# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _publ_contact_author_email mochida@chem.sci.toho-u.ac.jp _publ_contact_author_name 'Dr. Tomoyuki Mochida' _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _audit_creation_date 'Thu Feb 27 16:44:54 2003' _audit_creation_method 'by teXsan' _audit_update_record ? _publ_contact_author_address ; Department of Chemistry, Faculty of Science, Toho University Miyama 2-2-1, Funabashi, Chiba, 274-8510, Japan ; _publ_contact_author_fax ' +81-47-472-4406 ' _publ_contact_author_phone ' +81-47-472-4406 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_category ' FM ' _publ_section_title ; Supramolecular assembling of ferrocenes via hydrogen bonds: Dimensional variation in ferrocenylpyrimidine complexes with carboxylic acids and aromatic alcohols ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; loop_ _publ_author_name 'Tomoyuki Mochida' 'Ryo Horikoshi' 'Chisato Nambu' #------------------------------------------------------------------------------ data_compound_1 _database_code_CSD 206161 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C32 H30 Fe2 N4 O4 ' _chemical_formula_moiety ? _chemical_formula_weight 646.31 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _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 _cell_length_a 9.755(4) _cell_length_b 8.478(3) _cell_length_c 17.791(3) _cell_angle_alpha 90 _cell_angle_beta 95.72(2) _cell_angle_gamma 90 _cell_volume 1464.1(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.6 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.2 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.034 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.746 _exptl_absorpt_correction_T_max 0.998 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 3797 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 1.0482 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.0482 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% 0.03 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3522 _reflns_number_gt 2305 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1801 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2305 _refine_ls_number_parameters 191 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.15000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0011 _refine_diff_density_max 0.59 _refine_diff_density_min -0.49 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Fe Fe 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.99689(6) 0.17692(7) 0.72257(3) 0.0538(2) Uani 1.00 d . . . O(1) O 0.5581(4) -0.3344(4) 0.4671(3) 0.103(1) Uani 1.00 d . . . O(2) O 0.7060(4) -0.1727(5) 0.5279(3) 0.102(1) Uani 1.00 d . . . N(1) N 0.7619(4) 0.4529(5) 0.4870(2) 0.070(1) Uani 1.00 d . . . N(2) N 0.8828(5) 0.2457(6) 0.4367(2) 0.089(2) Uani 1.00 d . . . C(1) C 0.7867(6) 0.3545(7) 0.4328(3) 0.075(1) Uani 1.00 d . . . C(2) C 0.8412(5) 0.4418(5) 0.5520(2) 0.063(1) Uani 1.00 d . . . C(3) C 0.9450(4) 0.3324(5) 0.5640(2) 0.053(1) Uani 1.00 d . . . C(4) C 0.9624(6) 0.2365(7) 0.5026(3) 0.079(2) Uani 1.00 d . . . C(5) C 1.0332(5) 0.3204(5) 0.6364(3) 0.060(1) Uani 1.00 d . . . C(6) C 1.0208(5) 0.4109(6) 0.7029(3) 0.069(1) Uani 1.00 d . . . C(7) C 1.1241(6) 0.3584(7) 0.7590(3) 0.082(2) Uani 1.00 d . . . C(8) C 1.1993(5) 0.2395(8) 0.7278(3) 0.081(2) Uani 1.00 d . . . C(9) C 1.1452(5) 0.2151(6) 0.6523(3) 0.069(1) Uani 1.00 d . . . C(10) C 0.8367(6) 0.0363(9) 0.6867(4) 0.096(2) Uani 1.00 d . . . C(11) C 0.8025(7) 0.1382(8) 0.7463(9) 0.154(4) Uani 1.00 d . . . C(12) C 0.905(1) 0.084(1) 0.8093(4) 0.130(3) Uani 1.00 d . . . C(13) C 0.9807(7) -0.0278(10) 0.7820(4) 0.100(2) Uani 1.00 d . . . C(14) C 0.9418(8) -0.0527(7) 0.7125(4) 0.091(2) Uani 1.00 d . . . C(15) C 0.4842(5) -0.0742(6) 0.4814(3) 0.080(2) Uani 1.00 d . . . C(16) C 0.5945(5) -0.1962(6) 0.4942(3) 0.064(1) Uani 1.00 d . . . H(1) H 0.7297 0.3630 0.3865 0.0896 Uiso 1.00 calc . . . H(2) H 0.8255 0.5123 0.5918 0.0751 Uiso 1.00 calc . . . H(3) H 1.0343 0.1605 0.5073 0.0944 Uiso 1.00 calc . . . H(4) H 0.9548 0.4913 0.7088 0.0830 Uiso 1.00 calc . . . H(5) H 1.1388 0.3966 0.8093 0.0986 Uiso 1.00 calc . . . H(6) H 1.2738 0.1828 0.7536 0.0971 Uiso 1.00 calc . . . H(7) H 1.1775 0.1407 0.6183 0.0828 Uiso 1.00 calc . . . H(8) H 0.7913 0.0335 0.6369 0.1150 Uiso 1.00 calc . . . H(9) H 0.7281 0.2102 0.7473 0.1850 Uiso 1.00 calc . . . H(10) H 0.9128 0.1215 0.8598 0.1557 Uiso 1.00 calc . . . H(11) H 1.0555 -0.0799 0.8099 0.1200 Uiso 1.00 calc . . . H(12) H 0.9851 -0.1262 0.6822 0.1089 Uiso 1.00 calc . . . H(13) H 0.4664 -0.0570 0.4279 0.0760 Uiso 1.00 calc . . . H(14) H 0.4007 -0.1162 0.4986 0.0760 Uiso 1.00 calc . . . H(15) H 0.6213 -0.4200 0.4723 0.1231 Uiso 1.00 calc . . . 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 0.0495(4) 0.0578(4) 0.0540(4) -0.0051(3) 0.0049(2) 0.0003(3) O(1) 0.079(3) 0.073(2) 0.146(4) 0.022(2) -0.036(3) -0.026(2) O(2) 0.070(2) 0.106(3) 0.123(3) 0.022(2) -0.025(2) -0.038(2) N(1) 0.069(2) 0.069(2) 0.071(2) 0.013(2) 0.001(2) 0.005(2) N(2) 0.089(3) 0.109(3) 0.067(3) 0.026(3) -0.004(2) -0.023(3) C(1) 0.070(3) 0.094(4) 0.058(2) 0.009(3) 0.000(2) -0.005(2) C(2) 0.063(2) 0.064(3) 0.060(2) 0.012(2) 0.006(2) -0.002(2) C(3) 0.053(2) 0.055(2) 0.051(2) -0.004(2) 0.006(2) 0.002(2) C(4) 0.073(3) 0.083(3) 0.079(3) 0.027(3) 0.002(3) -0.018(3) C(5) 0.057(2) 0.061(2) 0.062(2) -0.009(2) 0.007(2) 0.012(2) C(6) 0.075(3) 0.058(2) 0.072(3) -0.005(2) 0.000(2) -0.002(2) C(7) 0.091(4) 0.072(3) 0.078(3) -0.027(3) -0.018(3) 0.001(2) C(8) 0.054(3) 0.097(4) 0.090(4) -0.009(3) -0.005(2) 0.027(3) C(9) 0.046(2) 0.089(3) 0.073(3) 0.005(2) 0.011(2) 0.017(3) C(10) 0.075(4) 0.106(5) 0.101(5) -0.034(4) -0.019(3) 0.024(4) C(11) 0.063(4) 0.066(4) 0.35(2) 0.003(3) 0.100(6) 0.014(6) C(12) 0.153(7) 0.162(8) 0.086(4) -0.086(6) 0.074(5) -0.042(5) C(13) 0.104(5) 0.111(5) 0.085(4) -0.029(4) 0.005(4) 0.036(4) C(14) 0.099(4) 0.063(3) 0.114(5) -0.020(3) 0.026(4) -0.002(3) C(15) 0.059(3) 0.069(3) 0.107(4) 0.008(2) -0.010(3) -0.001(3) C(16) 0.055(2) 0.072(3) 0.063(2) 0.011(2) 0.000(2) -0.001(2) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 C(5) 2.016(4) . . yes Fe C(6) 2.032(5) . . yes Fe C(7) 2.041(5) . . yes Fe C(8) 2.037(5) . . yes Fe C(9) 2.030(5) . . yes Fe C(10) 2.018(5) . . yes Fe C(11) 2.011(6) . . yes Fe C(12) 2.021(6) . . yes Fe C(13) 2.047(6) . . yes Fe C(14) 2.022(5) . . yes O(1) C(16) 1.304(6) . . yes O(2) C(16) 1.205(6) . . yes N(1) C(1) 1.316(6) . . yes N(1) C(2) 1.329(6) . . yes N(2) C(1) 1.312(7) . . yes N(2) C(4) 1.342(6) . . yes C(2) C(3) 1.374(6) . . yes C(3) C(4) 1.387(6) . . yes C(3) C(5) 1.479(6) . . yes C(5) C(6) 1.426(7) . . yes C(5) C(9) 1.418(7) . . yes C(6) C(7) 1.417(7) . . yes C(7) C(8) 1.394(9) . . yes C(8) C(9) 1.408(8) . . yes C(10) C(11) 1.43(1) . . yes C(10) C(14) 1.318(10) . . yes C(11) C(12) 1.50(1) . . yes C(12) C(13) 1.32(1) . . yes C(13) C(14) 1.275(8) . . yes C(15) C(15) 1.44(1) . 3_656 yes C(15) C(16) 1.494(7) . . 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 C(5) Fe C(6) 41.3(2) . . 0_555 yes C(5) Fe C(7) 68.9(2) . . 0_555 yes C(5) Fe C(8) 68.6(2) . . 0_555 yes C(5) Fe C(9) 41.0(2) . . 0_555 yes C(5) Fe C(10) 107.8(2) . . 0_555 yes C(5) Fe C(11) 119.9(4) . . 0_555 yes C(5) Fe C(12) 160.2(4) . . 0_555 yes C(5) Fe C(13) 158.9(3) . . 0_555 yes C(5) Fe C(14) 125.3(2) . . 0_555 yes C(6) Fe C(7) 40.7(2) . . 0_555 yes C(6) Fe C(8) 68.1(2) . . 0_555 yes C(6) Fe C(9) 68.7(2) . . 0_555 yes C(6) Fe C(10) 128.4(2) . . 0_555 yes C(6) Fe C(11) 108.8(3) . . 0_555 yes C(6) Fe C(12) 125.4(3) . . 0_555 yes C(6) Fe C(13) 158.9(3) . . 0_555 yes C(6) Fe C(14) 163.4(3) . . 0_555 yes C(7) Fe C(8) 40.0(3) . . 0_555 yes C(7) Fe C(9) 68.1(2) . . 0_555 yes C(7) Fe C(10) 166.6(3) . . 0_555 yes C(7) Fe C(11) 127.8(4) . . 0_555 yes C(7) Fe C(12) 110.7(3) . . 0_555 yes C(7) Fe C(13) 123.4(2) . . 0_555 yes C(7) Fe C(14) 154.3(3) . . 0_555 yes C(8) Fe C(9) 40.5(2) . . 0_555 yes C(8) Fe C(10) 152.2(3) . . 0_555 yes C(8) Fe C(11) 164.4(5) . . 0_555 yes C(8) Fe C(12) 124.7(3) . . 0_555 yes C(8) Fe C(13) 108.8(3) . . 0_555 yes C(8) Fe C(14) 120.1(3) . . 0_555 yes C(9) Fe C(10) 118.5(3) . . 0_555 yes C(9) Fe C(11) 154.2(5) . . 0_555 yes C(9) Fe C(12) 158.5(4) . . 0_555 yes C(9) Fe C(13) 123.4(3) . . 0_555 yes C(9) Fe C(14) 107.3(3) . . 0_555 yes C(10) Fe C(11) 41.6(4) . . 0_555 yes C(10) Fe C(12) 67.8(3) . . 0_555 yes C(10) Fe C(13) 64.2(2) . . 0_555 yes C(10) Fe C(14) 38.1(3) . . 0_555 yes C(11) Fe C(12) 43.6(4) . . 0_555 yes C(11) Fe C(13) 68.3(3) . . 0_555 yes C(11) Fe C(14) 67.3(3) . . 0_555 yes C(12) Fe C(13) 38.0(4) . . 0_555 yes C(12) Fe C(14) 63.8(3) . . 0_555 yes C(13) Fe C(14) 36.5(3) . . 0_555 yes C(1) N(1) C(2) 117.3(4) . . 0_555 yes C(1) N(2) C(4) 115.8(4) . . 0_555 yes N(1) C(1) N(2) 126.1(5) . . 0_555 yes N(1) C(2) C(3) 122.6(4) . . 0_555 yes C(2) C(3) C(4) 114.8(4) . . 0_555 yes C(2) C(3) C(5) 122.5(4) . . 0_555 yes C(4) C(3) C(5) 122.6(4) . . 0_555 yes N(2) C(4) C(3) 123.2(5) . . 0_555 yes Fe C(5) C(3) 124.9(3) . . 0_555 yes Fe C(5) C(6) 70.0(3) . . 0_555 yes Fe C(5) C(9) 70.0(3) . . 0_555 yes C(3) C(5) C(6) 126.6(4) . . 0_555 yes C(3) C(5) C(9) 126.0(4) . . 0_555 yes C(6) C(5) C(9) 107.5(4) . . 0_555 yes Fe C(6) C(5) 68.8(2) . . 0_555 yes Fe C(6) C(7) 70.0(3) . . 0_555 yes C(5) C(6) C(7) 107.6(5) . . 0_555 yes Fe C(7) C(6) 69.3(3) . . 0_555 yes Fe C(7) C(8) 69.9(3) . . 0_555 yes C(6) C(7) C(8) 108.2(5) . . 0_555 yes Fe C(8) C(7) 70.2(3) . . 0_555 yes Fe C(8) C(9) 69.5(3) . . 0_555 yes C(7) C(8) C(9) 108.9(5) . . 0_555 yes Fe C(9) C(5) 69.0(3) . . 0_555 yes Fe C(9) C(8) 70.0(3) . . 0_555 yes C(5) C(9) C(8) 107.9(5) . . 0_555 yes Fe C(10) C(11) 68.9(4) . . 0_555 yes Fe C(10) C(14) 71.1(3) . . 0_555 yes C(11) C(10) C(14) 108.6(7) . . 0_555 yes Fe C(11) C(10) 69.5(4) . . 0_555 yes Fe C(11) C(12) 68.6(3) . . 0_555 yes C(10) C(11) C(12) 100.5(5) . . 0_555 yes Fe C(12) C(11) 67.8(4) . . 0_555 yes Fe C(12) C(13) 72.1(4) . . 0_555 yes C(11) C(12) C(13) 107.5(6) . . 0_555 yes Fe C(13) C(12) 69.9(4) . . 0_555 yes Fe C(13) C(14) 70.7(4) . . 0_555 yes C(12) C(13) C(14) 110.5(7) . . 0_555 yes Fe C(14) C(10) 70.8(4) . . 0_555 yes Fe C(14) C(13) 72.8(4) . . 0_555 yes C(10) C(14) C(13) 112.9(7) . . 0_555 yes C(15) C(15) C(16) 114.6(5) 3_656 . 0_555 yes O(1) C(16) O(2) 122.1(4) . . 0_555 yes O(1) C(16) C(15) 113.6(4) . . 0_555 yes O(2) C(16) C(15) 124.2(5) . . 0_555 yes #------------------------------------------------------------------------------ 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe C(5) C(3) C(2) 92.9(5) 0_555 24_1 5_555 55_5 yes Fe C(5) C(3) C(4) -88.5(6) 0_555 24_1 5_555 55_5 yes Fe C(5) C(6) C(7) 59.5(4) 0_555 24_1 5_555 55_5 yes Fe C(5) C(9) C(8) -59.5(3) 0_555 24_1 5_555 55_5 yes Fe C(6) C(5) C(3) 119.2(4) 0_555 24_1 5_555 55_5 yes Fe C(6) C(5) C(9) -60.3(3) 0_555 24_1 5_555 55_5 yes Fe C(6) C(7) C(8) 59.2(4) 0_555 24_1 5_555 55_5 yes Fe C(7) C(6) C(5) -58.7(3) 0_555 24_1 5_555 55_5 yes Fe C(7) C(8) C(9) 58.8(4) 0_555 24_1 5_555 55_5 yes Fe C(8) C(7) C(6) -58.9(4) 0_555 24_1 5_555 55_5 yes Fe C(8) C(9) C(5) 58.8(3) 0_555 24_1 5_555 55_5 yes Fe C(9) C(5) C(3) -119.3(4) 0_555 24_1 5_555 55_5 yes Fe C(9) C(5) C(6) 60.2(3) 0_555 24_1 5_555 55_5 yes Fe C(9) C(8) C(7) -59.3(4) 0_555 24_1 5_555 55_5 yes Fe C(10) C(11) C(12) -62.2(4) 0_555 24_1 5_555 55_5 yes Fe C(10) C(14) C(13) 60.9(5) 0_555 24_1 5_555 55_5 yes Fe C(11) C(10) C(14) 60.3(5) 0_555 24_1 5_555 55_5 yes Fe C(11) C(12) C(13) -61.5(5) 0_555 24_1 5_555 55_5 yes Fe C(12) C(11) C(10) 62.9(4) 0_555 24_1 5_555 55_5 yes Fe C(12) C(13) C(14) -59.2(5) 0_555 24_1 5_555 55_5 yes Fe C(13) C(12) C(11) 58.8(5) 0_555 24_1 5_555 55_5 yes Fe C(13) C(14) C(10) -59.7(5) 0_555 24_1 5_555 55_5 yes Fe C(14) C(10) C(11) -58.9(4) 0_555 24_1 5_555 55_5 yes Fe C(14) C(13) C(12) 58.7(5) 0_555 24_1 5_555 55_5 yes O(1) C(16) C(15) C(15) 173.0(6) 0_555 24_1 5_555 55_5 yes O(2) C(16) C(15) C(15) -5(1) 0_555 24_1 5_555 55_5 yes N(1) C(1) N(2) C(4) -0.3(10) 0_555 24_1 5_555 55_5 yes N(1) C(2) C(3) C(4) 1.2(7) 0_555 24_1 5_555 55_5 yes N(1) C(2) C(3) C(5) 179.9(4) 0_555 24_1 5_555 55_5 yes N(2) C(1) N(1) C(2) 0.0(9) 0_555 24_1 5_555 55_5 yes N(2) C(4) C(3) C(2) -1.6(9) 0_555 24_1 5_555 55_5 yes N(2) C(4) C(3) C(5) 179.7(5) 0_555 24_1 5_555 55_5 yes C(1) N(1) C(2) C(3) -0.5(7) 0_555 24_1 5_555 55_5 yes C(1) N(2) C(4) C(3) 1.2(10) 0_555 24_1 5_555 55_5 yes C(2) C(3) C(5) C(6) 3.0(7) 0_555 24_1 5_555 55_5 yes C(2) C(3) C(5) C(9) -177.6(4) 0_555 24_1 5_555 55_5 yes C(3) C(5) Fe C(6) -121.2(5) 0_555 24_1 5_555 55_5 yes C(3) C(5) Fe C(7) -158.9(5) 0_555 24_1 5_555 55_5 yes C(3) C(5) Fe C(8) 158.1(5) 0_555 24_1 5_555 55_5 yes C(3) C(5) Fe C(9) 120.6(5) 0_555 24_1 5_555 55_5 yes C(3) C(5) Fe C(10) 7.3(5) 0_555 24_1 5_555 55_5 yes C(3) C(5) Fe C(11) -36.5(6) 0_555 24_1 5_555 55_5 yes C(3) C(5) Fe C(12) -66.2(8) 0_555 24_1 5_555 55_5 yes C(3) C(5) Fe C(13) 71.3(8) 0_555 24_1 5_555 55_5 yes C(3) C(5) Fe C(14) 45.5(5) 0_555 24_1 5_555 55_5 yes C(3) C(5) C(6) C(7) 178.7(4) 0_555 24_1 5_555 55_5 yes C(3) C(5) C(9) C(8) -178.7(4) 0_555 24_1 5_555 55_5 yes C(4) C(3) C(5) C(6) -178.3(5) 0_555 24_1 5_555 55_5 yes C(4) C(3) C(5) C(9) 1.1(7) 0_555 24_1 5_555 55_5 yes C(5) Fe C(6) C(7) -119.1(5) 0_555 24_1 5_555 55_5 yes C(5) Fe C(7) C(6) 38.2(3) 0_555 24_1 5_555 55_5 yes C(5) Fe C(7) C(8) -81.5(3) 0_555 24_1 5_555 55_5 yes C(5) Fe C(8) C(7) 82.2(3) 0_555 24_1 5_555 55_5 yes C(5) Fe C(8) C(9) -37.9(3) 0_555 24_1 5_555 55_5 yes C(5) Fe C(9) C(8) 119.3(5) 0_555 24_1 5_555 55_5 yes C(5) Fe C(10) C(11) -115.3(6) 0_555 24_1 5_555 55_5 yes C(5) Fe C(10) C(14) 125.1(4) 0_555 24_1 5_555 55_5 yes C(5) Fe C(11) C(10) 83.3(4) 0_555 24_1 5_555 55_5 yes C(5) Fe C(11) C(12) -165.9(4) 0_555 24_1 5_555 55_5 yes C(5) Fe C(12) C(11) 38.5(9) 0_555 24_1 5_555 55_5 yes C(5) Fe C(12) C(13) 156.8(6) 0_555 24_1 5_555 55_5 yes C(5) Fe C(13) C(12) -158.2(6) 0_555 24_1 5_555 55_5 yes C(5) Fe C(13) C(14) -36.7(9) 0_555 24_1 5_555 55_5 yes C(5) Fe C(14) C(10) -72.7(5) 0_555 24_1 5_555 55_5 yes C(5) Fe C(14) C(13) 164.7(4) 0_555 24_1 5_555 55_5 yes C(5) C(6) Fe C(7) 119.1(5) 0_555 24_1 5_555 55_5 yes C(5) C(6) Fe C(8) 82.1(3) 0_555 24_1 5_555 55_5 yes C(5) C(6) Fe C(9) 38.4(3) 0_555 24_1 5_555 55_5 yes C(5) C(6) Fe C(10) -71.8(4) 0_555 24_1 5_555 55_5 yes C(5) C(6) Fe C(11) -114.3(6) 0_555 24_1 5_555 55_5 yes C(5) C(6) Fe C(12) -160.1(4) 0_555 24_1 5_555 55_5 yes C(5) C(6) Fe C(13) 167.4(7) 0_555 24_1 5_555 55_5 yes C(5) C(6) Fe C(14) -40.9(9) 0_555 24_1 5_555 55_5 yes C(5) C(6) C(7) C(8) 0.5(6) 0_555 24_1 5_555 55_5 yes C(5) C(9) Fe C(6) -38.6(3) 0_555 24_1 5_555 55_5 yes C(5) C(9) Fe C(7) -82.5(3) 0_555 24_1 5_555 55_5 yes C(5) C(9) Fe C(8) -119.3(5) 0_555 24_1 5_555 55_5 yes C(5) C(9) Fe C(10) 84.6(4) 0_555 24_1 5_555 55_5 yes C(5) C(9) Fe C(11) 50.8(7) 0_555 24_1 5_555 55_5 yes C(5) C(9) Fe C(12) -173.7(6) 0_555 24_1 5_555 55_5 yes C(5) C(9) Fe C(13) 161.0(3) 0_555 24_1 5_555 55_5 yes C(5) C(9) Fe C(14) 124.3(3) 0_555 24_1 5_555 55_5 yes C(5) C(9) C(8) C(7) -0.5(6) 0_555 24_1 5_555 55_5 yes C(6) Fe C(5) C(9) 118.2(4) 0_555 24_1 5_555 55_5 yes C(6) Fe C(7) C(8) -119.6(5) 0_555 24_1 5_555 55_5 yes C(6) Fe C(8) C(7) 37.7(3) 0_555 24_1 5_555 55_5 yes C(6) Fe C(8) C(9) -82.5(3) 0_555 24_1 5_555 55_5 yes C(6) Fe C(9) C(8) 80.7(4) 0_555 24_1 5_555 55_5 yes C(6) Fe C(10) C(11) -74.2(6) 0_555 24_1 5_555 55_5 yes C(6) Fe C(10) C(14) 166.3(4) 0_555 24_1 5_555 55_5 yes C(6) Fe C(11) C(10) 127.2(4) 0_555 24_1 5_555 55_5 yes C(6) Fe C(11) C(12) -122.0(5) 0_555 24_1 5_555 55_5 yes C(6) Fe C(12) C(11) 80.1(5) 0_555 24_1 5_555 55_5 yes C(6) Fe C(12) C(13) -161.7(4) 0_555 24_1 5_555 55_5 yes C(6) Fe C(13) C(12) 45.3(9) 0_555 24_1 5_555 55_5 yes C(6) Fe C(13) C(14) 166.9(6) 0_555 24_1 5_555 55_5 yes C(6) Fe C(14) C(10) -40(1) 0_555 24_1 5_555 55_5 yes C(6) Fe C(14) C(13) -163.3(8) 0_555 24_1 5_555 55_5 yes C(6) C(5) Fe C(7) -37.7(3) 0_555 24_1 5_555 55_5 yes C(6) C(5) Fe C(8) -80.7(3) 0_555 24_1 5_555 55_5 yes C(6) C(5) Fe C(9) -118.2(4) 0_555 24_1 5_555 55_5 yes C(6) C(5) Fe C(10) 128.6(4) 0_555 24_1 5_555 55_5 yes C(6) C(5) Fe C(11) 84.7(5) 0_555 24_1 5_555 55_5 yes C(6) C(5) Fe C(12) 55.0(7) 0_555 24_1 5_555 55_5 yes C(6) C(5) Fe C(13) -167.4(6) 0_555 24_1 5_555 55_5 yes C(6) C(5) Fe C(14) 166.8(3) 0_555 24_1 5_555 55_5 yes C(6) C(5) C(9) C(8) 0.8(5) 0_555 24_1 5_555 55_5 yes C(6) C(7) Fe C(8) 119.6(5) 0_555 24_1 5_555 55_5 yes C(6) C(7) Fe C(9) 82.4(3) 0_555 24_1 5_555 55_5 yes C(6) C(7) Fe C(10) -39(1) 0_555 24_1 5_555 55_5 yes C(6) C(7) Fe C(11) -74.0(6) 0_555 24_1 5_555 55_5 yes C(6) C(7) Fe C(12) -120.7(5) 0_555 24_1 5_555 55_5 yes C(6) C(7) Fe C(13) -161.2(4) 0_555 24_1 5_555 55_5 yes C(6) C(7) Fe C(14) 167.0(5) 0_555 24_1 5_555 55_5 yes C(6) C(7) C(8) C(9) 0.0(6) 0_555 24_1 5_555 55_5 yes C(7) Fe C(5) C(9) 80.5(3) 0_555 24_1 5_555 55_5 yes C(7) Fe C(8) C(9) -120.2(5) 0_555 24_1 5_555 55_5 yes C(7) Fe C(9) C(8) 36.8(4) 0_555 24_1 5_555 55_5 yes C(7) Fe C(10) C(11) -42(1) 0_555 24_1 5_555 55_5 yes C(7) Fe C(10) C(14) -161.6(9) 0_555 24_1 5_555 55_5 yes C(7) Fe C(11) C(10) 168.7(3) 0_555 24_1 5_555 55_5 yes C(7) Fe C(11) C(12) -80.5(5) 0_555 24_1 5_555 55_5 yes C(7) Fe C(12) C(11) 123.6(5) 0_555 24_1 5_555 55_5 yes C(7) Fe C(12) C(13) -118.2(5) 0_555 24_1 5_555 55_5 yes C(7) Fe C(13) C(12) 81.0(6) 0_555 24_1 5_555 55_5 yes C(7) Fe C(13) C(14) -157.4(5) 0_555 24_1 5_555 55_5 yes C(7) Fe C(14) C(10) 170.3(6) 0_555 24_1 5_555 55_5 yes C(7) Fe C(14) C(13) 47.7(8) 0_555 24_1 5_555 55_5 yes C(7) C(6) Fe C(8) -37.0(4) 0_555 24_1 5_555 55_5 yes C(7) C(6) Fe C(9) -80.7(4) 0_555 24_1 5_555 55_5 yes C(7) C(6) Fe C(10) 169.1(4) 0_555 24_1 5_555 55_5 yes C(7) C(6) Fe C(11) 126.6(6) 0_555 24_1 5_555 55_5 yes C(7) C(6) Fe C(12) 80.8(5) 0_555 24_1 5_555 55_5 yes C(7) C(6) Fe C(13) 48.3(8) 0_555 24_1 5_555 55_5 yes C(7) C(6) Fe C(14) -160.0(8) 0_555 24_1 5_555 55_5 yes C(7) C(6) C(5) C(9) -0.8(5) 0_555 24_1 5_555 55_5 yes C(7) C(8) Fe C(9) 120.2(5) 0_555 24_1 5_555 55_5 yes C(7) C(8) Fe C(10) 169.9(4) 0_555 24_1 5_555 55_5 yes C(7) C(8) Fe C(11) -43(1) 0_555 24_1 5_555 55_5 yes C(7) C(8) Fe C(12) -81.1(5) 0_555 24_1 5_555 55_5 yes C(7) C(8) Fe C(13) -120.0(4) 0_555 24_1 5_555 55_5 yes C(7) C(8) Fe C(14) -158.4(4) 0_555 24_1 5_555 55_5 yes C(8) Fe C(5) C(9) 37.5(3) 0_555 24_1 5_555 55_5 yes C(8) Fe C(10) C(11) 167.0(6) 0_555 24_1 5_555 55_5 yes C(8) Fe C(10) C(14) 47.5(7) 0_555 24_1 5_555 55_5 yes C(8) Fe C(11) C(10) -157.1(8) 0_555 24_1 5_555 55_5 yes C(8) Fe C(11) C(12) -46(1) 0_555 24_1 5_555 55_5 yes C(8) Fe C(12) C(11) 166.3(5) 0_555 24_1 5_555 55_5 yes C(8) Fe C(12) C(13) -75.5(5) 0_555 24_1 5_555 55_5 yes C(8) Fe C(13) C(12) 122.8(5) 0_555 24_1 5_555 55_5 yes C(8) Fe C(13) C(14) -115.6(5) 0_555 24_1 5_555 55_5 yes C(8) Fe C(14) C(10) -156.6(4) 0_555 24_1 5_555 55_5 yes C(8) Fe C(14) C(13) 80.8(5) 0_555 24_1 5_555 55_5 yes C(8) C(7) Fe C(9) -37.3(3) 0_555 24_1 5_555 55_5 yes C(8) C(7) Fe C(10) -159.3(9) 0_555 24_1 5_555 55_5 yes C(8) C(7) Fe C(11) 166.4(6) 0_555 24_1 5_555 55_5 yes C(8) C(7) Fe C(12) 119.7(5) 0_555 24_1 5_555 55_5 yes C(8) C(7) Fe C(13) 79.2(5) 0_555 24_1 5_555 55_5 yes C(8) C(7) Fe C(14) 47.3(7) 0_555 24_1 5_555 55_5 yes C(8) C(9) Fe C(10) -156.1(4) 0_555 24_1 5_555 55_5 yes C(8) C(9) Fe C(11) 170.1(5) 0_555 24_1 5_555 55_5 yes C(8) C(9) Fe C(12) -54.4(8) 0_555 24_1 5_555 55_5 yes C(8) C(9) Fe C(13) -79.7(4) 0_555 24_1 5_555 55_5 yes C(8) C(9) Fe C(14) -116.4(4) 0_555 24_1 5_555 55_5 yes C(9) Fe C(10) C(11) -158.7(6) 0_555 24_1 5_555 55_5 yes C(9) Fe C(10) C(14) 81.8(4) 0_555 24_1 5_555 55_5 yes C(9) Fe C(11) C(10) 47.3(8) 0_555 24_1 5_555 55_5 yes C(9) Fe C(11) C(12) 158.1(6) 0_555 24_1 5_555 55_5 yes C(9) Fe C(12) C(11) -153.7(7) 0_555 24_1 5_555 55_5 yes C(9) Fe C(12) C(13) -35.5(9) 0_555 24_1 5_555 55_5 yes C(9) Fe C(13) C(12) 165.2(5) 0_555 24_1 5_555 55_5 yes C(9) Fe C(13) C(14) -73.2(5) 0_555 24_1 5_555 55_5 yes C(9) Fe C(14) C(10) -114.3(4) 0_555 24_1 5_555 55_5 yes C(9) Fe C(14) C(13) 123.1(5) 0_555 24_1 5_555 55_5 yes C(9) C(5) Fe C(10) -113.2(4) 0_555 24_1 5_555 55_5 yes C(9) C(5) Fe C(11) -157.1(5) 0_555 24_1 5_555 55_5 yes C(9) C(5) Fe C(12) 173.2(6) 0_555 24_1 5_555 55_5 yes C(9) C(5) Fe C(13) -49.2(7) 0_555 24_1 5_555 55_5 yes C(9) C(5) Fe C(14) -75.0(4) 0_555 24_1 5_555 55_5 yes C(9) C(8) Fe C(10) 49.7(6) 0_555 24_1 5_555 55_5 yes C(9) C(8) Fe C(11) -163.9(10) 0_555 24_1 5_555 55_5 yes C(9) C(8) Fe C(12) 158.7(4) 0_555 24_1 5_555 55_5 yes C(9) C(8) Fe C(13) 119.8(4) 0_555 24_1 5_555 55_5 yes C(9) C(8) Fe C(14) 81.4(4) 0_555 24_1 5_555 55_5 yes C(10) Fe C(11) C(12) 110.8(6) 0_555 24_1 5_555 55_5 yes C(10) Fe C(12) C(11) -42.1(5) 0_555 24_1 5_555 55_5 yes C(10) Fe C(12) C(13) 76.1(5) 0_555 24_1 5_555 55_5 yes C(10) Fe C(13) C(12) -86.3(5) 0_555 24_1 5_555 55_5 yes C(10) Fe C(13) C(14) 35.3(5) 0_555 24_1 5_555 55_5 yes C(10) Fe C(14) C(13) -122.6(7) 0_555 24_1 5_555 55_5 yes C(10) C(11) Fe C(12) -110.8(6) 0_555 24_1 5_555 55_5 yes C(10) C(11) Fe C(13) -75.1(4) 0_555 24_1 5_555 55_5 yes C(10) C(11) Fe C(14) -35.6(4) 0_555 24_1 5_555 55_5 yes C(10) C(11) C(12) C(13) 1.4(7) 0_555 24_1 5_555 55_5 yes C(10) C(14) Fe C(11) 38.8(6) 0_555 24_1 5_555 55_5 yes C(10) C(14) Fe C(12) 86.8(5) 0_555 24_1 5_555 55_5 yes C(10) C(14) Fe C(13) 122.6(7) 0_555 24_1 5_555 55_5 yes C(10) C(14) C(13) C(12) -1.0(8) 0_555 24_1 5_555 55_5 yes C(11) Fe C(10) C(14) -119.5(7) 0_555 24_1 5_555 55_5 yes C(11) Fe C(12) C(13) 118.2(7) 0_555 24_1 5_555 55_5 yes C(11) Fe C(13) C(12) -40.9(6) 0_555 24_1 5_555 55_5 yes C(11) Fe C(13) C(14) 80.7(6) 0_555 24_1 5_555 55_5 yes C(11) Fe C(14) C(13) -83.8(6) 0_555 24_1 5_555 55_5 yes C(11) C(10) Fe C(12) 44.2(5) 0_555 24_1 5_555 55_5 yes C(11) C(10) Fe C(13) 85.7(6) 0_555 24_1 5_555 55_5 yes C(11) C(10) Fe C(14) 119.5(7) 0_555 24_1 5_555 55_5 yes C(11) C(10) C(14) C(13) 2.0(8) 0_555 24_1 5_555 55_5 yes C(11) C(12) Fe C(13) -118.2(7) 0_555 24_1 5_555 55_5 yes C(11) C(12) Fe C(14) -83.8(6) 0_555 24_1 5_555 55_5 yes C(11) C(12) C(13) C(14) -0.3(8) 0_555 24_1 5_555 55_5 yes C(12) Fe C(10) C(14) -75.4(5) 0_555 24_1 5_555 55_5 yes C(12) Fe C(13) C(14) 121.6(7) 0_555 24_1 5_555 55_5 yes C(12) Fe C(14) C(13) -35.7(5) 0_555 24_1 5_555 55_5 yes C(12) C(11) Fe C(13) 35.7(5) 0_555 24_1 5_555 55_5 yes C(12) C(11) Fe C(14) 75.2(5) 0_555 24_1 5_555 55_5 yes C(12) C(11) C(10) C(14) -1.9(7) 0_555 24_1 5_555 55_5 yes C(12) C(13) Fe C(14) -121.6(7) 0_555 24_1 5_555 55_5 yes C(13) Fe C(10) C(14) -33.8(4) 0_555 24_1 5_555 55_5 yes C(13) C(12) Fe C(14) 34.4(4) 0_555 24_1 5_555 55_5 yes C(16) C(15) C(15) C(16) 180.0 0_555 24_1 5_555 55_5 yes C(16) C(15) C(15) C(16) 180.0 0_555 24_1 5_555 55_5 yes #------------------------------------------------------------------------------ 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(1) 2.681(5) . 1_545 ? O(1) O(1) 3.287(10) . 3_646 ? O(1) N(1) 3.455(7) . 3_656 ? O(1) C(13) 3.504(8) . 4_444 ? O(1) C(1) 3.546(7) . 1_545 ? O(1) C(2) 3.560(6) . 1_545 ? O(2) N(1) 3.314(6) . 1_545 ? O(2) C(4) 3.376(7) . 3_756 ? O(2) C(10) 3.468(7) . . ? O(2) C(2) 3.534(6) . 1_545 ? N(1) C(16) 3.402(6) . 1_565 ? N(1) C(3) 3.581(6) . 3_766 ? C(1) C(5) 3.554(7) . 3_766 ? C(2) C(4) 3.524(8) . 3_766 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #-----------END data_compound_2 _database_code_CSD 206162 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C34 H30 Fe2 N4 O2 ' _chemical_formula_moiety ? _chemical_formula_weight 638.33 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _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 _cell_length_a 10.801(5) _cell_length_b 7.696(5) _cell_length_c 17.052(4) _cell_angle_alpha 90 _cell_angle_beta 95.10(3) _cell_angle_gamma 90 _cell_volume 1411(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.8 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.8 _exptl_crystal_size_min 0.5 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.066 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.608 _exptl_absorpt_correction_T_max 0.999 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 3653 _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9991 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% 0.62 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3229 _reflns_number_gt 2729 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1478 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2729 _refine_ls_number_parameters 190 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.12500(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0003 _refine_diff_density_max 0.47 _refine_diff_density_min -0.86 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Fe Fe 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.51019(3) -0.34381(5) 0.24244(2) 0.0358(1) Uani 1.00 d . . . O(1) O 0.2371(2) -0.6352(3) 0.0241(2) 0.0687(8) Uani 1.00 d . . . N(1) N 0.3762(3) -0.2372(4) -0.0472(2) 0.0594(8) Uani 1.00 d . . . N(2) N 0.2882(2) 0.0099(4) 0.0081(2) 0.0506(7) Uani 1.00 d . . . C(1) C 0.2978(3) -0.1032(5) -0.0487(2) 0.0519(8) Uani 1.00 d . . . C(2) C 0.3627(3) -0.0137(4) 0.0733(2) 0.0416(7) Uani 1.00 d . . . C(3) C 0.4488(3) -0.1485(3) 0.0836(2) 0.0363(6) Uani 1.00 d . . . C(4) C 0.4508(3) -0.2567(4) 0.0190(2) 0.0522(8) Uani 1.00 d . . . C(5) C 0.5315(3) -0.1687(3) 0.1556(2) 0.0406(7) Uani 1.00 d . . . C(6) C 0.5210(3) -0.0813(4) 0.2291(2) 0.0527(9) Uani 1.00 d . . . C(7) C 0.6185(4) -0.1407(4) 0.2837(2) 0.061(1) Uani 1.00 d . . . C(8) C 0.6898(3) -0.2613(5) 0.2456(2) 0.0605(10) Uani 1.00 d . . . C(9) C 0.6379(3) -0.2795(5) 0.1671(2) 0.0522(8) Uani 1.00 d . . . C(10) C 0.3638(5) -0.4953(7) 0.2074(3) 0.090(2) Uani 1.00 d . . . C(11) C 0.3417(4) -0.4031(7) 0.2762(4) 0.106(2) Uani 1.00 d . . . C(12) C 0.4404(4) -0.4616(5) 0.3355(2) 0.066(1) Uani 1.00 d . . . C(13) C 0.5086(4) -0.5818(5) 0.2966(2) 0.061(1) Uani 1.00 d . . . C(14) C 0.4640(5) -0.5982(5) 0.2197(3) 0.073(1) Uani 1.00 d . . . C(15) C 0.0966(3) -0.4018(4) 0.0346(2) 0.0497(8) Uani 1.00 d . . . C(16) C 0.1185(3) -0.5706(4) 0.0120(2) 0.0449(7) Uani 1.00 d . . . C(17) C 0.0214(3) -0.6682(4) -0.0224(2) 0.0482(8) Uani 1.00 d . . . H(1) H 0.2438 -0.0881 -0.0952 0.0760 Uiso 1.00 calc . . . H(2) H 0.3570 0.0657 0.1155 0.0760 Uiso 1.00 calc . . . H(3) H 0.5084 -0.3501 0.0217 0.0760 Uiso 1.00 calc . . . H(4) H 0.4587 0.0005 0.2397 0.0760 Uiso 1.00 calc . . . H(5) H 0.6324 -0.1062 0.3372 0.0760 Uiso 1.00 calc . . . H(6) H 0.7602 -0.3216 0.2691 0.0760 Uiso 1.00 calc . . . H(7) H 0.6680 -0.3539 0.1286 0.0760 Uiso 1.00 calc . . . H(8) H 0.2754 -0.3254 0.2839 0.0760 Uiso 1.00 calc . . . H(9) H 0.4526 -0.4289 0.3893 0.0760 Uiso 1.00 calc . . . H(10) H 0.5806 -0.6390 0.3197 0.0760 Uiso 1.00 calc . . . H(11) H 0.4972 -0.6709 0.1818 0.0760 Uiso 1.00 calc . . . H(12) H 0.3153 -0.4839 0.1584 0.0760 Uiso 1.00 calc . . . H(13) H 0.1641 -0.3316 0.0581 0.0760 Uiso 1.00 calc . . . H(14) H 0.0362 -0.7851 -0.0391 0.0760 Uiso 1.00 calc . . . H(18) H 0.2545 -0.7506 0.0086 0.0760 Uiso 1.00 calc . . . 