . . -36.8(8) no C(26) Fe(2) C(30) C(29) . . . . 120(1) no C(26) C(27) Fe(2) C(28) . . . . 118(1) no C(26) C(27) Fe(2) C(29) . . . . 82.2(9) no C(26) C(27) Fe(2) C(30) . . . . 38.4(8) no C(26) C(27) C(28) C(29) . . . . -2(2) no C(26) C(30) Fe(2) C(27) . . . . -39.0(7) no C(26) C(30) Fe(2) C(28) . . . . -82.8(8) no C(26) C(30) Fe(2) C(29) . . . . -120(1) no C(26) C(30) C(29) C(28) . . . . -4(2) no C(27) Fe(2) C(26) C(30) . . . . 117(1) no C(27) Fe(2) C(28) C(29) . . . . -121(1) no C(27) Fe(2) C(29) C(28) . . . . 36.7(9) no C(27) Fe(2) C(29) C(30) . . . . -81.0(9) no C(27) Fe(2) C(30) C(29) . . . . 81.5(9) no C(27) C(26) Fe(2) C(28) . . . . -37.9(9) no C(27) C(26) Fe(2) C(29) . . . . -80.4(9) no C(27) C(26) Fe(2) C(30) . . . . -117(1) no C(27) C(26) C(30) C(29) . . . . 3(2) no C(27) C(28) Fe(2) C(29) . . . . 121(1) no C(27) C(28) Fe(2) C(30) . . . . 82(1) no C(27) C(28) C(29) C(30) . . . . 4(2) no C(28) Fe(2) C(26) C(30) . . . . 79.4(9) no C(28) Fe(2) C(29) C(30) . . . . -118(1) no C(28) Fe(2) C(30) C(29) . . . . 37.7(9) no C(28) C(27) Fe(2) C(29) . . . . -35.9(9) no C(28) C(27) Fe(2) C(30) . . . . -80(1) no C(28) C(27) C(26) C(30) . . . . -1(2) no C(28) C(29) Fe(2) C(30) . . . . 118(1) no C(29) Fe(2) C(26) C(30) . . . . 36.9(8) no C(29) C(28) Fe(2) C(30) . . . . -38.7(9) no #===END data_18 #----------------------------------------------------------------------- _audit_creation_date '1999-05-18' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #----------------------------------------------------------------------- _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Walker, N. & Stuart. D. (1983). Acta Cryst. A39, 158-166. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. ; #----------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item '_geom_extra_table_head_3' '_geom_bond_atom_site_label_D' '_geom_bond_atom_site_label_H' '_geom_contact_atom_site_label_A' '_geom_bond_distance_DH' '_geom_contact_distance_HA' '_geom_contact_distance_DA' '_geom_angle_DHA' '_geom_contact_site_symmetry_A' # # #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #----------------------------------------------------------------------- _cell_length_a 9.568(2) _cell_length_b 12.6641(9) _cell_length_c 16.383(2) _cell_angle_alpha 90.007(9) _cell_angle_beta 92.24(1) _cell_angle_gamma 90.01(1) _cell_volume 1983.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 25.8 _cell_measurement_theta_max 33.4 #----------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #----------------------------------------------------------------------- _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 432.30 _chemical_formula_analytical 'C22 H21 Fe N2 P S ' _chemical_formula_sum 'C22 H21 Fe N2 P S ' _chemical_formula_moiety 'C22 H21 Fe N2 P