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 0.0378(3) 0.0328(3) 0.0371(3) -0.0007(1) 0.0050(2) 0.0050(1) O(1) 0.049(1) 0.060(2) 0.094(2) 0.016(1) -0.008(1) -0.008(1) N(1) 0.070(2) 0.057(2) 0.051(1) 0.002(1) 0.001(1) -0.013(1) N(2) 0.046(1) 0.052(1) 0.053(1) 0.009(1) 0.001(1) 0.003(1) C(1) 0.049(2) 0.060(2) 0.046(2) -0.003(1) -0.002(1) 0.001(1) C(2) 0.045(1) 0.041(1) 0.039(1) 0.009(1) 0.006(1) 0.001(1) C(3) 0.038(1) 0.032(1) 0.039(1) -0.0020(9) 0.006(1) 0.0048(10) C(4) 0.057(2) 0.041(2) 0.059(2) 0.008(1) 0.006(1) -0.004(1) C(5) 0.042(1) 0.034(1) 0.046(1) -0.0016(10) 0.003(1) 0.010(1) C(6) 0.071(2) 0.030(1) 0.054(2) -0.003(1) -0.010(2) 0.002(1) C(7) 0.072(2) 0.045(2) 0.061(2) -0.014(2) -0.022(2) 0.008(1) C(8) 0.039(1) 0.069(2) 0.071(2) -0.009(1) -0.008(1) 0.029(2) C(9) 0.037(1) 0.064(2) 0.056(2) 0.007(1) 0.013(1) 0.020(2) C(10) 0.080(3) 0.107(4) 0.079(3) -0.057(3) -0.017(2) 0.031(3) C(11) 0.053(2) 0.080(3) 0.193(6) 0.013(2) 0.061(3) 0.058(4) C(12) 0.083(2) 0.063(2) 0.057(2) 0.009(2) 0.031(2) 0.019(2) C(13) 0.079(2) 0.046(2) 0.061(2) 0.002(2) 0.019(2) 0.017(2) C(14) 0.097(3) 0.050(2) 0.071(2) -0.020(2) 0.011(2) 0.003(2) C(15) 0.050(2) 0.040(1) 0.056(2) -0.002(1) -0.010(1) -0.005(1) C(16) 0.047(1) 0.041(1) 0.046(1) 0.008(1) 0.000(1) 0.003(1) C(17) 0.059(2) 0.035(1) 0.049(2) 0.008(1) -0.004(1) -0.009(1) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 C(5) 2.031(3) . . yes Fe C(6) 2.037(3) . . yes Fe C(7) 2.040(3) . . yes Fe C(8) 2.038(3) . . yes Fe C(9) 2.028(3) . . yes Fe C(10) 2.012(4) . . yes Fe C(11) 2.010(4) . . yes Fe C(12) 2.031(3) . . yes Fe C(13) 2.052(3) . . yes Fe C(14) 2.049(4) . . yes O(1) C(16) 1.373(4) . . yes N(1) C(1) 1.333(5) . . yes N(1) C(4) 1.336(4) . . yes N(2) C(1) 1.313(4) . . yes N(2) C(2) 1.325(4) . . yes C(2) C(3) 1.394(4) . . yes C(3) C(4) 1.383(4) . . yes C(3) C(5) 1.460(4) . . yes C(5) C(6) 1.436(4) . . yes C(5) C(9) 1.430(4) . . yes C(6) C(7) 1.419(5) . . yes C(7) C(8) 1.402(6) . . yes C(8) C(9) 1.412(5) . . yes C(10) C(11) 1.410(8) . . yes C(10) C(14) 1.342(7) . . yes C(11) C(12) 1.474(7) . . yes C(12) C(13) 1.388(5) . . yes C(13) C(14) 1.362(7) . . yes C(15) C(16) 1.381(4) . . yes C(15) C(17) 1.382(4) . 3_545 yes C(16) C(17) 1.378(4) . . 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 C(5) Fe C(6) 41.3(1) . . 0_555 yes C(5) Fe C(7) 69.2(1) . . 0_555 yes C(5) Fe C(8) 69.1(1) . . 0_555 yes C(5) Fe C(9) 41.3(1) . . 0_555 yes C(5) Fe C(10) 107.8(1) . . 0_555 yes C(5) Fe C(11) 121.6(2) . . 0_555 yes C(5) Fe C(12) 160.1(1) . . 0_555 yes C(5) Fe C(13) 157.9(1) . . 0_555 yes C(5) Fe C(14) 122.5(2) . . 0_555 yes C(6) Fe C(7) 40.7(1) . . 0_555 yes C(6) Fe C(8) 68.3(1) . . 0_555 yes C(6) Fe C(9) 68.8(2) . . 0_555 yes C(6) Fe C(10) 126.4(2) . . 0_555 yes C(6) Fe C(11) 108.6(2) . . 0_555 yes C(6) Fe C(12) 124.0(2) . . 0_555 yes C(6) Fe C(13) 159.7(1) . . 0_555 yes C(6) Fe C(14) 160.3(2) . . 0_555 yes C(7) Fe C(8) 40.2(2) . . 0_555 yes C(7) Fe C(9) 68.3(2) . . 0_555 yes C(7) Fe C(10) 163.3(2) . . 0_555 yes C(7) Fe C(11) 125.5(3) . . 0_555 yes C(7) Fe C(12) 108.3(2) . . 0_555 yes C(7) Fe C(13) 123.8(2) . . 0_555 yes C(7) Fe C(14) 156.9(2) . . 0_555 yes C(8) Fe C(9) 40.6(1) . . 0_555 yes C(8) Fe C(10) 155.5(2) . . 0_555 yes C(8) Fe C(11) 161.4(2) . . 0_555 yes C(8) Fe C(12) 122.5(2) . . 0_555 yes C(8) Fe C(13) 108.2(2) . . 0_555 yes C(8) Fe C(14) 121.2(2) . . 0_555 yes C(9) Fe C(10) 120.9(2) . . 0_555 yes C(9) Fe C(11) 157.1(2) . . 0_555 yes C(9) Fe C(12) 157.7(1) . . 0_555 yes C(9) Fe C(13) 122.4(1) . . 0_555 yes C(9) Fe C(14) 106.3(2) . . 0_555 yes C(10) Fe C(11) 41.0(2) . . 0_555 yes C(10) Fe C(12) 68.7(2) . . 0_555 yes C(10) Fe C(13) 65.1(2) . . 0_555 yes C(10) Fe C(14) 38.6(2) . . 0_555 yes C(11) Fe C(12) 42.8(2) . . 0_555 yes C(11) Fe C(13) 68.0(2) . . 0_555 yes C(11) Fe C(14) 68.0(2) . . 0_555 yes C(12) Fe C(13) 39.7(1) . . 0_555 yes C(12) Fe C(14) 67.7(2) . . 0_555 yes C(13) Fe C(14) 38.8(2) . . 0_555 yes C(1) N(1) C(4) 115.9(3) . . 0_555 yes C(1) N(2) C(2) 116.5(3) . . 0_555 yes N(1) C(1) N(2) 126.2(3) . . 0_555 yes N(2) C(2) C(3) 123.7(3) . . 0_555 yes C(2) C(3) C(4) 113.9(3) . . 0_555 yes C(2) C(3) C(5) 122.4(2) . . 0_555 yes C(4) C(3) C(5) 123.6(3) . . 0_555 yes N(1) C(4) C(3) 123.7(3) . . 0_555 yes Fe C(5) C(3) 125.7(2) . . 0_555 yes Fe C(5) C(6) 69.6(2) . . 0_555 yes Fe C(5) C(9) 69.2(2) . . 0_555 yes C(3) C(5) C(6) 126.4(3) . . 0_555 yes C(3) C(5) C(9) 127.1(3) . . 0_555 yes C(6) C(5) C(9) 106.5(3) . . 0_555 yes Fe C(6) C(5) 69.1(2) . . 0_555 yes Fe C(6) C(7) 69.7(2) . . 0_555 yes C(5) C(6) C(7) 108.1(3) . . 0_555 yes Fe C(7) C(6) 69.5(2) . . 0_555 yes Fe C(7) C(8) 69.8(2) . . 0_555 yes C(6) C(7) C(8) 108.4(3) . . 0_555 yes Fe C(8) C(7) 70.0(2) . . 0_555 yes Fe C(8) C(9) 69.3(2) . . 0_555 yes C(7) C(8) C(9) 108.4(3) . . 0_555 yes Fe C(9) C(5) 69.5(2) . . 0_555 yes Fe C(9) C(8) 70.1(2) . . 0_555 yes C(5) C(9) C(8) 108.6(3) . . 0_555 yes Fe C(10) C(11) 69.4(2) . . 0_555 yes Fe C(10) C(14) 72.2(2) . . 0_555 yes C(11) C(10) C(14) 111.2(4) . . 0_555 yes Fe C(11) C(10) 69.6(2) . . 0_555 yes Fe C(11) C(12) 69.4(2) . . 0_555 yes C(10) C(11) C(12) 104.5(4) . . 0_555 yes Fe C(12) C(11) 67.8(2) . . 0_555 yes Fe C(12) C(13) 71.0(2) . . 0_555 yes C(11) C(12) C(13) 105.0(4) . . 0_555 yes Fe C(13) C(12) 69.3(2) . . 0_555 yes Fe C(13) C(14) 70.5(2) . . 0_555 yes C(12) C(13) C(14) 111.4(4) . . 0_555 yes Fe C(14) C(10) 69.2(2) . . 0_555 yes Fe C(14) C(13) 70.7(2) . . 0_555 yes C(10) C(14) C(13) 107.9(4) . . 0_555 yes C(16) C(15) C(17) 120.2(3) . 3_545 0_555 yes O(1) C(16) C(15) 118.6(3) . . 0_555 yes O(1) C(16) C(17) 122.1(3) . . 0_555 yes C(15) C(16) C(17) 119.3(3) . . 0_555 yes C(15) C(17) C(16) 120.6(3) 3_545 . 0_555 yes #------------------------------------------------------------------------------ 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe C(5) C(3) C(2) 103.1(3) 0_555 20_1 5_555 55_5 yes Fe C(5) C(3) C(4) -78.9(4) 0_555 20_1 5_555 55_5 yes Fe C(5) C(6) C(7) 59.0(2) 0_555 20_1 5_555 55_5 yes Fe C(5) C(9) C(8) -59.4(2) 0_555 20_1 5_555 55_5 yes Fe C(6) C(5) C(3) 119.9(3) 0_555 20_1 5_555 55_5 yes Fe C(6) C(5) C(9) -59.7(2) 0_555 20_1 5_555 55_5 yes Fe C(6) C(7) C(8) 59.2(2) 0_555 20_1 5_555 55_5 yes Fe C(7) C(6) C(5) -58.6(2) 0_555 20_1 5_555 55_5 yes Fe C(7) C(8) C(9) 58.8(2) 0_555 20_1 5_555 55_5 yes Fe C(8) C(7) C(6) -59.0(2) 0_555 20_1 5_555 55_5 yes Fe C(8) C(9) C(5) 59.0(2) 0_555 20_1 5_555 55_5 yes Fe C(9) C(5) C(3) -119.7(3) 0_555 20_1 5_555 55_5 yes Fe C(9) C(5) C(6) 59.9(2) 0_555 20_1 5_555 55_5 yes Fe C(9) C(8) C(7) -59.2(2) 0_555 20_1 5_555 55_5 yes Fe C(10) C(11) C(12) -61.0(3) 0_555 20_1 5_555 55_5 yes Fe C(10) C(14) C(13) 60.4(3) 0_555 20_1 5_555 55_5 yes Fe C(11) C(10) C(14) 60.3(3) 0_555 20_1 5_555 55_5 yes Fe C(11) C(12) C(13) -61.7(3) 0_555 20_1 5_555 55_5 yes Fe C(12) C(11) C(10) 61.1(3) 0_555 20_1 5_555 55_5 yes Fe C(12) C(13) C(14) -57.9(3) 0_555 20_1 5_555 55_5 yes Fe C(13) C(12) C(11) 59.7(2) 0_555 20_1 5_555 55_5 yes Fe C(13) C(14) C(10) -59.5(3) 0_555 20_1 5_555 55_5 yes Fe C(14) C(10) C(11) -58.6(3) 0_555 20_1 5_555 55_5 yes Fe C(14) C(13) C(12) 57.2(3) 0_555 20_1 5_555 55_5 yes O(1) C(16) C(15) C(17) 179.1(3) 0_555 20_1 5_555 55_5 yes O(1) C(16) C(17) C(15) -179.1(3) 0_555 20_1 5_555 55_5 yes N(1) C(1) N(2) C(2) -1.0(5) 0_555 20_1 5_555 55_5 yes N(1) C(4) C(3) C(2) -1.1(5) 0_555 20_1 5_555 55_5 yes N(1) C(4) C(3) C(5) -179.2(3) 0_555 20_1 5_555 55_5 yes N(2) C(1) N(1) C(4) 0.4(6) 0_555 20_1 5_555 55_5 yes N(2) C(2) C(3) C(4) 0.4(4) 0_555 20_1 5_555 55_5 yes N(2) C(2) C(3) C(5) 178.6(3) 0_555 20_1 5_555 55_5 yes C(1) N(1) C(4) C(3) 0.7(5) 0_555 20_1 5_555 55_5 yes C(1) N(2) C(2) C(3) 0.5(5) 0_555 20_1 5_555 55_5 yes C(2) C(3) C(5) C(6) 13.3(4) 0_555 20_1 5_555 55_5 yes C(2) C(3) C(5) C(9) -167.2(3) 0_555 20_1 5_555 55_5 yes C(3) C(5) Fe C(6) -120.9(3) 0_555 20_1 5_555 55_5 yes C(3) C(5) Fe C(7) -158.2(3) 0_555 20_1 5_555 55_5 yes C(3) C(5) Fe C(8) 158.6(3) 0_555 20_1 5_555 55_5 yes C(3) C(5) Fe C(9) 121.4(3) 0_555 20_1 5_555 55_5 yes C(3) C(5) Fe C(10) 4.5(3) 0_555 20_1 5_555 55_5 yes C(3) C(5) Fe C(11) -38.4(4) 0_555 20_1 5_555 55_5 yes C(3) C(5) Fe C(12) -71.9(5) 0_555 20_1 5_555 55_5 yes C(3) C(5) Fe C(13) 71.7(5) 0_555 20_1 5_555 55_5 yes C(3) C(5) Fe C(14) 44.2(3) 0_555 20_1 5_555 55_5 yes C(3) C(5) C(6) C(7) 178.9(3) 0_555 20_1 5_555 55_5 yes C(3) C(5) C(9) C(8) -179.0(3) 0_555 20_1 5_555 55_5 yes C(4) C(3) C(5) C(6) -168.7(3) 0_555 20_1 5_555 55_5 yes C(4) C(3) C(5) C(9) 10.8(5) 0_555 20_1 5_555 55_5 yes C(5) Fe C(6) C(7) -119.7(3) 0_555 20_1 5_555 55_5 yes C(5) Fe C(7) C(6) 37.9(2) 0_555 20_1 5_555 55_5 yes C(5) Fe C(7) C(8) -81.9(2) 0_555 20_1 5_555 55_5 yes C(5) Fe C(8) C(7) 82.1(2) 0_555 20_1 5_555 55_5 yes C(5) Fe C(8) C(9) -37.8(2) 0_555 20_1 5_555 55_5 yes C(5) Fe C(9) C(8) 119.8(3) 0_555 20_1 5_555 55_5 yes C(5) Fe C(10) C(11) -118.0(3) 0_555 20_1 5_555 55_5 yes C(5) Fe C(10) C(14) 120.2(3) 0_555 20_1 5_555 55_5 yes C(5) Fe C(11) C(10) 80.8(3) 0_555 20_1 5_555 55_5 yes C(5) Fe C(11) C(12) -164.0(2) 0_555 20_1 5_555 55_5 yes C(5) Fe C(12) C(11) 43.8(6) 0_555 20_1 5_555 55_5 yes C(5) Fe C(12) C(13) 159.6(4) 0_555 20_1 5_555 55_5 yes C(5) Fe C(13) C(12) -161.6(3) 0_555 20_1 5_555 55_5 yes C(5) Fe C(13) C(14) -38.4(6) 0_555 20_1 5_555 55_5 yes C(5) Fe C(14) C(10) -77.4(3) 0_555 20_1 5_555 55_5 yes C(5) Fe C(14) C(13) 163.9(2) 0_555 20_1 5_555 55_5 yes C(5) C(6) Fe C(7) 119.7(3) 0_555 20_1 5_555 55_5 yes C(5) C(6) Fe C(8) 82.6(2) 0_555 20_1 5_555 55_5 yes C(5) C(6) Fe C(9) 38.8(2) 0_555 20_1 5_555 55_5 yes C(5) C(6) Fe C(10) -74.8(3) 0_555 20_1 5_555 55_5 yes C(5) C(6) Fe C(11) -117.0(3) 0_555 20_1 5_555 55_5 yes C(5) C(6) Fe C(12) -162.0(2) 0_555 20_1 5_555 55_5 yes C(5) C(6) Fe C(13) 166.4(4) 0_555 20_1 5_555 55_5 yes C(5) C(6) Fe C(14) -40.3(6) 0_555 20_1 5_555 55_5 yes C(5) C(6) C(7) C(8) 0.6(4) 0_555 20_1 5_555 55_5 yes C(5) C(9) Fe C(6) -38.8(2) 0_555 20_1 5_555 55_5 yes C(5) C(9) Fe C(7) -82.7(2) 0_555 20_1 5_555 55_5 yes C(5) C(9) Fe C(8) -119.8(3) 0_555 20_1 5_555 55_5 yes C(5) C(9) Fe C(10) 81.7(3) 0_555 20_1 5_555 55_5 yes C(5) C(9) Fe C(11) 48.9(6) 0_555 20_1 5_555 55_5 yes C(5) C(9) Fe C(12) -168.1(4) 0_555 20_1 5_555 55_5 yes C(5) C(9) Fe C(13) 160.1(2) 0_555 20_1 5_555 55_5 yes C(5) C(9) Fe C(14) 121.0(2) 0_555 20_1 5_555 55_5 yes C(5) C(9) C(8) C(7) -0.2(4) 0_555 20_1 5_555 55_5 yes C(6) Fe C(5) C(9) 117.7(3) 0_555 20_1 5_555 55_5 yes C(6) Fe C(7) C(8) -119.8(3) 0_555 20_1 5_555 55_5 yes C(6) Fe C(8) C(7) 37.6(2) 0_555 20_1 5_555 55_5 yes C(6) Fe C(8) C(9) -82.3(2) 0_555 20_1 5_555 55_5 yes C(6) Fe C(9) C(8) 81.0(2) 0_555 20_1 5_555 55_5 yes C(6) Fe C(10) C(11) -76.0(3) 0_555 20_1 5_555 55_5 yes C(6) Fe C(10) C(14) 162.2(3) 0_555 20_1 5_555 55_5 yes C(6) Fe C(11) C(10) 124.5(3) 0_555 20_1 5_555 55_5 yes C(6) Fe C(11) C(12) -120.3(2) 0_555 20_1 5_555 55_5 yes C(6) Fe C(12) C(11) 80.7(3) 0_555 20_1 5_555 55_5 yes C(6) Fe C(12) C(13) -163.5(2) 0_555 20_1 5_555 55_5 yes C(6) Fe C(13) C(12) 42.8(6) 0_555 20_1 5_555 55_5 yes C(6) Fe C(13) C(14) 166.0(4) 0_555 20_1 5_555 55_5 yes C(6) Fe C(14) C(10) -46.9(7) 0_555 20_1 5_555 55_5 yes C(6) Fe C(14) C(13) -165.6(4) 0_555 20_1 5_555 55_5 yes C(6) C(5) Fe C(7) -37.3(2) 0_555 20_1 5_555 55_5 yes C(6) C(5) Fe C(8) -80.5(2) 0_555 20_1 5_555 55_5 yes C(6) C(5) Fe C(9) -117.7(3) 0_555 20_1 5_555 55_5 yes C(6) C(5) Fe C(10) 125.3(3) 0_555 20_1 5_555 55_5 yes C(6) C(5) Fe C(11) 82.4(3) 0_555 20_1 5_555 55_5 yes C(6) C(5) Fe C(12) 49.0(5) 0_555 20_1 5_555 55_5 yes C(6) C(5) Fe C(13) -167.5(4) 0_555 20_1 5_555 55_5 yes C(6) C(5) Fe C(14) 165.0(2) 0_555 20_1 5_555 55_5 yes C(6) C(5) C(9) C(8) 0.5(4) 0_555 20_1 5_555 55_5 yes C(6) C(7) Fe C(8) 119.8(3) 0_555 20_1 5_555 55_5 yes C(6) C(7) Fe C(9) 82.3(2) 0_555 20_1 5_555 55_5 yes C(6) C(7) Fe C(10) -44.5(7) 0_555 20_1 5_555 55_5 yes C(6) C(7) Fe C(11) -76.8(3) 0_555 20_1 5_555 55_5 yes C(6) C(7) Fe C(12) -121.2(2) 0_555 20_1 5_555 55_5 yes C(6) C(7) Fe C(13) -162.4(2) 0_555 20_1 5_555 55_5 yes C(6) C(7) Fe C(14) 163.0(4) 0_555 20_1 5_555 55_5 yes C(6) C(7) C(8) C(9) -0.2(4) 0_555 20_1 5_555 55_5 yes C(7) Fe C(5) C(9) 80.4(2) 0_555 20_1 5_555 55_5 yes C(7) Fe C(8) C(9) -119.8(3) 0_555 20_1 5_555 55_5 yes C(7) Fe C(9) C(8) 37.1(2) 0_555 20_1 5_555 55_5 yes C(7) Fe C(10) C(11) -41.4(7) 0_555 20_1 5_555 55_5 yes C(7) Fe C(10) C(14) -163.1(5) 0_555 20_1 5_555 55_5 yes C(7) Fe C(11) C(10) 166.5(3) 0_555 20_1 5_555 55_5 yes C(7) Fe C(11) C(12) -78.2(3) 0_555 20_1 5_555 55_5 yes C(7) Fe C(12) C(11) 123.0(3) 0_555 20_1 5_555 55_5 yes C(7) Fe C(12) C(13) -121.2(3) 0_555 20_1 5_555 55_5 yes C(7) Fe C(13) C(12) 77.7(3) 0_555 20_1 5_555 55_5 yes C(7) Fe C(13) C(14) -159.2(3) 0_555 20_1 5_555 55_5 yes C(7) Fe C(14) C(10) 167.7(4) 0_555 20_1 5_555 55_5 yes C(7) Fe C(14) C(13) 49.0(6) 0_555 20_1 5_555 55_5 yes C(7) C(6) Fe C(8) -37.1(3) 0_555 20_1 5_555 55_5 yes C(7) C(6) Fe C(9) -80.9(3) 0_555 20_1 5_555 55_5 yes C(7) C(6) Fe C(10) 165.5(3) 0_555 20_1 5_555 55_5 yes C(7) C(6) Fe C(11) 123.3(3) 0_555 20_1 5_555 55_5 yes C(7) C(6) Fe C(12) 78.3(3) 0_555 20_1 5_555 55_5 yes C(7) C(6) Fe C(13) 46.7(6) 0_555 20_1 5_555 55_5 yes C(7) C(6) Fe C(14) -160.1(5) 0_555 20_1 5_555 55_5 yes C(7) C(6) C(5) C(9) -0.7(4) 0_555 20_1 5_555 55_5 yes C(7) C(8) Fe C(9) 119.8(3) 0_555 20_1 5_555 55_5 yes C(7) C(8) Fe C(10) 169.2(4) 0_555 20_1 5_555 55_5 yes C(7) C(8) Fe C(11) -46.4(6) 0_555 20_1 5_555 55_5 yes C(7) C(8) Fe C(12) -79.8(2) 0_555 20_1 5_555 55_5 yes C(7) C(8) Fe C(13) -121.2(2) 0_555 20_1 5_555 55_5 yes C(7) C(8) Fe C(14) -161.7(2) 0_555 20_1 5_555 55_5 yes C(8) Fe C(5) C(9) 37.2(2) 0_555 20_1 5_555 55_5 yes C(8) Fe C(10) C(11) 163.5(3) 0_555 20_1 5_555 55_5 yes C(8) Fe C(10) C(14) 41.8(5) 0_555 20_1 5_555 55_5 yes C(8) Fe C(11) C(10) -158.4(5) 0_555 20_1 5_555 55_5 yes C(8) Fe C(11) C(12) -43.1(6) 0_555 20_1 5_555 55_5 yes C(8) Fe C(12) C(11) 165.0(3) 0_555 20_1 5_555 55_5 yes C(8) Fe C(12) C(13) -79.2(3) 0_555 20_1 5_555 55_5 yes C(8) Fe C(13) C(12) 119.3(3) 0_555 20_1 5_555 55_5 yes C(8) Fe C(13) C(14) -117.5(3) 0_555 20_1 5_555 55_5 yes C(8) Fe C(14) C(10) -161.1(3) 0_555 20_1 5_555 55_5 yes C(8) Fe C(14) C(13) 80.1(3) 0_555 20_1 5_555 55_5 yes C(8) C(7) Fe C(9) -37.5(2) 0_555 20_1 5_555 55_5 yes C(8) C(7) Fe C(10) -164.3(5) 0_555 20_1 5_555 55_5 yes C(8) C(7) Fe C(11) 163.5(2) 0_555 20_1 5_555 55_5 yes C(8) C(7) Fe C(12) 119.0(2) 0_555 20_1 5_555 55_5 yes C(8) C(7) Fe C(13) 77.9(3) 0_555 20_1 5_555 55_5 yes C(8) C(7) Fe C(14) 43.2(5) 0_555 20_1 5_555 55_5 yes C(8) C(9) Fe C(10) -158.4(3) 0_555 20_1 5_555 55_5 yes C(8) C(9) Fe C(11) 168.8(5) 0_555 20_1 5_555 55_5 yes C(8) C(9) Fe C(12) -48.3(5) 0_555 20_1 5_555 55_5 yes C(8) C(9) Fe C(13) -80.1(3) 0_555 20_1 5_555 55_5 yes C(8) C(9) Fe C(14) -119.2(3) 0_555 20_1 5_555 55_5 yes C(9) Fe C(10) C(11) -161.3(3) 0_555 20_1 5_555 55_5 yes C(9) Fe C(10) C(14) 77.0(3) 0_555 20_1 5_555 55_5 yes C(9) Fe C(11) C(10) 45.0(6) 0_555 20_1 5_555 55_5 yes C(9) Fe C(11) C(12) 160.3(4) 0_555 20_1 5_555 55_5 yes C(9) Fe C(12) C(11) -159.8(4) 0_555 20_1 5_555 55_5 yes C(9) Fe C(12) C(13) -44.0(6) 0_555 20_1 5_555 55_5 yes C(9) Fe C(13) C(12) 161.8(2) 0_555 20_1 5_555 55_5 yes C(9) Fe C(13) C(14) -75.0(3) 0_555 20_1 5_555 55_5 yes C(9) Fe C(14) C(10) -119.5(3) 0_555 20_1 5_555 55_5 yes C(9) Fe C(14) C(13) 121.8(3) 0_555 20_1 5_555 55_5 yes C(9) C(5) Fe C(10) -117.0(3) 0_555 20_1 5_555 55_5 yes C(9) C(5) Fe C(11) -159.8(3) 0_555 20_1 5_555 55_5 yes C(9) C(5) Fe C(12) 166.7(4) 0_555 20_1 5_555 55_5 yes C(9) C(5) Fe C(13) -49.7(5) 0_555 20_1 5_555 55_5 yes C(9) C(5) Fe C(14) -77.3(3) 0_555 20_1 5_555 55_5 yes C(9) C(8) Fe C(10) 49.4(5) 0_555 20_1 5_555 55_5 yes C(9) C(8) Fe C(11) -166.3(5) 0_555 20_1 5_555 55_5 yes C(9) C(8) Fe C(12) 160.3(2) 0_555 20_1 5_555 55_5 yes C(9) C(8) Fe C(13) 119.0(2) 0_555 20_1 5_555 55_5 yes C(9) C(8) Fe C(14) 78.4(3) 0_555 20_1 5_555 55_5 yes C(10) Fe C(11) C(12) 115.2(4) 0_555 20_1 5_555 55_5 yes C(10) Fe C(12) C(11) -39.6(3) 0_555 20_1 5_555 55_5 yes C(10) Fe C(12) C(13) 76.2(3) 0_555 20_1 5_555 55_5 yes C(10) Fe C(13) C(12) -86.1(3) 0_555 20_1 5_555 55_5 yes C(10) Fe C(13) C(14) 37.1(3) 0_555 20_1 5_555 55_5 yes C(10) Fe C(14) C(13) -118.7(4) 0_555 20_1 5_555 55_5 yes C(10) C(11) Fe C(12) -115.2(4) 0_555 20_1 5_555 55_5 yes C(10) C(11) Fe C(13) -76.9(3) 0_555 20_1 5_555 55_5 yes C(10) C(11) Fe C(14) -34.9(3) 0_555 20_1 5_555 55_5 yes C(10) C(11) C(12) C(13) -0.6(4) 0_555 20_1 5_555 55_5 yes C(10) C(14) Fe C(11) 37.0(3) 0_555 20_1 5_555 55_5 yes C(10) C(14) Fe C(12) 83.4(3) 0_555 20_1 5_555 55_5 yes C(10) C(14) Fe C(13) 118.7(4) 0_555 20_1 5_555 55_5 yes C(10) C(14) C(13) C(12) -2.3(5) 0_555 20_1 5_555 55_5 yes C(11) Fe C(10) C(14) -121.8(4) 0_555 20_1 5_555 55_5 yes C(11) Fe C(12) C(13) 115.8(4) 0_555 20_1 5_555 55_5 yes C(11) Fe C(13) C(12) -41.3(3) 0_555 20_1 5_555 55_5 yes C(11) Fe C(13) C(14) 81.9(4) 0_555 20_1 5_555 55_5 yes C(11) Fe C(14) C(13) -81.7(3) 0_555 20_1 5_555 55_5 yes C(11) C(10) Fe C(12) 41.3(3) 0_555 20_1 5_555 55_5 yes C(11) C(10) Fe C(13) 84.5(3) 0_555 20_1 5_555 55_5 yes C(11) C(10) Fe C(14) 121.8(4) 0_555 20_1 5_555 55_5 yes C(11) C(10) C(14) C(13) 1.8(5) 0_555 20_1 5_555 55_5 yes C(11) C(12) Fe C(13) -115.8(4) 0_555 20_1 5_555 55_5 yes C(11) C(12) Fe C(14) -81.3(3) 0_555 20_1 5_555 55_5 yes C(11) C(12) C(13) C(14) 1.8(4) 0_555 20_1 5_555 55_5 yes C(12) Fe C(10) C(14) -80.5(3) 0_555 20_1 5_555 55_5 yes C(12) Fe C(13) C(14) 123.2(4) 0_555 20_1 5_555 55_5 yes C(12) Fe C(14) C(13) -35.3(3) 0_555 20_1 5_555 55_5 yes C(12) C(11) Fe C(13) 38.4(2) 0_555 20_1 5_555 55_5 yes C(12) C(11) Fe C(14) 80.4(3) 0_555 20_1 5_555 55_5 yes C(12) C(11) C(10) C(14) -0.7(5) 0_555 20_1 5_555 55_5 yes C(12) C(13) Fe C(14) -123.2(4) 0_555 20_1 5_555 55_5 yes C(13) Fe C(10) C(14) -37.3(3) 0_555 20_1 5_555 55_5 yes C(13) C(12) Fe C(14) 34.5(3) 0_555 20_1 5_555 55_5 yes C(13) C(12) Fe C(14) 34.5(3) 0_555 20_1 5_555 55_5 yes #------------------------------------------------------------------------------ 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(2) 2.805(4) . 1_545 ? O(1) C(2) 3.290(4) . 1_545 ? O(1) C(10) 3.471(6) . . ? N(1) C(2) 3.479(4) . 3_655 ? N(2) C(4) 3.463(4) . 3_655 ? N(2) C(3) 3.527(4) . 3_655 ? C(1) C(5) 3.420(4) . 3_655 ? C(1) C(3) 3.448(4) . 3_655 ? C(1) C(15) 3.545(5) . . ? C(2) C(4) 3.380(5) . 3_655 ? #------------------------------------------------------------------------------ loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_site_distance_DH _geom_hbond_site_distance_HA _geom_hbond_site_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O(1) H(18) N(2) . . 1_545 0.950 1.879 2.805(4) 164.075 no #------------------------------------------------------------------------------ #-----------END data_compound_3 _database_code_CSD 206163 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C34 H30 Fe2 N4 O2 ' _chemical_formula_moiety ? _chemical_formula_weight 638.33 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _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 _cell_length_a 10.766(3) _cell_length_b 7.576(3) _cell_length_c 17.452(4) _cell_angle_alpha 90 _cell_angle_beta 94.59(2) _cell_angle_gamma 90 _cell_volume 1418.9(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.8 _cell_measurement_theta_max 14.9 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.2 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.061 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.772 _exptl_absorpt_correction_T_max 0.999 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 3679 _diffrn_reflns_av_R_equivalents 0.066 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9981 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9981 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% 1.13 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3249 _reflns_number_gt 2071 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1430 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2071 _refine_ls_number_parameters 199 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.11000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0002 _refine_diff_density_max 0.46 _refine_diff_density_min -0.31 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Fe Fe 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.50822(5) 0.34450(8) 0.23889(4) 0.0384(2) Uani 1.00 d . . . O(1) O 0.4429(7) 0.3388(9) 0.5262(5) 0.072(2) Uani 0.50 d P . . O(2) O 0.2797(7) 0.1337(9) 0.4708(5) 0.072(3) Uani 0.50 d P . . N(1) N 0.2880(4) -0.0016(6) 0.0108(2) 0.056(1) Uani 1.00 d . . . N(2) N 0.3841(5) 0.2470(7) -0.0414(3) 0.067(2) Uani 1.00 d . . . C(1) C 0.3031(6) 0.1168(8) -0.0432(3) 0.068(2) Uani 1.00 d . . . C(2) C 0.4570(5) 0.2587(7) 0.0229(3) 0.062(2) Uani 1.00 d . . . C(3) C 0.4516(4) 0.1457(5) 0.0856(3) 0.042(1) Uani 1.00 d . . . C(4) C 0.3622(4) 0.0147(6) 0.0744(3) 0.046(1) Uani 1.00 d . . . C(5) C 0.5332(4) 0.1617(6) 0.1569(3) 0.045(1) Uani 1.00 d . . . C(6) C 0.6409(4) 0.2714(8) 0.1693(3) 0.058(1) Uani 1.00 d . . . C(7) C 0.6879(5) 0.2570(8) 0.2465(4) 0.064(2) Uani 1.00 d . . . C(8) C 0.6110(6) 0.1368(7) 0.2841(3) 0.065(2) Uani 1.00 d . . . C(9) C 0.5147(5) 0.0773(6) 0.2282(3) 0.055(1) Uani 1.00 d . . . C(10) C 0.3610(6) 0.4920(9) 0.1998(4) 0.080(2) Uani 1.00 d . . . C(11) C 0.4636(7) 0.6013(7) 0.2143(4) 0.073(2) Uani 1.00 d . . . C(12) C 0.5035(5) 0.5877(7) 0.2920(3) 0.061(2) Uani 1.00 d . . . C(13) C 0.4279(6) 0.4683(7) 0.3265(3) 0.064(2) Uani 1.00 d . . . C(14) C 0.3370(5) 0.4073(9) 0.2691(5) 0.083(2) Uani 1.00 d . . . C(15) C 0.5880(7) 0.1040(8) 0.5359(4) 0.080(2) Uani 1.00 d . . . C(16) C 0.4723(6) 0.1753(7) 0.5160(4) 0.069(2) Uani 1.00 d . . . C(17) C 0.3829(6) 0.0704(8) 0.4819(4) 0.073(2) Uani 1.00 d . . . H(1) H 0.2491 0.1067 -0.0888 0.0811 Uiso 1.00 calc . . . H(2) H 0.5173 0.3505 0.0267 0.0740 Uiso 1.00 calc . . . H(3) H 0.3539 -0.0679 0.1146 0.0550 Uiso 1.00 calc . . . H(4) H 0.6744 0.3442 0.1316 0.0699 Uiso 1.00 calc . . . H(5) H 0.7580 0.3183 0.2699 0.0773 Uiso 1.00 calc . . . H(6) H 0.6207 0.1036 0.3367 0.0779 Uiso 1.00 calc . . . H(7) H 0.4496 -0.0027 0.2374 0.0656 Uiso 1.00 calc . . . H(8) H 0.3142 0.4781 0.1517 0.0966 Uiso 1.00 calc . . . H(9) H 0.5000 0.6733 0.1776 0.0880 Uiso 1.00 calc . . . H(10) H 0.5733 0.6471 0.3168 0.0737 Uiso 1.00 calc . . . H(11) H 0.4350 0.4343 0.3791 0.0766 Uiso 1.00 calc . . . H(12) H 0.2709 0.3273 0.2763 0.0995 Uiso 1.00 calc . . . H(13) H 0.6583 0.1788 0.5459 0.0956 Uiso 1.00 calc . . . H(14) H 0.3610 0.3789 0.5110 0.0860 Uiso 0.50 calc P . . H(15) H 0.2623 0.2600 0.4645 0.0760 Uiso 0.50 calc P . . 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 0.0384(3) 0.0330(3) 0.0445(4) 0.0011(3) 0.0073(2) -0.0038(3) O(1) 0.061(4) 0.063(5) 0.085(5) 0.013(4) -0.029(4) -0.031(4) O(2) 0.060(4) 0.046(4) 0.105(6) 0.012(4) -0.023(4) -0.005(4) N(1) 0.055(2) 0.058(2) 0.054(3) 0.000(2) 0.001(2) -0.001(2) N(2) 0.081(3) 0.066(3) 0.055(3) -0.001(3) 0.009(2) 0.015(2) C(1) 0.070(3) 0.084(4) 0.048(3) 0.007(3) 0.003(3) -0.003(3) C(2) 0.070(3) 0.047(3) 0.071(4) -0.008(3) 0.020(3) 0.003(3) C(3) 0.046(2) 0.036(2) 0.047(2) 0.003(2) 0.013(2) -0.003(2) C(4) 0.051(3) 0.044(2) 0.043(3) -0.002(2) 0.009(2) -0.003(2) C(5) 0.042(2) 0.037(2) 0.056(3) 0.001(2) 0.007(2) -0.008(2) C(6) 0.044(2) 0.065(3) 0.069(3) -0.006(2) 0.023(2) -0.017(3) C(7) 0.039(2) 0.069(4) 0.085(4) 0.009(3) 0.001(3) -0.020(3) C(8) 0.071(3) 0.055(3) 0.065(3) 0.017(3) -0.019(3) -0.004(3) C(9) 0.065(3) 0.031(2) 0.066(3) 0.005(2) -0.004(2) 0.003(2) C(10) 0.077(4) 0.072(4) 0.088(5) 0.040(4) -0.022(4) -0.030(4) C(11) 0.109(5) 0.044(3) 0.068(4) 0.019(3) 0.012(4) 0.002(3) C(12) 0.072(3) 0.045(3) 0.069(3) 0.004(3) 0.019(3) -0.015(2) C(13) 0.076(4) 0.057(3) 0.062(3) 0.003(3) 0.029(3) -0.013(3) C(14) 0.048(3) 0.060(4) 0.146(7) 0.000(3) 0.039(4) -0.031(4) C(15) 0.089(5) 0.053(3) 0.097(5) -0.006(3) 0.007(4) -0.002(3) C(16) 0.082(4) 0.046(3) 0.080(4) 0.011(3) 0.014(3) 0.004(3) C(17) 0.076(4) 0.052(3) 0.093(4) 0.007(3) 0.014(3) 0.009(3) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS97 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 C(5) 2.025(4) . . yes Fe C(6) 2.025(4) . . yes Fe C(7) 2.039(5) . . yes Fe C(8) 2.045(5) . . yes Fe C(9) 2.035(5) . . yes Fe C(10) 2.013(5) . . yes Fe C(11) 2.042(6) . . yes Fe C(12) 2.065(5) . . yes Fe C(13) 2.044(5) . . yes Fe C(14) 2.014(5) . . yes O(1) C(16) 1.294(8) . . yes O(2) C(17) 1.212(9) . . yes N(1) C(1) 1.322(7) . . yes N(1) C(4) 1.320(6) . . yes N(2) C(1) 1.315(8) . . yes N(2) C(2) 1.320(7) . . yes C(2) C(3) 1.394(7) . . yes C(3) C(4) 1.385(6) . . yes C(3) C(5) 1.469(6) . . yes C(5) C(6) 1.429(6) . . yes C(5) C(9) 1.428(7) . . yes C(6) C(7) 1.406(7) . . yes C(7) C(8) 1.425(8) . . yes C(8) C(9) 1.437(7) . . yes C(10) C(11) 1.387(10) . . yes C(10) C(14) 1.411(10) . . yes C(11) C(12) 1.393(9) . . yes C(12) C(13) 1.387(8) . . yes C(13) C(14) 1.421(9) . . yes C(15) C(16) 1.377(9) . . yes C(15) C(17) 1.398(8) . 