S ' _chemical_formula_structural 'C22 H21 Fe N2 P S ' _chemical_compound_source - _exptl_crystal_F_000 896.00 _exptl_absorpt_coefficient_mu 7.903 _exptl_absorpt_correction_type ; \DF (DIFABS; Walker & Stuart, 1983) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.637 _exptl_special_details ; The scan width was (0.84+0.35tan\q)\% with an \w scan speed of 16\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #----------------------------------------------------------------------- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.79 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 4 1 0 4 2 0 4 -2 _diffrn_reflns_number 3319 _reflns_number_total 3143 _reflns_number_gt 1832 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.06996 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 60.07 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.05005 _diffrn_orient_matrix_UB_12 0.06305 _diffrn_orient_matrix_UB_13 -0.02342 _diffrn_orient_matrix_UB_21 -0.07719 _diffrn_orient_matrix_UB_22 -0.01109 _diffrn_orient_matrix_UB_23 0.03853 _diffrn_orient_matrix_UB_31 0.04978 _diffrn_orient_matrix_UB_32 0.04623 _diffrn_orient_matrix_UB_33 0.04121 #----------------------------------------------------------------------- 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 88 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 84 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 8 0.029 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 4 0.283 0.434 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 4 0.319 0.557 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Fe 0 4 -1.179 3.204 ;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_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Fe(1) 0.13074(9) 0.38206(6) -0.16233(6) 0.0637(3) 1.000 . Uani d ? S(1) 0.3792(2) 0.3708(1) 0.05338(8) 0.0625(5) 1.000 . Uani d ? P(1) 0.4137(1) 0.3021(1) -0.04978(8) 0.0478(4) 1.000 . Uani d ? N(11) 0.4827(4) 0.1817(3) -0.0454(2) 0.050(1) 1.000 . Uani d ? N(17) 0.5238(4) 0.3759(3) -0.0996(2) 0.049(1) 1.000 . Uani d ? C(1) 0.2569(5) 0.2742(4) -0.1077(3) 0.051(2) 1.000 . Uani d ? C(2) 0.1212(6) 0.2697(4) -0.0751(4) 0.067(2) 1.000 . Uani d ? C(3) 0.0233(7) 0.2479(5) -0.1386(5) 0.087(3) 1.000 . Uani d ? C(4) 0.0966(7) 0.2361(5) -0.2102(4) 0.087(3) 1.000 . Uani d ? C(5) 0.2400(6) 0.2522(4) -0.1930(3) 0.066(2) 1.000 . Uani d ? C(6) 0.2209(7) 0.5275(4) -0.1525(5) 0.082(3) 1.000 . Uani d ? C(7) 0.096(1) 0.5244(5) -0.1117(5) 0.099(3) 1.000 . Uani d ? C(8) -0.0117(9) 0.4998(7) -0.1663(8) 0.133(4) 1.000 . Uani d ? C(9) 0.048(1) 0.4880(7) -0.2421(6) 0.144(4) 1.000 . Uani d ? C(10) 0.195(1) 0.5033(5) -0.2323(5) 0.107(3) 1.000 . Uani d ? C(11) 0.6137(5) 0.1516(4) -0.0082(3) 0.050(2) 1.000 . Uani d ? C(12) 0.6973(6) 0.2195(4) 0.0385(3) 