3_656 yes C(16) C(17) 1.349(9) . . 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 C(5) Fe C(6) 41.3(2) . . 0_555 yes C(5) Fe C(7) 69.2(2) . . 0_555 yes C(5) Fe C(8) 69.4(2) . . 0_555 yes C(5) Fe C(9) 41.2(2) . . 0_555 yes C(5) Fe C(10) 106.6(2) . . 0_555 yes C(5) Fe C(11) 123.1(2) . . 0_555 yes C(5) Fe C(12) 159.5(2) . . 0_555 yes C(5) Fe C(13) 158.5(2) . . 0_555 yes C(5) Fe C(14) 121.5(2) . . 0_555 yes C(6) Fe C(7) 40.5(2) . . 0_555 yes C(6) Fe C(8) 68.6(2) . . 0_555 yes C(6) Fe C(9) 69.0(2) . . 0_555 yes C(6) Fe C(10) 121.5(3) . . 0_555 yes C(6) Fe C(11) 107.5(2) . . 0_555 yes C(6) Fe C(12) 123.8(2) . . 0_555 yes C(6) Fe C(13) 159.3(2) . . 0_555 yes C(6) Fe C(14) 157.8(3) . . 0_555 yes C(7) Fe C(8) 40.8(2) . . 0_555 yes C(7) Fe C(9) 69.1(2) . . 0_555 yes C(7) Fe C(10) 156.9(3) . . 0_555 yes C(7) Fe C(11) 122.0(3) . . 0_555 yes C(7) Fe C(12) 108.5(2) . . 0_555 yes C(7) Fe C(13) 123.8(3) . . 0_555 yes C(7) Fe C(14) 160.6(3) . . 0_555 yes C(8) Fe C(9) 41.2(2) . . 0_555 yes C(8) Fe C(10) 160.9(3) . . 0_555 yes C(8) Fe C(11) 157.7(3) . . 0_555 yes C(8) Fe C(12) 123.1(2) . . 0_555 yes C(8) Fe C(13) 108.3(2) . . 0_555 yes C(8) Fe C(14) 124.0(3) . . 0_555 yes C(9) Fe C(10) 123.6(2) . . 0_555 yes C(9) Fe C(11) 159.8(3) . . 0_555 yes C(9) Fe C(12) 158.6(2) . . 0_555 yes C(9) Fe C(13) 123.0(2) . . 0_555 yes C(9) Fe C(14) 107.3(2) . . 0_555 yes C(10) Fe C(11) 40.0(3) . . 0_555 yes C(10) Fe C(12) 67.0(2) . . 0_555 yes C(10) Fe C(13) 68.3(3) . . 0_555 yes C(10) Fe C(14) 41.0(3) . . 0_555 yes C(11) Fe C(12) 39.7(3) . . 0_555 yes C(11) Fe C(13) 67.2(2) . . 0_555 yes C(11) Fe C(14) 68.0(3) . . 0_555 yes C(12) Fe C(13) 39.4(2) . . 0_555 yes C(12) Fe C(14) 67.4(2) . . 0_555 yes C(13) Fe C(14) 41.0(3) . . 0_555 yes C(1) N(1) C(4) 115.9(5) . . 0_555 yes C(1) N(2) C(2) 114.8(5) . . 0_555 yes N(1) C(1) N(2) 127.6(5) . . 0_555 yes N(2) C(2) C(3) 124.5(5) . . 0_555 yes C(2) C(3) C(4) 113.7(4) . . 0_555 yes C(2) C(3) C(5) 123.6(4) . . 0_555 yes C(4) C(3) C(5) 122.7(4) . . 0_555 yes N(1) C(4) C(3) 123.5(4) . . 0_555 yes Fe C(5) C(3) 123.4(3) . . 0_555 yes Fe C(5) C(6) 69.3(3) . . 0_555 yes Fe C(5) C(9) 69.8(3) . . 0_555 yes C(3) C(5) C(6) 126.8(4) . . 0_555 yes C(3) C(5) C(9) 125.9(4) . . 0_555 yes C(6) C(5) C(9) 107.2(4) . . 0_555 yes Fe C(6) C(5) 69.3(2) . . 0_555 yes Fe C(6) C(7) 70.3(3) . . 0_555 yes C(5) C(6) C(7) 109.0(5) . . 0_555 yes Fe C(7) C(6) 69.2(3) . . 0_555 yes Fe C(7) C(8) 69.8(3) . . 0_555 yes C(6) C(7) C(8) 108.2(5) . . 0_555 yes Fe C(8) C(7) 69.4(3) . . 0_555 yes Fe C(8) C(9) 69.0(3) . . 0_555 yes C(7) C(8) C(9) 107.7(5) . . 0_555 yes Fe C(9) C(5) 69.0(3) . . 0_555 yes Fe C(9) C(8) 69.8(3) . . 0_555 yes C(5) C(9) C(8) 107.9(5) . . 0_555 yes Fe C(10) C(11) 71.1(3) . . 0_555 yes Fe C(10) C(14) 69.5(3) . . 0_555 yes C(11) C(10) C(14) 108.2(5) . . 0_555 yes Fe C(11) C(10) 68.9(3) . . 0_555 yes Fe C(11) C(12) 71.1(3) . . 0_555 yes C(10) C(11) C(12) 108.2(6) . . 0_555 yes Fe C(12) C(11) 69.3(3) . . 0_555 yes Fe C(12) C(13) 69.5(3) . . 0_555 yes C(11) C(12) C(13) 108.9(6) . . 0_555 yes Fe C(13) C(12) 71.1(3) . . 0_555 yes Fe C(13) C(14) 68.4(3) . . 0_555 yes C(12) C(13) C(14) 107.5(6) . . 0_555 yes Fe C(14) C(10) 69.5(3) . . 0_555 yes Fe C(14) C(13) 70.6(3) . . 0_555 yes C(10) C(14) C(13) 107.0(5) . . 0_555 yes C(16) C(15) C(17) 121.9(6) . 3_656 0_555 yes O(1) C(16) C(15) 124.6(7) . . 0_555 yes O(1) C(16) C(17) 116.8(6) . . 0_555 yes C(15) C(16) C(17) 118.6(5) . . 0_555 yes O(2) C(17) C(15) 123.9(7) . 3_656 0_555 yes O(2) C(17) C(16) 116.7(7) . . 0_555 yes C(15) C(17) C(16) 119.4(6) 3_656 . 0_555 yes #------------------------------------------------------------------------------ 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe C(5) C(3) C(2) 77.1(5) 0_555 19_1 5_555 55_5 yes Fe C(5) C(3) C(4) -103.3(5) 0_555 19_1 5_555 55_5 yes Fe C(5) C(6) C(7) 59.3(4) 0_555 19_1 5_555 55_5 yes Fe C(5) C(9) C(8) -59.1(3) 0_555 19_1 5_555 55_5 yes Fe C(6) C(5) C(3) 117.0(4) 0_555 19_1 5_555 55_5 yes Fe C(6) C(5) C(9) -59.7(3) 0_555 19_1 5_555 55_5 yes Fe C(6) C(7) C(8) 59.1(4) 0_555 19_1 5_555 55_5 yes Fe C(7) C(6) C(5) -58.7(3) 0_555 19_1 5_555 55_5 yes Fe C(7) C(8) C(9) 58.5(4) 0_555 19_1 5_555 55_5 yes Fe C(8) C(7) C(6) -58.7(4) 0_555 19_1 5_555 55_5 yes Fe C(8) C(9) C(5) 58.7(3) 0_555 19_1 5_555 55_5 yes Fe C(9) C(5) C(3) -117.3(4) 0_555 19_1 5_555 55_5 yes Fe C(9) C(5) C(6) 59.5(3) 0_555 19_1 5_555 55_5 yes Fe C(9) C(8) C(7) -58.8(4) 0_555 19_1 5_555 55_5 yes Fe C(10) C(11) C(12) -60.5(4) 0_555 19_1 5_555 55_5 yes Fe C(10) C(14) C(13) 61.0(4) 0_555 19_1 5_555 55_5 yes Fe C(11) C(10) C(14) 59.9(4) 0_555 19_1 5_555 55_5 yes Fe C(11) C(12) C(13) -58.2(4) 0_555 19_1 5_555 55_5 yes Fe C(12) C(11) C(10) 59.1(4) 0_555 19_1 5_555 55_5 yes Fe C(12) C(13) C(14) -58.9(4) 0_555 19_1 5_555 55_5 yes Fe C(13) C(12) C(11) 58.1(4) 0_555 19_1 5_555 55_5 yes Fe C(13) C(14) C(10) -60.2(4) 0_555 19_1 5_555 55_5 yes Fe C(14) C(10) C(11) -60.8(4) 0_555 19_1 5_555 55_5 yes Fe C(14) C(13) C(12) 60.6(4) 0_555 19_1 5_555 55_5 yes O(1) C(16) C(15) C(17) -175.0(8) 0_555 19_1 5_555 55_5 yes O(1) C(16) C(17) O(2) -7(1) 0_555 19_1 5_555 55_5 yes O(1) C(16) C(17) C(15) 175.2(7) 0_555 19_1 5_555 55_5 yes O(2) C(17) C(15) C(16) -173.9(8) 0_555 19_1 5_555 55_5 yes O(2) C(17) C(16) C(15) 174.2(8) 0_555 19_1 5_555 55_5 yes N(1) C(1) N(2) C(2) -0.6(9) 0_555 19_1 5_555 55_5 yes N(1) C(4) C(3) C(2) -0.6(7) 0_555 19_1 5_555 55_5 yes N(1) C(4) C(3) C(5) 179.9(4) 0_555 19_1 5_555 55_5 yes N(2) C(1) N(1) C(4) 0.9(9) 0_555 19_1 5_555 55_5 yes N(2) C(2) C(3) C(4) 0.9(8) 0_555 19_1 5_555 55_5 yes N(2) C(2) C(3) C(5) -179.6(5) 0_555 19_1 5_555 55_5 yes C(1) N(1) C(4) C(3) -0.2(7) 0_555 19_1 5_555 55_5 yes C(1) N(2) C(2) C(3) -0.3(8) 0_555 19_1 5_555 55_5 yes C(2) C(3) C(5) C(6) -10.9(7) 0_555 19_1 5_555 55_5 yes C(2) C(3) C(5) C(9) 165.2(5) 0_555 19_1 5_555 55_5 yes C(3) C(5) Fe C(6) -121.2(5) 0_555 19_1 5_555 55_5 yes C(3) C(5) Fe C(7) -158.0(4) 0_555 19_1 5_555 55_5 yes C(3) C(5) Fe C(8) 158.1(4) 0_555 19_1 5_555 55_5 yes C(3) C(5) Fe C(9) 120.3(5) 0_555 19_1 5_555 55_5 yes C(3) C(5) Fe C(10) -2.1(5) 0_555 19_1 5_555 55_5 yes C(3) C(5) Fe C(11) -42.6(5) 0_555 19_1 5_555 55_5 yes C(3) C(5) Fe C(12) -70.6(7) 0_555 19_1 5_555 55_5 yes C(3) C(5) Fe C(13) 70.6(7) 0_555 19_1 5_555 55_5 yes C(3) C(5) Fe C(14) 40.1(5) 0_555 19_1 5_555 55_5 yes C(3) C(5) C(6) C(7) 176.2(4) 0_555 19_1 5_555 55_5 yes C(3) C(5) C(9) C(8) -176.4(4) 0_555 19_1 5_555 55_5 yes C(4) C(3) C(5) C(6) 168.6(4) 0_555 19_1 5_555 55_5 yes C(4) C(3) C(5) C(9) -15.3(7) 0_555 19_1 5_555 55_5 yes C(5) Fe C(6) C(7) -120.3(5) 0_555 19_1 5_555 55_5 yes C(5) Fe C(7) C(6) 37.6(3) 0_555 19_1 5_555 55_5 yes C(5) Fe C(7) C(8) -82.1(3) 0_555 19_1 5_555 55_5 yes C(5) Fe C(8) C(7) 81.7(3) 0_555 19_1 5_555 55_5 yes C(5) Fe C(8) C(9) -37.8(3) 0_555 19_1 5_555 55_5 yes C(5) Fe C(9) C(8) 119.5(5) 0_555 19_1 5_555 55_5 yes C(5) Fe C(10) C(11) -122.0(4) 0_555 19_1 5_555 55_5 yes C(5) Fe C(10) C(14) 119.2(4) 0_555 19_1 5_555 55_5 yes C(5) Fe C(11) C(10) 75.8(5) 0_555 19_1 5_555 55_5 yes C(5) Fe C(11) C(12) -165.1(3) 0_555 19_1 5_555 55_5 yes C(5) Fe C(12) C(11) 38.0(8) 0_555 19_1 5_555 55_5 yes C(5) Fe C(12) C(13) 158.8(5) 0_555 19_1 5_555 55_5 yes C(5) Fe C(13) C(12) -159.8(5) 0_555 19_1 5_555 55_5 yes C(5) Fe C(13) C(14) -41.2(8) 0_555 19_1 5_555 55_5 yes C(5) Fe C(14) C(10) -78.8(4) 0_555 19_1 5_555 55_5 yes C(5) Fe C(14) C(13) 163.6(3) 0_555 19_1 5_555 55_5 yes C(5) C(6) Fe C(7) 120.3(5) 0_555 19_1 5_555 55_5 yes C(5) C(6) Fe C(8) 82.7(3) 0_555 19_1 5_555 55_5 yes C(5) C(6) Fe C(9) 38.3(3) 0_555 19_1 5_555 55_5 yes C(5) C(6) Fe C(10) -79.1(4) 0_555 19_1 5_555 55_5 yes C(5) C(6) Fe C(11) -120.5(3) 0_555 19_1 5_555 55_5 yes C(5) C(6) Fe C(12) -161.0(3) 0_555 19_1 5_555 55_5 yes C(5) C(6) Fe C(13) 167.8(6) 0_555 19_1 5_555 55_5 yes C(5) C(6) Fe C(14) -46.2(8) 0_555 19_1 5_555 55_5 yes C(5) C(6) C(7) C(8) 0.4(6) 0_555 19_1 5_555 55_5 yes C(5) C(9) Fe C(6) -38.4(3) 0_555 19_1 5_555 55_5 yes C(5) C(9) Fe C(7) -81.9(3) 0_555 19_1 5_555 55_5 yes C(5) C(9) Fe C(8) -119.5(5) 0_555 19_1 5_555 55_5 yes C(5) C(9) Fe C(10) 76.2(4) 0_555 19_1 5_555 55_5 yes C(5) C(9) Fe C(11) 45.2(8) 0_555 19_1 5_555 55_5 yes C(5) C(9) Fe C(12) -169.5(5) 0_555 19_1 5_555 55_5 yes C(5) C(9) Fe C(13) 160.5(3) 0_555 19_1 5_555 55_5 yes C(5) C(9) Fe C(14) 118.3(4) 0_555 19_1 5_555 55_5 yes C(5) C(9) C(8) C(7) -0.1(6) 0_555 19_1 5_555 55_5 yes C(6) Fe C(5) C(9) 118.5(4) 0_555 19_1 5_555 55_5 yes C(6) Fe C(7) C(8) -119.7(5) 0_555 19_1 5_555 55_5 yes C(6) Fe C(8) C(7) 37.3(3) 0_555 19_1 5_555 55_5 yes C(6) Fe C(8) C(9) -82.2(4) 0_555 19_1 5_555 55_5 yes C(6) Fe C(9) C(8) 81.0(4) 0_555 19_1 5_555 55_5 yes C(6) Fe C(10) C(11) -79.5(4) 0_555 19_1 5_555 55_5 yes C(6) Fe C(10) C(14) 161.8(3) 0_555 19_1 5_555 55_5 yes C(6) Fe C(11) C(10) 118.5(4) 0_555 19_1 5_555 55_5 yes C(6) Fe C(11) C(12) -122.4(4) 0_555 19_1 5_555 55_5 yes C(6) Fe C(12) C(11) 75.9(5) 0_555 19_1 5_555 55_5 yes C(6) Fe C(12) C(13) -163.3(4) 0_555 19_1 5_555 55_5 yes C(6) Fe C(13) C(12) 42.6(8) 0_555 19_1 5_555 55_5 yes C(6) Fe C(13) C(14) 161.1(6) 0_555 19_1 5_555 55_5 yes C(6) Fe C(14) C(10) -44.8(8) 0_555 19_1 5_555 55_5 yes C(6) Fe C(14) C(13) -162.4(5) 0_555 19_1 5_555 55_5 yes C(6) C(5) Fe C(7) -36.8(3) 0_555 19_1 5_555 55_5 yes C(6) C(5) Fe C(8) -80.6(3) 0_555 19_1 5_555 55_5 yes C(6) C(5) Fe C(9) -118.5(4) 0_555 19_1 5_555 55_5 yes C(6) C(5) Fe C(10) 119.1(4) 0_555 19_1 5_555 55_5 yes C(6) C(5) Fe C(11) 78.6(4) 0_555 19_1 5_555 55_5 yes C(6) C(5) Fe C(12) 50.6(7) 0_555 19_1 5_555 55_5 yes C(6) C(5) Fe C(13) -168.2(6) 0_555 19_1 5_555 55_5 yes C(6) C(5) Fe C(14) 161.3(4) 0_555 19_1 5_555 55_5 yes C(6) C(5) C(9) C(8) 0.3(5) 0_555 19_1 5_555 55_5 yes C(6) C(7) Fe C(8) 119.7(5) 0_555 19_1 5_555 55_5 yes C(6) C(7) Fe C(9) 81.8(4) 0_555 19_1 5_555 55_5 yes C(6) C(7) Fe C(10) -46.0(7) 0_555 19_1 5_555 55_5 yes C(6) C(7) Fe C(11) -79.2(4) 0_555 19_1 5_555 55_5 yes C(6) C(7) Fe C(12) -120.8(4) 0_555 19_1 5_555 55_5 yes C(6) C(7) Fe C(13) -161.7(3) 0_555 19_1 5_555 55_5 yes C(6) C(7) Fe C(14) 164.6(6) 0_555 19_1 5_555 55_5 yes C(6) C(7) C(8) C(9) -0.2(6) 0_555 19_1 5_555 55_5 yes C(7) Fe C(5) C(9) 81.6(3) 0_555 19_1 5_555 55_5 yes C(7) Fe C(8) C(9) -119.5(5) 0_555 19_1 5_555 55_5 yes C(7) Fe C(9) C(8) 37.6(4) 0_555 19_1 5_555 55_5 yes C(7) Fe C(10) C(11) -46.3(7) 0_555 19_1 5_555 55_5 yes C(7) Fe C(10) C(14) -165.0(5) 0_555 19_1 5_555 55_5 yes C(7) Fe C(11) C(10) 160.4(4) 0_555 19_1 5_555 55_5 yes C(7) Fe C(11) C(12) -80.4(4) 0_555 19_1 5_555 55_5 yes C(7) Fe C(12) C(11) 118.1(4) 0_555 19_1 5_555 55_5 yes C(7) Fe C(12) C(13) -121.1(4) 0_555 19_1 5_555 55_5 yes C(7) Fe C(13) C(12) 77.8(4) 0_555 19_1 5_555 55_5 yes C(7) Fe C(13) C(14) -163.7(4) 0_555 19_1 5_555 55_5 yes C(7) Fe C(14) C(10) 162.2(6) 0_555 19_1 5_555 55_5 yes C(7) Fe C(14) C(13) 44.6(8) 0_555 19_1 5_555 55_5 yes C(7) C(6) Fe C(8) -37.6(3) 0_555 19_1 5_555 55_5 yes C(7) C(6) Fe C(9) -82.0(4) 0_555 19_1 5_555 55_5 yes C(7) C(6) Fe C(10) 160.6(4) 0_555 19_1 5_555 55_5 yes C(7) C(6) Fe C(11) 119.2(4) 0_555 19_1 5_555 55_5 yes C(7) C(6) Fe C(12) 78.7(4) 0_555 19_1 5_555 55_5 yes C(7) C(6) Fe C(13) 47.5(8) 0_555 19_1 5_555 55_5 yes C(7) C(6) Fe C(14) -166.5(6) 0_555 19_1 5_555 55_5 yes C(7) C(6) C(5) C(9) -0.5(6) 0_555 19_1 5_555 55_5 yes C(7) C(8) Fe C(9) 119.5(5) 0_555 19_1 5_555 55_5 yes C(7) C(8) Fe C(10) 162.8(7) 0_555 19_1 5_555 55_5 yes C(7) C(8) Fe C(11) -46.6(8) 0_555 19_1 5_555 55_5 yes C(7) C(8) Fe C(12) -80.0(4) 0_555 19_1 5_555 55_5 yes C(7) C(8) Fe C(13) -121.0(3) 0_555 19_1 5_555 55_5 yes C(7) C(8) Fe C(14) -163.5(3) 0_555 19_1 5_555 55_5 yes C(8) Fe C(5) C(9) 37.8(3) 0_555 19_1 5_555 55_5 yes C(8) Fe C(10) C(11) 163.2(7) 0_555 19_1 5_555 55_5 yes C(8) Fe C(10) C(14) 44.4(9) 0_555 19_1 5_555 55_5 yes C(8) Fe C(11) C(10) -165.5(6) 0_555 19_1 5_555 55_5 yes C(8) Fe C(11) C(12) -46.4(9) 0_555 19_1 5_555 55_5 yes C(8) Fe C(12) C(11) 160.9(4) 0_555 19_1 5_555 55_5 yes C(8) Fe C(12) C(13) -78.3(4) 0_555 19_1 5_555 55_5 yes C(8) Fe C(13) C(12) 120.2(4) 0_555 19_1 5_555 55_5 yes C(8) Fe C(13) C(14) -121.2(4) 0_555 19_1 5_555 55_5 yes C(8) Fe C(14) C(10) -163.9(3) 0_555 19_1 5_555 55_5 yes C(8) Fe C(14) C(13) 78.4(4) 0_555 19_1 5_555 55_5 yes C(8) C(7) Fe C(9) -37.9(3) 0_555 19_1 5_555 55_5 yes C(8) C(7) Fe C(10) -165.7(5) 0_555 19_1 5_555 55_5 yes C(8) C(7) Fe C(11) 161.1(3) 0_555 19_1 5_555 55_5 yes C(8) C(7) Fe C(12) 119.5(3) 0_555 19_1 5_555 55_5 yes C(8) C(7) Fe C(13) 78.6(4) 0_555 19_1 5_555 55_5 yes C(8) C(7) Fe C(14) 44.9(8) 0_555 19_1 5_555 55_5 yes C(8) C(9) Fe C(10) -164.3(4) 0_555 19_1 5_555 55_5 yes C(8) C(9) Fe C(11) 164.7(7) 0_555 19_1 5_555 55_5 yes C(8) C(9) Fe C(12) -50.1(8) 0_555 19_1 5_555 55_5 yes C(8) C(9) Fe C(13) -80.0(4) 0_555 19_1 5_555 55_5 yes C(8) C(9) Fe C(14) -122.2(4) 0_555 19_1 5_555 55_5 yes C(9) Fe C(10) C(11) -163.9(3) 0_555 19_1 5_555 55_5 yes C(9) Fe C(10) C(14) 77.3(4) 0_555 19_1 5_555 55_5 yes C(9) Fe C(11) C(10) 41.9(9) 0_555 19_1 5_555 55_5 yes C(9) Fe C(11) C(12) 161.0(6) 0_555 19_1 5_555 55_5 yes C(9) Fe C(12) C(11) -162.0(6) 0_555 19_1 5_555 55_5 yes C(9) Fe C(12) C(13) -41.2(8) 0_555 19_1 5_555 55_5 yes C(9) Fe C(13) C(12) 163.4(3) 0_555 19_1 5_555 55_5 yes C(9) Fe C(13) C(14) -78.1(5) 0_555 19_1 5_555 55_5 yes C(9) Fe C(14) C(10) -121.6(4) 0_555 19_1 5_555 55_5 yes C(9) Fe C(14) C(13) 120.7(4) 0_555 19_1 5_555 55_5 yes C(9) C(5) Fe C(10) -122.4(4) 0_555 19_1 5_555 55_5 yes C(9) C(5) Fe C(11) -163.0(4) 0_555 19_1 5_555 55_5 yes C(9) C(5) Fe C(12) 169.1(6) 0_555 19_1 5_555 55_5 yes C(9) C(5) Fe C(13) -49.8(7) 0_555 19_1 5_555 55_5 yes C(9) C(5) Fe C(14) -80.2(4) 0_555 19_1 5_555 55_5 yes C(9) C(8) Fe C(10) 43.4(9) 0_555 19_1 5_555 55_5 yes C(9) C(8) Fe C(11) -166.0(6) 0_555 19_1 5_555 55_5 yes C(9) C(8) Fe C(12) 160.5(3) 0_555 19_1 5_555 55_5 yes C(9) C(8) Fe C(13) 119.6(4) 0_555 19_1 5_555 55_5 yes C(9) C(8) Fe C(14) 77.0(4) 0_555 19_1 5_555 55_5 yes C(10) Fe C(11) C(12) 119.1(6) 0_555 19_1 5_555 55_5 yes C(10) Fe C(12) C(11) -37.6(4) 0_555 19_1 5_555 55_5 yes C(10) Fe C(12) C(13) 83.2(4) 0_555 19_1 5_555 55_5 yes C(10) Fe C(13) C(12) -79.8(4) 0_555 19_1 5_555 55_5 yes C(10) Fe C(13) C(14) 38.7(4) 0_555 19_1 5_555 55_5 yes C(10) Fe C(14) C(13) -117.6(5) 0_555 19_1 5_555 55_5 yes C(10) C(11) Fe C(12) -119.1(6) 0_555 19_1 5_555 55_5 yes C(10) C(11) Fe C(13) -82.9(4) 0_555 19_1 5_555 55_5 yes C(10) C(11) Fe C(14) -38.4(4) 0_555 19_1 5_555 55_5 yes C(10) C(11) C(12) C(13) 0.9(6) 0_555 19_1 5_555 55_5 yes C(10) C(14) Fe C(11) 37.4(4) 0_555 19_1 5_555 55_5 yes C(10) C(14) Fe C(12) 80.4(4) 0_555 19_1 5_555 55_5 yes C(10) C(14) Fe C(13) 117.6(5) 0_555 19_1 5_555 55_5 yes C(10) C(14) C(13) C(12) 0.4(6) 0_555 19_1 5_555 55_5 yes C(11) Fe C(10) C(14) -118.8(5) 0_555 19_1 5_555 55_5 yes C(11) Fe C(12) C(13) 120.8(6) 0_555 19_1 5_555 55_5 yes C(11) Fe C(13) C(12) -36.5(4) 0_555 19_1 5_555 55_5 yes C(11) Fe C(13) C(14) 82.1(4) 0_555 19_1 5_555 55_5 yes C(11) Fe C(14) C(13) -80.2(4) 0_555 19_1 5_555 55_5 yes C(11) C(10) Fe C(12) 37.3(4) 0_555 19_1 5_555 55_5 yes C(11) C(10) Fe C(13) 80.0(4) 0_555 19_1 5_555 55_5 yes C(11) C(10) Fe C(14) 118.8(5) 0_555 19_1 5_555 55_5 yes C(11) C(10) C(14) C(13) 0.1(7) 0_555 19_1 5_555 55_5 yes C(11) C(12) Fe C(13) -120.8(6) 0_555 19_1 5_555 55_5 yes C(11) C(12) Fe C(14) -82.2(5) 0_555 19_1 5_555 55_5 yes C(11) C(12) C(13) C(14) -0.8(6) 0_555 19_1 5_555 55_5 yes C(12) Fe C(10) C(14) -81.5(4) 0_555 19_1 5_555 55_5 yes C(12) Fe C(13) C(14) 118.6(6) 0_555 19_1 5_555 55_5 yes C(12) Fe C(14) C(13) -37.2(3) 0_555 19_1 5_555 55_5 yes C(12) C(11) Fe C(13) 36.3(4) 0_555 19_1 5_555 55_5 yes C(12) C(11) Fe C(14) 80.8(4) 0_555 19_1 5_555 55_5 yes C(12) C(11) C(10) C(14) -0.6(7) 0_555 19_1 5_555 55_5 yes C(12) C(13) Fe C(14) -118.6(6) 0_555 19_1 5_555 55_5 yes C(13) Fe C(10) C(14) -38.7(4) 0_555 19_1 5_555 55_5 yes C(13) C(12) Fe C(14) 38.6(4) 0_555 19_1 5_555 55_5 yes C(13) C(12) Fe C(14) 38.6(4) 0_555 19_1 5_555 55_5 yes #------------------------------------------------------------------------------ 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(1) 2.793(8) . 2_555 ? O(1) O(1) 2.92(2) . 3_666 ? O(1) C(13) 3.180(9) . 3_666 ? O(1) C(12) 3.228(10) . 3_666 ? O(1) C(1) 3.415(10) . 2_555 ? O(2) N(1) 2.882(8) . 2_555 ? O(2) C(4) 3.331(8) . 2_555 ? O(2) C(10) 3.40(1) . 2_545 ? N(1) C(2) 3.455(7) . 3_655 ? N(1) C(3) 3.555(6) . 3_655 ? N(2) C(4) 3.461(7) . 3_655 ? N(2) C(3) 3.577(7) . 3_655 ? C(1) C(3) 3.434(7) . 3_655 ? C(1) C(5) 3.472(7) . 3_655 ? C(1) C(15) 3.501(9) . 4_454 ? C(2) C(4) 3.390(7) . 3_655 ? #------------------------------------------------------------------------------ loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_site_distance_DH _geom_hbond_site_distance_HA _geom_hbond_site_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O(1) H(14) O(2) . . . 0.950 2.147 2.48(1) 99.161 no O(1) H(14) N(1) . . 2_555 0.950 1.854 2.793(8) 168.952 no #------------------------------------------------------------------------------ #-----------END #------------------------------------------------------------------------------ data_compound_4 _database_code_CSD 206164 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C32 H30 Fe2 N4 O4 S ' _chemical_formula_moiety ? _chemical_formula_weight 678.37 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _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 _cell_length_a 7.406(3) _cell_length_b 19.131(7) _cell_length_c 20.727(3) _cell_angle_alpha 90 _cell_angle_beta 92.42(3) _cell_angle_gamma 90 _cell_volume 2933(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.7 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.2 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.104 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.776 _exptl_absorpt_correction_T_max 0.999 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 7461 _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9984 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9984 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% 0.29 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6729 _reflns_number_gt 4327 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1287 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4327 _refine_ls_number_parameters 388 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.10000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0003 _refine_diff_density_max 0.28 _refine_diff_density_min -0.33 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S S 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Fe Fe 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe(1) Fe 0.23455(7) 0.78693(3) 0.08693(2) 0.0305(1) Uani 1.00 d . . . Fe(2) Fe 0.22708(6) 0.28611(3) 0.16411(2) 0.0287(1) Uani 1.00 d . . . S S 0.2215(2) -0.00165(6) 0.23772(6) 0.0488(3) Uani 1.00 d . . . O(1) O 0.3640(5) -0.0166(2) 0.3865(1) 0.0566(10) Uani 1.00 d . . . O(2) O 0.3180(6) 0.0975(2) 0.3796(2) 0.074(1) Uani 1.00 d . . . O(3) O -0.2039(5) 0.0951(2) 0.1731(2) 0.067(1) Uani 1.00 d . . . O(4) O -0.1528(6) -0.0146(2) 0.1970(3) 0.099(2) Uani 1.00 d . . . N(1) N 0.2532(5) 0.5021(2) 0.0080(2) 0.049(1) Uani 1.00 d . . . N(2) N 0.1710(6) 0.5405(2) 0.1120(2) 0.058(1) Uani 1.00 d . . . N(3) N 0.5116(5) 1.0423(2) 0.1040(2) 0.0446(10) Uani 1.00 d . . . N(4) N 0.2271(5) 1.0486(2) 0.0474(2) 0.056(1) Uani 1.00 d . . . C(1) C 0.2321(7) 0.5509(2) 0.0534(3) 0.057(1) Uani 1.00 d . . . C(2) C 0.1258(7) 0.4748(2) 0.1257(2) 0.050(1) Uani 1.00 d . . . C(3) C 0.1406(5) 0.4197(2) 0.0827(2) 0.0348(10) Uani 1.00 d . . . C(4) C 0.2062(6) 0.4367(2) 0.0229(2) 0.043(1) Uani 1.00 d . . . C(5) C 0.0893(5) 0.3482(2) 0.0994(2) 0.0329(9) Uani 1.00 d . . . C(6) C 0.1431(5) 0.2844(2) 0.0692(2) 0.039(1) Uani 1.00 d . . . C(7) C 0.0663(5) 0.2278(2) 0.1018(2) 0.041(1) Uani 1.00 d . . . C(8) C -0.0361(5) 0.2547(2) 0.1526(2) 0.042(1) Uani 1.00 d . . . C(9) C -0.0246(5) 0.3288(2) 0.1512(2) 0.040(1) Uani 1.00 d . . . C(10) C 0.4517(7) 0.3399(3) 0.1930(3) 0.061(1) Uani 1.00 d . . . C(11) C 0.4997(5) 0.2737(3) 0.1699(2) 0.060(1) Uani 1.00 d . . . C(12) C 0.4192(6) 0.2230(2) 0.2079(2) 0.048(1) Uani 1.00 d . . . C(13) C 0.3202(6) 0.2572(3) 0.2547(2) 0.048(1) Uani 1.00 d . . . C(14) C 0.3393(7) 0.3302(3) 0.2455(2) 0.057(1) Uani 1.00 d . . . C(15) C 0.3680(6) 1.0766(2) 0.0792(2) 0.049(1) Uani 1.00 d . . . C(16) C 0.2341(6) 0.9797(2) 0.0385(2) 0.048(1) Uani 1.00 d . . . C(17) C 0.3782(5) 0.9378(2) 0.0598(2) 0.0334(9) Uani 1.00 d . . . C(18) C 0.5152(5) 0.9735(2) 0.0941(2) 0.040(1) Uani 1.00 d . . . C(19) C 0.3874(5) 0.8628(2) 0.0471(2) 0.0339(9) Uani 1.00 d . . . C(20) C 0.2869(5) 0.8249(2) -0.0016(2) 0.039(1) Uani 1.00 d . . . C(21) C 0.3374(6) 0.7540(2) 0.0029(2) 0.044(1) Uani 1.00 d . . . C(22) C 0.4680(5) 0.7470(2) 0.0538(2) 0.044(1) Uani 1.00 d . . . C(23) C 0.5007(5) 0.8134(2) 0.0815(2) 0.037(1) Uani 1.00 d . . . C(24) C 0.0569(7) 0.8350(3) 0.1446(3) 0.057(1) Uani 1.00 d . . . C(25) C -0.0356(6) 0.7919(3) 0.0991(3) 0.066(2) Uani 1.00 d . . . C(26) C 0.0221(7) 0.7240(3) 0.1079(3) 0.063(2) Uani 1.00 d . . . C(27) C 0.1513(8) 0.7232(3) 0.1583(3) 0.064(2) Uani 1.00 d . . . C(28) C 0.1749(7) 0.7916(3) 0.1814(2) 0.062(2) Uani 1.00 d . . . C(29) C 0.3586(6) 0.0432(2) 0.3555(2) 0.043(1) Uani 1.00 d . . . C(30) C 0.4046(6) 0.0369(3) 0.2860(2) 0.049(1) Uani 1.00 d . . . C(31) C 0.0612(6) 0.0693(2) 0.2356(2) 0.049(1) Uani 1.00 d . . . C(32) C -0.1078(6) 0.0452(2) 0.1993(2) 0.047(1) Uani 1.00 d . . . H(1) H 0.2641 0.5975 0.0427 0.0685 Uiso 1.00 calc . . . H(2) H 0.0811 0.4652 0.1672 0.0606 Uiso 1.00 calc . . . H(3) H 0.2181 0.4009 -0.0084 0.0512 Uiso 1.00 calc . . . H(4) H 0.2194 0.2809 0.0335 0.0471 Uiso 1.00 calc . . . H(5) H 0.0828 0.1797 0.0922 0.0489 Uiso 1.00 calc . . . H(6) H -0.1006 0.2278 0.1826 0.0505 Uiso 1.00 calc . . . H(7) H -0.0802 0.3601 0.1799 0.0478 Uiso 1.00 calc . . . H(8) H 0.4890 0.3836 0.1763 0.0733 Uiso 1.00 calc . . . H(9) H 0.5746 0.2648 0.1347 0.0716 Uiso 1.00 calc . . . H(10) H 0.4288 0.1738 0.2026 0.0582 Uiso 1.00 calc . . . H(11) H 0.2512 0.2353 0.2867 0.0578 Uiso 1.00 calc . . . H(12) H 0.2872 0.3660 0.2705 0.0688 Uiso 1.00 calc . . . H(13) H 0.3665 1.1259 0.0852 0.0588 Uiso 1.00 calc . . . H(14) H 0.1345 0.9578 0.0162 0.0579 Uiso 1.00 calc . . . H(15) H 0.6158 0.9476 0.1112 0.0482 Uiso 1.00 calc . . . H(16) H 0.2004 0.8441 -0.0319 0.0473 Uiso 1.00 calc . . . H(17) H 0.2906 0.7171 -0.0236 0.0529 Uiso 1.00 calc . . . H(18) H 0.5236 0.7045 0.0676 0.0535 Uiso 1.00 calc . . . H(19) H 0.5822 0.8235 0.1170 0.0445 Uiso 1.00 calc . . . H(20) H 0.0416 0.8840 0.1498 0.0682 Uiso 1.00 calc . . . H(21) H -0.1237 0.8073 0.0675 0.0791 Uiso 1.00 calc . . . H(22) H -0.0189 0.6846 0.0835 0.0757 Uiso 1.00 calc . . . H(23) H 0.2136 0.6829 0.1743 0.0771 Uiso 1.00 calc . . . H(24) H 0.2544 0.8059 0.2161 0.0744 Uiso 1.00 calc . . . H(25) H 0.3370 -0.0183 0.4308 0.0680 Uiso 1.00 calc . . . H(26) H 0.5091 0.0083 0.2831 0.0595 Uiso 1.00 calc . . . H(27) H 0.4294 0.0821 0.2696 0.0595 Uiso 1.00 calc . . . H(28) H 0.1106 0.1085 0.2143 0.0585 Uiso 1.00 calc . . . H(29) H 0.0334 0.0821 0.2783 0.0585 Uiso 1.00 calc . . . H(30) H -0.3127 0.0847 0.1493 0.0805 Uiso 1.00 calc . . . 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) 0.0226(2) 0.0354(3) 0.0337(3) -0.0026(2) 0.0034(2) -0.0026(2) Fe(2) 0.0224(2) 0.0315(3) 0.0321(3) -0.0018(2) -0.0003(2) -0.0005(2) S 0.0491(6) 0.0520(7) 0.0451(6) 0.0066(5) 0.0006(5) -0.0053(5) O(1) 0.084(2) 0.040(2) 0.047(2) 0.015(2) 0.012(2) 0.000(1) O(2) 0.100(3) 0.043(2) 0.078(2) 0.011(2) 0.004(2) -0.010(2) O(3) 0.055(2) 0.037(2) 0.107(3) -0.009(2) -0.033(2) 0.007(2) O(4) 0.085(3) 0.039(2) 0.167(5) -0.016(2) -0.061(3) 0.009(2) N(1) 0.052(2) 0.050(2) 0.046(2) -0.006(2) -0.001(2) 0.014(2) N(2) 0.070(3) 0.036(2) 0.069(3) -0.001(2) 0.009(2) 0.002(2) N(3) 0.041(2) 0.040(2) 0.053(2) -0.010(2) 0.003(2) -0.004(2) N(4) 0.045(2) 0.045(2) 0.076(3) 0.003(2) -0.010(2) -0.006(2) C(1) 0.058(3) 0.043(3) 0.068(3) -0.004(2) -0.007(2) 0.016(2) C(2) 0.058(3) 0.042(2) 0.052(3) -0.001(2) 0.012(2) 0.000(2) C(3) 0.030(2) 0.039(2) 0.035(2) -0.001(2) -0.005(1) 0.006(2) C(4) 0.047(2) 0.042(2) 0.039(2) -0.001(2) -0.003(2) 0.005(2) C(5) 0.027(2) 0.035(2) 0.036(2) 0.001(2) -0.004(1) 0.002(2) C(6) 0.035(2) 0.045(2) 0.037(2) 0.003(2) -0.007(2) -0.007(2) C(7) 0.036(2) 0.033(2) 0.052(2) -0.002(2) -0.010(2) -0.008(2) C(8) 0.022(2) 0.043(2) 0.060(3) -0.005(2) -0.002(2) 0.006(2) C(9) 0.025(2) 0.040(2) 0.054(2) 0.003(2) 0.003(2) 0.001(2) C(10) 0.051(3) 0.057(3) 0.073(3) -0.029(2) -0.031(2) 0.020(3) C(11) 0.020(2) 0.105(4) 0.054(3) -0.001(2) -0.002(2) 0.006(3) C(12) 0.046(2) 0.043(3) 0.055(3) 0.008(2) -0.012(2) 0.002(2) C(13) 0.043(2) 0.065(3) 0.036(2) -0.002(2) -0.003(2) 0.009(2) C(14) 0.064(3) 0.055(3) 0.051(3) 0.008(2) -0.023(2) -0.016(2) C(15) 0.048(2) 0.036(2) 0.063(3) 0.001(2) 0.006(2) -0.005(2) C(16) 0.035(2) 0.040(2) 0.069(3) 0.001(2) -0.009(2) -0.004(2) C(17) 0.027(2) 0.036(2) 0.037(2) -0.006(2) 0.000(1) -0.002(2) C(18) 0.029(2) 0.042(2) 0.049(2) -0.003(2) -0.002(2) 0.000(2) C(19) 0.024(2) 0.045(2) 0.033(2) -0.005(2) 0.001(1) -0.001(2) C(20) 0.038(2) 0.045(2) 0.036(2) -0.006(2) -0.001(2) -0.001(2) C(21) 0.051(2) 0.043(2) 0.039(2) -0.004(2) 0.014(2) -0.010(2) C(22) 0.035(2) 0.049(3) 0.050(2) 0.005(2) 0.014(2) 0.001(2) C(23) 0.021(2) 0.046(2) 0.044(2) 0.000(2) 0.002(2) 0.003(2) C(24) 0.050(3) 0.053(3) 0.070(3) 0.000(2) 0.029(2) -0.016(2) C(25) 0.023(2) 0.108(5) 0.067(3) 0.000(2) 0.011(2) -0.013(3) C(26) 0.055(3) 0.061(3) 0.075(3) -0.029(3) 0.027(3) -0.018(3) C(27) 0.068(3) 0.063(3) 0.065(3) -0.001(3) 0.030(3) 0.019(3) C(28) 0.048(3) 0.101(4) 0.039(2) -0.020(3) 0.013(2) -0.009(2) C(29) 0.039(2) 0.044(2) 0.047(2) 0.002(2) -0.003(2) -0.004(2) C(30) 0.036(2) 0.063(3) 0.049(3) -0.003(2) 0.002(2) 0.011(2) C(31) 0.045(2) 0.041(2) 0.059(3) -0.005(2) -0.006(2) 0.002(2) C(32) 0.044(2) 0.036(2) 0.060(3) -0.006(2) -0.005(2) 0.002(2) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS97 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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(19) 2.036(4) . . yes Fe(1) C(20) 2.026(4) . . yes Fe(1) C(21) 2.030(4) . . yes Fe(1) C(22) 2.036(4) . . yes Fe(1) C(23) 2.043(4) . . yes Fe(1) C(24) 2.035(4) . . yes Fe(1) C(25) 2.029(4) . . yes Fe(1) C(26) 2.043(4) . . yes Fe(1) C(27) 2.034(4) . . yes Fe(1) C(28) 2.027(4) . . yes Fe(2) C(5) 2.034(4) . . yes Fe(2) C(6) 2.039(4) . . yes Fe(2) C(7) 2.049(4) . . yes Fe(2) C(8) 2.044(4) . . yes Fe(2) C(9) 2.042(4) . . yes Fe(2) C(10) 2.025(4) . . yes Fe(2) C(11) 2.032(4) . . yes Fe(2) C(12) 2.049(4) . . yes Fe(2) C(13) 2.048(4) . . yes Fe(2) C(14) 2.032(4) . . yes S C(30) 1.808(5) . . yes S C(31) 1.802(5) . . yes O(1) C(29) 1.312(5) . . yes O(2) C(29) 1.198(5) . . yes O(3) C(32) 1.296(5) . . yes O(4) C(32) 1.192(5) . . yes N(1) C(1) 1.340(7) . . yes N(1) C(4) 1.337(5) . . yes N(2) C(1) 1.330(6) . . yes N(2) C(2) 1.333(6) . . yes N(3) C(15) 1.334(6) . . yes N(3) C(18) 1.332(5) . . yes N(4) C(15) 1.324(6) . . yes N(4) C(16) 1.333(6) . . yes C(2) C(3) 1.389(6) . . yes C(3) C(4) 1.389(5) . . yes C(3) C(5) 1.464(5) . . yes C(5) C(6) 1.436(5) . . yes C(5) C(9) 1.442(5) . . yes C(6) C(7) 1.409(6) . . yes C(7) C(8) 1.420(6) . . yes C(8) C(9) 1.420(6) . . yes C(10) C(11) 1.406(8) . . yes C(10) C(14) 1.410(8) . . yes C(11) C(12) 1.398(7) . . yes C(12) C(13) 1.402(6) . . yes C(13) C(14) 1.417(7) . . yes C(16) C(17) 1.391(6) . . yes C(17) C(18) 1.394(5) . . yes C(17) C(19) 1.460(5) . . yes C(19) C(20) 1.427(5) . . yes C(19) C(23) 1.434(5) . . yes C(20) C(21) 1.409(6) . . yes C(21) C(22) 1.407(6) . . yes C(22) C(23) 1.411(6) . . yes C(24) C(25) 1.409(7) . . yes C(24) C(28) 1.406(7) . . yes C(25) C(26) 1.378(7) . . yes C(26) C(27) 1.386(8) . . yes C(27) C(28) 1.403(7) . . yes C(29) C(30) 1.499(6) . . yes C(31) C(32) 1.506(6) . . 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 C(19) Fe(1) C(20) 41.1(1) . . 0_555 yes C(19) Fe(1) C(21) 68.8(2) . . 0_555 yes C(19) Fe(1) C(22) 68.7(2) . . 0_555 yes C(19) Fe(1) C(23) 41.1(1) . . 0_555 yes C(19) Fe(1) C(24) 107.5(2) . . 0_555 yes C(19) Fe(1) C(25) 125.7(2) . . 0_555 yes C(19) Fe(1) C(26) 162.3(2) . . 0_555 yes C(19) Fe(1) C(27) 155.9(2) . . 0_555 yes C(19) Fe(1) C(28) 120.4(2) . . 0_555 yes C(20) Fe(1) C(21) 40.7(2) . . 0_555 yes C(20) Fe(1) C(22) 68.4(2) . . 0_555 yes C(20) Fe(1) C(23) 68.9(2) . . 0_555 yes C(20) Fe(1) C(24) 121.6(2) . . 0_555 yes C(20) Fe(1) C(25) 108.8(2) . . 0_555 yes C(20) Fe(1) C(26) 125.7(2) . . 0_555 yes C(20) Fe(1) C(27) 161.7(2) . . 0_555 yes C(20) Fe(1) C(28) 156.4(2) . . 0_555 yes C(21) Fe(1) C(22) 40.5(2) . . 0_555 yes C(21) Fe(1) C(23) 68.4(2) . . 0_555 yes C(21) Fe(1) C(24) 156.9(2) . . 0_555 yes C(21) Fe(1) C(25) 121.9(2) . . 0_555 yes C(21) Fe(1) C(26) 108.7(2) . . 0_555 yes C(21) Fe(1) C(27) 125.0(2) . . 0_555 yes C(21) Fe(1) C(28) 161.3(2) . . 0_555 yes C(22) Fe(1) C(23) 40.5(2) . . 0_555 yes C(22) Fe(1) C(24) 161.3(2) . . 0_555 yes C(22) Fe(1) C(25) 156.3(2) . . 0_555 yes C(22) Fe(1) C(26) 121.6(2) . . 0_555 yes C(22) Fe(1) C(27) 108.0(2) . . 0_555 yes C(22) Fe(1) C(28) 124.4(2) . . 0_555 yes C(23) Fe(1) C(24) 124.7(2) . . 0_555 yes C(23) Fe(1) C(25) 162.5(2) . . 0_555 yes C(23) Fe(1) C(26) 155.7(2) . . 0_555 yes C(23) Fe(1) C(27) 120.8(2) . . 0_555 yes C(23) Fe(1) C(28) 107.0(2) . . 0_555 yes C(24) Fe(1) C(25) 40.6(2) . . 0_555 yes C(24) Fe(1) C(26) 67.6(2) . . 0_555 yes C(24) Fe(1) C(27) 67.7(2) . . 0_555 yes C(24) Fe(1) C(28) 40.5(2) . . 0_555 yes C(25) Fe(1) C(26) 39.6(2) . . 0_555 yes C(25) Fe(1) C(27) 66.9(2) . . 0_555 yes C(25) Fe(1) C(28) 67.8(2) . . 0_555 yes C(26) Fe(1) C(27) 39.8(2) . . 0_555 yes C(26) Fe(1) C(28) 67.6(2) . . 0_555 yes C(27) Fe(1) C(28) 40.4(2) . . 0_555 yes C(5) Fe(2) C(6) 41.3(1) . . 0_555 yes C(5) Fe(2) C(7) 68.9(2) . . 0_555 yes C(5) Fe(2) C(8) 69.2(2) . . 0_555 yes C(5) Fe(2) C(9) 41.4(2) . . 0_555 yes C(5) Fe(2) C(10) 106.3(2) . . 0_555 yes C(5) Fe(2) C(11) 125.3(2) . . 0_555 yes C(5) Fe(2) C(12) 163.0(2) . . 0_555 yes C(5) Fe(2) C(13) 154.5(2) . . 0_555 yes C(5) Fe(2) C(14) 118.8(2) . . 0_555 yes C(6) Fe(2) C(7) 40.3(2) . . 0_555 yes C(6) Fe(2) C(8) 68.4(2) . . 0_555 yes C(6) Fe(2) C(9) 68.9(2) . . 0_555 yes C(6) Fe(2) C(10) 120.4(2) . . 0_555 yes C(6) Fe(2) C(11) 108.5(2) . . 0_555 yes C(6) Fe(2) C(12) 126.6(2) . . 0_555 yes C(6) Fe(2) C(13) 163.2(2) . . 0_555 yes C(6) Fe(2) C(14) 154.9(2) . . 0_555 yes C(7) Fe(2) C(8) 40.6(2) . . 0_555 yes C(7) Fe(2) C(9) 68.4(2) . . 0_555 yes C(7) Fe(2) C(10) 155.7(2) . . 0_555 yes C(7) Fe(2) C(11) 121.5(2) . . 0_555 yes C(7) Fe(2) C(12) 109.4(2) . . 0_555 yes C(7) Fe(2) C(13) 126.5(2) . . 0_555 yes C(7) Fe(2) C(14) 162.8(2) . . 0_555 yes C(8) Fe(2) C(9) 40.7(2) . . 0_555 yes C(8) Fe(2) C(10) 162.0(2) . . 0_555 yes C(8) Fe(2) C(11) 155.9(2) . . 0_555 yes C(8) Fe(2) C(12) 121.3(2) . . 0_555 yes C(8) Fe(2) C(13) 108.0(2) . . 0_555 yes C(8) Fe(2) C(14) 125.0(2) . . 0_555 yes C(9) Fe(2) C(10) 124.7(2) . . 0_555 yes C(9) Fe(2) C(11) 162.6(2) . . 0_555 yes C(9) Fe(2) C(12) 155.0(2) . . 0_555 yes C(9) Fe(2) C(13) 119.9(2) . . 0_555 yes C(9) Fe(2) C(14) 106.4(2) . . 0_555 yes C(10) Fe(2) C(11) 40.6(2) . . 0_555 yes C(10) Fe(2) C(12) 67.8(2) . . 0_555 yes C(10) Fe(2) C(13) 68.0(2) . . 0_555 yes C(10) Fe(2) C(14) 40.7(2) . . 0_555 yes C(11) Fe(2) C(12) 40.1(2) . . 0_555 yes C(11) Fe(2) C(13) 67.6(2) . . 0_555 yes C(11) Fe(2) C(14) 68.2(2) . . 0_555 yes C(12) Fe(2) C(13) 40.0(2) . . 0_555 yes C(12) Fe(2) C(14) 67.9(2) . . 0_555 yes C(13) Fe(2) C(14) 40.6(2) . . 0_555 yes C(30) S C(31) 100.6(2) . . 0_555 yes C(1) N(1) C(4) 116.9(4) . . 0_555 yes C(1) N(2) C(2) 115.7(4) . . 0_555 yes C(15) N(3) C(18) 116.6(4) . . 0_555 yes C(15) N(4) C(16) 115.8(4) . . 0_555 yes N(1) C(1) N(2) 126.2(4) . . 0_555 yes N(2) C(2) C(3) 123.5(4) . . 0_555 yes C(2) C(3) C(4) 115.7(4) . . 0_555 yes C(2) C(3) C(5) 122.0(4) . . 0_555 yes C(4) C(3) C(5) 122.3(4) . . 0_555 yes N(1) C(4) C(3) 122.0(4) . . 0_555 yes Fe(2) C(5) C(3) 125.0(3) . . 0_555 yes Fe(2) C(5) C(6) 69.5(2) . . 0_555 yes Fe(2) C(5) C(9) 69.6(2) . . 0_555 yes C(3) C(5) C(6) 127.7(3) . . 0_555 yes C(3) C(5) C(9) 125.6(3) . . 0_555 yes C(6) C(5) C(9) 106.7(3) . . 0_555 yes Fe(2) C(6) C(5) 69.2(2) . . 0_555 yes Fe(2) C(6) C(7) 70.2(2) . . 0_555 yes C(5) C(6) C(7) 108.6(3) . . 0_555 yes Fe(2) C(7) C(6) 69.4(2) . . 0_555 yes Fe(2) C(7) C(8) 69.5(2) . . 0_555 yes C(6) C(7) C(8) 108.5(3) . . 0_555 yes Fe(2) C(8) C(7) 69.9(2) . . 0_555 yes Fe(2) C(8) C(9) 69.6(2) . . 0_555 yes C(7) C(8) C(9) 108.1(3) . . 0_555 yes Fe(2) C(9) C(5) 69.0(2) . . 0_555 yes Fe(2) C(9) C(8) 69.7(2) . . 0_555 yes C(5) C(9) C(8) 108.1(3) . . 0_555 yes Fe(2) C(10) C(11) 70.0(2) . . 0_555 yes Fe(2) C(10) C(14) 69.9(3) . . 0_555 yes C(11) C(10) C(14) 108.0(4) . . 0_555 yes Fe(2) C(11) C(10) 69.5(3) . . 0_555 yes Fe(2) C(11) C(12) 70.6(2) . . 0_555 yes C(10) C(11) C(12) 108.3(4) . . 0_555 yes Fe(2) C(12) C(11) 69.3(2) . . 0_555 yes Fe(2) C(12) C(13) 70.0(2) . . 0_555 yes C(11) C(12) C(13) 108.3(4) . . 0_555 yes Fe(2) C(13) C(12) 70.0(2) . . 0_555 yes Fe(2) C(13) C(14) 69.1(2) . . 0_555 yes C(12) C(13) C(14) 108.0(4) . . 0_555 yes Fe(2) C(14) C(10) 69.4(3) . . 0_555 yes Fe(2) C(14) C(13) 70.3(2) . . 0_555 yes C(10) C(14) C(13) 107.4(4) . . 0_555 yes N(3) C(15) N(4) 126.2(4) . . 0_555 yes N(4) C(16) C(17) 124.1(4) . . 0_555 yes C(16) C(17) C(18) 114.3(4) . . 0_555 yes C(16) C(17) C(19) 123.4(3) . . 0_555 yes C(18) C(17) C(19) 122.4(3) . . 0_555 yes N(3) C(18) C(17) 123.0(4) . . 0_555 yes Fe(1) C(19) C(17) 126.6(3) . . 0_555 yes Fe(1) C(19) C(20) 69.1(2) . . 0_555 yes Fe(1) C(19) C(23) 69.7(2) . . 0_555 yes C(17) C(19) C(20) 126.8(3) . . 0_555 yes C(17) C(19) C(23) 126.1(3) . . 0_555 yes C(20) C(19) C(23) 107.1(3) . . 0_555 yes Fe(1) C(20) C(19) 69.8(2) . . 0_555 yes Fe(1) C(20) C(21) 69.8(2) . . 0_555 yes C(19) C(20) C(21) 108.2(3) . . 0_555 yes Fe(1) C(21) C(20) 69.5(2) . . 0_555 yes Fe(1) C(21) C(22) 70.0(2) . . 0_555 yes C(20) C(21) C(22) 108.3(4) . . 0_555 yes Fe(1) C(22) C(21) 69.5(2) . . 0_555 yes Fe(1) C(22) C(23) 70.0(2) . . 0_555 yes C(21) C(22) C(23) 108.7(4) . . 0_555 yes Fe(1) C(23) C(19) 69.2(2) . . 0_555 yes Fe(1) C(23) C(22) 69.5(2) . . 0_555 yes C(19) C(23) C(22) 107.7(3) . . 0_555 yes Fe(1) C(24) C(25) 69.5(3) . . 0_555 yes Fe(1) C(24) C(28) 69.5(3) . . 0_555 yes C(25) C(24) C(28) 107.0(5) . . 0_555 yes Fe(1) C(25) C(24) 69.9(3) . . 0_555 yes Fe(1) C(25) C(26) 70.8(3) . . 0_555 yes C(24) C(25) C(26) 108.8(5) . . 0_555 yes Fe(1) C(26) C(25) 69.7(3) . . 0_555 yes Fe(1) C(26) C(27) 69.8(3) . . 0_555 yes C(25) C(26) C(27) 108.1(5) . . 0_555 yes Fe(1) C(27) C(26) 70.5(3) . . 0_555 yes Fe(1) C(27) C(28) 69.5(3) . . 0_555 yes C(26) C(27) C(28) 108.6(5) . . 0_555 yes Fe(1) C(28) C(24) 70.0(3) . . 0_555 yes Fe(1) C(28) C(27) 70.0(3) . . 0_555 yes C(24) C(28) C(27) 107.5(4) . . 0_555 yes O(1) C(29) O(2) 123.8(4) . . 0_555 yes O(1) C(29) C(30) 113.4(4) . . 0_555 yes O(2) C(29) C(30) 122.8(4) . . 0_555 yes S C(30) C(29) 111.6(3) . . 0_555 yes S C(31) C(32) 108.3(3) . . 0_555 yes O(3) C(32) O(4) 123.0(4) . . 0_555 yes O(3) C(32) C(31) 114.4(4) . . 0_555 yes O(4) C(32) C(31) 122.6(4) . . 0_555 yes #------------------------------------------------------------------------------ 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe(1) C(19) C(17) C(16) -70.8(5) 0_555 22_1 5_555 55_5 yes Fe(1) C(19) C(17) C(18) 109.8(4) 0_555 22_1 5_555 55_5 yes Fe(1) C(19) C(20) C(21) -59.4(3) 0_555 22_1 5_555 55_5 yes Fe(1) C(19) C(23) C(22) 59.0(3) 0_555 22_1 5_555 55_5 yes Fe(1) C(20) C(19) C(17) -120.8(4) 0_555 22_1 5_555 55_5 yes Fe(1) C(20) C(19) C(23) 59.6(2) 0_555 22_1 5_555 55_5 yes Fe(1) C(20) C(21) C(22) -59.5(3) 0_555 22_1 5_555 55_5 yes Fe(1) C(21) C(20) C(19) 59.4(3) 0_555 22_1 5_555 55_5 yes Fe(1) C(21) C(22) C(23) -59.3(3) 0_555 22_1 5_555 55_5 yes Fe(1) C(22) C(21) C(20) 59.2(3) 0_555 22_1 5_555 55_5 yes Fe(1) C(22) C(23) C(19) -58.8(2) 0_555 22_1 5_555 55_5 yes Fe(1) C(23) C(19) C(17) 121.1(4) 0_555 22_1 5_555 55_5 yes Fe(1) C(23) C(19) C(20) -59.2(3) 0_555 22_1 5_555 55_5 yes Fe(1) C(23) C(22) C(21) 58.9(3) 0_555 22_1 5_555 55_5 yes Fe(1) C(24) C(25) C(26) 60.3(3) 0_555 22_1 5_555 55_5 yes Fe(1) C(24) C(28) C(27) -60.3(3) 0_555 22_1 5_555 55_5 yes Fe(1) C(25) C(24) C(28) -59.6(3) 0_555 22_1 5_555 55_5 yes Fe(1) C(25) C(26) C(27) 59.4(3) 0_555 22_1 5_555 55_5 yes Fe(1) C(26) C(25) C(24) -59.8(3) 0_555 22_1 5_555 55_5 yes Fe(1) C(26) C(27) C(28) 59.3(3) 0_555 22_1 5_555 55_5 yes Fe(1) C(27) C(26) C(25) -59.3(3) 0_555 22_1 5_555 55_5 yes Fe(1) C(27) C(28) C(24) 60.3(3) 0_555 22_1 5_555 55_5 yes Fe(1) C(28) C(24) C(25) 59.6(3) 0_555 22_1 5_555 55_5 yes Fe(1) C(28) C(27) C(26) -59.9(3) 0_555 22_1 5_555 55_5 yes Fe(2) C(5) C(3) C(2) -70.4(5) 0_555 22_1 5_555 55_5 yes Fe(2) C(5) C(3) C(4) 109.8(4) 0_555 22_1 5_555 55_5 yes Fe(2) C(5) C(6) C(7) 59.4(3) 0_555 22_1 5_555 55_5 yes Fe(2) C(5) C(9) C(8) -58.9(3) 0_555 22_1 5_555 55_5 yes Fe(2) C(6) C(5) C(3) 119.0(4) 0_555 22_1 5_555 55_5 yes Fe(2) C(6) C(5) C(9) -59.9(3) 0_555 22_1 5_555 55_5 yes Fe(2) C(6) C(7) C(8) 58.7(3) 0_555 22_1 5_555 55_5 yes Fe(2) C(7) C(6) C(5) -58.7(3) 0_555 22_1 5_555 55_5 yes Fe(2) C(7) C(8) C(9) 59.3(3) 0_555 22_1 5_555 55_5 yes Fe(2) C(8) C(7) C(6) -58.7(3) 0_555 22_1 5_555 55_5 yes Fe(2) C(8) C(9) C(5) 58.5(3) 0_555 22_1 5_555 55_5 yes Fe(2) C(9) C(5) C(3) -119.0(4) 0_555 22_1 5_555 55_5 yes Fe(2) C(9) C(5) C(6) 59.9(2) 0_555 22_1 5_555 55_5 yes Fe(2) C(9) C(8) C(7) -59.5(3) 0_555 22_1 5_555 55_5 yes Fe(2) C(10) C(11) C(12) -60.2(3) 0_555 22_1 5_555 55_5 yes Fe(2) C(10) C(14) C(13) 60.3(3) 0_555 22_1 5_555 55_5 yes Fe(2) C(11) C(10) C(14) 59.8(3) 0_555 22_1 5_555 55_5 yes Fe(2) C(11) C(12) C(13) -59.3(3) 0_555 22_1 5_555 55_5 yes Fe(2) C(12) C(11) C(10) 59.5(3) 0_555 22_1 5_555 55_5 yes Fe(2) C(12) C(13) C(14) -58.8(3) 0_555 22_1 5_555 55_5 yes Fe(2) C(13) C(12) C(11) 58.9(3) 0_555 22_1 5_555 55_5 yes Fe(2) C(13) C(14) C(10) -59.7(3) 0_555 22_1 5_555 55_5 yes Fe(2) C(14) C(10) C(11) -59.9(3) 0_555 22_1 5_555 55_5 yes Fe(2) C(14) C(13) C(12) 59.4(3) 0_555 22_1 5_555 55_5 yes S C(30) C(29) O(1) 74.7(4) 0_555 22_1 5_555 55_5 yes S C(30) C(29) O(2) -104.1(5) 0_555 22_1 5_555 55_5 yes S C(31) C(32) O(3) -155.2(4) 0_555 22_1 5_555 55_5 yes S C(31) C(32) O(4) 27.6(7) 0_555 22_1 5_555 55_5 yes N(1) C(1) N(2) C(2) -0.6(8) 0_555 22_1 5_555 55_5 yes N(1) C(4) C(3) C(2) 0.4(6) 0_555 22_1 5_555 55_5 yes N(1) C(4) C(3) C(5) -179.8(4) 0_555 22_1 5_555 55_5 yes N(2) C(1) N(1) C(4) 0.9(7) 0_555 22_1 5_555 55_5 yes N(2) C(2) C(3) C(4) -0.2(7) 0_555 22_1 5_555 55_5 yes N(2) C(2) C(3) C(5) -179.9(4) 0_555 22_1 5_555 55_5 yes N(3) C(15) N(4) C(16) -1.6(8) 0_555 22_1 5_555 55_5 yes N(3) C(18) C(17) C(16) -1.9(6) 0_555 22_1 5_555 55_5 yes N(3) C(18) C(17) C(19) 177.5(4) 0_555 22_1 5_555 55_5 yes N(4) C(15) N(3) C(18) 2.0(7) 0_555 22_1 5_555 55_5 yes N(4) C(16) C(17) C(18) 2.3(7) 0_555 22_1 5_555 55_5 yes N(4) C(16) C(17) C(19) -177.1(4) 0_555 22_1 5_555 55_5 yes C(1) N(1) C(4) C(3) -0.7(6) 0_555 22_1 5_555 55_5 yes C(1) N(2) C(2) C(3) 0.2(7) 0_555 22_1 5_555 55_5 yes C(2) C(3) C(5) C(6) -160.5(4) 0_555 22_1 5_555 55_5 yes C(2) C(3) C(5) C(9) 18.2(6) 0_555 22_1 5_555 55_5 yes C(3) C(5) Fe(2) C(6) -122.4(4) 0_555 22_1 5_555 55_5 yes C(3) C(5) Fe(2) C(7) -159.3(4) 0_555 22_1 5_555 55_5 yes C(3) C(5) Fe(2) C(8) 157.1(4) 0_555 22_1 5_555 55_5 yes C(3) C(5) Fe(2) C(9) 119.8(4) 0_555 22_1 5_555 55_5 yes C(3) C(5) Fe(2) C(10) -4.6(4) 0_555 22_1 5_555 55_5 yes C(3) C(5) Fe(2) C(11) -44.9(4) 0_555 22_1 5_555 55_5 yes C(3) C(5) Fe(2) C(12) -71.7(7) 0_555 22_1 5_555 55_5 yes C(3) C(5) Fe(2) C(13) 68.5(5) 0_555 22_1 5_555 55_5 yes C(3) C(5) Fe(2) C(14) 37.6(4) 0_555 22_1 5_555 55_5 yes C(3) C(5) C(6) C(7) 178.4(4) 0_555 22_1 5_555 55_5 yes C(3) C(5) C(9) C(8) -178.0(3) 0_555 22_1 5_555 55_5 yes C(4) C(3) C(5) C(6) 19.8(6) 0_555 22_1 5_555 55_5 yes C(4) C(3) C(5) C(9) -161.5(4) 0_555 22_1 5_555 55_5 yes C(5) Fe(2) C(6) C(7) -119.9(3) 0_555 22_1 5_555 55_5 yes C(5) Fe(2) C(7) C(6) 37.8(2) 0_555 22_1 5_555 55_5 yes C(5) Fe(2) C(7) C(8) -82.3(2) 0_555 22_1 5_555 55_5 yes C(5) Fe(2) C(8) C(7) 81.4(2) 0_555 22_1 5_555 55_5 yes C(5) Fe(2) C(8) C(9) -37.9(2) 0_555 22_1 5_555 55_5 yes C(5) Fe(2) C(9) C(8) 119.7(3) 0_555 22_1 5_555 55_5 yes C(5) Fe(2) C(10) C(11) -125.7(3) 0_555 22_1 5_555 55_5 yes C(5) Fe(2) C(10) C(14) 115.4(3) 0_555 22_1 5_555 55_5 yes C(5) Fe(2) C(11) C(10) 72.7(3) 0_555 22_1 5_555 55_5 yes C(5) Fe(2) C(11) C(12) -168.1(2) 0_555 22_1 5_555 55_5 yes C(5) Fe(2) C(12) C(11) 35.0(7) 0_555 22_1 5_555 55_5 yes C(5) Fe(2) C(12) C(13) 154.7(5) 0_555 22_1 5_555 55_5 yes C(5) Fe(2) C(13) C(12) -163.1(3) 0_555 22_1 5_555 55_5 yes C(5) Fe(2) C(13) C(14) -43.7(5) 0_555 22_1 5_555 55_5 yes C(5) Fe(2) C(14) C(10) -81.5(3) 0_555 22_1 5_555 55_5 yes C(5) Fe(2) C(14) C(13) 160.1(2) 0_555 22_1 5_555 55_5 yes C(5) C(6) Fe(2) C(7) 119.9(3) 0_555 22_1 5_555 55_5 yes C(5) C(6) Fe(2) C(8) 82.7(2) 0_555 22_1 5_555 55_5 yes C(5) C(6) Fe(2) C(9) 38.9(2) 0_555 22_1 5_555 55_5 yes C(5) C(6) Fe(2) C(10) -79.9(3) 0_555 22_1 5_555 55_5 yes C(5) C(6) Fe(2) C(11) -122.8(3) 0_555 22_1 5_555 55_5 yes C(5) C(6) Fe(2) C(12) -163.6(2) 0_555 22_1 5_555 55_5 yes C(5) C(6) Fe(2) C(13) 163.6(5) 0_555 22_1 5_555 55_5 yes C(5) C(6) Fe(2) C(14) -44.9(5) 0_555 22_1 5_555 55_5 yes C(5) C(6) C(7) C(8) 0.0(4) 0_555 22_1 5_555 55_5 yes C(5) C(9) Fe(2) C(6) -38.7(2) 0_555 22_1 5_555 55_5 yes C(5) C(9) Fe(2) C(7) -82.1(2) 0_555 22_1 5_555 55_5 yes C(5) C(9) Fe(2) C(8) -119.7(3) 0_555 22_1 5_555 55_5 yes C(5) C(9) Fe(2) C(10) 74.5(3) 0_555 22_1 5_555 55_5 yes C(5) C(9) Fe(2) C(11) 46.0(7) 0_555 22_1 5_555 55_5 yes C(5) C(9) Fe(2) C(12) -172.0(4) 0_555 22_1 5_555 55_5 yes C(5) C(9) Fe(2) C(13) 157.2(2) 0_555 22_1 5_555 55_5 yes C(5) C(9) Fe(2) C(14) 115.2(3) 0_555 22_1 5_555 55_5 yes C(5) C(9) C(8) C(7) -1.0(5) 0_555 22_1 5_555 55_5 yes C(6) Fe(2) C(5) C(9) 117.8(3) 0_555 22_1 5_555 55_5 yes C(6) Fe(2) C(7) C(8) -120.1(3) 0_555 22_1 5_555 55_5 yes C(6) Fe(2) C(8) C(7) 37.0(2) 0_555 22_1 5_555 55_5 yes C(6) Fe(2) C(8) C(9) -82.3(3) 0_555 22_1 5_555 55_5 yes C(6) Fe(2) C(9) C(8) 81.0(3) 0_555 22_1 5_555 55_5 yes C(6) Fe(2) C(10) C(11) -83.1(3) 0_555 22_1 5_555 55_5 yes C(6) Fe(2) C(10) C(14) 158.0(3) 0_555 22_1 5_555 55_5 yes C(6) Fe(2) C(11) C(10) 115.5(3) 0_555 22_1 5_555 55_5 yes C(6) Fe(2) C(11) C(12) -125.4(3) 0_555 22_1 5_555 55_5 yes C(6) Fe(2) C(12) C(11) 74.4(3) 0_555 22_1 5_555 55_5 yes C(6) Fe(2) C(12) C(13) -165.9(3) 0_555 22_1 5_555 55_5 yes C(6) Fe(2) C(13) C(12) 42.5(7) 0_555 22_1 5_555 55_5 yes C(6) Fe(2) C(13) C(14) 161.9(5) 0_555 22_1 5_555 55_5 yes C(6) Fe(2) C(14) C(10) -49.4(6) 0_555 22_1 5_555 55_5 yes C(6) Fe(2) C(14) C(13) -167.8(4) 0_555 22_1 5_555 55_5 yes C(6) C(5) Fe(2) C(7) -37.0(2) 0_555 22_1 5_555 55_5 yes C(6) C(5) Fe(2) C(8) -80.6(2) 0_555 22_1 5_555 55_5 yes C(6) C(5) Fe(2) C(9) -117.8(3) 0_555 22_1 5_555 55_5 yes C(6) C(5) Fe(2) C(10) 117.8(3) 0_555 22_1 5_555 55_5 yes C(6) C(5) Fe(2) C(11) 77.5(3) 0_555 22_1 5_555 55_5 yes C(6) C(5) Fe(2) C(12) 50.6(6) 0_555 22_1 5_555 55_5 yes C(6) C(5) Fe(2) C(13) -169.1(4) 0_555 22_1 5_555 55_5 yes C(6) C(5) Fe(2) C(14) 160.0(3) 0_555 22_1 5_555 55_5 yes C(6) C(5) C(9) C(8) 1.0(4) 0_555 22_1 5_555 55_5 yes C(6) C(7) Fe(2) C(8) 120.1(3) 0_555 22_1 5_555 55_5 yes C(6) C(7) Fe(2) C(9) 82.5(2) 0_555 22_1 5_555 55_5 yes C(6) C(7) Fe(2) C(10) -45.2(5) 0_555 22_1 5_555 55_5 yes C(6) C(7) Fe(2) C(11) -81.5(3) 0_555 22_1 5_555 55_5 yes C(6) C(7) Fe(2) C(12) -124.1(3) 0_555 22_1 5_555 55_5 yes C(6) C(7) Fe(2) C(13) -165.6(2) 0_555 22_1 5_555 55_5 yes C(6) C(7) Fe(2) C(14) 157.8(6) 0_555 22_1 5_555 55_5 yes C(6) C(7) C(8) C(9) 0.7(5) 0_555 22_1 5_555 55_5 yes C(7) Fe(2) C(5) C(9) 80.9(2) 0_555 22_1 5_555 55_5 yes C(7) Fe(2) C(8) C(9) -119.3(4) 0_555 22_1 5_555 55_5 yes C(7) Fe(2) C(9) C(8) 37.6(2) 0_555 22_1 5_555 55_5 yes C(7) Fe(2) C(10) C(11) -50.9(5) 0_555 22_1 5_555 55_5 yes C(7) Fe(2) C(10) C(14) -169.8(4) 0_555 22_1 5_555 55_5 yes C(7) Fe(2) C(11) C(10) 157.9(3) 0_555 22_1 5_555 55_5 yes C(7) Fe(2) C(11) C(12) -82.9(3) 0_555 22_1 5_555 55_5 yes C(7) Fe(2) C(12) C(11) 116.2(3) 0_555 22_1 5_555 55_5 yes C(7) Fe(2) C(12) C(13) -124.1(3) 0_555 22_1 5_555 55_5 yes C(7) Fe(2) C(13) C(12) 76.3(3) 0_555 22_1 5_555 55_5 yes C(7) Fe(2) C(13) C(14) -164.3(3) 0_555 22_1 5_555 55_5 yes C(7) Fe(2) C(14) C(10) 165.7(5) 0_555 22_1 5_555 55_5 yes C(7) Fe(2) C(14) C(13) 47.4(7) 0_555 22_1 5_555 55_5 yes C(7) C(6) Fe(2) C(8) -37.3(2) 0_555 22_1 5_555 55_5 yes C(7) C(6) Fe(2) C(9) -81.1(3) 0_555 22_1 5_555 55_5 yes C(7) C(6) Fe(2) C(10) 160.2(3) 0_555 22_1 5_555 55_5 yes C(7) C(6) Fe(2) C(11) 117.3(3) 0_555 22_1 5_555 55_5 yes C(7) C(6) Fe(2) C(12) 76.5(3) 0_555 22_1 5_555 55_5 yes C(7) C(6) Fe(2) C(13) 43.7(7) 0_555 22_1 5_555 55_5 yes C(7) C(6) Fe(2) C(14) -164.8(4) 0_555 22_1 5_555 55_5 yes C(7) C(6) C(5) C(9) -0.6(4) 0_555 22_1 5_555 55_5 yes C(7) C(8) Fe(2) C(9) 119.3(4) 0_555 22_1 5_555 55_5 yes C(7) C(8) Fe(2) C(10) 160.2(5) 0_555 22_1 5_555 55_5 yes C(7) C(8) Fe(2) C(11) -50.2(5) 0_555 22_1 5_555 55_5 yes C(7) C(8) Fe(2) C(12) -83.7(3) 0_555 22_1 5_555 55_5 yes C(7) C(8) Fe(2) C(13) -125.5(3) 0_555 22_1 5_555 55_5 yes C(7) C(8) Fe(2) C(14) -167.3(3) 0_555 22_1 5_555 55_5 yes C(8) Fe(2) C(5) C(9) 37.2(2) 0_555 22_1 5_555 55_5 yes C(8) Fe(2) C(10) C(11) 161.5(5) 0_555 22_1 5_555 55_5 yes C(8) Fe(2) C(10) C(14) 42.6(7) 0_555 22_1 5_555 55_5 yes C(8) Fe(2) C(11) C(10) -166.1(4) 0_555 22_1 5_555 55_5 yes C(8) Fe(2) C(11) C(12) -47.0(5) 0_555 22_1 5_555 55_5 yes C(8) Fe(2) C(12) C(11) 159.6(3) 0_555 22_1 5_555 55_5 yes C(8) Fe(2) C(12) C(13) -80.8(3) 0_555 22_1 5_555 55_5 yes C(8) Fe(2) C(13) C(12) 117.5(3) 0_555 22_1 5_555 55_5 yes C(8) Fe(2) C(13) C(14) -123.1(3) 0_555 22_1 5_555 55_5 yes C(8) Fe(2) C(14) C(10) -165.2(3) 0_555 22_1 5_555 55_5 yes C(8) Fe(2) C(14) C(13) 76.4(3) 0_555 22_1 5_555 55_5 yes C(8) C(7) Fe(2) C(9) -37.7(2) 0_555 22_1 5_555 55_5 yes C(8) C(7) Fe(2) C(10) -165.3(4) 0_555 22_1 5_555 55_5 yes C(8) C(7) Fe(2) C(11) 158.4(3) 0_555 22_1 5_555 55_5 yes C(8) C(7) Fe(2) C(12) 115.7(3) 0_555 22_1 5_555 55_5 yes C(8) C(7) Fe(2) C(13) 74.3(3) 0_555 22_1 5_555 55_5 yes C(8) C(7) Fe(2) C(14) 37.7(7) 0_555 22_1 5_555 55_5 yes C(8) C(9) Fe(2) C(10) -165.8(3) 0_555 22_1 5_555 55_5 yes C(8) C(9) Fe(2) C(11) 165.7(6) 0_555 22_1 5_555 55_5 yes C(8) C(9) Fe(2) C(12) -52.3(5) 0_555 22_1 5_555 55_5 yes C(8) C(9) Fe(2) C(13) -83.1(3) 0_555 22_1 5_555 55_5 yes C(8) C(9) Fe(2) C(14) -125.1(3) 0_555 22_1 5_555 55_5 yes C(9) Fe(2) C(10) C(11) -167.3(3) 0_555 22_1 5_555 55_5 yes C(9) Fe(2) C(10) C(14) 73.8(3) 0_555 22_1 5_555 55_5 yes C(9) Fe(2) C(11) C(10) 37.1(7) 0_555 22_1 5_555 55_5 yes C(9) Fe(2) C(11) C(12) 156.2(5) 0_555 22_1 5_555 55_5 yes C(9) Fe(2) C(12) C(11) -163.4(4) 0_555 22_1 5_555 55_5 yes C(9) Fe(2) C(12) C(13) -43.7(5) 0_555 22_1 5_555 55_5 yes C(9) Fe(2) C(13) C(12) 160.4(3) 0_555 22_1 5_555 55_5 yes C(9) Fe(2) C(13) C(14) -80.2(3) 0_555 22_1 5_555 55_5 yes C(9) Fe(2) C(14) C(10) -124.6(3) 0_555 22_1 5_555 55_5 yes C(9) Fe(2) C(14) C(13) 117.0(3) 0_555 22_1 5_555 55_5 yes C(9) C(5) Fe(2) C(10) -124.4(3) 0_555 22_1 5_555 55_5 yes C(9) C(5) Fe(2) C(11) -164.7(3) 0_555 22_1 5_555 55_5 yes C(9) C(5) Fe(2) C(12) 168.4(5) 0_555 22_1 5_555 55_5 yes C(9) C(5) Fe(2) C(13) -51.3(5) 0_555 22_1 5_555 55_5 yes C(9) C(5) Fe(2) C(14) -82.2(3) 0_555 22_1 5_555 55_5 yes C(9) C(8) Fe(2) C(10) 40.8(7) 0_555 22_1 5_555 55_5 yes C(9) C(8) Fe(2) C(11) -169.6(4) 0_555 22_1 5_555 55_5 yes C(9) C(8) Fe(2) C(12) 157.0(3) 0_555 22_1 5_555 55_5 yes C(9) C(8) Fe(2) C(13) 115.2(3) 0_555 22_1 5_555 55_5 yes C(9) C(8) Fe(2) C(14) 73.4(3) 0_555 22_1 5_555 55_5 yes C(10) Fe(2) C(11) C(12) 119.1(4) 0_555 22_1 5_555 55_5 yes C(10) Fe(2) C(12) C(11) -37.8(3) 0_555 22_1 5_555 55_5 yes C(10) Fe(2) C(12) C(13) 81.8(3) 0_555 22_1 5_555 55_5 yes C(10) Fe(2) C(13) C(12) -81.2(3) 0_555 22_1 5_555 55_5 yes C(10) Fe(2) C(13) C(14) 38.2(3) 0_555 22_1 5_555 55_5 yes C(10) Fe(2) C(14) C(13) -118.4(4) 0_555 22_1 5_555 55_5 yes C(10) C(11) Fe(2) C(12) -119.1(4) 0_555 22_1 5_555 55_5 yes C(10) C(11) Fe(2) C(13) -81.9(3) 0_555 22_1 5_555 55_5 yes C(10) C(11) Fe(2) C(14) -37.9(3) 0_555 22_1 5_555 55_5 yes C(10) C(11) C(12) C(13) 0.2(5) 0_555 22_1 5_555 55_5 yes C(10) C(14) Fe(2) C(11) 37.8(3) 0_555 22_1 5_555 55_5 yes C(10) C(14) Fe(2) C(12) 81.2(3) 0_555 22_1 5_555 55_5 yes C(10) C(14) Fe(2) C(13) 118.4(4) 0_555 22_1 5_555 55_5 yes C(10) C(14) C(13) C(12) -0.3(5) 0_555 22_1 5_555 55_5 yes C(11) Fe(2) C(10) C(14) -118.9(4) 0_555 22_1 5_555 55_5 yes C(11) Fe(2) C(12) C(13) 119.7(4) 0_555 22_1 5_555 55_5 yes C(11) Fe(2) C(13) C(12) -37.2(3) 0_555 22_1 5_555 55_5 yes C(11) Fe(2) C(13) C(14) 82.2(3) 0_555 22_1 5_555 55_5 yes C(11) Fe(2) C(14) C(13) -80.5(3) 0_555 22_1 5_555 55_5 yes C(11) C(10) Fe(2) C(12) 37.4(3) 0_555 22_1 5_555 55_5 yes C(11) C(10) Fe(2) C(13) 80.7(3) 0_555 22_1 5_555 55_5 yes C(11) C(10) Fe(2) C(14) 118.9(4) 0_555 22_1 5_555 55_5 yes C(11) C(10) C(14) C(13) 0.4(5) 0_555 22_1 5_555 55_5 yes C(11) C(12) Fe(2) C(13) -119.7(4) 0_555 22_1 5_555 55_5 yes C(11) C(12) Fe(2) C(14) -81.9(3) 0_555 22_1 5_555 55_5 yes C(11) C(12) C(13) C(14) 0.1(5) 0_555 22_1 5_555 55_5 yes C(12) Fe(2) C(10) C(14) -81.5(3) 0_555 22_1 5_555 55_5 yes C(12) Fe(2) C(13) C(14) 119.4(4) 0_555 22_1 5_555 55_5 yes C(12) Fe(2) C(14) C(13) -37.2(3) 0_555 22_1 5_555 55_5 yes C(12) C(11) Fe(2) C(13) 37.2(3) 0_555 22_1 5_555 55_5 yes C(12) C(11) Fe(2) C(14) 81.2(3) 0_555 22_1 5_555 55_5 yes C(12) C(11) C(10) C(14) -0.4(5) 0_555 22_1 5_555 55_5 yes C(12) C(13) Fe(2) C(14) -119.4(4) 0_555 22_1 5_555 55_5 yes C(13) Fe(2) C(10) C(14) -38.2(3) 0_555 22_1 5_555 55_5 yes C(13) C(12) Fe(2) C(14) 37.8(3) 0_555 22_1 5_555 55_5 yes C(15) N(3) C(18) C(17) 0.0(6) 0_555 22_1 5_555 55_5 yes C(15) N(4) C(16) C(17) -0.7(7) 0_555 22_1 5_555 55_5 yes C(16) C(17) C(19) C(20) 19.2(6) 0_555 22_1 5_555 55_5 yes C(16) C(17) C(19) C(23) -161.1(4) 0_555 22_1 5_555 55_5 yes C(17) C(19) Fe(1) C(20) 121.0(4) 0_555 22_1 5_555 55_5 yes C(17) C(19) Fe(1) C(21) 158.5(4) 0_555 22_1 5_555 55_5 yes C(17) C(19) Fe(1) C(22) -157.9(4) 0_555 22_1 5_555 55_5 yes C(17) C(19) Fe(1) C(23) -120.5(4) 0_555 22_1 5_555 55_5 yes C(17) C(19) Fe(1) C(24) 2.7(4) 0_555 22_1 5_555 55_5 yes C(17) C(19) Fe(1) C(25) 43.7(4) 0_555 22_1 5_555 55_5 yes C(17) C(19) Fe(1) C(26) 73.4(7) 0_555 22_1 5_555 55_5 yes C(17) C(19) Fe(1) C(27) -71.4(6) 0_555 22_1 5_555 55_5 yes