0.070(2) 1.000 . Uani d ? C(13) 0.8233(6) 0.1853(5) 0.0732(4) 0.078(2) 1.000 . Uani d ? C(14) 0.8668(6) 0.0830(5) 0.0622(4) 0.076(2) 1.000 . Uani d ? C(15) 0.7871(6) 0.0159(4) 0.0156(3) 0.067(2) 1.000 . Uani d ? C(16) 0.6599(5) 0.0488(4) -0.0208(3) 0.054(2) 1.000 . Uani d ? C(17) 0.5822(5) 0.3615(4) -0.1774(3) 0.047(2) 1.000 . Uani d ? C(18) 0.6065(5) 0.4511(4) -0.2237(3) 0.055(2) 1.000 . Uani d ? C(19) 0.6702(6) 0.4425(4) -0.2976(3) 0.064(2) 1.000 . Uani d ? C(20) 0.7086(6) 0.3450(5) -0.3270(3) 0.066(2) 1.000 . Uani d ? C(21) 0.6802(6) 0.2571(4) -0.2823(3) 0.066(2) 1.000 . Uani d ? C(22) 0.6193(6) 0.2644(4) -0.2085(3) 0.062(2) 1.000 . Uani d ? H(2) 0.1004 0.2800 -0.0194 0.080 1.000 . Uiso c ? H(3) -0.0751 0.2419 -0.1339 0.103 1.000 . Uiso c ? H(4) 0.0556 0.2200 -0.2625 0.105 1.000 . Uiso c ? H(5) 0.3125 0.2490 -0.2310 0.079 1.000 . Uiso c ? H(6) 0.3102 0.5438 -0.1284 0.099 1.000 . Uiso c ? H(7) 0.0871 0.5370 -0.0551 0.120 1.000 . Uiso c ? H(8) -0.1080 0.4925 -0.1550 0.159 1.000 . Uiso c ? H(9) -0.0017 0.4721 -0.2921 0.173 1.000 . Uiso c ? H(10) 0.2616 0.4978 -0.2738 0.128 1.000 . Uiso c ? H(11) 0.4507 0.1091 -0.0640 0.100 1.000 . Uiso c ? H(12) 0.6680 0.2903 0.0465 0.084 1.000 . Uiso c ? H(13) 0.8798 0.2327 0.1051 0.093 1.000 . Uiso c ? H(14) 0.9526 0.0593 0.0871 0.091 1.000 . Uiso c ? H(15) 0.8178 -0.0546 0.0079 0.081 1.000 . Uiso c ? H(16) 0.6056 0.0015 -0.0539 0.064 1.000 . Uiso c ? H(17) 0.5251 0.4449 -0.0791 0.100 1.000 . Uiso c ? H(18) 0.5792 0.5184 -0.2044 0.066 1.000 . Uiso c ? H(19) 0.6875 0.5043 -0.3284 0.077 1.000 . Uiso c ? H(20) 0.7538 0.3392 -0.3774 0.079 1.000 . Uiso c ? H(21) 0.7035 0.1895 -0.3029 0.079 1.000 . Uiso c ? H(22) 0.6020 0.2022 -0.1783 0.074 1.000 . Uiso c ? 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) 0.0533(6) 0.0490(5) 0.0874(7) 0.0030(5) -0.0166(5) 0.0042(5) S(1) 0.075(1) 0.0572(9) 0.0560(9) -0.0092(8) 0.0139(7) -0.0052(8) P(1) 0.0461(8) 0.0414(7) 0.0555(9) -0.0008(7) -0.0012(6) 0.0018(7) N(11) 0.050(3) 0.033(2) 0.066(3) 0.002(2) -0.011(2) -0.005(2) N(17) 0.055(3) 0.041(2) 0.052(3) -0.005(2) 0.008(2) -0.004(2) C(1) 0.039(3) 0.043(3) 0.071(4) 0.004(3) -0.007(3) -0.003(3) C(2) 0.048(4) 0.055(4) 0.097(5) -0.006(3) -0.004(3) 0.007(3) C(3) 0.056(4) 0.061(4) 0.141(7) -0.003(3) -0.019(5) 0.013(5) C(4) 0.075(5) 0.062(4) 0.121(6) 0.003(4) -0.044(5) -0.018(4) C(5) 0.060(4) 0.064(4) 0.074(4) 0.006(3) -0.013(3) -0.012(3) C(6) 0.072(5) 0.041(3) 0.131(7) -0.001(3) -0.021(5) 0.005(4) C(7) 0.101(6) 0.050(4) 0.147(7) 0.022(4) 0.005(6) -0.001(4) C(8) 0.062(5) 0.087(6) 0.25(1) 0.025(5) -0.021(8) 0.042(9) C(9) 0.19(1) 0.072(5) 0.164(9) -0.016(7) -0.117(9) 0.050(7) C(10) 0.146(9) 0.064(5) 0.109(7) -0.009(5) -0.010(6) 0.018(5) C(11) 0.046(3) 0.054(3) 0.050(3) -0.001(3) -0.002(3) 0.002(3) C(12) 