C(17) C(19) Fe(1) C(28) -39.6(4) 0_555 22_1 5_555 55_5 yes C(17) C(19) C(20) C(21) 179.8(3) 0_555 22_1 5_555 55_5 yes C(17) C(19) C(23) C(22) -179.9(3) 0_555 22_1 5_555 55_5 yes C(18) C(17) C(19) C(20) -160.2(4) 0_555 22_1 5_555 55_5 yes C(18) C(17) C(19) C(23) 19.5(6) 0_555 22_1 5_555 55_5 yes C(19) Fe(1) C(20) C(21) 119.4(3) 0_555 22_1 5_555 55_5 yes C(19) Fe(1) C(21) C(20) -37.9(2) 0_555 22_1 5_555 55_5 yes C(19) Fe(1) C(21) C(22) 81.5(3) 0_555 22_1 5_555 55_5 yes C(19) Fe(1) C(22) C(21) -82.0(3) 0_555 22_1 5_555 55_5 yes C(19) Fe(1) C(22) C(23) 38.0(2) 0_555 22_1 5_555 55_5 yes C(19) Fe(1) C(23) C(22) -119.3(3) 0_555 22_1 5_555 55_5 yes C(19) Fe(1) C(24) C(25) 125.0(3) 0_555 22_1 5_555 55_5 yes C(19) Fe(1) C(24) C(28) -116.7(3) 0_555 22_1 5_555 55_5 yes C(19) Fe(1) C(25) C(24) -74.2(4) 0_555 22_1 5_555 55_5 yes C(19) Fe(1) C(25) C(26) 166.3(3) 0_555 22_1 5_555 55_5 yes C(19) Fe(1) C(26) C(25) -39.1(7) 0_555 22_1 5_555 55_5 yes C(19) Fe(1) C(26) C(27) -158.5(5) 0_555 22_1 5_555 55_5 yes C(19) Fe(1) C(27) C(26) 164.1(4) 0_555 22_1 5_555 55_5 yes C(19) Fe(1) C(27) C(28) 44.6(6) 0_555 22_1 5_555 55_5 yes C(19) Fe(1) C(28) C(24) 81.2(3) 0_555 22_1 5_555 55_5 yes C(19) Fe(1) C(28) C(27) -160.6(3) 0_555 22_1 5_555 55_5 yes C(19) C(20) Fe(1) C(21) -119.4(3) 0_555 22_1 5_555 55_5 yes C(19) C(20) Fe(1) C(22) -81.9(2) 0_555 22_1 5_555 55_5 yes C(19) C(20) Fe(1) C(23) -38.3(2) 0_555 22_1 5_555 55_5 yes C(19) C(20) Fe(1) C(24) 80.3(3) 0_555 22_1 5_555 55_5 yes C(19) C(20) Fe(1) C(25) 123.2(3) 0_555 22_1 5_555 55_5 yes C(19) C(20) Fe(1) C(26) 164.0(3) 0_555 22_1 5_555 55_5 yes C(19) C(20) Fe(1) C(27) -163.7(6) 0_555 22_1 5_555 55_5 yes C(19) C(20) Fe(1) C(28) 45.8(5) 0_555 22_1 5_555 55_5 yes C(19) C(20) C(21) C(22) -0.1(4) 0_555 22_1 5_555 55_5 yes C(19) C(23) Fe(1) C(20) 38.3(2) 0_555 22_1 5_555 55_5 yes C(19) C(23) Fe(1) C(21) 82.1(2) 0_555 22_1 5_555 55_5 yes C(19) C(23) Fe(1) C(22) 119.3(3) 0_555 22_1 5_555 55_5 yes C(19) C(23) Fe(1) C(24) -76.2(3) 0_555 22_1 5_555 55_5 yes C(19) C(23) Fe(1) C(25) -47.4(7) 0_555 22_1 5_555 55_5 yes C(19) C(23) Fe(1) C(26) 169.8(4) 0_555 22_1 5_555 55_5 yes C(19) C(23) Fe(1) C(27) -159.0(3) 0_555 22_1 5_555 55_5 yes C(19) C(23) Fe(1) C(28) -117.1(3) 0_555 22_1 5_555 55_5 yes C(19) C(23) C(22) C(21) 0.1(4) 0_555 22_1 5_555 55_5 yes C(20) Fe(1) C(19) C(23) -118.5(3) 0_555 22_1 5_555 55_5 yes C(20) Fe(1) C(21) C(22) 119.5(4) 0_555 22_1 5_555 55_5 yes C(20) Fe(1) C(22) C(21) -37.6(2) 0_555 22_1 5_555 55_5 yes C(20) Fe(1) C(22) C(23) 82.4(3) 0_555 22_1 5_555 55_5 yes C(20) Fe(1) C(23) C(22) -81.0(3) 0_555 22_1 5_555 55_5 yes C(20) Fe(1) C(24) C(25) 82.2(4) 0_555 22_1 5_555 55_5 yes C(20) Fe(1) C(24) C(28) -159.6(3) 0_555 22_1 5_555 55_5 yes C(20) Fe(1) C(25) C(24) -116.9(3) 0_555 22_1 5_555 55_5 yes C(20) Fe(1) C(25) C(26) 123.7(3) 0_555 22_1 5_555 55_5 yes C(20) Fe(1) C(26) C(25) -75.8(4) 0_555 22_1 5_555 55_5 yes C(20) Fe(1) C(26) C(27) 164.8(3) 0_555 22_1 5_555 55_5 yes C(20) Fe(1) C(27) C(26) -42.8(8) 0_555 22_1 5_555 55_5 yes C(20) Fe(1) C(27) C(28) -162.4(5) 0_555 22_1 5_555 55_5 yes C(20) Fe(1) C(28) C(24) 48.1(6) 0_555 22_1 5_555 55_5 yes C(20) Fe(1) C(28) C(27) 166.3(4) 0_555 22_1 5_555 55_5 yes C(20) C(19) Fe(1) C(21) 37.5(2) 0_555 22_1 5_555 55_5 yes C(20) C(19) Fe(1) C(22) 81.1(3) 0_555 22_1 5_555 55_5 yes C(20) C(19) Fe(1) C(23) 118.5(3) 0_555 22_1 5_555 55_5 yes C(20) C(19) Fe(1) C(24) -118.3(3) 0_555 22_1 5_555 55_5 yes C(20) C(19) Fe(1) C(25) -77.3(3) 0_555 22_1 5_555 55_5 yes C(20) C(19) Fe(1) C(26) -47.6(7) 0_555 22_1 5_555 55_5 yes C(20) C(19) Fe(1) C(27) 167.5(5) 0_555 22_1 5_555 55_5 yes C(20) C(19) Fe(1) C(28) -160.6(3) 0_555 22_1 5_555 55_5 yes C(20) C(19) C(23) C(22) -0.2(4) 0_555 22_1 5_555 55_5 yes C(20) C(21) Fe(1) C(22) -119.5(4) 0_555 22_1 5_555 55_5 yes C(20) C(21) Fe(1) C(23) -82.3(2) 0_555 22_1 5_555 55_5 yes C(20) C(21) Fe(1) C(24) 47.1(5) 0_555 22_1 5_555 55_5 yes C(20) C(21) Fe(1) C(25) 81.9(3) 0_555 22_1 5_555 55_5 yes C(20) C(21) Fe(1) C(26) 123.4(3) 0_555 22_1 5_555 55_5 yes C(20) C(21) Fe(1) C(27) 164.5(3) 0_555 22_1 5_555 55_5 yes C(20) C(21) Fe(1) C(28) -161.4(5) 0_555 22_1 5_555 55_5 yes C(20) C(21) C(22) C(23) 0.0(4) 0_555 22_1 5_555 55_5 yes C(21) Fe(1) C(19) C(23) -81.0(3) 0_555 22_1 5_555 55_5 yes C(21) Fe(1) C(22) C(23) 120.0(4) 0_555 22_1 5_555 55_5 yes C(21) Fe(1) C(23) C(22) -37.2(3) 0_555 22_1 5_555 55_5 yes C(21) Fe(1) C(24) C(25) 48.2(6) 0_555 22_1 5_555 55_5 yes C(21) Fe(1) C(24) C(28) 166.4(4) 0_555 22_1 5_555 55_5 yes C(21) Fe(1) C(25) C(24) -159.9(3) 0_555 22_1 5_555 55_5 yes C(21) Fe(1) C(25) C(26) 80.7(4) 0_555 22_1 5_555 55_5 yes C(21) Fe(1) C(26) C(25) -117.8(3) 0_555 22_1 5_555 55_5 yes C(21) Fe(1) C(26) C(27) 122.8(3) 0_555 22_1 5_555 55_5 yes C(21) Fe(1) C(27) C(26) -76.6(4) 0_555 22_1 5_555 55_5 yes C(21) Fe(1) C(27) C(28) 163.9(3) 0_555 22_1 5_555 55_5 yes C(21) Fe(1) C(28) C(24) -163.3(5) 0_555 22_1 5_555 55_5 yes C(21) Fe(1) C(28) C(27) -45.1(7) 0_555 22_1 5_555 55_5 yes C(21) C(20) Fe(1) C(22) 37.5(2) 0_555 22_1 5_555 55_5 yes C(21) C(20) Fe(1) C(23) 81.1(3) 0_555 22_1 5_555 55_5 yes C(21) C(20) Fe(1) C(24) -160.3(3) 0_555 22_1 5_555 55_5 yes C(21) C(20) Fe(1) C(25) -117.4(3) 0_555 22_1 5_555 55_5 yes C(21) C(20) Fe(1) C(26) -76.6(3) 0_555 22_1 5_555 55_5 yes C(21) C(20) Fe(1) C(27) -44.3(7) 0_555 22_1 5_555 55_5 yes C(21) C(20) Fe(1) C(28) 165.1(4) 0_555 22_1 5_555 55_5 yes C(21) C(20) C(19) C(23) 0.1(4) 0_555 22_1 5_555 55_5 yes C(21) C(22) Fe(1) C(23) -120.0(4) 0_555 22_1 5_555 55_5 yes C(21) C(22) Fe(1) C(24) -163.4(5) 0_555 22_1 5_555 55_5 yes C(21) C(22) Fe(1) C(25) 50.1(6) 0_555 22_1 5_555 55_5 yes C(21) C(22) Fe(1) C(26) 81.9(3) 0_555 22_1 5_555 55_5 yes C(21) C(22) Fe(1) C(27) 123.4(3) 0_555 22_1 5_555 55_5 yes C(21) C(22) Fe(1) C(28) 164.9(3) 0_555 22_1 5_555 55_5 yes C(22) Fe(1) C(19) C(23) -37.4(2) 0_555 22_1 5_555 55_5 yes C(22) Fe(1) C(24) C(25) -160.0(5) 0_555 22_1 5_555 55_5 yes C(22) Fe(1) C(24) C(28) -41.8(7) 0_555 22_1 5_555 55_5 yes C(22) Fe(1) C(25) C(24) 164.2(4) 0_555 22_1 5_555 55_5 yes C(22) Fe(1) C(25) C(26) 44.8(7) 0_555 22_1 5_555 55_5 yes C(22) Fe(1) C(26) C(25) -160.6(3) 0_555 22_1 5_555 55_5 yes C(22) Fe(1) C(26) C(27) 80.1(4) 0_555 22_1 5_555 55_5 yes C(22) Fe(1) C(27) C(26) -118.1(3) 0_555 22_1 5_555 55_5 yes C(22) Fe(1) C(27) C(28) 122.4(3) 0_555 22_1 5_555 55_5 yes C(22) Fe(1) C(28) C(24) 165.0(3) 0_555 22_1 5_555 55_5 yes C(22) Fe(1) C(28) C(27) -76.8(4) 0_555 22_1 5_555 55_5 yes C(22) C(21) Fe(1) C(23) 37.2(3) 0_555 22_1 5_555 55_5 yes C(22) C(21) Fe(1) C(24) 166.5(4) 0_555 22_1 5_555 55_5 yes C(22) C(21) Fe(1) C(25) -158.7(3) 0_555 22_1 5_555 55_5 yes C(22) C(21) Fe(1) C(26) -117.1(3) 0_555 22_1 5_555 55_5 yes C(22) C(21) Fe(1) C(27) -76.0(3) 0_555 22_1 5_555 55_5 yes C(22) C(21) Fe(1) C(28) -41.9(7) 0_555 22_1 5_555 55_5 yes C(22) C(23) Fe(1) C(24) 164.5(3) 0_555 22_1 5_555 55_5 yes C(22) C(23) Fe(1) C(25) -166.7(6) 0_555 22_1 5_555 55_5 yes C(22) C(23) Fe(1) C(26) 50.5(5) 0_555 22_1 5_555 55_5 yes C(22) C(23) Fe(1) C(27) 81.7(3) 0_555 22_1 5_555 55_5 yes C(22) C(23) Fe(1) C(28) 123.5(3) 0_555 22_1 5_555 55_5 yes C(23) Fe(1) C(24) C(25) 167.1(3) 0_555 22_1 5_555 55_5 yes C(23) Fe(1) C(24) C(28) -74.7(3) 0_555 22_1 5_555 55_5 yes C(23) Fe(1) C(25) C(24) -37.6(8) 0_555 22_1 5_555 55_5 yes C(23) Fe(1) C(25) C(26) -157.0(6) 0_555 22_1 5_555 55_5 yes C(23) Fe(1) C(26) C(25) 163.4(4) 0_555 22_1 5_555 55_5 yes C(23) Fe(1) C(26) C(27) 44.1(6) 0_555 22_1 5_555 55_5 yes C(23) Fe(1) C(27) C(26) -160.6(3) 0_555 22_1 5_555 55_5 yes C(23) Fe(1) C(27) C(28) 79.9(4) 0_555 22_1 5_555 55_5 yes C(23) Fe(1) C(28) C(24) 124.0(3) 0_555 22_1 5_555 55_5 yes C(23) Fe(1) C(28) C(27) -117.8(3) 0_555 22_1 5_555 55_5 yes C(23) C(19) Fe(1) C(24) 123.2(3) 0_555 22_1 5_555 55_5 yes C(23) C(19) Fe(1) C(25) 164.2(3) 0_555 22_1 5_555 55_5 yes C(23) C(19) Fe(1) C(26) -166.1(6) 0_555 22_1 5_555 55_5 yes C(23) C(19) Fe(1) C(27) 49.0(5) 0_555 22_1 5_555 55_5 yes C(23) C(19) Fe(1) C(28) 80.9(3) 0_555 22_1 5_555 55_5 yes C(23) C(22) Fe(1) C(24) -43.4(7) 0_555 22_1 5_555 55_5 yes C(23) C(22) Fe(1) C(25) 170.1(5) 0_555 22_1 5_555 55_5 yes C(23) C(22) Fe(1) C(26) -158.1(3) 0_555 22_1 5_555 55_5 yes C(23) C(22) Fe(1) C(27) -116.7(3) 0_555 22_1 5_555 55_5 yes C(23) C(22) Fe(1) C(28) -75.1(3) 0_555 22_1 5_555 55_5 yes C(24) Fe(1) C(25) C(26) -119.4(5) 0_555 22_1 5_555 55_5 yes C(24) Fe(1) C(26) C(25) 37.8(3) 0_555 22_1 5_555 55_5 yes C(24) Fe(1) C(26) C(27) -81.6(4) 0_555 22_1 5_555 55_5 yes C(24) Fe(1) C(27) C(26) 81.3(4) 0_555 22_1 5_555 55_5 yes C(24) Fe(1) C(27) C(28) -38.2(3) 0_555 22_1 5_555 55_5 yes C(24) Fe(1) C(28) C(27) 118.2(4) 0_555 22_1 5_555 55_5 yes C(24) C(25) Fe(1) C(26) 119.4(5) 0_555 22_1 5_555 55_5 yes C(24) C(25) Fe(1) C(27) 82.1(4) 0_555 22_1 5_555 55_5 yes C(24) C(25) Fe(1) C(28) 38.2(3) 0_555 22_1 5_555 55_5 yes C(24) C(25) C(26) C(27) -0.4(6) 0_555 22_1 5_555 55_5 yes C(24) C(28) Fe(1) C(25) -38.2(3) 0_555 22_1 5_555 55_5 yes C(24) C(28) Fe(1) C(26) -81.2(3) 0_555 22_1 5_555 55_5 yes C(24) C(28) Fe(1) C(27) -118.2(4) 0_555 22_1 5_555 55_5 yes C(24) C(28) C(27) C(26) 0.4(5) 0_555 22_1 5_555 55_5 yes C(25) Fe(1) C(24) C(28) 118.2(5) 0_555 22_1 5_555 55_5 yes C(25) Fe(1) C(26) C(27) -119.4(5) 0_555 22_1 5_555 55_5 yes C(25) Fe(1) C(27) C(26) 37.1(3) 0_555 22_1 5_555 55_5 yes C(25) Fe(1) C(27) C(28) -82.4(4) 0_555 22_1 5_555 55_5 yes C(25) Fe(1) C(28) C(27) 79.9(4) 0_555 22_1 5_555 55_5 yes C(25) C(24) Fe(1) C(26) -36.9(3) 0_555 22_1 5_555 55_5 yes C(25) C(24) Fe(1) C(27) -80.0(4) 0_555 22_1 5_555 55_5 yes C(25) C(24) Fe(1) C(28) -118.2(5) 0_555 22_1 5_555 55_5 yes C(25) C(24) C(28) C(27) -0.7(5) 0_555 22_1 5_555 55_5 yes C(25) C(26) Fe(1) C(27) 119.4(5) 0_555 22_1 5_555 55_5 yes C(25) C(26) Fe(1) C(28) 81.8(4) 0_555 22_1 5_555 55_5 yes C(25) C(26) C(27) C(28) 0.0(6) 0_555 22_1 5_555 55_5 yes C(26) Fe(1) C(24) C(28) 81.3(3) 0_555 22_1 5_555 55_5 yes C(26) Fe(1) C(27) C(28) -119.5(5) 0_555 22_1 5_555 55_5 yes C(26) Fe(1) C(28) C(27) 37.0(3) 0_555 22_1 5_555 55_5 yes C(26) C(25) Fe(1) C(27) -37.3(3) 0_555 22_1 5_555 55_5 yes C(26) C(25) Fe(1) C(28) -81.3(4) 0_555 22_1 5_555 55_5 yes C(26) C(25) C(24) C(28) 0.7(5) 0_555 22_1 5_555 55_5 yes C(26) C(27) Fe(1) C(28) 119.5(5) 0_555 22_1 5_555 55_5 yes C(27) Fe(1) C(24) C(28) 38.2(3) 0_555 22_1 5_555 55_5 yes C(27) C(26) Fe(1) C(28) -37.6(3) 0_555 22_1 5_555 55_5 yes C(29) C(30) S C(31) 72.1(4) 0_555 22_1 5_555 55_5 yes C(30) S C(31) C(32) -177.3(3) 0_555 22_1 5_555 55_5 yes C(30) S C(31) C(32) -177.3(3) 0_555 22_1 5_555 55_5 yes #------------------------------------------------------------------------------ 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(1) 2.697(5) . 4_555 ? O(1) C(1) 3.443(6) . 2_645 ? O(1) C(4) 3.461(5) . 4_555 ? O(1) C(10) 3.506(6) . 2_645 ? O(1) N(1) 3.525(5) . 2_645 ? O(2) C(4) 3.186(6) . 4_555 ? O(2) N(1) 3.325(6) . 4_555 ? O(2) C(26) 3.510(6) . 2_545 ? O(2) C(22) 3.523(6) . 2_645 ? O(3) N(3) 2.695(5) . 1_445 ? O(3) C(8) 3.330(5) . . ? O(3) C(18) 3.484(5) . 1_445 ? O(3) C(7) 3.589(6) . . ? O(4) C(18) 3.195(6) . 1_445 ? O(4) N(3) 3.267(6) . 1_445 ? O(4) C(24) 3.465(6) . 1_545 ? O(4) C(14) 3.504(6) . 2_545 ? N(1) C(29) 3.401(6) . 4_554 ? N(2) C(29) 3.521(6) . 2_655 ? N(3) C(32) 3.373(6) . 1_665 ? N(3) C(17) 3.546(5) . 3_675 ? N(3) C(16) 3.594(6) . 3_675 ? N(4) C(18) 3.591(6) . 3_675 ? C(1) C(29) 3.507(7) . 2_655 ? C(1) C(4) 3.559(7) . 3_565 ? C(7) C(20) 3.423(6) . 3_565 ? C(8) C(11) 3.490(6) . 1_455 ? C(15) C(19) 3.448(6) . 3_675 ? C(15) C(17) 3.518(6) . 3_675 ? C(16) C(18) 3.498(6) . 3_675 ? C(23) C(25) 3.463(6) . 1_655 ? #------------------------------------------------------------------------------ loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_site_distance_DH _geom_hbond_site_distance_HA _geom_hbond_site_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O(1) H(25) N(1) . . 4_555 0.950 1.768 2.698(5) 165.130 no #------------------------------------------------------------------------------ #-----------END data_compound_5 _database_code_CSD 206165 #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C34 H26 Fe N2 O2 ' _chemical_formula_moiety 'C34 H26 Fe N2 O2 ' _chemical_formula_weight 550.44 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-z #------------------------------------------------------------------------------ _cell_length_a 9.320(4) _cell_length_b 10.951(5) _cell_length_c 13.149(4) _cell_angle_alpha 90 _cell_angle_beta 99.32(3) _cell_angle_gamma 90 _cell_volume 1324.3(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.9 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.3 #------------------------------------------------------------------------------ _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 572.00 _exptl_absorpt_coefficient_mu 0.604 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.758 _exptl_absorpt_correction_T_max 0.886 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 3391 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9991 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.58 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3346 _reflns_number_gt 2050 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1370 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3385 _refine_ls_number_parameters 353 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0130 _refine_diff_density_max 0.29 _refine_diff_density_min -0.42 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 0 Friedel Pairs' _refine_ls_abs_structure_Flack -0.03(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Fe Fe 0.346 0.844 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe(1) Fe -0.47218(8) -0.5328(3) -0.87286(6) 0.0490(2) Uani 1.00 1 d . . . O(1) O 0.0133(4) -0.2185(4) -0.5464(3) 0.053(1) Uani 1.00 1 d . . . O(2) O -0.1678(5) 0.1188(4) -0.5967(3) 0.047(1) Uani 1.00 1 d . . . N(1) N -0.9304(6) -0.5664(5) -0.7344(4) 0.062(2) Uani 1.00 1 d . . . N(2) N -0.7931(6) -0.4865(5) -0.5812(4) 0.054(2) Uani 1.00 1 d . . . C(1) C -0.9158(7) -0.5125(6) -0.6429(5) 0.056(2) Uani 1.00 1 d . . . C(2) C -0.6715(6) -0.5160(6) -0.6154(4) 0.047(2) Uani 1.00 1 d . . . C(3) C -0.6706(6) -0.5732(5) -0.7096(4) 0.045(2) Uani 1.00 1 d . . . C(4) C -0.8066(8) -0.5957(7) -0.7656(5) 0.058(2) Uani 1.00 1 d . . . C(5) C -0.5345(7) -0.6069(6) -0.7461(4) 0.048(2) Uani 1.00 1 d . . . C(6) C -0.3964(6) -0.5487(8) -0.7196(4) 0.055(2) Uani 1.00 1 d . . . C(7) C -0.2986(7) -0.6062(9) -0.7761(5) 0.069(2) Uani 1.00 1 d . . . C(8) C -0.3721(8) -0.6990(8) -0.8370(5) 0.072(2) Uani 1.00 1 d . . . C(9) C -0.5192(8) -0.7006(6) -0.8199(5) 0.059(2) Uani 1.00 1 d . . . C(10) C -0.628(1) -0.416(1) -0.935(1) 0.128(5) Uani 1.00 1 d . . . C(11) C -0.494(2) -0.3536(9) -0.9076(8) 0.123(5) Uani 1.00 1 d . . . C(12) C -0.395(1) -0.404(1) -0.9637(7) 0.088(3) Uani 1.00 1 d . . . C(13) C -0.465(1) -0.4958(9) -1.0239(6) 0.084(3) Uani 1.00 1 d . . . C(14) C -0.606(1) -0.502(1) -1.0077(8) 0.103(4) Uani 1.00 1 d . . . C(15) C -0.1341(6) -0.2198(5) -0.5563(4) 0.040(1) Uani 1.00 1 d . . . C(16) C -0.2113(6) -0.1426(5) -0.6271(4) 0.035(1) Uani 1.00 1 d . . . C(17) C -0.3660(6) -0.1351(5) -0.6350(4) 0.036(1) Uani 1.00 1 d . . . C(18) C -0.4524(6) -0.0543(6) -0.7021(4) 0.048(2) Uani 1.00 1 d . . . C(19) C -0.6015(6) -0.0478(9) -0.7047(5) 0.059(2) Uani 1.00 1 d . . . C(20) C -0.6697(7) -0.1197(8) -0.6396(5) 0.065(2) Uani 1.00 1 d . . . C(21) C -0.5904(7) -0.1993(7) -0.5741(5) 0.055(2) Uani 1.00 1 d . . . C(22) C -0.4377(6) -0.2108(6) -0.5690(4) 0.045(2) Uani 1.00 1 d . . . C(23) C -0.3521(7) -0.2918(6) -0.5010(4) 0.049(2) Uani 1.00 1 d . . . C(24) C -0.2058(7) -0.2967(6) -0.4945(5) 0.049(2) Uani 1.00 1 d . . . C(25) C -0.1173(6) 0.0602(6) -0.6767(4) 0.038(1) Uani 1.00 1 d . . . C(26) C -0.1348(6) -0.0641(5) -0.6941(4) 0.034(1) Uani 1.00 1 d . . . C(27) C -0.0733(6) -0.1157(6) -0.7780(4) 0.039(1) Uani 1.00 1 d . . . C(28) C -0.0782(7) -0.2430(6) -0.8000(4) 0.052(2) Uani 1.00 1 d . . . C(29) C -0.0169(8) -0.2888(8) -0.8787(5) 0.068(2) Uani 1.00 1 d . . . C(30) C 0.0532(8) -0.2140(9) -0.9403(5) 0.071(2) Uani 1.00 1 d . . . C(31) C 0.0594(7) -0.0940(8) -0.9215(5) 0.062(2) Uani 1.00 1 d . . . C(32) C -0.0014(5) -0.0394(8) -0.8402(4) 0.047(1) Uani 1.00 1 d . . . C(33) C 0.0102(7) 0.0866(7) -0.8197(5) 0.053(2) Uani 1.00 1 d . . . C(34) C -0.0481(6) 0.1349(6) -0.7411(5) 0.049(2) Uani 1.00 1 d . . . H(1) H -1.0031 -0.4900 -0.6192 0.0671 Uiso 1.00 1 c . . . H(2) H -0.5811 -0.4972 -0.5737 0.0564 Uiso 1.00 1 c . . . H(3) H -0.8118 -0.6346 -0.8306 0.0691 Uiso 1.00 1 c . . . H(4) H -0.3741 -0.4832 -0.6723 0.0661 Uiso 1.00 1 c . . . H(5) H -0.1997 -0.5842 -0.7743 0.0834 Uiso 1.00 1 c . . . H(6) H -0.3317 -0.7502 -0.8834 0.0860 Uiso 1.00 1 c . . . H(7) H -0.5934 -0.7543 -0.8514 0.0706 Uiso 1.00 1 c . . . H(8) H -0.7164 -0.3991 -0.9109 0.1537 Uiso 1.00 1 c . . . H(9) H -0.4756 -0.2878 -0.8602 0.1476 Uiso 1.00 1 c . . . H(10) H -0.2964 -0.3804 -0.9605 0.1053 Uiso 1.00 1 c . . . H(11) H -0.4222 -0.5465 -1.0695 0.1011 Uiso 1.00 1 c . . . H(12) H -0.6774 -0.5572 -1.0407 0.1233 Uiso 1.00 1 c . . . H(13) H 0.0694 -0.2703 -0.4973 0.0760 Uiso 1.00 1 c . . . H(14) H -0.4078 -0.0033 -0.7464 0.0577 Uiso 1.00 1 c . . . H(15) H -0.6577 0.0065 -0.7516 0.0712 Uiso 1.00 1 c . . . H(16) H -0.7717 -0.1131 -0.6410 0.0785 Uiso 1.00 1 c . . . H(17) H -0.6383 -0.2485 -0.5304 0.0663 Uiso 1.00 1 c . . . H(18) H -0.3984 -0.3441 -0.4587 0.0588 Uiso 1.00 1 c . . . H(19) H -0.1511 -0.3523 -0.4480 0.0586 Uiso 1.00 1 c . . . H(20) H -0.1376 0.0707 -0.5370 0.0760 Uiso 1.00 1 c . . . H(21) H -0.1251 -0.2967 -0.7590 0.0622 Uiso 1.00 1 c . . . H(22) H -0.0219 -0.3741 -0.8919 0.0811 Uiso 1.00 1 c . . . H(23) H 0.0960 -0.2475 -0.9949 0.0851 Uiso 1.00 1 c . . . H(24) H 0.1066 -0.0430 -0.9644 0.0744 Uiso 1.00 1 c . . . H(25) H 0.0592 0.1378 -0.8613 0.0631 Uiso 1.00 1 c . . . H(26) H -0.0422 0.2205 -0.7292 0.0593 Uiso 1.00 1 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) 0.0440(4) 0.0577(5) 0.0460(4) 0.0040(6) 0.0096(3) 0.0003(5) O(1) 0.038(2) 0.058(3) 0.062(2) 0.006(2) 0.008(2) 0.019(2) O(2) 0.056(3) 0.038(2) 0.047(2) -0.002(2) 0.014(2) -0.004(2) N(1) 0.052(3) 0.069(4) 0.068(3) -0.013(3) 0.018(3) 0.001(3) N(2) 0.071(4) 0.043(3) 0.056(3) 0.002(2) 0.030(3) 0.007(2) C(1) 0.054(3) 0.045(4) 0.073(4) -0.001(3) 0.023(3) 0.006(3) C(2) 0.059(3) 0.043(4) 0.039(3) -0.003(3) 0.012(2) 0.007(3) C(3) 0.051(3) 0.041(3) 0.044(3) -0.001(3) 0.014(3) 0.004(2) C(4) 0.063(4) 0.054(4) 0.058(4) -0.013(3) 0.014(3) -0.003(3) C(5) 0.056(4) 0.048(4) 0.039(3) 0.005(3) 0.006(3) 0.002(3) C(6) 0.042(3) 0.071(5) 0.049(3) 0.002(4) -0.000(2) -0.003(4) C(7) 0.045(3) 0.097(6) 0.065(4) 0.016(4) 0.001(3) -0.001(4) C(8) 0.076(5) 0.080(5) 0.059(4) 0.033(4) 0.011(4) -0.003(4) C(9) 0.075(4) 0.043(4) 0.060(4) 0.008(4) 0.016(3) -0.004(3) C(10) 0.094(7) 0.17(1) 0.14(1) 0.079(8) 0.071(7) 0.11(1) C(11) 0.22(2) 0.066(6) 0.088(6) 0.031(8) 0.051(9) 0.026(5) C(12) 0.086(6) 0.100(7) 0.078(5) -0.021(6) 0.016(5) 0.021(5) C(13) 0.095(6) 0.105(8) 0.054(4) -0.006(5) 0.017(4) 0.010(4) C(14) 0.076(5) 0.13(1) 0.087(6) -0.015(7) -0.018(5) 0.047(7) C(15) 0.046(3) 0.034(3) 0.040(3) 0.001(3) 0.009(2) 0.001(2) C(16) 0.038(3) 0.033(3) 0.034(3) -0.008(2) 0.006(2) -0.001(2) C(17) 0.039(3) 0.036(3) 0.036(3) -0.004(2) 0.010(2) -0.006(2) C(18) 0.045(3) 0.059(5) 0.038(3) -0.009(3) 0.003(2) 0.001(3) C(19) 0.036(3) 0.079(5) 0.061(3) 0.007(4) 0.000(2) 0.004(4) C(20) 0.035(3) 0.088(6) 0.075(5) -0.014(4) 0.014(3) -0.008(4) C(21) 0.043(3) 0.059(4) 0.068(4) -0.013(3) 0.022(3) -0.001(3) C(22) 0.042(3) 0.050(3) 0.044(3) -0.012(3) 0.010(2) -0.008(3) C(23) 0.060(4) 0.044(3) 0.045(3) -0.018(3) 0.016(3) 0.003(3) C(24) 0.060(4) 0.038(3) 0.050(3) -0.001(3) 0.013(3) 0.008(3) C(25) 0.030(3) 0.040(3) 0.042(3) -0.003(2) 0.001(2) 0.007(3) C(26) 0.030(2) 0.037(3) 0.035(3) -0.001(2) 0.002(2) 0.004(2) C(27) 0.034(3) 0.048(3) 0.036(3) 0.001(2) 0.007(2) 0.004(2) C(28) 0.051(3) 0.056(4) 0.049(3) -0.002(3) 0.008(3) -0.009(3) C(29) 0.067(4) 0.077(5) 0.059(4) 0.009(4) 0.011(4) -0.021(4) C(30) 0.059(4) 0.109(7) 0.050(4) 0.013(5) 0.023(3) -0.008(4) C(31) 0.052(4) 0.088(6) 0.049(3) 0.006(4) 0.018(3) 0.010(4) C(32) 0.035(2) 0.068(4) 0.038(2) 0.000(4) 0.005(2) 0.006(4) C(33) 0.048(3) 0.060(4) 0.051(3) -0.006(3) 0.012(3) 0.018(3) C(34) 0.045(3) 0.040(3) 0.063(4) -0.009(3) 0.007(3) 0.016(3) #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Fe(1) C(5) 2.022(6) yes . . Fe(1) C(6) 2.032(5) yes . . Fe(1) C(7) 2.053(7) yes . . Fe(1) C(8) 2.064(9) yes . . Fe(1) C(9) 2.037(7) yes . . Fe(1) C(10) 2.01(1) yes . . Fe(1) C(11) 2.02(1) yes . . Fe(1) C(12) 2.05(1) yes . . Fe(1) C(13) 2.039(8) yes . . Fe(1) C(14) 2.02(1) yes . . O(1) C(15) 1.359(7) yes . . O(2) C(25) 1.378(7) yes . . N(1) C(1) 1.327(9) yes . . N(1) C(4) 1.325(9) yes . . N(2) C(1) 1.321(8) yes . . N(2) C(2) 1.325(8) yes . . C(2) C(3) 1.389(8) yes . . C(3) C(4) 1.382(8) yes . . C(3) C(5) 1.474(9) yes . . C(5) C(6) 1.428(9) yes . . C(5) C(9) 1.436(9) yes . . C(6) C(7) 1.41(1) yes . . C(7) C(8) 1.40(1) yes . . C(8) C(9) 1.42(1) yes . . C(10) C(11) 1.42(2) yes . . C(10) C(14) 1.38(2) yes . . C(11) C(12) 1.38(2) yes . . C(12) C(13) 1.38(1) yes . . C(13) C(14) 1.37(1) yes . . C(15) C(16) 1.372(7) yes . . C(15) C(24) 1.412(9) yes . . C(16) C(17) 1.431(8) yes . . C(16) C(26) 1.491(8) yes . . C(17) C(18) 1.407(8) yes . . C(17) C(22) 1.440(8) yes . . C(18) C(19) 1.386(8) yes . . C(19) C(20) 1.39(1) yes . . C(20) C(21) 1.36(1) yes . . C(21) C(22) 1.420(8) yes . . C(22) C(23) 1.411(8) yes . . C(23) C(24) 1.353(9) yes . . C(25) C(26) 1.386(8) yes . . C(25) C(34) 1.408(9) yes . . C(26) C(27) 1.438(8) yes . . C(27) C(28) 1.423(9) yes . . C(27) C(32) 1.413(9) yes . . C(28) C(29) 1.36(1) yes . . C(29) C(30) 1.39(1) yes . . C(30) C(31) 1.34(1) yes . . C(31) C(32) 1.421(9) yes . . C(32) C(33) 1.41(1) yes . . C(33) C(34) 1.35(1) yes . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C(5) Fe(1) C(6) 41.3(2) yes . . . C(5) Fe(1) C(7) 68.6(3) yes . . . C(5) Fe(1) C(8) 68.8(3) yes . . . C(5) Fe(1) C(9) 41.4(3) yes . . . C(5) Fe(1) C(10) 107.9(4) yes . . . C(5) Fe(1) C(11) 123.0(4) yes . . . C(5) Fe(1) C(12) 158.5(3) yes . . . C(5) Fe(1) C(13) 160.4(3) yes . . . C(5) Fe(1) C(14) 124.8(4) yes . . . C(6) Fe(1) C(7) 40.5(3) yes . . . C(6) Fe(1) C(8) 68.1(3) yes . . . C(6) Fe(1) C(9) 69.1(3) yes . . . C(6) Fe(1) C(10) 124.9(5) yes . . . C(6) Fe(1) C(11) 108.3(4) yes . . . C(6) Fe(1) C(12) 122.6(3) yes . . . C(6) Fe(1) C(13) 157.2(3) yes . . . C(6) Fe(1) C(14) 161.6(4) yes . . . C(7) Fe(1) C(8) 39.8(3) yes . . . C(7) Fe(1) C(9) 68.1(3) yes . . . C(7) Fe(1) C(10) 161.3(5) yes . . . C(7) Fe(1) C(11) 124.1(5) yes . . . C(7) Fe(1) C(12) 108.4(3) yes . . . C(7) Fe(1) C(13) 122.3(3) yes . . . C(7) Fe(1) C(14) 156.9(4) yes . . . C(8) Fe(1) C(9) 40.6(3) yes . . . C(8) Fe(1) C(10) 157.7(5) yes . . . C(8) Fe(1) C(11) 159.1(5) yes . . . C(8) Fe(1) C(12) 123.4(4) yes . . . C(8) Fe(1) C(13) 108.2(3) yes . . . C(8) Fe(1) C(14) 122.6(4) yes . . . C(9) Fe(1) C(10) 122.2(5) yes . . . C(9) Fe(1) C(11) 159.3(5) yes . . . C(9) Fe(1) C(12) 159.0(4) yes . . . C(9) Fe(1) C(13) 123.7(3) yes . . . C(9) Fe(1) C(14) 108.3(4) yes . . . C(10) Fe(1) C(11) 41.3(6) yes . . . C(10) Fe(1) C(12) 67.8(5) yes . . . C(10) Fe(1) C(13) 67.2(5) yes . . . C(10) Fe(1) C(14) 40.0(5) yes . . . C(11) Fe(1) C(12) 39.8(5) yes . . . C(11) Fe(1) C(13) 66.7(4) yes . . . C(11) Fe(1) C(14) 67.3(5) yes . . . C(12) Fe(1) C(13) 39.3(4) yes . . . C(12) Fe(1) C(14) 66.4(4) yes . . . C(13) Fe(1) C(14) 39.3(4) yes . . . C(1) N(1) C(4) 115.0(5) yes . . . C(1) N(2) C(2) 116.2(5) yes . . . N(1) C(1) N(2) 127.1(6) yes . . . C(3) C(2) N(2) 122.8(5) yes . . . C(4) C(3) C(5) 123.1(5) yes . . . C(4) C(3) C(2) 114.7(6) yes . . . C(5) C(3) C(2) 122.2(5) yes . . . N(1) C(4) C(3) 124.2(6) yes . . . C(6) C(5) C(9) 107.4(6) yes . . . C(6) C(5) Fe(1) 69.8(4) yes . . . C(6) C(5) C(3) 126.7(6) yes . . . C(9) C(5) Fe(1) 69.9(4) yes . . . C(9) C(5) C(3) 125.8(6) yes . . . Fe(1) C(5) C(3) 123.0(4) yes . . . C(7) C(6) Fe(1) 70.6(4) yes . . . C(5) C(6) C(7) 107.8(6) yes . . . C(5) C(6) Fe(1) 69.0(3) yes . . . C(8) C(7) Fe(1) 70.5(4) yes . . . C(6) C(7) C(8) 109.1(6) yes . . . C(6) C(7) Fe(1) 69.0(4) yes . . . C(9) C(8) Fe(1) 68.7(4) yes . . . C(7) C(8) C(9) 108.2(7) yes . . . C(7) C(8) Fe(1) 69.7(5) yes . . . C(5) C(9) Fe(1) 68.7(4) yes . . . C(5) C(9) C(8) 107.6(6) yes . . . C(8) C(9) Fe(1) 70.7(4) yes . . . C(11) C(10) C(14) 106(1) yes . . . C(11) C(10) Fe(1) 69.8(7) yes . . . C(14) C(10) Fe(1) 70.7(7) yes . . . C(12) C(11) Fe(1) 71.4(6) yes . . . C(10) C(11) C(12) 107(1) yes . . . C(10) C(11) Fe(1) 68.9(8) yes . . . C(13) C(12) Fe(1) 69.9(6) yes . . . C(11) C(12) C(13) 107.8(9) yes . . . C(11) C(12) Fe(1) 68.8(6) yes . . . C(14) C(13) Fe(1) 69.8(5) yes . . . C(12) C(13) C(14) 108.9(9) yes . . . C(12) C(13) Fe(1) 70.8(5) yes . . . C(10) C(14) Fe(1) 69.3(7) yes . . . C(10) C(14) C(13) 109(1) yes . . . C(13) C(14) Fe(1) 70.9(5) yes . . . C(16) C(15) C(24) 120.9(5) yes . . . C(16) C(15) O(1) 118.0(5) yes . . . C(24) C(15) O(1) 121.1(5) yes . . . C(17) C(16) C(26) 119.8(4) yes . . . C(17) C(16) C(15) 119.7(5) yes . . . C(26) C(16) C(15) 120.5(5) yes . . . C(18) C(17) C(22) 117.8(5) yes . . . C(18) C(17) C(16) 123.3(5) yes . . . C(22) C(17) C(16) 118.9(5) yes . . . C(19) C(18) C(17) 121.1(6) yes . . . C(20) C(19) C(18) 120.8(6) yes . . . C(21) C(20) C(19) 119.9(6) yes . . . C(22) C(21) C(20) 121.7(6) yes . . . C(23) C(22) C(17) 118.3(5) yes . . . C(23) C(22) C(21) 123.0(6) yes . . . C(17) C(22) C(21) 118.7(5) yes . . . C(24) C(23) C(22) 121.7(6) yes . . . C(15) C(24) C(23) 120.3(5) yes . . . C(26) C(25) C(34) 121.7(5) yes . . . C(26) C(25) O(2) 122.5(5) yes . . . C(34) C(25) O(2) 115.8(5) yes . . . C(27) C(26) C(16) 121.0(5) yes . . . C(27) C(26) C(25) 117.5(5) yes . . . C(16) C(26) C(25) 121.6(5) yes . . . C(28) C(27) C(32) 117.6(6) yes . . . C(28) C(27) C(26) 122.5(5) yes . . . C(32) C(27) C(26) 119.8(6) yes . . . C(29) C(28) C(27) 120.9(6) yes . . . C(30) C(29) C(28) 121.6(8) yes . . . C(31) C(30) C(29) 118.9(7) yes . . . C(32) C(31) C(30) 122.8(7) yes . . . C(33) C(32) C(27) 119.9(5) yes . . . C(33) C(32) C(31) 122.0(6) yes . . . C(27) C(32) C(31) 118.2(7) yes . . . C(34) C(33) C(32) 120.2(6) yes . . . C(25) C(34) C(33) 120.9(6) yes . . . 