0.068(4) 0.058(4) 0.082(4) 0.000(3) -0.024(3) -0.005(3) C(13) 0.063(4) 0.089(5) 0.079(5) -0.001(4) -0.023(4) -0.013(4) C(14) 0.056(4) 0.092(5) 0.077(4) 0.016(4) -0.013(3) 0.007(4) C(15) 0.063(4) 0.059(4) 0.079(4) 0.012(3) 0.000(3) 0.011(3) C(16) 0.044(3) 0.055(3) 0.061(4) 0.006(3) -0.003(3) 0.003(3) C(17) 0.040(3) 0.049(3) 0.050(3) -0.003(3) -0.007(2) -0.006(3) C(18) 0.053(4) 0.051(3) 0.059(4) -0.004(3) -0.005(3) -0.006(3) C(19) 0.069(4) 0.077(4) 0.047(4) -0.011(4) 0.002(3) 0.003(3) C(20) 0.070(4) 0.078(4) 0.049(4) 0.001(4) 0.004(3) -0.010(3) C(21) 0.070(4) 0.062(4) 0.066(4) 0.007(3) 0.001(3) -0.011(3) C(22) 0.073(4) 0.055(3) 0.058(4) 0.005(3) 0.011(3) -0.003(3) #----------------------------------------------------------------------- _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.000007078 _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 1832 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0345 _refine_ls_goodness_of_fit_ref 1.984 _refine_ls_shift/esd_max 0.0050 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -0.22 _refine_diff_density_max 0.26 #----------------------------------------------------------------------- _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) C(1) 2.011(5) . . yes Fe(1) C(2) 2.022(5) . . yes Fe(1) C(3) 2.031(6) . . yes Fe(1) C(4) 2.030(6) . . yes Fe(1) C(5) 2.023(5) . . yes Fe(1) C(6) 2.037(6) . . yes Fe(1) C(7) 2.016(6) . . yes Fe(1) C(8) 2.019(8) . . yes Fe(1) C(9) 2.015(7) . . yes Fe(1) C(10) 2.026(7) . . yes S(1) P(1) 1.941(2) . . yes P(1) N(11) 1.662(4) . . yes P(1) N(17) 1.649(4) . . yes P(1) C(1) 1.779(5) . . yes N(11) C(11) 1.424(6) . . yes N(11) H(11) 1.01 . . no N(17) C(17) 1.423(6) . . yes N(17) H(17) 0.94 . . no C(1) C(2) 1.424(7) . . yes C(1) C(5) 1.429(7) . . yes C(2) C(3) 1.400(8) . . yes C(2) H(2) 0.95 . . no C(3) C(4) 1.399(9) . . yes C(3) H(3) 0.95 . . no C(4) C(5) 1.405(8) . . yes C(4) H(4) 0.95 . . no C(5) H(5) 0.95 . . no C(6) C(7) 1.391(9) . . yes C(6) C(10) 1.356(9) . . yes C(6) H(6) 0.95 . . no C(7) C(8) 1.37(1) . . yes C(7) H(7) 0.95 . . no C(8) C(9) 1.39(1) . . yes C(8) H(8) 0.95 . . no C(9) C(10) 1.43(1) . . yes C(9) H(9) 0.95 . . no C(10) H(10) 0.95 . . no C(11) C(12) 1.384(7) . . yes C(11) C(16) 1.393(6) . . yes C(12) C(13) 1.383(7) . . yes C(12) H(12) 0.95 . . no C(13) C(14) 1.375(7) . . yes C(13) H(13) 0.95 . . no C(14) C(15) 1.356(7) . . yes C(14) H(14) 0.95 . . no C(15) C(16) 1.398(7) . . yes C(15) H(15) 0.95 . . no C(16) H(16) 0.95 . . no C(17) C(18) 1.389(6) . . yes C(17) C(22) 1.383(6) . . yes C(18) C(19) 1.380(7) . . yes C(18) H(18) 0.95 . . no C(19) C(20) 1.380(7) . . yes C(19) H(19) 0.95 . . no C(20) C(21) 1.365(7) . . yes C(20) H(20) 0.95 . . no C(21) C(22) 1.366(7) . . yes C(21) H(21) 0.95 . . no C(22) H(22) 0.95 . . no #----------------------------------------------------------------------- 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 C(1) Fe(1) C(2) 41.4(2) . . . yes C(1) Fe(1) C(3) 69.2(2) . . . yes C(1) Fe(1) C(4) 68.8(2) . . . yes C(1) Fe(1) C(5) 41.5(2) . . . yes C(1) Fe(1) C(6) 109.5(2) . . . yes C(1) Fe(1) C(7) 122.0(3) . . . yes C(1) Fe(1) C(8) 155.4(4) . . . yes C(1) Fe(1) C(9) 163.0(4) . . . yes C(1) Fe(1) C(10) 125.2(3) . . . yes C(2) Fe(1) C(3) 40.4(2) . . . yes C(2) Fe(1) C(4) 67.8(2) . . . yes C(2) Fe(1) C(5) 69.0(2) . . . yes C(2) Fe(1) C(6) 127.7(3) . . . yes C(2) Fe(1) C(7) 109.0(3) . . . yes C(2) Fe(1) C(8) 119.6(4) . . . yes C(2) Fe(1) C(9) 154.2(4) . . . yes C(2) Fe(1) C(10) 163.1(3) . . . yes C(3) Fe(1) C(4) 40.3(2) . . . yes C(3) Fe(1) C(5) 68.8(3) . . . yes C(3) Fe(1) C(6) 163.1(3) . . . yes C(3) Fe(1) C(7) 125.2(3) . . . yes C(3) Fe(1) C(8) 106.1(3) . . . yes C(3) Fe(1) C(9) 119.5(4) . . . yes C(3) Fe(1) C(10) 155.4(3) . . . yes C(4) Fe(1) C(5) 40.6(2) . . . yes C(4) Fe(1) C(6) 156.2(3) . . . yes C(4) Fe(1) C(7) 161.2(3) . . . yes C(4) Fe(1) C(8) 124.2(4) . . . yes C(4) Fe(1) C(9) 107.6(3) . . . yes C(4) Fe(1) C(10) 121.3(3) . . . yes C(5) Fe(1) C(6) 122.2(3) . . . yes C(5) Fe(1) C(7) 157.5(3) . . . yes C(5) Fe(1) C(8) 161.3(4) . . . yes C(5) Fe(1) C(9) 125.1(4) . . . yes C(5) Fe(1) C(10) 107.7(3) . . . yes C(6) Fe(1) C(7) 40.1(3) . . . yes C(6) Fe(1) C(8) 67.6(3) . . . yes C(6) Fe(1) C(9) 66.7(3) . . . yes C(6) Fe(1) C(10) 39.0(3) . . . yes C(7) Fe(1) C(8) 39.8(3) . . . yes C(7) Fe(1) C(9) 66.7(4) . . . yes C(7) Fe(1) C(10) 67.3(3) . . . yes C(8) Fe(1) C(9) 40.4(3) . . . yes C(8) Fe(1) C(10) 69.0(4) . . . yes C(9) Fe(1) C(10) 41.3(3) . . . yes S(1) P(1) N(11) 117.0(2) . . . yes S(1) P(1) N(17) 108.1(1) . . . yes S(1) P(1) C(1) 112.6(2) . . . yes N(11) P(1) N(17) 106.4(2) . . . yes N(11) P(1) C(1) 99.6(2) . . . yes N(17) P(1) C(1) 113.0(2) . . . yes P(1) N(11) C(11) 127.2(3) . . . yes P(1) N(11) H(11) 134.8 . . . no C(11) N(11) H(11) 97.9 . . . no P(1) N(17) C(17) 130.7(3) . . . yes P(1) N(17) H(17) 110.6 . . . no C(17) N(17) H(17) 116.2 . . . no Fe(1) C(1) P(1) 125.6(3) . . . yes Fe(1) C(1) C(2) 69.7(3) . . . yes Fe(1) C(1) C(5) 69.7(3) . . . yes P(1) C(1) C(2) 124.8(4) . . . yes P(1) C(1) C(5) 128.4(4) . . . yes C(2) C(1) C(5) 106.8(5) . . . yes Fe(1) C(2) C(1) 68.9(3) . . . yes Fe(1) C(2) C(3) 70.2(4) . . . yes Fe(1) C(2) H(2) 126.9 . . . no C(1) C(2) C(3) 108.8(6) . . . yes C(1) C(2) H(2) 125.6 . . . no C(3) C(2) H(2) 125.6 . . . no Fe(1) C(3) C(2) 69.4(3) . . . yes Fe(1) C(3) C(4) 69.8(4) . . . yes Fe(1) C(3) H(3) 126.3 . . . no C(2) C(3) C(4) 107.6(6) . . . yes C(2) C(3) H(3) 126.3 . . . no C(4) C(3) H(3) 126.1 . . . no Fe(1) C(4) C(3) 69.9(4) . . . yes Fe(1) C(4) C(5) 69.5(3) . . . yes