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 _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(6) Fe(1) C(5) C(3) 121.4(6) yes . . . . C(6) Fe(1) C(5) C(9) -118.4(5) yes . . . . C(7) Fe(1) C(5) C(3) 159.0(5) yes . . . . C(7) Fe(1) C(5) C(6) 37.7(4) yes . . . . C(7) Fe(1) C(5) C(9) -80.7(4) yes . . . . C(8) Fe(1) C(5) C(3) -158.1(5) yes . . . . C(8) Fe(1) C(5) C(6) 80.5(4) yes . . . . C(8) Fe(1) C(5) C(9) -37.8(3) yes . . . . C(9) Fe(1) C(5) C(3) -120.3(6) yes . . . . C(9) Fe(1) C(5) C(6) 118.4(5) yes . . . . C(10) Fe(1) C(5) C(3) -1.5(5) yes . . . . C(10) Fe(1) C(5) C(6) -122.9(4) yes . . . . C(10) Fe(1) C(5) C(9) 118.8(4) yes . . . . C(11) Fe(1) C(5) C(3) 41.4(5) yes . . . . C(11) Fe(1) C(5) C(6) -80.0(4) yes . . . . C(11) Fe(1) C(5) C(9) 161.7(3) yes . . . . C(12) Fe(1) C(5) C(3) 73.2(7) yes . . . . C(12) Fe(1) C(5) C(6) -48.2(7) yes . . . . C(12) Fe(1) C(5) C(9) -166.5(4) yes . . . . C(13) Fe(1) C(5) C(3) -73.4(9) yes . . . . C(13) Fe(1) C(5) C(6) 165.2(6) yes . . . . C(13) Fe(1) C(5) C(9) 46.9(8) yes . . . . C(14) Fe(1) C(5) C(3) -42.4(6) yes . . . . C(14) Fe(1) C(5) C(6) -163.8(4) yes . . . . C(14) Fe(1) C(5) C(9) 77.9(4) yes . . . . C(5) Fe(1) C(6) C(7) 118.8(6) yes . . . . C(7) Fe(1) C(6) C(5) -118.8(6) yes . . . . C(8) Fe(1) C(6) C(5) -82.3(4) yes . . . . C(8) Fe(1) C(6) C(7) 36.5(4) yes . . . . C(9) Fe(1) C(6) C(5) -38.6(3) yes . . . . C(9) Fe(1) C(6) C(7) 80.3(5) yes . . . . C(10) Fe(1) C(6) C(5) 76.9(5) yes . . . . C(10) Fe(1) C(6) C(7) -164.3(4) yes . . . . C(11) Fe(1) C(6) C(5) 119.6(4) yes . . . . C(11) Fe(1) C(6) C(7) -121.6(4) yes . . . . C(12) Fe(1) C(6) C(5) 161.1(3) yes . . . . C(12) Fe(1) C(6) C(7) -80.1(5) yes . . . . C(13) Fe(1) C(6) C(5) -167.2(6) yes . . . . C(13) Fe(1) C(6) C(7) -48(1) yes . . . . C(14) Fe(1) C(6) C(5) 46(1) yes . . . . C(14) Fe(1) C(6) C(7) 165.4(8) yes . . . . C(5) Fe(1) C(7) C(6) -38.4(4) yes . . . . C(5) Fe(1) C(7) C(8) 82.1(4) yes . . . . C(6) Fe(1) C(7) C(8) 120.5(6) yes . . . . C(8) Fe(1) C(7) C(6) -120.5(6) yes . . . . C(9) Fe(1) C(7) C(6) -83.1(4) yes . . . . C(9) Fe(1) C(7) C(8) 37.4(4) yes . . . . C(10) Fe(1) C(7) C(6) 44(1) yes . . . . C(10) Fe(1) C(7) C(8) 164.5(6) yes . . . . C(11) Fe(1) C(7) C(6) 77.8(5) yes . . . . C(11) Fe(1) C(7) C(8) -161.7(4) yes . . . . C(12) Fe(1) C(7) C(6) 119.0(4) yes . . . . C(12) Fe(1) C(7) C(8) -120.5(4) yes . . . . C(13) Fe(1) C(7) C(6) 160.0(4) yes . . . . C(13) Fe(1) C(7) C(8) -79.5(5) yes . . . . C(14) Fe(1) C(7) C(6) -168.3(6) yes . . . . C(14) Fe(1) C(7) C(8) -47.8(9) yes . . . . C(5) Fe(1) C(8) C(7) -81.6(4) yes . . . . C(5) Fe(1) C(8) C(9) 38.5(3) yes . . . . C(6) Fe(1) C(8) C(9) 83.1(4) yes . . . . C(7) Fe(1) C(8) C(9) 120.1(5) yes . . . . C(9) Fe(1) C(8) C(7) -120.1(5) yes . . . . C(10) Fe(1) C(8) C(7) -167.0(4) yes . . . . C(10) Fe(1) C(8) C(9) -46.9(7) yes . . . . C(11) Fe(1) C(8) C(7) 46.9(8) yes . . . . C(11) Fe(1) C(8) C(9) 167.0(4) yes . . . . C(12) Fe(1) C(8) C(7) 78.4(5) yes . . . . C(12) Fe(1) C(8) C(9) -161.5(3) yes . . . . C(13) Fe(1) C(8) C(7) 119.0(4) yes . . . . C(13) Fe(1) C(8) C(9) -120.9(3) yes . . . . C(14) Fe(1) C(8) C(7) 159.9(4) yes . . . . C(14) Fe(1) C(8) C(9) -80.0(4) yes . . . . C(5) Fe(1) C(9) C(8) -118.7(5) yes . . . . C(6) Fe(1) C(9) C(5) 38.4(3) yes . . . . C(6) Fe(1) C(9) C(8) -80.3(4) yes . . . . C(7) Fe(1) C(9) C(5) 82.0(3) yes . . . . C(7) Fe(1) C(9) C(8) -36.7(3) yes . . . . C(8) Fe(1) C(9) C(5) 118.7(4) yes . . . . C(10) Fe(1) C(9) C(5) -80.5(4) yes . . . . C(10) Fe(1) C(9) C(8) 160.9(3) yes . . . . C(11) Fe(1) C(9) C(5) -48.2(7) yes . . . . C(11) Fe(1) C(9) C(8) -166.9(4) yes . . . . C(12) Fe(1) C(9) C(5) 166.2(4) yes . . . . C(12) Fe(1) C(9) C(8) 47.6(7) yes . . . . C(13) Fe(1) C(9) C(5) -162.9(3) yes . . . . C(13) Fe(1) C(9) C(8) 78.4(4) yes . . . . C(14) Fe(1) C(9) C(5) -122.3(3) yes . . . . C(14) Fe(1) C(9) C(8) 119.1(4) yes . . . . C(5) Fe(1) C(10) C(11) 120.1(7) yes . . . . C(5) Fe(1) C(10) C(14) -123.2(7) yes . . . . C(6) Fe(1) C(10) C(11) 77.6(8) yes . . . . C(6) Fe(1) C(10) C(14) -165.7(6) yes . . . . C(7) Fe(1) C(10) C(11) 44(1) yes . . . . C(7) Fe(1) C(10) C(14) 161.0(9) yes . . . . C(8) Fe(1) C(10) C(11) -162.5(8) yes . . . . C(8) Fe(1) C(10) C(14) -45(1) yes . . . . C(9) Fe(1) C(10) C(11) 163.4(6) yes . . . . C(9) Fe(1) C(10) C(14) -80.0(8) yes . . . . C(11) Fe(1) C(10) C(14) 116.7(9) yes . . . . C(12) Fe(1) C(10) C(11) -37.5(6) yes . . . . C(12) Fe(1) C(10) C(14) 79.2(7) yes . . . . C(13) Fe(1) C(10) C(11) -80.2(7) yes . . . . C(13) Fe(1) C(10) C(14) 36.5(6) yes . . . . C(14) Fe(1) C(10) C(11) -116(1) yes . . . . C(5) Fe(1) C(11) C(10) -79.3(7) yes . . . . C(5) Fe(1) C(11) C(12) 162.4(4) yes . . . . C(6) Fe(1) C(11) C(10) -122.4(7) yes . . . . C(6) Fe(1) C(11) C(12) 119.3(5) yes . . . . C(7) Fe(1) C(11) C(10) -164.3(6) yes . . . . C(7) Fe(1) C(11) C(12) 77.3(6) yes . . . . C(8) Fe(1) C(11) C(10) 161.3(8) yes . . . . C(8) Fe(1) C(11) C(12) 42(1) yes . . . . C(9) Fe(1) C(11) C(10) -43(1) yes . . . . C(9) Fe(1) C(11) C(12) -161.5(6) yes . . . . C(10) Fe(1) C(11) C(12) -118.3(7) yes . . . . C(12) Fe(1) C(11) C(10) 118.3(8) yes . . . . C(13) Fe(1) C(11) C(10) 81.4(7) yes . . . . C(13) Fe(1) C(11) C(12) -36.9(5) yes . . . . C(14) Fe(1) C(11) C(10) 38.5(7) yes . . . . C(14) Fe(1) C(11) C(12) -79.8(5) yes . . . . C(5) Fe(1) C(12) C(11) -43(1) yes . . . . C(5) Fe(1) C(12) C(13) -163.1(6) yes . . . . C(6) Fe(1) C(12) C(11) -79.3(7) yes . . . . C(6) Fe(1) C(12) C(13) 161.3(5) yes . . . . C(7) Fe(1) C(12) C(11) -121.7(6) yes . . . . C(7) Fe(1) C(12) C(13) 118.9(5) yes . . . . C(8) Fe(1) C(12) C(11) -163.1(6) yes . . . . C(8) Fe(1) C(12) C(13) 77.6(6) yes . . . . C(9) Fe(1) C(12) C(11) 161.8(7) yes . . . . C(9) Fe(1) C(12) C(13) 42(1) yes . . . . C(10) Fe(1) C(12) C(11) 38.8(6) yes . . . . C(10) Fe(1) C(12) C(13) -80.6(5) yes . . . . C(11) Fe(1) C(12) C(13) -119.4(7) yes . . . . C(13) Fe(1) C(12) C(11) 119.4(8) yes . . . . C(14) Fe(1) C(12) C(11) 82.4(7) yes . . . . C(14) Fe(1) C(12) C(13) -37.0(5) yes . . . . C(5) Fe(1) C(13) C(12) 161.4(8) yes . . . . C(5) Fe(1) C(13) C(14) 41(1) yes . . . . C(6) Fe(1) C(13) C(12) -44(1) yes . . . . C(6) Fe(1) C(13) C(14) -163.9(8) yes . . . . C(7) Fe(1) C(13) C(12) -79.4(6) yes . . . . C(7) Fe(1) C(13) C(14) 161.0(6) yes . . . . C(8) Fe(1) C(13) C(12) -120.9(5) yes . . . . C(8) Fe(1) C(13) C(14) 119.5(6) yes . . . . C(9) Fe(1) C(13) C(12) -163.1(5) yes . . . . C(9) Fe(1) C(13) C(14) 77.3(7) yes . . . . C(10) Fe(1) C(13) C(12) 82.4(6) yes . . . . C(10) Fe(1) C(13) C(14) -37.2(6) yes . . . . C(11) Fe(1) C(13) C(12) 37.4(5) yes . . . . C(11) Fe(1) C(13) C(14) -82.2(6) yes . . . . C(12) Fe(1) C(13) C(14) -119.6(8) yes . . . . C(14) Fe(1) C(13) C(12) 119.6(7) yes . . . . C(5) Fe(1) C(14) C(10) 75.7(8) yes . . . . C(5) Fe(1) C(14) C(13) -164.2(5) yes . . . . C(6) Fe(1) C(14) C(10) 40(1) yes . . . . C(6) Fe(1) C(14) C(13) 160.1(9) yes . . . . C(7) Fe(1) C(14) C(10) -164.6(8) yes . . . . C(7) Fe(1) C(14) C(13) -44(1) yes . . . . C(8) Fe(1) C(14) C(10) 161.2(7) yes . . . . C(8) Fe(1) C(14) C(13) -78.8(7) yes . . . . C(9) Fe(1) C(14) C(10) 118.7(7) yes . . . . C(9) Fe(1) C(14) C(13) -121.2(6) yes . . . . C(10) Fe(1) C(14) C(13) 120.1(8) yes . . . . C(11) Fe(1) C(14) C(10) -39.7(7) yes . . . . C(11) Fe(1) C(14) C(13) 80.4(6) yes . . . . C(12) Fe(1) C(14) C(10) -83.1(8) yes . . . . C(12) Fe(1) C(14) C(13) 37.0(5) yes . . . . C(13) Fe(1) C(14) C(10) -120(1) yes . . . . C(4) N(1) C(1) N(2) 0(1) yes . . . . C(1) N(1) C(4) C(3) 0(1) yes . . . . C(2) N(2) C(1) N(1) 1(1) yes . . . . C(1) N(2) C(2) C(3) -1.3(9) yes . . . . N(2) C(2) C(3) C(4) 0.8(9) yes . . . . N(2) C(2) C(3) C(5) -179.2(6) yes . . . . C(2) C(3) C(4) N(1) 0(1) yes . . . . C(5) C(3) C(4) N(1) 179(719) yes . . . . C(2) C(3) C(5) Fe(1) -115.7(5) yes . . . . C(2) C(3) C(5) C(6) -27.4(9) yes . . . . C(2) C(3) C(5) C(9) 156.5(6) yes . . . . C(4) C(3) C(5) Fe(1) 64.3(7) yes . . . . C(4) C(3) C(5) C(6) 152.6(6) yes . . . . C(4) C(3) C(5) C(9) -23.5(9) yes . . . . Fe(1) C(5) C(6) C(7) -60.2(5) yes . . . . C(3) C(5) C(6) Fe(1) -116.7(6) yes . . . . C(3) C(5) C(6) C(7) -176.9(6) yes . . . . C(9) C(5) C(6) Fe(1) 60.0(4) yes . . . . C(9) C(5) C(6) C(7) -0.2(7) yes . . . . Fe(1) C(5) C(9) C(8) 60.3(5) yes . . . . C(3) C(5) C(9) Fe(1) 116.9(6) yes . . . . C(3) C(5) C(9) C(8) 177.2(6) yes . . . . C(6) C(5) C(9) Fe(1) -59.9(4) yes . . . . C(6) C(5) C(9) C(8) 0.4(7) yes . . . . Fe(1) C(6) C(7) C(8) -59.2(6) yes . . . . C(5) C(6) C(7) Fe(1) 59.2(5) yes . . . . C(5) C(6) C(7) C(8) -0.1(9) yes . . . . Fe(1) C(7) C(8) C(9) -58.0(6) yes . . . . C(6) C(7) C(8) Fe(1) 58.3(6) yes . . . . C(6) C(7) C(8) C(9) 0.3(9) yes . . . . Fe(1) C(8) C(9) C(5) -59.0(5) yes . . . . C(7) C(8) C(9) Fe(1) 58.6(5) yes . . . . C(7) C(8) C(9) C(5) -0.4(8) yes . . . . Fe(1) C(10) C(11) C(12) 61.2(9) yes . . . . C(14) C(10) C(11) Fe(1) -61(1) yes . . . . C(14) C(10) C(11) C(12) 0(1) yes . . . . Fe(1) C(10) C(14) C(13) -59.9(9) yes . . . . C(11) C(10) C(14) Fe(1) 61.0(9) yes . . . . C(11) C(10) C(14) C(13) 1(1) yes . . . . Fe(1) C(11) C(12) C(13) 59.2(8) yes . . . . C(10) C(11) C(12) Fe(1) -59.6(7) yes . . . . C(10) C(11) C(12) C(13) 0(1) yes . . . . Fe(1) C(12) C(13) C(14) 59.6(8) yes . . . . C(11) C(12) C(13) Fe(1) -58.5(7) yes . . . . C(11) C(12) C(13) C(14) 1(1) yes . . . . Fe(1) C(13) C(14) C(10) 58.9(9) yes . . . . C(12) C(13) C(14) Fe(1) -60.2(6) yes . . . . C(12) C(13) C(14) C(10) -1(1) yes . . . . O(1) C(15) C(16) C(17) -175.7(5) yes . . . . O(1) C(15) C(16) C(26) 2.7(8) yes . . . . C(24) C(15) C(16) C(17) 3.2(8) yes . . . . C(24) C(15) C(16) C(26) -178.4(5) yes . . . . O(1) C(15) C(24) C(23) 176.1(6) yes . . . . C(16) C(15) C(24) C(23) -2.8(9) yes . . . . C(15) C(16) C(17) C(18) 177.0(5) yes . . . . C(15) C(16) C(17) C(22) -1.0(8) yes . . . . C(26) C(16) C(17) C(18) -1.5(8) yes . . . . C(26) C(16) C(17) C(22) -179.5(5) yes . . . . C(15) C(16) C(26) C(25) -105.3(6) yes . . . . C(15) C(16) C(26) C(27) 73.3(7) yes . . . . C(17) C(16) C(26) C(25) 73.2(6) yes . . . . C(17) C(16) C(26) C(27) -108.3(6) yes . . . . C(16) C(17) C(18) C(19) -178.1(6) yes . . . . C(22) C(17) C(18) C(19) -0.0(9) yes . . . . C(16) C(17) C(22) C(21) 177.4(5) yes . . . . C(16) C(17) C(22) C(23) -1.6(8) yes . . . . C(18) C(17) C(22) C(21) -0.7(8) yes . . . . C(18) C(17) C(22) C(23) -179.7(5) yes . . . . C(17) C(18) C(19) C(20) 1(1) yes . . . . C(18) C(19) C(20) C(21) -1(1) yes . . . . C(19) C(20) C(21) C(22) 0(1) yes . . . . C(20) C(21) C(22) C(17) 0.5(9) yes . . . . C(20) C(21) C(22) C(23) 179.3(6) yes . . . . C(17) C(22) C(23) C(24) 2.0(9) yes . . . . C(21) C(22) C(23) C(24) -176.9(6) yes . . . . C(22) C(23) C(24) C(15) 0.1(9) yes . . . . O(2) C(25) C(26) C(16) 0.6(8) yes . . . . O(2) C(25) C(26) C(27) -178.0(5) yes . . . . C(34) C(25) C(26) C(16) -178.5(5) yes . . . . C(34) C(25) C(26) C(27) 2.9(7) yes . . . . O(2) C(25) C(34) C(33) 177.6(5) yes . . . . C(26) C(25) C(34) C(33) -3.2(8) yes . . . . C(16) C(26) C(27) C(28) -1.8(7) yes . . . . C(16) C(26) C(27) C(32) 179(881) yes . . . . C(25) C(26) C(27) C(28) 176.8(5) yes . . . . C(25) C(26) C(27) C(32) -1.4(7) yes . . . . C(26) C(27) C(28) C(29) -178.9(5) yes . . . . C(32) C(27) C(28) C(29) -0.6(8) yes . . . . C(26) C(27) C(32) C(31) 179.2(5) yes . . . . C(26) C(27) C(32) C(33) 0.2(7) yes . . . . C(28) C(27) C(32) C(31) 0.9(7) yes . . . . C(28) C(27) C(32) C(33) -178.1(5) yes . . . . C(27) C(28) C(29) C(30) 0(1) yes . . . . C(28) C(29) C(30) C(31) 0(1) yes . . . . C(29) C(30) C(31) C(32) 0(1) yes . . . . C(30) C(31) C(32) C(27) -1.0(8) yes . . . . C(30) C(31) C(32) C(33) 178.0(6) yes . . . . C(27) C(32) C(33) C(34) -0.5(8) yes . . . . C(31) C(32) C(33) C(34) -179.4(5) yes . . . . C(32) C(33) C(34) C(25) 1.9(9) yes . . . . #------------------------------------------------------------------------------ #-----------END data_compound_6 _database_code_CSD 206166 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C23 H18 Fe N2 O6 ' _chemical_formula_moiety ? _chemical_formula_weight 474.25 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 11.037(2) _cell_length_b 12.652(4) _cell_length_c 7.518(5) _cell_angle_alpha 104.42(3) _cell_angle_beta 96.41(3) _cell_angle_gamma 88.21(3) _cell_volume 1010.4(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.3 _cell_measurement_theta_max 14.9 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.791 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.783 _exptl_absorpt_correction_T_max 0.999 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 4892 _diffrn_reflns_av_R_equivalents 0.014 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 1.0011 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.0011 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% 0.69 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4651 _reflns_number_gt 2935 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1119 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2935 _refine_ls_number_parameters 289 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.07500(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0006 _refine_diff_density_max 0.41 _refine_diff_density_min -0.30 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Fe Fe 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe -1.11764(4) -0.19347(4) -0.33750(7) 0.0397(1) Uani 1.00 d . . . O(1) O -0.4965(2) -0.6354(2) -0.3736(3) 0.0449(6) Uani 1.00 d . . . O(2) O -0.3516(2) -0.5129(2) -0.3439(3) 0.0487(7) Uani 1.00 d . . . O(3) O -0.4091(2) -0.1467(2) 0.0494(4) 0.0559(7) Uani 1.00 d . . . O(4) O -0.5670(3) -0.1070(2) 0.2107(4) 0.0658(8) Uani 1.00 d . . . O(5) O -0.8950(2) -0.3867(2) 0.0994(3) 0.0488(7) Uani 1.00 d . . . O(6) O -0.8862(2) -0.5371(2) -0.1282(4) 0.0539(7) Uani 1.00 d . . . N(1) N -0.6562(2) -0.2184(2) -0.4474(4) 0.0424(8) Uani 1.00 d . . . N(2) N -0.6821(2) -0.0500(2) -0.2347(4) 0.0422(7) Uani 1.00 d . . . C(1) C -0.6220(3) -0.1177(3) -0.3596(5) 0.0413(9) Uani 1.00 d . . . C(2) C -0.7856(3) -0.0865(3) -0.1968(5) 0.0430(9) Uani 1.00 d . . . C(3) C -0.8320(3) -0.1891(2) -0.2832(4) 0.0333(8) Uani 1.00 d . . . C(4) C -0.7611(3) -0.2534(2) -0.4087(5) 0.0396(9) Uani 1.00 d . . . C(5) C -0.9460(3) -0.2286(3) -0.2385(5) 0.0390(9) Uani 1.00 d . . . C(6) C -1.0146(3) -0.1763(3) -0.0897(5) 0.051(1) Uani 1.00 d . . . C(7) C -1.1188(4) -0.2412(4) -0.0981(6) 0.065(1) Uani 1.00 d . . . C(8) C -1.1143(4) -0.3333(3) -0.2484(7) 0.064(1) Uani 1.00 d . . . C(9) C -1.0094(3) -0.3263(3) -0.3362(5) 0.050(1) Uani 1.00 d . . . C(10) C -1.1108(4) -0.1142(4) -0.5394(7) 0.074(2) Uani 1.00 d . . . C(11) C -1.1594(5) -0.0453(3) -0.3882(7) 0.074(1) Uani 1.00 d . . . C(12) C -1.2645(4) -0.0953(4) -0.3608(7) 0.077(2) Uani 1.00 d . . . C(13) C -1.2801(4) -0.1923(4) -0.4934(8) 0.080(2) Uani 1.00 d . . . C(14) C -1.1852(5) -0.2061(4) -0.6037(6) 0.077(2) Uani 1.00 d . . . C(15) C -0.4911(3) -0.3529(2) -0.1202(4) 0.0332(8) Uani 1.00 d . . . C(16) C -0.5614(3) -0.2795(2) -0.0041(4) 0.0327(8) Uani 1.00 d . . . C(17) C -0.6760(3) -0.3105(2) 0.0261(4) 0.0325(8) Uani 1.00 d . . . C(18) C -0.7199(3) -0.4138(2) -0.0625(4) 0.0336(8) Uani 1.00 d . . . C(19) C -0.6496(3) -0.4868(2) -0.1792(4) 0.0338(8) Uani 1.00 d . . . C(20) C -0.5345(3) -0.4571(2) -0.2056(4) 0.0326(8) Uani 1.00 d . . . C(21) C -0.4507(3) -0.5365(2) -0.3168(4) 0.0338(8) Uani 1.00 d . . . C(22) C -0.5145(3) -0.1682(2) 0.0971(4) 0.0383(8) Uani 1.00 d . . . C(23) C -0.8415(3) -0.4504(2) -0.0327(4) 0.0366(8) Uani 1.00 d . . . H(1) H -0.5486 -0.0918 -0.3888 0.0496 Uiso 1.00 calc . . . H(2) H -0.8296 -0.0399 -0.1058 0.0514 Uiso 1.00 calc . . . H(3) H -0.7876 -0.3254 -0.4697 0.0475 Uiso 1.00 calc . . . H(4) H -0.9945 -0.1092 -0.0016 0.0607 Uiso 1.00 calc . . . H(5) H -1.1806 -0.2252 -0.0167 0.0791 Uiso 1.00 calc . . . H(6) H -1.1734 -0.3899 -0.2862 0.0771 Uiso 1.00 calc . . . H(7) H -0.9852 -0.3776 -0.4422 0.0605 Uiso 1.00 calc . . . H(8) H -1.0393 -0.1010 -0.5900 0.0892 Uiso 1.00 calc . . . H(9) H -1.1275 0.0231 -0.3179 0.0882 Uiso 1.00 calc . . . H(10) H -1.3164 -0.0670 -0.2674 0.0922 Uiso 1.00 calc . . . H(11) H -1.3448 -0.2422 -0.5055 0.0966 Uiso 1.00 calc . . . H(12) H -1.1745 -0.2659 -0.7060 0.0915 Uiso 1.00 calc . . . H(13) H -0.4130 -0.3317 -0.1415 0.0395 Uiso 1.00 calc . . . H(14) H -0.7238 -0.2609 0.1072 0.0393 Uiso 1.00 calc . . . H(15) H -0.6804 -0.5573 -0.2408 0.0408 Uiso 1.00 calc . . . H(16) H -0.4521 -0.6925 -0.4451 0.0546 Uiso 1.00 calc . . . H(17) H -0.3708 -0.0787 0.1039 0.0683 Uiso 1.00 calc . . . H(18) H -0.9726 -0.4055 0.1255 0.0590 Uiso 1.00 calc . . . 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 0.0271(2) 0.0402(3) 0.0507(3) -0.0049(2) 0.0058(2) 0.0077(2) O(1) 0.033(1) 0.031(1) 0.063(1) -0.0020(9) 0.018(1) -0.008(1) O(2) 0.037(1) 0.041(1) 0.065(2) -0.007(1) 0.024(1) 0.000(1) O(3) 0.046(1) 0.037(1) 0.075(2) -0.015(1) 0.026(1) -0.015(1) O(4) 0.062(2) 0.039(1) 0.085(2) -0.009(1) 0.037(2) -0.018(1) O(5) 0.035(1) 0.049(1) 0.059(2) -0.005(1) 0.021(1) 0.000(1) O(6) 0.038(1) 0.045(1) 0.074(2) -0.010(1) 0.024(1) -0.003(1) N(1) 0.036(1) 0.035(1) 0.054(2) 0.000(1) 0.016(1) 0.000(1) N(2) 0.032(1) 0.033(1) 0.056(2) -0.005(1) 0.008(1) 0.000(1) C(1) 0.032(2) 0.038(2) 0.052(2) -0.003(1) 0.009(1) 0.003(1) C(2) 0.036(2) 0.036(2) 0.051(2) 0.002(1) 0.011(2) -0.002(1) C(3) 0.028(1) 0.032(2) 0.039(2) 0.001(1) 0.005(1) 0.004(1) C(4) 0.037(2) 0.030(2) 0.048(2) -0.001(1) 0.010(1) -0.001(1) C(5) 0.027(1) 0.037(2) 0.054(2) 0.001(1) 0.007(1) 0.014(1) C(6) 0.039(2) 0.069(2) 0.046(2) 0.000(2) 0.010(2) 0.014(2) C(7) 0.046(2) 0.091(3) 0.071(3) -0.002(2) 0.022(2) 0.036(2) C(8) 0.042(2) 0.058(2) 0.105(3) -0.011(2) 0.010(2) 0.040(2) C(9) 0.038(2) 0.037(2) 0.076(3) -0.003(1) 0.009(2) 0.014(2) C(10) 0.062(3) 0.094(3) 0.083(3) -0.005(3) 0.009(2) 0.051(3) C(11) 0.088(3) 0.042(2) 0.083(3) -0.006(2) -0.017(3) 0.010(2) C(12) 0.055(3) 0.080(3) 0.089(3) 0.028(2) 0.009(2) 0.011(3) C(13) 0.046(2) 0.079(3) 0.106(4) -0.018(2) -0.023(3) 0.017(3) C(14) 0.097(4) 0.068(3) 0.054(3) 0.008(3) -0.011(3) 0.003(2) C(15) 0.027(1) 0.035(2) 0.038(2) -0.003(1) 0.008(1) 0.007(1) C(16) 0.032(1) 0.030(1) 0.034(2) -0.001(1) 0.005(1) 0.004(1) C(17) 0.030(1) 0.030(1) 0.035(2) 0.002(1) 0.008(1) 0.003(1) C(18) 0.027(1) 0.033(2) 0.042(2) 0.000(1) 0.008(1) 0.009(1) C(19) 0.029(1) 0.031(2) 0.040(2) -0.001(1) 0.006(1) 0.005(1) C(20) 0.028(1) 0.030(1) 0.039(2) 0.001(1) 0.008(1) 0.004(1) C(21) 0.030(1) 0.034(2) 0.036(2) 0.001(1) 0.007(1) 0.005(1) C(22) 0.037(2) 0.030(2) 0.045(2) -0.003(1) 0.006(1) 0.002(1) C(23) 0.031(2) 0.033(2) 0.046(2) 0.002(1) 0.010(1) 0.009(1) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 C(5) 2.034(3) . . yes Fe C(6) 2.038(4) . . yes Fe C(7) 2.037(4) . . yes Fe C(8) 2.040(4) . . yes Fe C(9) 2.033(4) . . yes Fe C(10) 2.026(4) . . yes Fe C(11) 2.034(4) . . yes Fe C(12) 2.030(4) . . yes Fe C(13) 2.032(4) . . yes Fe C(14) 2.025(4) . . yes O(1) C(21) 1.315(4) . . yes O(2) C(21) 1.194(4) . . yes O(3) C(22) 1.311(4) . . yes O(4) C(22) 1.190(4) . . yes O(5) C(23) 1.299(4) . . yes O(6) C(23) 1.234(4) . . yes N(1) C(1) 1.326(4) . . yes N(1) C(4) 1.339(4) . . yes N(2) C(1) 1.325(4) . . yes N(2) C(2) 1.331(4) . . yes C(2) C(3) 1.384(4) . . yes C(3) C(4) 1.382(4) . . yes C(3) C(5) 1.471(4) . . yes C(5) C(6) 1.432(4) . . yes C(5) C(9) 1.430(5) . . yes C(6) C(7) 1.421(5) . . yes C(7) C(8) 1.411(6) . . yes C(8) C(9) 1.411(5) . . yes C(10) C(11) 1.398(7) . . yes C(10) C(14) 1.397(7) . . yes C(11) C(12) 1.397(7) . . yes C(12) C(13) 1.377(7) . . yes C(13) C(14) 1.388(7) . . yes C(15) C(16) 1.389(4) . . yes C(15) C(20) 1.389(4) . . yes C(16) C(17) 1.394(4) . . yes C(16) C(22) 1.501(4) . . yes C(17) C(18) 1.387(4) . . yes C(18) C(19) 1.389(4) . . yes C(18) C(23) 1.492(4) . . yes C(19) C(20) 1.384(4) . . yes C(20) C(21) 1.504(4) . . 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 C(5) Fe C(6) 41.2(1) . . 0_555 yes C(5) Fe C(7) 69.1(1) . . 0_555 yes C(5) Fe C(8) 68.7(1) . . 0_555 yes C(5) Fe C(9) 41.2(1) . . 0_555 yes C(5) Fe C(10) 110.0(2) . . 0_555 yes C(5) Fe C(11) 121.2(2) . . 0_555 yes C(5) Fe C(12) 154.8(2) . . 0_555 yes C(5) Fe C(13) 164.7(2) . . 0_555 yes C(5) Fe C(14) 128.0(2) . . 0_555 yes C(6) Fe C(7) 40.8(2) . . 0_555 yes C(6) Fe C(8) 68.3(2) . . 0_555 yes C(6) Fe C(9) 68.9(2) . . 0_555 yes C(6) Fe C(10) 130.7(2) . . 0_555 yes C(6) Fe C(11) 110.8(2) . . 0_555 yes C(6) Fe C(12) 120.1(2) . . 0_555 yes C(6) Fe C(13) 151.9(2) . . 0_555 yes C(6) Fe C(14) 167.6(2) . . 0_555 yes C(7) Fe C(8) 40.5(2) . . 0_555 yes C(7) Fe C(9) 68.6(2) . . 0_555 yes C(7) Fe C(10) 167.9(2) . . 0_555 yes C(7) Fe C(11) 129.0(2) . . 0_555 yes C(7) Fe C(12) 107.9(2) . . 0_555 yes C(7) Fe C(13) 117.1(2) . . 0_555 yes C(7) Fe C(14) 149.7(2) . . 0_555 yes C(8) Fe C(9) 40.5(1) . . 0_555 yes C(8) Fe C(10) 151.4(2) . . 0_555 yes C(8) Fe C(11) 165.0(2) . . 0_555 yes C(8) Fe C(12) 126.2(2) . . 0_555 yes C(8) Fe C(13) 106.2(2) . . 0_555 yes C(8) Fe C(14) 116.4(2) . . 0_555 yes C(9) Fe C(10) 119.3(2) . . 0_555 yes C(9) Fe C(11) 154.3(2) . . 0_555 yes C(9) Fe C(12) 163.0(2) . . 0_555 yes C(9) Fe C(13) 125.8(2) . . 0_555 yes C(9) Fe C(14) 106.6(2) . . 0_555 yes C(10) Fe C(11) 40.3(2) . . 0_555 yes C(10) Fe C(12) 67.4(2) . . 0_555 yes C(10) Fe C(13) 67.0(2) . . 0_555 yes C(10) Fe C(14) 40.3(2) . . 0_555 yes C(11) Fe C(12) 40.2(2) . . 0_555 yes C(11) Fe C(13) 67.1(2) . . 0_555 yes C(11) Fe C(14) 67.9(2) . . 0_555 yes C(12) Fe C(13) 39.6(2) . . 0_555 yes C(12) Fe C(14) 67.5(2) . . 0_555 yes C(13) Fe C(14) 40.0(2) . . 0_555 yes C(1) N(1) C(4) 117.0(3) . . 0_555 yes C(1) N(2) C(2) 116.9(3) . . 0_555 yes N(1) C(1) N(2) 125.3(3) . . 0_555 yes N(2) C(2) C(3) 123.0(3) . . 0_555 yes C(2) C(3) C(4) 115.3(3) . . 0_555 yes C(2) C(3) C(5) 122.3(3) . . 0_555 yes C(4) C(3) C(5) 122.3(3) . . 0_555 yes N(1) C(4) C(3) 122.5(3) . . 0_555 yes Fe C(5) C(3) 126.1(2) . . 0_555 yes Fe C(5) C(6) 69.6(2) . . 0_555 yes Fe C(5) C(9) 69.4(2) . . 0_555 yes C(3) C(5) C(6) 126.5(3) . . 0_555 yes C(3) C(5) C(9) 126.4(3) . . 0_555 yes C(6) C(5) C(9) 107.1(3) . . 0_555 yes Fe C(6) C(5) 69.3(2) . . 0_555 yes Fe C(6) C(7) 69.6(2) . . 0_555 yes C(5) C(6) C(7) 108.1(3) . . 0_555 yes Fe C(7) C(6) 69.6(2) . . 0_555 yes Fe C(7) C(8) 69.8(2) . . 0_555 yes C(6) C(7) C(8) 107.9(3) . . 0_555 yes Fe C(8) C(7) 69.7(2) . . 0_555 yes Fe C(8) C(9) 69.5(2) . . 0_555 yes C(7) C(8) C(9) 108.8(3) . . 0_555 yes Fe C(9) C(5) 69.5(2) . . 0_555 yes Fe C(9) C(8) 70.0(2) . . 0_555 yes C(5) C(9) C(8) 108.1(3) . . 0_555 yes Fe C(10) C(11) 70.2(2) . . 0_555 yes Fe C(10) C(14) 69.8(3) . . 0_555 yes C(11) C(10) C(14) 108.4(4) . . 0_555 yes Fe C(11) C(10) 69.6(2) . . 0_555 yes Fe C(11) C(12) 69.7(2) . . 0_555 yes C(10) C(11) C(12) 107.2(4) . . 0_555 yes Fe C(12) C(11) 70.0(2) . . 0_555 yes Fe C(12) C(13) 70.2(3) . . 0_555 yes C(11) C(12) C(13) 108.2(4) . . 0_555 yes Fe C(13) C(12) 70.1(3) . . 0_555 yes Fe C(13) C(14) 69.7(3) . . 0_555 yes C(12) C(13) C(14) 109.1(4) . . 0_555 yes Fe C(14) C(10) 69.9(2) . . 0_555 yes Fe C(14) C(13) 70.2(3) . . 0_555 yes C(10) C(14) C(13) 107.1(4) . . 0_555 yes C(16) C(15) C(20) 120.1(3) . . 0_555 yes C(15) C(16) C(17) 119.9(3) . . 0_555 yes C(15) C(16) C(22) 121.3(3) . . 0_555 yes C(17) C(16) C(22) 118.7(3) . . 0_555 yes C(16) C(17) C(18) 119.7(3) . . 0_555 yes C(17) C(18) C(19) 120.2(3) . . 0_555 yes C(17) C(18) C(23) 121.4(3) . . 0_555 yes C(19) C(18) C(23) 118.3(3) . . 0_555 yes C(18) C(19) C(20) 120.0(3) . . 0_555 yes C(15) C(20) C(19) 120.0(3) . . 0_555 yes C(15) C(20) C(21) 118.0(3) . . 0_555 yes C(19) C(20) C(21) 121.9(3) . . 0_555 yes O(1) C(21) O(2) 124.0(3) . . 0_555 yes O(1) C(21) C(20) 112.4(2) . . 0_555 yes O(2) C(21) C(20) 123.5(3) . . 0_555 yes O(3) C(22) O(4) 123.8(3) . . 0_555 yes O(3) C(22) C(16) 112.9(3) . . 0_555 yes O(4) C(22) C(16) 123.3(3) . . 0_555 yes O(5) C(23) O(6) 123.1(3) . . 0_555 yes O(5) C(23) C(18) 116.0(3) . . 0_555 yes O(6) C(23) C(18) 120.9(3) . . 0_555 yes #------------------------------------------------------------------------------ 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe C(5) C(3) C(2) 81.3(4) 0_555 20_1 5_555 55_5 yes Fe C(5) C(3) C(4) -101.4(3) 0_555 20_1 5_555 55_5 yes Fe C(5) C(6) C(7) 58.9(3) 0_555 20_1 5_555 55_5 yes Fe C(5) C(9) C(8) -59.6(3) 0_555 20_1 5_555 55_5 yes Fe C(6) C(5) C(3) 120.4(3) 0_555 20_1 5_555 55_5 yes Fe C(6) C(5) C(9) -59.4(2) 0_555 20_1 5_555 55_5 yes Fe C(6) C(7) C(8) 59.6(3) 0_555 20_1 5_555 55_5 yes Fe C(7) C(6) C(5) -58.7(3) 0_555 20_1 5_555 55_5 yes Fe C(7) C(8) C(9) 58.6(3) 0_555 20_1 5_555 55_5 yes Fe C(8) C(7) C(6) -59.4(3) 0_555 20_1 5_555 55_5 yes Fe C(8) C(9) C(5) 59.2(2) 0_555 20_1 5_555 55_5 yes Fe C(9) C(5) C(3) -120.3(3) 0_555 20_1 5_555 55_5 yes Fe C(9) C(5) C(6) 59.6(2) 0_555 20_1 5_555 55_5 yes Fe C(9) C(8) C(7) -58.7(3) 0_555 20_1 5_555 55_5 yes Fe C(10) C(11) C(12) -59.9(3) 0_555 20_1 5_555 55_5 yes Fe C(10) C(14) C(13) 60.7(3) 0_555 20_1 5_555 55_5 yes Fe C(11) C(10) C(14) 59.5(3) 0_555 20_1 5_555 55_5 yes Fe C(11) C(12) C(13) -60.1(3) 0_555 20_1 5_555 55_5 yes Fe C(12) C(11) C(10) 59.7(3) 0_555 20_1 5_555 55_5 yes Fe C(12) C(13) C(14) -59.0(3) 0_555 20_1 5_555 55_5 yes Fe C(13) C(12) C(11) 60.0(3) 0_555 20_1 5_555 55_5 yes Fe C(13) C(14) C(10) -60.5(3) 0_555 20_1 5_555 55_5 yes Fe C(14) C(10) C(11) -59.8(3) 0_555 20_1 5_555 55_5 yes Fe C(14) C(13) C(12) 59.3(4) 0_555 20_1 5_555 55_5 yes O(1) C(21) C(20) C(15) 172.9(3) 0_555 20_1 5_555 55_5 yes O(1) C(21) C(20) C(19) -3.7(4) 0_555 20_1 5_555 55_5 yes O(2) C(21) C(20) C(15) -4.3(5) 0_555 20_1 5_555 55_5 yes O(2) C(21) C(20) C(19) 179.0(3) 0_555 20_1 5_555 55_5 yes O(3) C(22) C(16) C(15) 6.2(4) 0_555 20_1 5_555 55_5 yes O(3) C(22) C(16) C(17) -176.5(3) 0_555 20_1 5_555 55_5 yes O(4) C(22) C(16) C(15) -172.7(3) 0_555 20_1 5_555 55_5 yes O(4) C(22) C(16) C(17) 4.6(5) 0_555 20_1 5_555 55_5 yes O(5) C(23) C(18) C(17) -9.6(4) 0_555 20_1 5_555 55_5 yes O(5) C(23) C(18) C(19) 169.1(3) 0_555 20_1 5_555 55_5 yes O(6) C(23) C(18) C(17) 171.2(3) 0_555 20_1 5_555 55_5 yes O(6) C(23) C(18) C(19) -10.1(5) 0_555 20_1 5_555 55_5 yes N(1) C(1) N(2) C(2) -0.7(5) 0_555 20_1 5_555 55_5 yes N(1) C(4) C(3) C(2) -1.4(5) 0_555 20_1 5_555 55_5 yes N(1) C(4) C(3) C(5) -178.8(3) 0_555 20_1 5_555 55_5 yes N(2) C(1) N(1) C(4) 1.3(5) 0_555 20_1 5_555 55_5 yes N(2) C(2) C(3) C(4) 2.0(5) 0_555 20_1 5_555 55_5 yes N(2) C(2) C(3) C(5) 179.5(3) 0_555 20_1 5_555 55_5 yes C(1) N(1) C(4) C(3) -0.1(5) 0_555 20_1 5_555 55_5 yes C(1) N(2) C(2) C(3) -1.1(5) 0_555 20_1 5_555 55_5 yes C(2) C(3) C(5) C(6) -8.7(5) 0_555 20_1 5_555 55_5 yes C(2) C(3) C(5) C(9) 171.0(3) 0_555 20_1 5_555 55_5 yes C(3) C(5) Fe C(6) -120.9(4) 0_555 20_1 5_555 55_5 yes C(3) C(5) Fe C(7) -158.3(3) 0_555 20_1 5_555 55_5 yes C(3) C(5) Fe C(8) 158.1(3) 0_555 20_1 5_555 55_5 yes C(3) C(5) Fe C(9) 120.6(4) 0_555 20_1 5_555 55_5 yes C(3) C(5) Fe C(10) 8.7(3) 0_555 20_1 5_555 55_5 yes C(3) C(5) Fe C(11) -34.5(4) 0_555 20_1 5_555 55_5 yes C(3) C(5) Fe C(12) -70.5(5) 0_555 20_1 5_555 55_5 yes C(3) C(5) Fe C(13) 84.8(7) 0_555 20_1 5_555 55_5 yes C(3) C(5) Fe C(14) 50.6(4) 0_555 20_1 5_555 55_5 yes C(3) C(5) C(6) C(7) 179.3(3) 0_555 20_1 5_555 55_5 yes C(3) C(5) C(9) C(8) -179.9(3) 0_555 20_1 5_555 55_5 yes C(4) C(3) C(5) C(6) 168.5(3) 0_555 20_1 5_555 55_5 yes C(4) C(3) C(5) C(9) -11.7(5) 0_555 20_1 5_555 55_5 yes C(5) Fe C(6) C(7) -119.7(3) 0_555 20_1 5_555 55_5 yes C(5) Fe C(7) C(6) 37.8(2) 0_555 20_1 5_555 55_5 yes C(5) Fe C(7) C(8) -81.3(2) 0_555 20_1 5_555 55_5 yes C(5) Fe C(8) C(7) 82.3(2) 0_555 20_1 5_555 55_5 yes C(5) Fe C(8) C(9) -38.0(2) 0_555 20_1 5_555 55_5 yes C(5) Fe C(9) C(8) 119.3(3) 0_555 20_1 5_555 55_5 yes C(5) Fe C(10) C(11) -115.0(3) 0_555 20_1 5_555 55_5 yes C(5) Fe C(10) C(14) 125.6(3) 0_555 20_1 5_555 55_5 yes C(5) Fe C(11) C(10) 84.5(3) 0_555 20_1 5_555 55_5 yes C(5) Fe C(11) C(12) -157.1(3) 0_555 20_1 5_555 55_5 yes C(5) Fe C(12) C(11) 51.2(5) 0_555 20_1 5_555 55_5 yes C(5) Fe C(12) C(13) 170.1(4) 0_555 20_1 5_555 55_5 yes C(5) Fe C(13) C(12) -163.8(5) 0_555 20_1 5_555 55_5 yes C(5) Fe C(13) C(14) -43.5(8) 0_555 20_1 5_555 55_5 yes C(5) Fe C(14) C(10) -75.7(3) 0_555 20_1 5_555 55_5 yes C(5) Fe C(14) C(13) 166.7(3) 0_555 20_1 5_555 55_5 yes C(5) C(6) Fe C(7) 119.7(3) 0_555 20_1 5_555 55_5 yes C(5) C(6) Fe C(8) 82.0(2) 0_555 20_1 5_555 55_5 yes C(5) C(6) Fe C(9) 38.3(2) 0_555 20_1 5_555 55_5 yes C(5) C(6) Fe C(10) -72.7(3) 0_555 20_1 5_555 55_5 yes C(5) C(6) Fe C(11) -114.1(3) 0_555 20_1 5_555 55_5 yes C(5) C(6) Fe C(12) -157.7(2) 0_555 20_1 5_555 55_5 yes C(5) C(6) Fe C(13) 165.9(3) 0_555 20_1 5_555 55_5 yes C(5) C(6) Fe C(14) -32.6(9) 0_555 20_1 5_555 55_5 yes C(5) C(6) C(7) C(8) 0.9(5) 0_555 20_1 5_555 55_5 yes C(5) C(9) Fe C(6) -38.4(2) 0_555 20_1 5_555 55_5 yes C(5) C(9) Fe C(7) -82.3(2) 0_555 20_1 5_555 55_5 yes C(5) C(9) Fe C(8) -119.3(3) 0_555 20_1 5_555 55_5 yes C(5) C(9) Fe C(10) 87.5(3) 0_555 20_1 5_555 55_5 yes C(5) C(9) Fe C(11) 55.9(5) 0_555 20_1 5_555 55_5 yes C(5) C(9) Fe C(12) -163.6(6) 0_555 20_1 5_555 55_5 yes C(5) C(9) Fe C(13) 169.0(2) 0_555 20_1 5_555 55_5 yes C(5) C(9) Fe C(14) 129.4(3) 0_555 20_1 5_555 55_5 yes C(5) C(9) C(8) C(7) 0.6(5) 0_555 20_1 5_555 55_5 yes C(6) Fe C(5) C(9) 118.5(3) 0_555 20_1 5_555 55_5 yes C(6) Fe C(7) C(8) -119.1(3) 0_555 20_1 5_555 55_5 yes C(6) Fe C(8) C(7) 37.9(2) 0_555 20_1 5_555 55_5 yes C(6) Fe C(8) C(9) -82.5(2) 0_555 20_1 5_555 55_5 yes C(6) Fe C(9) C(8) 80.9(3) 0_555 20_1 5_555 55_5 yes C(6) Fe C(10) C(11) -73.0(3) 0_555 20_1 5_555 55_5 yes C(6) Fe C(10) C(14) 167.6(3) 0_555 20_1 5_555 55_5 yes C(6) Fe C(11) C(10) 129.2(3) 0_555 20_1 5_555 55_5 yes C(6) Fe C(11) C(12) -112.5(3) 0_555 20_1 5_555 55_5 yes C(6) Fe C(12) C(11) 87.1(3) 0_555 20_1 5_555 55_5 yes C(6) Fe C(12) C(13) -154.0(3) 0_555 20_1 5_555 55_5 yes C(6) Fe C(13) C(12) 53.6(5) 0_555 20_1 5_555 55_5 yes C(6) Fe C(13) C(14) 173.9(3) 0_555 20_1 5_555 55_5 yes C(6) Fe C(14) C(10) -48.9(9) 0_555 20_1 5_555 55_5 yes C(6) Fe C(14) C(13) -166.6(7) 0_555 20_1 5_555 55_5 yes C(6) C(5) Fe C(7) -37.4(2) 0_555 20_1 5_555 55_5 yes C(6) C(5) Fe C(8) -81.0(2) 0_555 20_1 5_555 55_5 yes C(6) C(5) Fe C(9) -118.5(3) 0_555 20_1 5_555 55_5 yes C(6) C(5) Fe C(10) 129.6(3) 0_555 20_1 5_555 55_5 yes C(6) C(5) Fe C(11) 86.4(3) 0_555 20_1 5_555 55_5 yes C(6) C(5) Fe C(12) 50.4(5) 0_555 20_1 5_555 55_5 yes C(6) C(5) Fe C(13) -154.3(6) 0_555 20_1 5_555 55_5 yes C(6) C(5) Fe C(14) 171.5(3) 0_555 20_1 5_555 55_5 yes C(6) C(5) C(9) C(8) 0.0(4) 0_555 20_1 5_555 55_5 yes C(6) C(7) Fe C(8) 119.1(3) 0_555 20_1 5_555 55_5 yes C(6) C(7) Fe C(9) 82.1(2) 0_555 20_1 5_555 55_5 yes C(6) C(7) Fe C(10) -50.5(9) 0_555 20_1 5_555 55_5 yes C(6) C(7) Fe C(11) -76.1(3) 0_555 20_1 5_555 55_5 yes C(6) C(7) Fe C(12) -115.6(3) 0_555 20_1 5_555 55_5 yes C(6) C(7) Fe C(13) -157.6(2) 0_555 20_1 5_555 55_5 yes C(6) C(7) Fe C(14) 168.5(3) 0_555 20_1 5_555 55_5 yes C(6) C(7) C(8) C(9) -0.9(5) 0_555 20_1 5_555 55_5 yes C(7) Fe C(5) C(9) 81.0(2) 0_555 20_1 5_555 55_5 yes C(7) Fe C(8) C(9) -120.4(3) 0_555 20_1 5_555 55_5 yes C(7) Fe C(9) C(8) 37.0(3) 0_555 20_1 5_555 55_5 yes C(7) Fe C(10) C(11) -31.3(10) 0_555 20_1 5_555 55_5 yes C(7) Fe C(10) C(14) -150.7(8) 0_555 20_1 5_555 55_5 yes C(7) Fe C(11) C(10) 171.9(3) 0_555 20_1 5_555 55_5 yes C(7) Fe C(11) C(12) -69.8(3) 0_555 20_1 5_555 55_5 yes C(7) Fe C(12) C(11) 130.0(3) 0_555 20_1 5_555 55_5 yes C(7) Fe C(12) C(13) -111.1(3) 0_555 20_1 5_555 55_5 yes C(7) Fe C(13) C(12) 85.6(4) 0_555 20_1 5_555 55_5 yes C(7) Fe C(13) C(14) -154.1(3) 0_555 20_1 5_555 55_5 yes C(7) Fe C(14) C(10) 168.2(3) 0_555 20_1 5_555 55_5 yes C(7) Fe C(14) C(13) 50.5(5) 0_555 20_1 5_555 55_5 yes C(7) C(6) Fe C(8) -37.6(2) 0_555 20_1 5_555 55_5 yes C(7) C(6) Fe C(9) -81.3(3) 0_555 20_1 5_555 55_5 yes C(7) C(6) Fe C(10) 167.6(3) 0_555 20_1 5_555 55_5 yes C(7) C(6) Fe C(11) 126.3(3) 0_555 20_1 5_555 55_5 yes C(7) C(6) Fe C(12) 82.7(3) 0_555 20_1 5_555 55_5 yes C(7) C(6) Fe C(13) 46.2(5) 0_555 20_1 5_555 55_5 yes C(7) C(6) Fe C(14) -152.3(8) 0_555 20_1 5_555 55_5 yes C(7) C(6) C(5) C(9) -0.5(4) 0_555 20_1 5_555 55_5 yes C(7) C(8) Fe C(9) 120.4(3) 0_555 20_1 5_555 55_5 yes C(7) C(8) Fe C(10) 175.4(3) 0_555 20_1 5_555 55_5 yes C(7) C(8) Fe C(11) -51.6(8) 0_555 20_1 5_555 55_5 yes C(7) C(8) Fe C(12) -74.3(3) 0_555 20_1 5_555 55_5 yes C(7) C(8) Fe C(13) -112.9(3) 0_555 20_1 5_555 55_5 yes C(7) C(8) Fe C(14) -154.7(3) 0_555 20_1 5_555 55_5 yes C(8) Fe C(5) C(9) 37.5(2) 0_555 20_1 5_555 55_5 yes C(8) Fe C(10) C(11) 162.9(3) 0_555 20_1 5_555 55_5 yes C(8) Fe C(10) C(14) 43.6(5) 0_555 20_1 5_555 55_5 yes C(8) Fe C(11) C(10) -147.2(7) 0_555 20_1 5_555 55_5 yes C(8) Fe C(11) C(12) -28.8(8) 0_555 20_1 5_555 55_5 yes C(8) Fe C(12) C(11) 171.1(3) 0_555 20_1 5_555 55_5 yes C(8) Fe C(12) C(13) -70.0(4) 0_555 20_1 5_555 55_5 yes C(8) Fe C(13) C(12) 127.8(3) 0_555 20_1 5_555 55_5 yes C(8) Fe C(13) C(14) -111.9(3) 0_555 20_1 5_555 55_5 yes C(8) Fe C(14) C(10) -158.4(3) 0_555 20_1 5_555 55_5 yes C(8) Fe C(14) C(13) 83.9(3) 0_555 20_1 5_555 55_5 yes C(8) C(7) Fe C(9) -37.0(2) 0_555 20_1 5_555 55_5 yes C(8) C(7) Fe C(10) -169.5(8) 0_555 20_1 5_555 55_5 yes C(8) C(7) Fe C(11) 164.8(3) 0_555 20_1 5_555 55_5 yes C(8) C(7) Fe C(12) 125.3(3) 0_555 20_1 5_555 55_5 yes C(8) C(7) Fe C(13) 83.3(3) 0_555 20_1 5_555 55_5 yes C(8) C(7) Fe C(14) 49.5(5) 0_555 20_1 5_555 55_5 yes C(8) C(9) Fe C(10) -153.2(3) 0_555 20_1 5_555 55_5 yes C(8) C(9) Fe C(11) 175.2(4) 0_555 20_1 5_555 55_5 yes C(8) C(9) Fe C(12) -44.3(7) 0_555 20_1 5_555 55_5 yes C(8) C(9) Fe C(13) -71.7(3) 0_555 20_1 5_555 55_5 yes C(8) C(9) Fe C(14) -111.3(3) 0_555 20_1 5_555 55_5 yes C(9) Fe C(10) C(11) -159.4(3) 0_555 20_1 5_555 55_5 yes C(9) Fe C(10) C(14) 81.2(3) 0_555 20_1 5_555 55_5 yes C(9) Fe C(11) C(10) 44.9(5) 0_555 20_1 5_555 55_5 yes C(9) Fe C(11) C(12) 163.2(4) 0_555 20_1 5_555 55_5 yes C(9) Fe C(12) C(11) -154.7(5) 0_555 20_1 5_555 55_5 yes C(9) Fe C(12) C(13) -35.8(8) 0_555 20_1 5_555 55_5 yes C(9) Fe C(13) C(12) 167.8(3) 0_555 20_1 5_555 55_5 yes C(9) Fe C(13) C(14) -71.9(3) 0_555 20_1 5_555 55_5 yes C(9) Fe C(14) C(10) -115.9(3) 0_555 20_1 5_555 55_5 yes C(9) Fe C(14) C(13) 126.4(3) 0_555 20_1 5_555 55_5 yes C(9) C(5) Fe C(10) -111.9(3) 0_555 20_1 5_555 55_5 yes C(9) C(5) Fe C(11) -155.1(2) 0_555 20_1 5_555 55_5 yes C(9) C(5) Fe C(12) 168.8(4) 0_555 20_1 5_555 55_5 yes C(9) C(5) Fe C(13) -35.8(7) 0_555 20_1 5_555 55_5 yes C(9) C(5) Fe C(14) -70.0(3) 0_555 20_1 5_555 55_5 yes C(9) C(8) Fe C(10) 55.1(5) 0_555 20_1 5_555 55_5 yes C(9) C(8) Fe C(11) -172.0(6) 0_555 20_1 5_555 55_5 yes C(9) C(8) Fe C(12) 165.3(2) 0_555 20_1 5_555 55_5 yes C(9) C(8) Fe C(13) 126.7(3) 0_555 20_1 5_555 55_5 yes C(9) C(8) Fe C(14) 84.9(3) 0_555 20_1 5_555 55_5 yes C(10) Fe C(11) C(12) 118.3(4) 0_555 20_1 5_555 55_5 yes C(10) Fe C(12) C(11) -38.1(3) 0_555 20_1 5_555 55_5 yes C(10) Fe C(12) C(13) 80.8(3) 0_555 20_1 5_555 55_5 yes C(10) Fe C(13) C(12) -81.8(3) 0_555 20_1 5_555 55_5 yes C(10) Fe C(13) C(14) 38.5(3) 0_555 20_1 5_555 55_5 yes C(10) Fe C(14) C(13) -117.7(4) 0_555 20_1 5_555 55_5 yes C(10) C(11) Fe C(12) -118.3(4) 0_555 20_1 5_555 55_5 yes C(10) C(11) Fe C(13) -81.0(3) 0_555 20_1 5_555 55_5 yes C(10) C(11) Fe C(14) -37.5(3) 0_555 20_1 5_555 55_5 yes C(10) C(11) C(12) C(13) -0.4(5) 0_555 20_1 5_555 55_5 yes C(10) C(14) Fe C(11) 37.5(3) 0_555 20_1 5_555 55_5 yes C(10) C(14) Fe C(12) 81.1(3) 0_555 20_1 5_555 55_5 yes C(10) C(14) Fe C(13) 117.7(4) 0_555 20_1 5_555 55_5 yes C(10) C(14) C(13) C(12) -1.2(6) 0_555 20_1 5_555 55_5 yes C(11) Fe C(10) C(14) -119.4(4) 0_555 20_1 5_555 55_5 yes C(11) Fe C(12) C(13) 118.9(4) 0_555 20_1 5_555 55_5 yes C(11) Fe C(13) C(12) -37.9(3) 0_555 20_1 5_555 55_5 yes C(11) Fe C(13) C(14) 82.4(3) 0_555 20_1 5_555 55_5 yes C(11) Fe C(14) C(13) -80.2(3) 0_555 20_1 5_555 55_5 yes C(11) C(10) Fe C(12) 38.0(3) 0_555 20_1 5_555 55_5 yes C(11) C(10) Fe C(13) 81.2(3) 0_555 20_1 5_555 55_5 yes C(11) C(10) Fe C(14) 119.4(4) 0_555 20_1 5_555 55_5 yes C(11) C(10) C(14) C(13) 0.9(5) 0_555 20_1 5_555 55_5 yes C(11) C(12) Fe C(13) -118.9(4) 0_555 20_1 5_555 55_5 yes C(11) C(12) Fe C(14) -81.9(3) 0_555 20_1 5_555 55_5 yes C(11) C(12) C(13) C(14) 1.0(6) 0_555 20_1 5_555 55_5 yes C(12) Fe C(10) C(14) -81.4(3) 0_555 20_1 5_555 55_5 yes C(12) Fe C(13) C(14) 120.3(4) 0_555 20_1 5_555 55_5 yes C(12) Fe C(14) C(13) -36.6(3) 0_555 20_1 5_555 55_5 yes C(12) C(11) Fe C(13) 37.3(3) 0_555 20_1 5_555 55_5 yes C(12) C(11) Fe C(14) 80.8(3) 0_555 20_1 5_555 55_5 yes C(12) C(11) C(10) C(14) -0.3(5) 0_555 20_1 5_555 55_5 yes C(12) C(13) Fe C(14) -120.3(4) 0_555 20_1 5_555 55_5 yes C(13) Fe C(10) C(14) -38.2(3) 0_555 20_1 5_555 55_5 yes C(13) C(12) Fe C(14) 37.0(3) 0_555 20_1 5_555 55_5 yes C(15) C(16) C(17) C(18) -1.1(5) 0_555 20_1 5_555 55_5 yes C(15) C(20) C(19) C(18) -2.1(5) 0_555 20_1 5_555 55_5 yes C(16) C(15) C(20) C(19) 1.8(5) 0_555 20_1 5_555 55_5 yes C(16) C(15) C(20) C(21) -174.9(3) 0_555 20_1 5_555 55_5 yes C(16) C(17) C(18) C(19) 0.8(5) 0_555 20_1 5_555 55_5 yes C(16) C(17) C(18) C(23) 179.5(3) 0_555 20_1 5_555 55_5 yes C(17) C(16) C(15) C(20) -0.2(5) 0_555 20_1 5_555 55_5 yes C(17) C(18) C(19) C(20) 0.8(5) 0_555 20_1 5_555 55_5 yes C(18) C(17) C(16) C(22) -178.5(3) 0_555 20_1 5_555 55_5 yes C(18) C(19) C(20) C(21) 174.4(3) 0_555 20_1 5_555 55_5 yes C(20) C(15) C(16) C(22) 177.1(3) 0_555 20_1 5_555 55_5 yes C(20) C(19) C(18) C(23) -177.9(3) 0_555 20_1 5_555 55_5 yes C(20) C(19) C(18) C(23) -177.9(3) 0_555 20_1 5_555 55_5 yes #------------------------------------------------------------------------------ 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(1) 2.673(3) . 2_444 ? O(1) C(13) 3.245(5) . 2_344 ? O(1) C(17) 3.259(4) . 2_445 ? O(1) C(16) 3.272(4) . 2_445 ? O(1) O(2) 3.440(4) . 2_444 ? O(1) C(4) 3.519(4) . 2_444 ? O(1) C(21) 3.553(4) . 2_444 ? O(1) C(1) 3.565(4) . 2_444 ? O(2) C(21) 3.335(4) . 2_444 ? O(2) C(4) 3.361(4) . 2_444 ? O(2) N(1) 3.374(3) . 2_444 ? O(2) C(20) 3.411(4) . 2_444 ? O(2) C(18) 3.412(4) . 2_445 ? O(2) C(8) 3.417(4) . 1_655 ? O(2) C(23) 3.467(4) . 2_445 ? O(2) O(5) 3.497(4) . 2_445 ? O(2) C(19) 3.586(4) . 2_444 ? O(3) N(2) 2.695(3) . 2_455 ? O(3) C(1) 3.570(4) . 2_455 ? O(3) C(2) 3.576(4) . 2_455 ? O(3) C(7) 3.581(5) . 1_655 ? O(3) C(14) 3.591(6) . 1_656 ? O(4) C(12) 3.165(5) . 2_355 ? O(4) C(1) 3.389(4) . 1_556 ? O(4) N(2) 3.405(4) . 2_455 ? O(4) C(1) 3.457(4) . 2_455 ? O(4) N(1) 3.467(4) . 1_556 ? O(5) O(6) 2.678(3) . 2_345 ? O(5) C(7) 3.458(5) . . ? O(5) C(6) 3.477(5) . . ? O(5) C(23) 3.534(4) . 2_345 ? O(5) C(8) 3.538(5) . . ? O(5) C(5) 3.594(4) . . ? O(6) O(6) 3.307(4) . 2_345 ? O(6) C(23) 3.384(4) . 2_345 ? O(6) C(14) 3.489(5) . 2_344 ? O(6) C(9) 3.575(4) . . ? N(1) C(21) 3.413(4) . 2_444 ? N(2) C(22) 3.444(4) . 2_455 ? N(2) C(22) 3.541(4) . . ? C(3) C(17) 3.384(4) . . ? C(4) C(17) 3.541(5) . . ? C(9) C(23) 3.430(5) . . ? C(15) C(19) 3.589(4) . 2_445 ? C(17) C(21) 3.426(4) . 2_445 ? C(18) C(21) 3.419(4) . 2_445 ? C(19) C(20) 3.552(4) . 2_445 ? C(20) C(20) 3.523(6) . 2_445 ? C(20) C(21) 3.557(4) . 2_444 ? C(21) C(21) 3.187(6) . 2_444 ? #------------------------------------------------------------------------------ loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_site_distance_DH _geom_hbond_site_distance_HA _geom_hbond_site_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O(1) H(16) N(1) . . 2_444 0.946 1.741 2.673(3) 167.946 no #------------------------------------------------------------------------------ #-----------END data_compound_7 _database_code_CSD 206167 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C38 H30 Fe2 N4 O8 ' _chemical_formula_moiety ? _chemical_formula_weight 782.37 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 12.474(4) _cell_length_b 13.687(3) _cell_length_c 19.390(3) _cell_angle_alpha 90 _cell_angle_beta 94.10(2) _cell_angle_gamma 90 _cell_volume 3302(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.7 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.5 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.941 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.872 _exptl_absorpt_correction_T_max 0.998 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 4115 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 1.0000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.0000 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% 0.97 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3777 _reflns_number_gt 3026 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1638 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3026 _refine_ls_number_parameters 235 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.15000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0002 _refine_diff_density_max 0.48 _refine_diff_density_min -1.04 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Fe Fe 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.77894(3) 0.18137(3) 0.70097(2) 0.0292(1) Uani 1.00 d . . . O(1) O 1.0058(2) -0.1062(2) 0.9806(1) 0.0423(6) Uani 1.00 d . . . O(2) O 1.0143(2) -0.1884(2) 0.8822(1) 0.0636(9) Uani 1.00 d . . . O(3) O 1.0635(2) -0.4166(2) 1.0737(2) 0.0708(9) Uani 1.00 d . . . O(4) O 0.9657(2) -0.3133(2) 1.0110(2) 0.0657(9) Uani 1.00 d . . . N(1) N 0.8176(2) -0.0194(2) 0.9252(1) 0.0327(6) Uani 1.00 d . . . N(2) N 0.6304(2) -0.0008(2) 0.9028(2) 0.0395(7) Uani 1.00 d . . . C(1) C 0.7160(3) -0.0446(2) 0.9327(2) 0.0352(8) Uani 1.00 d . . . C(2) C 0.6472(2) 0.0760(3) 0.8622(2) 0.0375(8) Uani 1.00 d . . . C(3) C 0.7497(2) 0.1088(2) 0.8502(1) 0.0282(7) Uani 1.00 d . . . C(4) C 0.8327(2) 0.0569(2) 0.8842(2) 0.0330(7) Uani 1.00 d . . . C(5) C 0.7667(3) 0.1925(2) 0.8047(2) 0.0309(7) Uani 1.00 d . . . C(6) C 0.8683(3) 0.2285(2) 0.7861(2) 0.0377(8) Uani 1.00 d . . . C(7) C 0.8498(4) 0.3066(2) 0.7390(2) 0.0453(9) Uani 1.00 d . . . C(8) C 0.7357(4) 0.3193(2) 0.7283(2) 0.048(1) Uani 1.00 d . . . C(9) C 0.6854(3) 0.2495(2) 0.7681(2) 0.0405(9) Uani 1.00 d . . . C(10) C 0.7421(5) 0.0431(3) 0.6703(2) 0.066(1) Uani 1.00 d . . . C(11) C 0.8498(4) 0.0630(4) 0.6599(2) 0.066(1) Uani 1.00 d . . . C(12) C 0.8517(4) 0.1427(4) 0.6144(2) 0.063(1) Uani 1.00 d . . . C(13) C 0.7462(4) 0.1713(3) 0.5974(2) 0.057(1) Uani 1.00 d . . . C(14) C 0.6775(4) 0.1107(3) 0.6308(2) 0.057(1) Uani 1.00 d . . . C(15) C 1.1518(2) -0.2125(2) 0.9723(1) 0.0246(6) Uani 1.00 d . . . C(16) C 1.1541(2) -0.2938(2) 1.0166(1) 0.0244(6) Uani 1.00 d . . . C(17) C 1.2475(2) -0.1700(2) 0.9559(2) 0.0275(7) Uani 1.00 d . . . C(18) C 1.0479(2) -0.1693(2) 0.9403(2) 0.0288(7) Uani 1.00 d . . . C(19) C 1.0511(2) -0.3416(2) 1.0328(2) 0.0287(7) Uani 1.00 d . . . H(1) H 0.7041 -0.0986 0.9620 0.0425 Uiso 1.00 calc . . . H(2) H 0.5868 0.1093 0.8408 0.0451 Uiso 1.00 calc . . . H(3) H 0.9043 0.0768 0.8780 0.0397 Uiso 1.00 calc . . . H(4) H 0.9368 0.2037 0.8024 0.0454 Uiso 1.00 calc . . . H(5) H 0.9031 0.3436 0.7180 0.0543 Uiso 1.00 calc . . . H(6) H 0.7000 0.3660 0.6985 0.0581 Uiso 1.00 calc . . . H(7) H 0.6101 0.2413 0.7701 0.0485 Uiso 1.00 calc . . . H(8) H 0.7168 -0.0076 0.6985 0.0791 Uiso 1.00 calc . . . H(9) H 0.9105 0.0287 0.6798 0.0792 Uiso 1.00 calc . . . H(10) H 0.9142 0.1719 0.5982 0.0762 Uiso 1.00 calc . . . H(11) H 0.7248 0.2238 0.5675 0.0689 Uiso 1.00 calc . . . H(12) H 0.6013 0.1139 0.6276 0.0683 Uiso 1.00 calc . . . H(13) H 0.9405 -0.0742 0.9661 0.0506 Uiso 1.00 calc . . . H(14) H 1.0027 -0.4517 1.0870 0.0860 Uiso 1.00 calc . . . H(15) H 1.2462 -0.1155 0.9256 0.0760 Uiso 1.00 calc . . . 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 0.0277(3) 0.0304(3) 0.0299(3) -0.0011(2) 0.0061(2) 0.0013(1) O(1) 0.028(1) 0.043(1) 0.056(1) 0.0177(10) -0.0052(10) -0.006(1) O(2) 0.041(1) 0.105(3) 0.043(2) 0.030(1) -0.011(1) -0.013(1) O(3) 0.024(1) 0.080(2) 0.108(3) -0.007(1) 0.001(1) 0.066(2) O(4) 0.020(1) 0.061(2) 0.116(3) -0.004(1) 0.000(1) 0.049(2) N(1) 0.023(1) 0.034(1) 0.041(1) 0.003(1) 0.004(1) 0.004(1) N(2) 0.022(1) 0.044(1) 0.053(2) -0.004(1) 0.006(1) 0.014(1) C(1) 0.030(1) 0.032(1) 0.045(2) -0.001(1) 0.008(1) 0.009(1) C(2) 0.022(1) 0.043(2) 0.048(2) 0.004(1) 0.006(1) 0.014(1) C(3) 0.026(1) 0.030(1) 0.030(1) 0.000(1) 0.007(1) 0.000(1) C(4) 0.019(1) 0.039(1) 0.041(2) -0.002(1) 0.006(1) 0.001(1) C(5) 0.032(2) 0.031(1) 0.031(1) -0.001(1) 0.007(1) -0.002(1) C(6) 0.037(2) 0.040(2) 0.037(2) -0.013(1) 0.004(1) 0.003(1) C(7) 0.058(2) 0.038(2) 0.040(2) -0.015(2) 0.010(2) 0.004(1) C(8) 0.068(3) 0.032(2) 0.046(2) 0.010(2) 0.015(2) 0.005(1) C(9) 0.042(2) 0.037(2) 0.044(2) 0.011(1) 0.016(2) 0.005(1) C(10) 0.112(4) 0.035(2) 0.051(2) -0.019(2) 0.009(3) -0.004(2) C(11) 0.073(3) 0.065(3) 0.061(3) 0.033(2) 0.005(2) -0.020(2) C(12) 0.064(3) 0.084(3) 0.044(2) -0.008(2) 0.023(2) -0.017(2) C(13) 0.082(3) 0.056(2) 0.034(2) -0.012(2) -0.004(2) 0.000(1) C(14) 0.050(2) 0.066(3) 0.054(2) -0.011(2) -0.007(2) -0.018(2) C(15) 0.016(1) 0.024(1) 0.034(1) 0.0018(10) 0.003(1) 0.0020(10) C(16) 0.016(1) 0.025(1) 0.033(1) 0.0000(10) 0.005(1) 0.001(1) C(17) 0.017(1) 0.028(1) 0.037(2) 0.0008(10) 0.006(1) 0.006(1) C(18) 0.019(1) 0.033(1) 0.035(2) 0.000(1) 0.004(1) 0.006(1) C(19) 0.019(1) 0.029(1) 0.039(2) -0.003(1) 0.005(1) 0.005(1) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS97 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 C(5) 2.034(3) . . yes Fe C(6) 2.031(3) . . yes Fe C(7) 2.041(4) . . yes Fe C(8) 2.043(3) . . yes Fe C(9) 2.035(3) . . yes Fe C(10) 2.027(4) . . yes Fe C(11) 2.035(4) . . yes Fe C(12) 2.035(4) . . yes Fe C(13) 2.026(4) . . yes Fe C(14) 2.036(4) . . yes O(1) C(18) 1.300(4) . . yes O(2) C(18) 1.202(4) . . yes O(3) C(19) 1.299(4) . . yes O(4) C(19) 1.183(4) . . yes N(1) C(1) 1.331(4) . . yes N(1) C(4) 1.335(4) . . yes N(2) C(1) 1.322(4) . . yes N(2) C(2) 1.339(4) . . yes C(2) C(3) 1.390(4) . . yes C(3) C(4) 1.383(4) . . yes C(3) C(5) 1.470(4) . . yes C(5) C(6) 1.430(4) . . yes C(5) C(9) 1.428(5) . . yes C(6) C(7) 1.415(5) . . yes C(7) C(8) 1.434(6) . . yes C(8) C(9) 1.404(5) . . yes C(10) C(11) 1.400(7) . . yes C(10) C(14) 1.415(7) . . yes C(11) C(12) 1.405(7) . . yes C(12) C(13) 1.391(7) . . yes C(13) C(14) 1.386(6) . . yes C(15) C(16) 1.405(4) . . yes C(15) C(17) 1.386(4) . . yes C(15) C(18) 1.517(4) . . yes C(16) C(17) 1.393(4) . 7_747 yes C(16) C(19) 1.496(4) . . 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 C(5) Fe C(6) 41.2(1) . . 0_555 yes C(5) Fe C(7) 69.0(1) . . 0_555 yes C(5) Fe C(8) 68.6(1) . . 0_555 yes C(5) Fe C(9) 41.1(1) . . 0_555 yes C(5) Fe C(10) 109.2(2) . . 0_555 yes C(5) Fe C(11) 120.8(2) . . 0_555 yes C(5) Fe C(12) 154.8(2) . . 0_555 yes C(5) Fe C(13) 164.1(2) . . 0_555 yes C(5) Fe C(14) 127.6(2) . . 0_555 yes C(6) Fe C(7) 40.7(1) . . 0_555 yes C(6) Fe C(8) 68.6(2) . . 0_555 yes C(6) Fe C(9) 69.0(1) . . 0_555 yes C(6) Fe C(10) 129.4(2) . . 0_555 yes C(6) Fe C(11) 110.0(2) . . 0_555 yes C(6) Fe C(12) 120.1(2) . . 0_555 yes C(6) Fe C(13) 152.6(2) . . 0_555 yes C(6) Fe C(14) 166.8(2) . . 0_555 yes C(7) Fe C(8) 41.1(2) . . 0_555 yes C(7) Fe C(9) 68.8(2) . . 0_555 yes C(7) Fe C(10) 166.7(2) . . 0_555 yes C(7) Fe C(11) 128.4(2) . . 0_555 yes C(7) Fe C(12) 108.0(2) . . 0_555 yes C(7) Fe C(13) 117.8(2) . . 0_555 yes C(7) Fe C(14) 150.8(2) . . 0_555 yes C(8) Fe C(9) 40.3(1) . . 0_555 yes C(8) Fe C(10) 151.7(2) . . 0_555 yes C(8) Fe C(11) 165.2(2) . . 0_555 yes C(8) Fe C(12) 126.6(2) . . 0_555 yes C(8) Fe C(13) 106.4(2) . . 0_555 yes C(8) Fe C(14) 116.7(2) . . 0_555 yes C(9) Fe C(10) 119.1(2) . . 0_555 yes C(9) Fe C(11) 154.1(2) . . 0_555 yes C(9) Fe C(12) 163.1(2) . . 0_555 yes C(9) Fe C(13) 125.5(2) . . 0_555 yes C(9) Fe C(14) 106.7(2) . . 0_555 yes C(10) Fe C(11) 40.3(2) . . 0_555 yes C(10) Fe C(12) 67.7(2) . . 0_555 yes C(10) Fe C(13) 67.7(2) . . 0_555 yes C(10) Fe C(14) 40.8(2) . . 0_555 yes C(11) Fe C(12) 40.4(2) . . 0_555 yes C(11) Fe C(13) 67.7(2) . . 0_555 yes C(11) Fe C(14) 68.0(2) . . 0_555 yes C(12) Fe C(13) 40.1(2) . . 0_555 yes C(12) Fe C(14) 67.5(2) . . 0_555 yes C(13) Fe C(14) 39.9(2) . . 0_555 yes C(1) N(1) C(4) 116.3(3) . . 0_555 yes C(1) N(2) C(2) 117.3(3) . . 0_555 yes N(1) C(1) N(2) 125.5(3) . . 0_555 yes N(2) C(2) C(3) 122.4(3) . . 0_555 yes C(2) C(3) C(4) 114.9(3) . . 0_555 yes C(2) C(3) C(5) 121.7(3) . . 0_555 yes C(4) C(3) C(5) 123.4(3) . . 0_555 yes N(1) C(4) C(3) 123.6(3) . . 0_555 yes Fe C(5) C(3) 124.0(2) . . 0_555 yes Fe C(5) C(6) 69.3(2) . . 0_555 yes Fe C(5) C(9) 69.5(2) . . 0_555 yes C(3) C(5) C(6) 126.0(3) . . 0_555 yes C(3) C(5) C(9) 126.6(3) . . 0_555 yes C(6) C(5) C(9) 107.3(3) . . 0_555 yes Fe C(6) C(5) 69.5(2) . . 0_555 yes Fe C(6) C(7) 70.1(2) . . 0_555 yes C(5) C(6) C(7) 108.4(3) . . 0_555 yes Fe C(7) C(6) 69.3(2) . . 0_555 yes Fe C(7) C(8) 69.5(2) . . 0_555 yes C(6) C(7) C(8) 107.4(3) . . 0_555 yes Fe C(8) C(7) 69.4(2) . . 0_555 yes Fe C(8) C(9) 69.5(2) . . 0_555 yes C(7) C(8) C(9) 108.4(3) . . 0_555 yes Fe C(9) C(5) 69.4(2) . . 0_555 yes Fe C(9) C(8) 70.2(2) . . 0_555 yes C(5) C(9) C(8) 108.4(3) . . 0_555 yes Fe C(10) C(11) 70.2(2) . . 0_555 yes Fe C(10) C(14) 69.9(2) . . 0_555 yes C(11) C(10) C(14) 108.0(4) . . 0_555 yes Fe C(11) C(10) 69.5(2) . . 0_555 yes Fe C(11) C(12) 69.8(3) . . 0_555 yes C(10) C(11) C(12) 107.5(4) . . 0_555 yes Fe C(12) C(11) 69.8(2) . . 0_555 yes Fe C(12) C(13) 69.6(2) . . 0_555 yes C(11) C(12) C(13) 108.0(4) . . 0_555 yes Fe C(13) C(12) 70.3(2) . . 0_555 yes Fe C(13) C(14) 70.4(2) . . 0_555 yes C(12) C(13) C(14) 109.1(4) . . 0_555 yes Fe C(14) C(10) 69.3(2) . . 0_555 yes Fe C(14) C(13) 69.7(2) . . 0_555 yes C(10) C(14) C(13) 107.3(4) . . 0_555 yes C(16) C(15) C(17) 119.5(2) . . 0_555 yes C(16) C(15) C(18) 122.7(2) . . 0_555 yes C(17) C(15) C(18) 117.9(2) . . 0_555 yes C(15) C(16) C(17) 119.7(2) . 7_747 0_555 yes C(15) C(16) C(19) 119.6(2) . . 0_555 yes C(17) C(16) C(19) 120.7(2) 7_747 . 0_555 yes C(15) C(17) C(16) 120.9(2) . 7_747 0_555 yes O(1) C(18) O(2) 125.4(3) . . 0_555 yes O(1) C(18) C(15) 112.5(3) . . 0_555 yes O(2) C(18) C(15) 122.0(3) . . 0_555 yes O(3) C(19) O(4) 122.8(3) . . 0_555 yes O(3) C(19) C(16) 114.0(2) . . 0_555 yes O(4) C(19) C(16) 123.1(3) . . 