Fe(1) C(4) H(4) 126.8 . . . no C(3) C(4) C(5) 109.5(6) . . . yes C(3) C(4) H(4) 125.2 . . . no C(5) C(4) H(4) 125.3 . . . no Fe(1) C(5) C(1) 68.8(3) . . . yes Fe(1) C(5) C(4) 70.0(4) . . . yes Fe(1) C(5) H(5) 126.5 . . . no C(1) C(5) C(4) 107.3(6) . . . yes C(1) C(5) H(5) 126.3 . . . no C(4) C(5) H(5) 126.4 . . . no Fe(1) C(6) C(7) 69.1(4) . . . yes Fe(1) C(6) C(10) 70.1(4) . . . yes Fe(1) C(6) H(6) 126.9 . . . no C(7) C(6) C(10) 109.2(7) . . . yes C(7) C(6) H(6) 125.5 . . . no C(10) C(6) H(6) 125.3 . . . no Fe(1) C(7) C(6) 70.7(4) . . . yes Fe(1) C(7) C(8) 70.2(5) . . . yes Fe(1) C(7) H(7) 125.1 . . . no C(6) C(7) C(8) 109.3(8) . . . yes C(6) C(7) H(7) 125.3 . . . no C(8) C(7) H(7) 125.4 . . . no Fe(1) C(8) C(7) 70.0(4) . . . yes Fe(1) C(8) C(9) 69.6(5) . . . yes Fe(1) C(8) H(8) 125.4 . . . no C(7) C(8) C(9) 106.4(9) . . . yes C(7) C(8) H(8) 127.1 . . . no C(9) C(8) H(8) 126.6 . . . no Fe(1) C(9) C(8) 69.9(5) . . . yes Fe(1) C(9) C(10) 69.8(4) . . . yes Fe(1) C(9) H(9) 126.0 . . . no C(8) C(9) C(10) 108.7(9) . . . yes C(8) C(9) H(9) 125.7 . . . no C(10) C(9) H(9) 125.6 . . . no Fe(1) C(10) C(6) 70.9(4) . . . yes Fe(1) C(10) C(9) 68.9(5) . . . yes Fe(1) C(10) H(10) 125.1 . . . no C(6) C(10) C(9) 106.3(8) . . . yes C(6) C(10) H(10) 127.0 . . . no C(9) C(10) H(10) 126.6 . . . no N(11) C(11) C(12) 123.4(5) . . . yes N(11) C(11) C(16) 117.8(5) . . . yes C(12) C(11) C(16) 118.8(5) . . . yes C(11) C(12) C(13) 120.6(5) . . . yes C(11) C(12) H(12) 119.7 . . . no C(13) C(12) H(12) 119.7 . . . no C(12) C(13) C(14) 120.3(6) . . . yes C(12) C(13) H(13) 119.8 . . . no C(14) C(13) H(13) 119.9 . . . no C(13) C(14) C(15) 119.8(6) . . . yes C(13) C(14) H(14) 120.1 . . . no C(15) C(14) H(14) 120.1 . . . no C(14) C(15) C(16) 121.0(5) . . . yes C(14) C(15) H(15) 119.6 . . . no C(16) C(15) H(15) 119.4 . . . no C(11) C(16) C(15) 119.5(5) . . . yes C(11) C(16) H(16) 120.3 . . . no C(15) C(16) H(16) 120.3 . . . no N(17) C(17) C(18) 117.7(4) . . . yes N(17) C(17) C(22) 124.0(5) . . . yes C(18) C(17) C(22) 118.3(5) . . . yes C(17) C(18) C(19) 120.3(5) . . . yes C(17) C(18) H(18) 119.7 . . . no C(19) C(18) H(18) 120.0 . . . no C(18) C(19) C(20) 120.6(5) . . . yes C(18) C(19) H(19) 119.6 . . . no C(20) C(19) H(19) 119.8 . . . no C(19) C(20) C(21) 118.8(5) . . . yes C(19) C(20) H(20) 120.6 . . . no C(21) C(20) H(20) 120.7 . . . no C(20) C(21) C(22) 121.3(5) . . . yes C(20) C(21) H(21) 119.4 . . . no C(22) C(21) H(21) 119.3 . . . no C(17) C(22) C(21) 120.7(5) . . . yes C(17) C(22) H(22) 119.6 . . . no C(21) C(22) H(22) 119.7 . . . 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) N(17) 3.416(4) . 3_665 no S(1) C(18) 3.587(5) . 3_665 no N(11) C(16) 3.416(6) . 3_655 no C(5) C(10) 3.446(9) . 2_544 no C(16) C(16) 3.39(1) . 3_655 no #===END