0_555 yes #------------------------------------------------------------------------------ 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe C(5) C(3) C(2) -88.6(4) 0_555 23_1 5_555 55_5 yes Fe C(5) C(3) C(4) 91.6(4) 0_555 23_1 5_555 55_5 yes Fe C(5) C(6) C(7) 59.5(2) 0_555 23_1 5_555 55_5 yes Fe C(5) C(9) C(8) -59.6(2) 0_555 23_1 5_555 55_5 yes Fe C(6) C(5) C(3) 117.6(3) 0_555 23_1 5_555 55_5 yes Fe C(6) C(5) C(9) -59.3(2) 0_555 23_1 5_555 55_5 yes Fe C(6) C(7) C(8) 59.3(3) 0_555 23_1 5_555 55_5 yes Fe C(7) C(6) C(5) -59.1(2) 0_555 23_1 5_555 55_5 yes Fe C(7) C(8) C(9) 58.7(3) 0_555 23_1 5_555 55_5 yes Fe C(8) C(7) C(6) -59.1(2) 0_555 23_1 5_555 55_5 yes Fe C(8) C(9) C(5) 59.1(2) 0_555 23_1 5_555 55_5 yes Fe C(9) C(5) C(3) -117.7(3) 0_555 23_1 5_555 55_5 yes Fe C(9) C(5) C(6) 59.2(2) 0_555 23_1 5_555 55_5 yes Fe C(9) C(8) C(7) -58.6(3) 0_555 23_1 5_555 55_5 yes Fe C(10) C(11) C(12) -59.7(3) 0_555 23_1 5_555 55_5 yes Fe C(10) C(14) C(13) 59.5(3) 0_555 23_1 5_555 55_5 yes Fe C(11) C(10) C(14) 59.9(3) 0_555 23_1 5_555 55_5 yes Fe C(11) C(12) C(13) -59.3(3) 0_555 23_1 5_555 55_5 yes Fe C(12) C(11) C(10) 59.6(3) 0_555 23_1 5_555 55_5 yes Fe C(12) C(13) C(14) -60.0(3) 0_555 23_1 5_555 55_5 yes Fe C(13) C(12) C(11) 59.5(3) 0_555 23_1 5_555 55_5 yes Fe C(13) C(14) C(10) -59.3(3) 0_555 23_1 5_555 55_5 yes Fe C(14) C(10) C(11) -60.1(3) 0_555 23_1 5_555 55_5 yes Fe C(14) C(13) C(12) 60.0(3) 0_555 23_1 5_555 55_5 yes O(1) C(18) C(15) C(16) 85.9(3) 0_555 23_1 5_555 55_5 yes O(1) C(18) C(15) C(17) -95.1(3) 0_555 23_1 5_555 55_5 yes O(2) C(18) C(15) C(16) -98.5(4) 0_555 23_1 5_555 55_5 yes O(2) C(18) C(15) C(17) 80.5(4) 0_555 23_1 5_555 55_5 yes O(3) C(19) C(16) C(15) 179.4(3) 0_555 23_1 5_555 55_5 yes O(3) C(19) C(16) C(17) 0.3(5) 0_555 23_1 5_555 55_5 yes O(4) C(19) C(16) C(15) -1.3(5) 0_555 23_1 5_555 55_5 yes O(4) C(19) C(16) C(17) 179.7(4) 0_555 23_1 5_555 55_5 yes N(1) C(1) N(2) C(2) -0.8(6) 0_555 23_1 5_555 55_5 yes N(1) C(4) C(3) C(2) 0.6(5) 0_555 23_1 5_555 55_5 yes N(1) C(4) C(3) C(5) -179.6(3) 0_555 23_1 5_555 55_5 yes N(2) C(1) N(1) C(4) 0.4(5) 0_555 23_1 5_555 55_5 yes N(2) C(2) C(3) C(4) -1.0(5) 0_555 23_1 5_555 55_5 yes N(2) C(2) C(3) C(5) 179.2(3) 0_555 23_1 5_555 55_5 yes C(1) N(1) C(4) C(3) -0.3(5) 0_555 23_1 5_555 55_5 yes C(1) N(2) C(2) C(3) 1.1(5) 0_555 23_1 5_555 55_5 yes C(2) C(3) C(5) C(6) -176.4(3) 0_555 23_1 5_555 55_5 yes C(2) C(3) C(5) C(9) -0.1(5) 0_555 23_1 5_555 55_5 yes C(3) C(5) Fe C(6) -120.2(3) 0_555 23_1 5_555 55_5 yes C(3) C(5) Fe C(7) -157.6(3) 0_555 23_1 5_555 55_5 yes C(3) C(5) Fe C(8) 158.2(3) 0_555 23_1 5_555 55_5 yes C(3) C(5) Fe C(9) 121.0(4) 0_555 23_1 5_555 55_5 yes C(3) C(5) Fe C(10) 8.3(3) 0_555 23_1 5_555 55_5 yes C(3) C(5) Fe C(11) -34.6(4) 0_555 23_1 5_555 55_5 yes C(3) C(5) Fe C(12) -69.8(5) 0_555 23_1 5_555 55_5 yes C(3) C(5) Fe C(13) 84.1(6) 0_555 23_1 5_555 55_5 yes C(3) C(5) Fe C(14) 50.3(3) 0_555 23_1 5_555 55_5 yes C(3) C(5) C(6) C(7) 177.1(3) 0_555 23_1 5_555 55_5 yes C(3) C(5) C(9) C(8) -177.3(3) 0_555 23_1 5_555 55_5 yes C(4) C(3) C(5) C(6) 3.7(5) 0_555 23_1 5_555 55_5 yes C(4) C(3) C(5) C(9) -179.9(3) 0_555 23_1 5_555 55_5 yes C(5) Fe C(6) C(7) -119.6(3) 0_555 23_1 5_555 55_5 yes C(5) Fe C(7) C(6) 37.8(2) 0_555 23_1 5_555 55_5 yes C(5) Fe C(7) C(8) -81.1(2) 0_555 23_1 5_555 55_5 yes C(5) Fe C(8) C(7) 82.2(2) 0_555 23_1 5_555 55_5 yes C(5) Fe C(8) C(9) -37.9(2) 0_555 23_1 5_555 55_5 yes C(5) Fe C(9) C(8) 119.5(3) 0_555 23_1 5_555 55_5 yes C(5) Fe C(10) C(11) -115.3(3) 0_555 23_1 5_555 55_5 yes C(5) Fe C(10) C(14) 125.8(3) 0_555 23_1 5_555 55_5 yes C(5) Fe C(11) C(10) 83.6(3) 0_555 23_1 5_555 55_5 yes C(5) Fe C(11) C(12) -157.7(3) 0_555 23_1 5_555 55_5 yes C(5) Fe C(12) C(11) 50.0(5) 0_555 23_1 5_555 55_5 yes C(5) Fe C(12) C(13) 169.2(3) 0_555 23_1 5_555 55_5 yes C(5) Fe C(13) C(12) -163.1(5) 0_555 23_1 5_555 55_5 yes C(5) Fe C(13) C(14) -43.4(6) 0_555 23_1 5_555 55_5 yes C(5) Fe C(14) C(10) -75.1(3) 0_555 23_1 5_555 55_5 yes C(5) Fe C(14) C(13) 166.2(3) 0_555 23_1 5_555 55_5 yes C(5) C(6) Fe C(7) 119.6(3) 0_555 23_1 5_555 55_5 yes C(5) C(6) Fe C(8) 81.4(2) 0_555 23_1 5_555 55_5 yes C(5) C(6) Fe C(9) 38.1(2) 0_555 23_1 5_555 55_5 yes C(5) C(6) Fe C(10) -73.0(3) 0_555 23_1 5_555 55_5 yes C(5) C(6) Fe C(11) -114.3(2) 0_555 23_1 5_555 55_5 yes C(5) C(6) Fe C(12) -157.7(2) 0_555 23_1 5_555 55_5 yes C(5) C(6) Fe C(13) 165.8(3) 0_555 23_1 5_555 55_5 yes C(5) C(6) Fe C(14) -35.1(8) 0_555 23_1 5_555 55_5 yes C(5) C(6) C(7) C(8) 0.1(4) 0_555 23_1 5_555 55_5 yes C(5) C(9) Fe C(6) -38.2(2) 0_555 23_1 5_555 55_5 yes C(5) C(9) Fe C(7) -81.9(2) 0_555 23_1 5_555 55_5 yes C(5) C(9) Fe C(8) -119.5(3) 0_555 23_1 5_555 55_5 yes C(5) C(9) Fe C(10) 86.2(3) 0_555 23_1 5_555 55_5 yes C(5) C(9) Fe C(11) 54.6(5) 0_555 23_1 5_555 55_5 yes C(5) C(9) Fe C(12) -164.0(5) 0_555 23_1 5_555 55_5 yes C(5) C(9) Fe C(13) 168.3(2) 0_555 23_1 5_555 55_5 yes C(5) C(9) Fe C(14) 128.6(2) 0_555 23_1 5_555 55_5 yes C(5) C(9) C(8) C(7) 0.5(4) 0_555 23_1 5_555 55_5 yes C(6) Fe C(5) C(9) 118.8(3) 0_555 23_1 5_555 55_5 yes C(6) Fe C(7) C(8) -118.9(3) 0_555 23_1 5_555 55_5 yes C(6) Fe C(8) C(7) 37.8(2) 0_555 23_1 5_555 55_5 yes C(6) Fe C(8) C(9) -82.3(2) 0_555 23_1 5_555 55_5 yes C(6) Fe C(9) C(8) 81.3(2) 0_555 23_1 5_555 55_5 yes C(6) Fe C(10) C(11) -73.5(3) 0_555 23_1 5_555 55_5 yes C(6) Fe C(10) C(14) 167.6(2) 0_555 23_1 5_555 55_5 yes C(6) Fe C(11) C(10) 128.0(3) 0_555 23_1 5_555 55_5 yes C(6) Fe C(11) C(12) -113.3(3) 0_555 23_1 5_555 55_5 yes C(6) Fe C(12) C(11) 85.9(3) 0_555 23_1 5_555 55_5 yes C(6) Fe C(12) C(13) -154.9(2) 0_555 23_1 5_555 55_5 yes C(6) Fe C(13) C(12) 53.1(5) 0_555 23_1 5_555 55_5 yes C(6) Fe C(13) C(14) 172.7(3) 0_555 23_1 5_555 55_5 yes C(6) Fe C(14) C(10) -46.5(8) 0_555 23_1 5_555 55_5 yes C(6) Fe C(14) C(13) -165.2(6) 0_555 23_1 5_555 55_5 yes C(6) C(5) Fe C(7) -37.4(2) 0_555 23_1 5_555 55_5 yes C(6) C(5) Fe C(8) -81.6(2) 0_555 23_1 5_555 55_5 yes C(6) C(5) Fe C(9) -118.8(3) 0_555 23_1 5_555 55_5 yes C(6) C(5) Fe C(10) 128.6(2) 0_555 23_1 5_555 55_5 yes C(6) C(5) Fe C(11) 85.7(3) 0_555 23_1 5_555 55_5 yes C(6) C(5) Fe C(12) 50.4(4) 0_555 23_1 5_555 55_5 yes C(6) C(5) Fe C(13) -155.7(5) 0_555 23_1 5_555 55_5 yes C(6) C(5) Fe C(14) 170.5(2) 0_555 23_1 5_555 55_5 yes C(6) C(5) C(9) C(8) -0.4(4) 0_555 23_1 5_555 55_5 yes C(6) C(7) Fe C(8) 118.9(3) 0_555 23_1 5_555 55_5 yes C(6) C(7) Fe C(9) 82.0(2) 0_555 23_1 5_555 55_5 yes C(6) C(7) Fe C(10) -46.8(8) 0_555 23_1 5_555 55_5 yes C(6) C(7) Fe C(11) -75.5(3) 0_555 23_1 5_555 55_5 yes C(6) C(7) Fe C(12) -115.6(3) 0_555 23_1 5_555 55_5 yes C(6) C(7) Fe C(13) -158.0(2) 0_555 23_1 5_555 55_5 yes C(6) C(7) Fe C(14) 168.5(3) 0_555 23_1 5_555 55_5 yes C(6) C(7) C(8) C(9) -0.4(4) 0_555 23_1 5_555 55_5 yes C(7) Fe C(5) C(9) 81.4(2) 0_555 23_1 5_555 55_5 yes C(7) Fe C(8) C(9) -120.1(3) 0_555 23_1 5_555 55_5 yes C(7) Fe C(9) C(8) 37.6(2) 0_555 23_1 5_555 55_5 yes C(7) Fe C(10) C(11) -35.5(8) 0_555 23_1 5_555 55_5 yes C(7) Fe C(10) C(14) -154.4(6) 0_555 23_1 5_555 55_5 yes C(7) Fe C(11) C(10) 170.2(2) 0_555 23_1 5_555 55_5 yes C(7) Fe C(11) C(12) -71.2(3) 0_555 23_1 5_555 55_5 yes C(7) Fe C(12) C(11) 128.7(3) 0_555 23_1 5_555 55_5 yes C(7) Fe C(12) C(13) -112.1(3) 0_555 23_1 5_555 55_5 yes C(7) Fe C(13) C(12) 85.2(3) 0_555 23_1 5_555 55_5 yes C(7) Fe C(13) C(14) -155.2(3) 0_555 23_1 5_555 55_5 yes C(7) Fe C(14) C(10) 168.2(3) 0_555 23_1 5_555 55_5 yes C(7) Fe C(14) C(13) 49.6(5) 0_555 23_1 5_555 55_5 yes C(7) C(6) Fe C(8) -38.2(2) 0_555 23_1 5_555 55_5 yes C(7) C(6) Fe C(9) -81.5(2) 0_555 23_1 5_555 55_5 yes C(7) C(6) Fe C(10) 167.4(3) 0_555 23_1 5_555 55_5 yes C(7) C(6) Fe C(11) 126.1(3) 0_555 23_1 5_555 55_5 yes C(7) C(6) Fe C(12) 82.7(3) 0_555 23_1 5_555 55_5 yes C(7) C(6) Fe C(13) 46.2(4) 0_555 23_1 5_555 55_5 yes C(7) C(6) Fe C(14) -154.7(7) 0_555 23_1 5_555 55_5 yes C(7) C(6) C(5) C(9) 0.2(4) 0_555 23_1 5_555 55_5 yes C(7) C(8) Fe C(9) 120.1(3) 0_555 23_1 5_555 55_5 yes C(7) C(8) Fe C(10) 173.1(3) 0_555 23_1 5_555 55_5 yes C(7) C(8) Fe C(11) -49.8(8) 0_555 23_1 5_555 55_5 yes C(7) C(8) Fe C(12) -74.6(3) 0_555 23_1 5_555 55_5 yes C(7) C(8) Fe C(13) -113.8(2) 0_555 23_1 5_555 55_5 yes C(7) C(8) Fe C(14) -155.4(2) 0_555 23_1 5_555 55_5 yes C(8) Fe C(5) C(9) 37.2(2) 0_555 23_1 5_555 55_5 yes C(8) Fe C(10) C(11) 164.4(3) 0_555 23_1 5_555 55_5 yes C(8) Fe C(10) C(14) 45.6(5) 0_555 23_1 5_555 55_5 yes C(8) Fe C(11) C(10) -150.0(6) 0_555 23_1 5_555 55_5 yes C(8) Fe C(11) C(12) -31.3(8) 0_555 23_1 5_555 55_5 yes C(8) Fe C(12) C(11) 170.5(3) 0_555 23_1 5_555 55_5 yes C(8) Fe C(12) C(13) -70.3(3) 0_555 23_1 5_555 55_5 yes C(8) Fe C(13) C(12) 128.0(3) 0_555 23_1 5_555 55_5 yes C(8) Fe C(13) C(14) -112.3(3) 0_555 23_1 5_555 55_5 yes C(8) Fe C(14) C(10) -157.7(3) 0_555 23_1 5_555 55_5 yes C(8) Fe C(14) C(13) 83.7(3) 0_555 23_1 5_555 55_5 yes C(8) C(7) Fe C(9) -36.9(2) 0_555 23_1 5_555 55_5 yes C(8) C(7) Fe C(10) -165.7(6) 0_555 23_1 5_555 55_5 yes C(8) C(7) Fe C(11) 165.6(2) 0_555 23_1 5_555 55_5 yes C(8) C(7) Fe C(12) 125.5(3) 0_555 23_1 5_555 55_5 yes C(8) C(7) Fe C(13) 83.1(3) 0_555 23_1 5_555 55_5 yes C(8) C(7) Fe C(14) 49.6(4) 0_555 23_1 5_555 55_5 yes C(8) C(9) Fe C(10) -154.3(3) 0_555 23_1 5_555 55_5 yes C(8) C(9) Fe C(11) 174.1(4) 0_555 23_1 5_555 55_5 yes C(8) C(9) Fe C(12) -44.5(7) 0_555 23_1 5_555 55_5 yes C(8) C(9) Fe C(13) -72.1(3) 0_555 23_1 5_555 55_5 yes C(8) C(9) Fe C(14) -111.8(3) 0_555 23_1 5_555 55_5 yes C(9) Fe C(10) C(11) -159.3(3) 0_555 23_1 5_555 55_5 yes C(9) Fe C(10) C(14) 81.8(3) 0_555 23_1 5_555 55_5 yes C(9) Fe C(11) C(10) 45.1(5) 0_555 23_1 5_555 55_5 yes C(9) Fe C(11) C(12) 163.7(3) 0_555 23_1 5_555 55_5 yes C(9) Fe C(12) C(11) -155.2(5) 0_555 23_1 5_555 55_5 yes C(9) Fe C(12) C(13) -35.9(7) 0_555 23_1 5_555 55_5 yes C(9) Fe C(13) C(12) 167.9(3) 0_555 23_1 5_555 55_5 yes C(9) Fe C(13) C(14) -72.4(3) 0_555 23_1 5_555 55_5 yes C(9) Fe C(14) C(10) -115.5(3) 0_555 23_1 5_555 55_5 yes C(9) Fe C(14) C(13) 125.9(3) 0_555 23_1 5_555 55_5 yes C(9) C(5) Fe C(10) -112.7(3) 0_555 23_1 5_555 55_5 yes C(9) C(5) Fe C(11) -155.6(2) 0_555 23_1 5_555 55_5 yes C(9) C(5) Fe C(12) 169.2(4) 0_555 23_1 5_555 55_5 yes C(9) C(5) Fe C(13) -36.9(6) 0_555 23_1 5_555 55_5 yes C(9) C(5) Fe C(14) -70.7(3) 0_555 23_1 5_555 55_5 yes C(9) C(8) Fe C(10) 53.0(4) 0_555 23_1 5_555 55_5 yes C(9) C(8) Fe C(11) -169.9(6) 0_555 23_1 5_555 55_5 yes C(9) C(8) Fe C(12) 165.3(2) 0_555 23_1 5_555 55_5 yes C(9) C(8) Fe C(13) 126.2(3) 0_555 23_1 5_555 55_5 yes C(9) C(8) Fe C(14) 84.5(3) 0_555 23_1 5_555 55_5 yes C(10) Fe C(11) C(12) 118.7(4) 0_555 23_1 5_555 55_5 yes C(10) Fe C(12) C(11) -37.8(3) 0_555 23_1 5_555 55_5 yes C(10) Fe C(12) C(13) 81.4(3) 0_555 23_1 5_555 55_5 yes C(10) Fe C(13) C(12) -81.4(3) 0_555 23_1 5_555 55_5 yes C(10) Fe C(13) C(14) 38.3(3) 0_555 23_1 5_555 55_5 yes C(10) Fe C(14) C(13) -118.7(4) 0_555 23_1 5_555 55_5 yes C(10) C(11) Fe C(12) -118.7(4) 0_555 23_1 5_555 55_5 yes C(10) C(11) Fe C(13) -81.3(3) 0_555 23_1 5_555 55_5 yes C(10) C(11) Fe C(14) -38.1(3) 0_555 23_1 5_555 55_5 yes C(10) C(11) C(12) C(13) 0.2(5) 0_555 23_1 5_555 55_5 yes C(10) C(14) Fe C(11) 37.6(3) 0_555 23_1 5_555 55_5 yes C(10) C(14) Fe C(12) 81.4(3) 0_555 23_1 5_555 55_5 yes C(10) C(14) Fe C(13) 118.7(4) 0_555 23_1 5_555 55_5 yes C(10) C(14) C(13) C(12) 0.7(5) 0_555 23_1 5_555 55_5 yes C(11) Fe C(10) C(14) -118.9(4) 0_555 23_1 5_555 55_5 yes C(11) Fe C(12) C(13) 119.2(4) 0_555 23_1 5_555 55_5 yes C(11) Fe C(13) C(12) -37.7(3) 0_555 23_1 5_555 55_5 yes C(11) Fe C(13) C(14) 82.0(3) 0_555 23_1 5_555 55_5 yes C(11) Fe C(14) C(13) -81.0(3) 0_555 23_1 5_555 55_5 yes C(11) C(10) Fe C(12) 37.9(3) 0_555 23_1 5_555 55_5 yes C(11) C(10) Fe C(13) 81.4(3) 0_555 23_1 5_555 55_5 yes C(11) C(10) Fe C(14) 118.9(4) 0_555 23_1 5_555 55_5 yes C(11) C(10) C(14) C(13) -0.5(5) 0_555 23_1 5_555 55_5 yes C(11) C(12) Fe C(13) -119.2(4) 0_555 23_1 5_555 55_5 yes C(11) C(12) Fe C(14) -82.1(3) 0_555 23_1 5_555 55_5 yes C(11) C(12) C(13) C(14) -0.5(5) 0_555 23_1 5_555 55_5 yes C(12) Fe C(10) C(14) -81.0(3) 0_555 23_1 5_555 55_5 yes C(12) Fe C(13) C(14) 119.7(4) 0_555 23_1 5_555 55_5 yes C(12) Fe C(14) C(13) -37.2(3) 0_555 23_1 5_555 55_5 yes C(12) C(11) Fe C(13) 37.4(3) 0_555 23_1 5_555 55_5 yes C(12) C(11) Fe C(14) 80.6(3) 0_555 23_1 5_555 55_5 yes C(12) C(11) C(10) C(14) 0.2(5) 0_555 23_1 5_555 55_5 yes C(12) C(13) Fe C(14) -119.7(4) 0_555 23_1 5_555 55_5 yes C(13) Fe C(10) C(14) -37.5(3) 0_555 23_1 5_555 55_5 yes C(13) C(12) Fe C(14) 37.1(3) 0_555 23_1 5_555 55_5 yes C(15) C(17) C(16) C(19) -178.3(3) 0_555 23_1 5_555 55_5 yes C(16) C(17) C(15) C(18) 179.9(3) 0_555 23_1 5_555 55_5 yes C(17) C(15) C(16) C(19) -178.3(3) 0_555 23_1 5_555 55_5 yes C(17) C(16) C(15) C(18) -179.8(3) 0_555 23_1 5_555 55_5 yes C(18) C(15) C(16) C(19) 0.7(4) 0_555 23_1 5_555 55_5 yes C(18) C(15) C(16) C(19) 0.7(4) 0_555 23_1 5_555 55_5 yes #------------------------------------------------------------------------------ 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(1) 2.778(3) . . ? O(1) O(1) 3.010(4) . 3_757 ? O(1) N(1) 3.251(4) . 3_757 ? O(1) C(4) 3.260(4) . 3_757 ? O(1) C(12) 3.374(5) . 4_555 ? O(1) C(4) 3.545(4) . . ? O(2) C(9) 3.293(4) . 5_545 ? O(2) N(1) 3.515(4) . . ? O(3) N(2) 2.737(4) . 7_647 ? O(3) C(14) 3.175(5) . 8_545 ? O(3) C(10) 3.297(5) . 8_545 ? O(3) C(1) 3.520(4) . 7_647 ? O(4) C(1) 3.235(4) . 7_647 ? O(4) C(13) 3.263(6) . 6_646 ? O(4) N(2) 3.316(4) . 7_647 ? O(4) C(14) 3.335(6) . 6_646 ? O(4) C(12) 3.450(6) . 4_555 ? N(1) C(18) 3.524(4) . . ? N(2) C(19) 3.426(4) . 7_647 ? N(2) C(19) 3.528(4) . 5_455 ? N(2) C(16) 3.591(4) . 5_455 ? C(2) C(16) 3.480(4) . 5_455 ? C(2) C(15) 3.595(5) . 5_455 ? C(4) C(15) 3.498(4) . 3_757 ? C(5) C(17) 3.506(4) . 5_455 ? #------------------------------------------------------------------------------ loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_site_distance_DH _geom_hbond_site_distance_HA _geom_hbond_site_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O(1) H(13) N(1) . . 1_555 0.950 1.835 2.778(3) 171.470 no #------------------------------------------------------------------------------ #-----------END #------------------------------------------------------------------------------ data_compound_8 _database_code_CSD 206168 _publ_section_exptl_refinement ; Hydrogen atoms bonded to O2 and O3 are disordered and not located. ; #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C20 H22 Fe N2 O5 ' _chemical_formula_moiety ? _chemical_formula_weight 426.25 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcm _symmetry_Int_Tables_number 57 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,1/2+z x,1/2-y,-z -x,1/2+y,1/2-z -x,-y,-z x,y,1/2-z -x,1/2+y,z x,1/2-y,1/2+z _cell_length_a 7.997(3) _cell_length_b 14.278(2) _cell_length_c 17.219(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1966.3(10) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.2 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.8 _exptl_crystal_size_min 0.2 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.800 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.818 _exptl_absorpt_correction_T_max 1.000 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 2703 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 1.0000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.0000 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.58 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2343 _reflns_number_gt 1437 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1707 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1437 _refine_ls_number_parameters 136 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.12500(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0019 _refine_diff_density_max 0.39 _refine_diff_density_min -0.35 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Fe Fe 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe -0.0713(1) -0.19417(6) -0.7500 0.0523(2) Uani 1.00 d S . . O(1) O -0.5888(3) -0.3984(2) -0.5601(2) 0.0676(10) Uani 1.00 d . . . O(2) O -0.0699(4) -0.2500 -0.5000 0.059(1) Uani 1.00 d S . . O(3) O 0.0829(4) -0.4195(3) -0.5088(3) 0.104(2) Uani 1.00 d . . . N N 0.4241(5) 0.0187(3) -0.6817(3) 0.068(1) Uani 1.00 d . . . C(1) C 0.4687(8) 0.0528(5) -0.7500 0.069(2) Uani 1.00 d S . . C(2) C 0.3299(6) -0.0580(4) -0.6824(3) 0.064(1) Uani 1.00 d . . . C(3) C 0.2788(7) -0.1020(4) -0.7500 0.054(2) Uani 1.00 d S . . C(4) C 0.1808(8) -0.1891(4) -0.7500 0.058(2) Uani 1.00 d S . . C(5) C 0.1214(6) -0.2379(3) -0.6840(3) 0.064(1) Uani 1.00 d . . . C(6) C 0.0279(7) -0.3159(3) -0.7091(3) 0.073(2) Uani 1.00 d . . . C(7) C -0.159(1) -0.0615(5) -0.7500 0.103(3) Uani 1.00 d S . . C(8) C -0.2205(8) -0.1100(5) -0.6846(4) 0.093(2) Uani 1.00 d . . . C(9) C -0.3109(7) -0.1846(4) -0.7099(4) 0.087(2) Uani 1.00 d . . . C(10) C -0.5881(6) -0.2500 -0.5000 0.047(1) Uani 1.00 d S . . C(11) C -0.5001(4) -0.3251(3) -0.5300(2) 0.046(1) Uani 1.00 d . . . C(12) C -0.3254(4) -0.3266(3) -0.5296(2) 0.046(1) Uani 1.00 d . . . C(13) C -0.2426(6) -0.2500 -0.5000 0.043(1) Uani 1.00 d S . . H(1) H 0.5401 0.1082 -0.7500 0.0760 Uiso 1.00 calc S . . H(2) H 0.2961 -0.0842 -0.6343 0.0772 Uiso 1.00 calc . . . H(3) H 0.1405 -0.2206 -0.6315 0.0773 Uiso 1.00 calc . . . H(4) H -0.0310 -0.3601 -0.6748 0.0760 Uiso 1.00 calc . . . H(5) H -0.0903 -0.0059 -0.7500 0.0760 Uiso 1.00 calc S . . H(6) H -0.2018 -0.0930 -0.6301 0.1100 Uiso 1.00 calc . . . H(7) H -0.3665 -0.2288 -0.6764 0.0760 Uiso 1.00 calc . . . H(8) H -0.7083 -0.2500 -0.5000 0.0760 Uiso 1.00 calc S . . H(9) H -0.2658 -0.3790 -0.5491 0.0548 Uiso 1.00 calc . . . H(10) H -0.7076 -0.3967 -0.5601 0.0810 Uiso 1.00 calc . . . 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 0.0672(6) 0.0396(4) 0.0500(5) -0.0011(4) 0.0000 0.0000 O(1) 0.035(1) 0.070(2) 0.098(3) -0.009(1) 0.007(1) -0.037(2) O(2) 0.028(2) 0.061(3) 0.087(3) 0.0000 0.0000 -0.006(2) O(3) 0.062(2) 0.070(2) 0.181(5) -0.009(2) 0.045(2) -0.009(3) N 0.066(2) 0.064(2) 0.074(3) 0.001(2) 0.000(2) -0.016(2) C(1) 0.054(3) 0.058(4) 0.095(5) 0.005(3) 0.0000 0.0000 C(2) 0.065(3) 0.072(3) 0.055(3) -0.008(2) 0.002(2) -0.005(2) C(3) 0.053(3) 0.054(3) 0.054(3) 0.004(3) 0.0000 0.0000 C(4) 0.066(4) 0.051(3) 0.055(3) 0.009(3) 0.0000 0.0000 C(5) 0.080(3) 0.055(3) 0.057(3) 0.007(2) -0.006(2) 0.010(2) C(6) 0.092(4) 0.045(3) 0.082(3) 0.004(2) 0.007(3) 0.014(2) C(7) 0.071(5) 0.040(4) 0.20(1) 0.005(4) 0.0000 0.0000 C(8) 0.097(4) 0.096(4) 0.086(4) 0.035(4) 0.003(3) -0.025(4) C(9) 0.080(3) 0.086(4) 0.096(4) 0.002(3) 0.017(3) 0.016(3) C(10) 0.027(2) 0.052(3) 0.061(3) 0.0000 0.0000 -0.009(3) C(11) 0.037(2) 0.048(2) 0.052(2) -0.007(2) 0.003(2) -0.006(2) C(12) 0.035(2) 0.046(2) 0.056(2) 0.003(1) 0.005(2) -0.010(2) C(13) 0.029(2) 0.054(3) 0.046(3) 0.0000 0.0000 0.000(2) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 C(4) 2.017(7) . . yes Fe C(5) 2.015(5) . . yes Fe C(5) 2.015(5) . 6_553 yes Fe C(6) 2.036(5) . . yes Fe C(6) 2.036(5) . 6_553 yes Fe C(7) 2.019(8) . . yes Fe C(8) 2.034(5) . . yes Fe C(8) 2.034(5) . 6_553 yes Fe C(9) 2.042(6) . . yes Fe C(9) 2.042(6) . 6_553 yes O(1) C(11) 1.366(5) . . yes O(2) C(13) 1.381(6) . . yes N C(1) 1.322(5) . . yes N C(2) 1.329(6) . . yes C(2) C(3) 1.384(6) . . yes C(3) C(4) 1.471(9) . . yes C(4) C(5) 1.415(6) . . yes C(4) C(5) 1.415(6) . 6_553 yes C(5) C(6) 1.409(7) . . yes C(6) C(6) 1.41(1) . 6_553 yes C(7) C(8) 1.412(8) . . yes C(7) C(8) 1.412(8) . 6_553 yes C(8) C(9) 1.359(9) . . yes C(9) C(9) 1.38(1) . 6_553 yes C(10) C(11) 1.383(4) . . yes C(10) C(11) 1.383(4) . 3_544 yes C(11) C(12) 1.397(5) . . yes C(12) C(13) 1.377(4) . . 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 C(4) Fe C(5) 41.1(2) . . 0_555 yes C(4) Fe C(5) 41.1(2) . 6_553 0_555 yes C(4) Fe C(6) 69.0(2) . . 0_555 yes C(4) Fe C(6) 69.0(2) . 6_553 0_555 yes C(4) Fe C(7) 108.2(3) . . 0_555 yes C(4) Fe C(8) 124.4(2) . . 0_555 yes C(4) Fe C(8) 124.4(2) . 6_553 0_555 yes C(4) Fe C(9) 159.3(2) . . 0_555 yes C(4) Fe C(9) 159.3(2) . 6_553 0_555 yes C(5) Fe C(5) 68.7(3) . 6_553 0_555 yes C(5) Fe C(6) 40.7(2) . . 0_555 yes C(5) Fe C(6) 68.4(2) . 6_553 0_555 yes C(5) Fe C(7) 123.8(2) . . 0_555 yes C(5) Fe C(8) 108.6(2) . . 0_555 yes C(5) Fe C(8) 160.8(3) . 6_553 0_555 yes C(5) Fe C(9) 123.2(2) . . 0_555 yes C(5) Fe C(9) 158.4(2) . 6_553 0_555 yes C(5) Fe C(6) 68.4(2) 6_553 . 0_555 yes C(5) Fe C(6) 40.7(2) 6_553 6_553 0_555 yes C(5) Fe C(7) 123.8(2) 6_553 . 0_555 yes C(5) Fe C(8) 160.8(3) 6_553 . 0_555 yes C(5) Fe C(8) 108.6(2) 6_553 6_553 0_555 yes C(5) Fe C(9) 158.4(2) 6_553 . 0_555 yes C(5) Fe C(9) 123.2(2) 6_553 6_553 0_555 yes C(6) Fe C(6) 40.5(3) . 6_553 0_555 yes C(6) Fe C(7) 159.3(2) . . 0_555 yes C(6) Fe C(8) 122.7(2) . . 0_555 yes C(6) Fe C(8) 157.6(3) . 6_553 0_555 yes C(6) Fe C(9) 107.8(2) . . 0_555 yes C(6) Fe C(9) 122.7(2) . 6_553 0_555 yes C(6) Fe C(7) 159.3(2) 6_553 . 0_555 yes C(6) Fe C(8) 157.6(3) 6_553 . 0_555 yes C(6) Fe C(8) 122.7(2) 6_553 6_553 0_555 yes C(6) Fe C(9) 122.7(2) 6_553 . 0_555 yes C(6) Fe C(9) 107.8(2) 6_553 6_553 0_555 yes C(7) Fe C(8) 40.8(2) . . 0_555 yes C(7) Fe C(8) 40.8(2) . 6_553 0_555 yes C(7) Fe C(9) 67.2(3) . . 0_555 yes C(7) Fe C(9) 67.2(3) . 6_553 0_555 yes C(8) Fe C(8) 67.3(4) . 6_553 0_555 yes C(8) Fe C(9) 39.0(3) . . 0_555 yes C(8) Fe C(9) 66.2(3) . 6_553 0_555 yes C(8) Fe C(9) 66.2(3) 6_553 . 0_555 yes C(8) Fe C(9) 39.0(3) 6_553 6_553 0_555 yes C(9) Fe C(9) 39.5(4) . 6_553 0_555 yes C(1) N C(2) 116.6(5) . . 0_555 yes N C(1) N 125.7(7) . 6_553 0_555 yes N C(2) C(3) 123.3(5) . . 0_555 yes C(2) C(3) C(2) 114.5(6) . 6_553 0_555 yes C(2) C(3) C(4) 122.8(3) . . 0_555 yes C(2) C(3) C(4) 122.8(3) 6_553 . 0_555 yes Fe C(4) C(3) 124.2(4) . . 0_555 yes Fe C(4) C(5) 69.3(3) . . 0_555 yes Fe C(4) C(5) 69.3(3) . 6_553 0_555 yes C(3) C(4) C(5) 126.5(3) . . 0_555 yes C(3) C(4) C(5) 126.5(3) . 6_553 0_555 yes C(5) C(4) C(5) 106.9(6) . 6_553 0_555 yes Fe C(5) C(4) 69.6(3) . . 0_555 yes Fe C(5) C(6) 70.5(3) . . 0_555 yes C(4) C(5) C(6) 108.7(5) . . 0_555 yes Fe C(6) C(5) 68.8(3) . . 0_555 yes Fe C(6) C(6) 69.7(2) . 6_553 0_555 yes C(5) C(6) C(6) 107.8(3) . 6_553 0_555 yes Fe C(7) C(8) 70.2(4) . . 0_555 yes Fe C(7) C(8) 70.2(4) . 6_553 0_555 yes C(8) C(7) C(8) 105.9(7) . 6_553 0_555 yes Fe C(8) C(7) 69.0(4) . . 0_555 yes Fe C(8) C(9) 70.8(4) . . 0_555 yes C(7) C(8) C(9) 108.3(6) . . 0_555 yes Fe C(9) C(8) 70.2(3) . . 0_555 yes Fe C(9) C(9) 70.2(2) . 6_553 0_555 yes C(8) C(9) C(9) 108.7(4) . 6_553 0_555 yes C(11) C(10) C(11) 118.8(4) . 3_544 0_555 yes O(1) C(11) C(10) 118.1(3) . . 0_555 yes O(1) C(11) C(12) 120.6(3) . . 0_555 yes C(10) C(11) C(12) 121.3(4) . . 0_555 yes C(11) C(12) C(13) 118.1(3) . . 0_555 yes O(2) C(13) C(12) 118.8(2) . . 0_555 yes O(2) C(13) C(12) 118.8(2) . 3_544 0_555 yes C(12) C(13) C(12) 122.5(4) . 3_544 0_555 yes #------------------------------------------------------------------------------ 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe C(4) C(3) C(2) 90.5(5) 0_555 22_1 5_555 44_5 yes Fe C(4) C(3) C(2) -90.5(5) 0_555 22_1 5_555 44_5 yes Fe C(4) C(5) C(6) 59.8(4) 0_555 22_1 5_555 44_5 yes Fe C(4) C(5) C(6) -59.8(4) 0_555 22_1 5_555 44_5 yes Fe C(5) C(4) C(3) 118.0(6) 0_555 22_1 5_555 44_5 yes Fe C(5) C(4) C(5) -59.4(4) 0_555 22_1 5_555 44_5 yes Fe C(5) C(6) C(6) 59.0(1) 0_555 22_1 5_555 44_5 yes Fe C(5) C(4) C(3) -118.0(6) 0_555 22_1 5_555 44_5 yes Fe C(5) C(4) C(5) 59.4(4) 0_555 22_1 5_555 44_5 yes Fe C(5) C(6) C(6) -59.0(1) 0_555 22_1 5_555 44_5 yes Fe C(6) C(5) C(4) -59.2(4) 0_555 22_1 5_555 44_5 yes Fe C(6) C(6) C(5) 58.4(3) 0_555 22_1 5_555 44_5 yes Fe C(6) C(5) C(4) 59.2(4) 0_555 22_1 5_555 44_5 yes Fe C(6) C(6) C(5) -58.4(3) 0_555 22_1 5_555 44_5 yes Fe C(7) C(8) C(9) -60.1(5) 0_555 22_1 5_555 44_5 yes Fe C(7) C(8) C(9) 60.1(5) 0_555 22_1 5_555 44_5 yes Fe C(8) C(7) C(8) 61.5(5) 0_555 22_1 5_555 44_5 yes Fe C(8) C(9) C(9) -59.9(2) 0_555 22_1 5_555 44_5 yes Fe C(8) C(7) C(8) -61.5(5) 0_555 22_1 5_555 44_5 yes Fe C(8) C(9) C(9) 59.9(2) 0_555 22_1 5_555 44_5 yes Fe C(9) C(8) C(7) 59.0(5) 0_555 22_1 5_555 44_5 yes Fe C(9) C(9) C(8) -59.9(3) 0_555 22_1 5_555 44_5 yes Fe C(9) C(8) C(7) -59.0(5) 0_555 22_1 5_555 44_5 yes Fe C(9) C(9) C(8) 59.9(3) 0_555 22_1 5_555 44_5 yes O(1) C(11) C(10) C(11) -179.4(4) 0_555 22_1 5_555 44_5 yes O(1) C(11) C(12) C(13) 178.7(3) 0_555 22_1 5_555 44_5 yes O(2) C(13) C(12) C(11) -179.3(3) 0_555 22_1 5_555 44_5 yes O(2) C(13) C(12) C(11) -179.3(3) 0_555 22_1 5_555 44_5 yes N C(1) N C(2) -2.0(10) 0_555 22_1 5_555 44_5 yes N C(2) C(3) C(2) -1.8(9) 0_555 22_1 5_555 44_5 yes N C(2) C(3) C(4) 177.2(5) 0_555 22_1 5_555 44_5 yes C(1) N C(2) C(3) 0.1(8) 0_555 22_1 5_555 44_5 yes C(1) N C(2) C(3) -0.1(8) 0_555 22_1 5_555 44_5 yes C(2) C(3) C(4) C(5) 2.1(10) 0_555 22_1 5_555 44_5 yes C(2) C(3) C(4) C(5) 179.0(5) 0_555 22_1 5_555 44_5 yes C(3) C(4) Fe C(5) -120.9(3) 0_555 22_1 5_555 44_5 yes C(3) C(4) Fe C(5) 120.9(3) 0_555 22_1 5_555 44_5 yes C(3) C(4) Fe C(6) -158.2(2) 0_555 22_1 5_555 44_5 yes C(3) C(4) Fe C(6) 158.2(2) 0_555 22_1 5_555 44_5 yes C(3) C(4) Fe C(7) 0.0 0_555 22_1 5_555 44_5 yes C(3) C(4) Fe C(8) -42.2(3) 0_555 22_1 5_555 44_5 yes C(3) C(4) Fe C(8) 42.2(3) 0_555 22_1 5_555 44_5 yes C(3) C(4) Fe C(9) -73.5(7) 0_555 22_1 5_555 44_5 yes C(3) C(4) Fe C(9) 73.5(7) 0_555 22_1 5_555 44_5 yes C(3) C(4) C(5) C(6) 177.8(6) 0_555 22_1 5_555 44_5 yes C(3) C(4) C(5) C(6) -177.8(6) 0_555 22_1 5_555 44_5 yes C(4) Fe C(5) C(6) -119.7(4) 0_555 22_1 5_555 44_5 yes C(4) Fe C(5) C(6) 119.7(4) 0_555 22_1 5_555 44_5 yes C(4) Fe C(6) C(5) 37.7(3) 0_555 22_1 5_555 44_5 yes C(4) Fe C(6) C(6) -81.8(1) 0_555 22_1 5_555 44_5 yes C(4) Fe C(6) C(5) -37.7(3) 0_555 22_1 5_555 44_5 yes C(4) Fe C(6) C(6) 81.8(1) 0_555 22_1 5_555 44_5 yes C(4) Fe C(7) C(8) -122.0(4) 0_555 22_1 5_555 44_5 yes C(4) Fe C(7) C(8) 122.0(4) 0_555 22_1 5_555 44_5 yes C(4) Fe C(8) C(7) 77.6(4) 0_555 22_1 5_555 44_5 yes C(4) Fe C(8) C(9) -163.1(4) 0_555 22_1 5_555 44_5 yes C(4) Fe C(8) C(7) -77.6(4) 0_555 22_1 5_555 44_5 yes C(4) Fe C(8) C(9) 163.1(4) 0_555 22_1 5_555 44_5 yes C(4) Fe C(9) C(8) 43.0(9) 0_555 22_1 5_555 44_5 yes C(4) Fe C(9) C(9) 162.4(7) 0_555 22_1 5_555 44_5 yes C(4) Fe C(9) C(8) -43.0(9) 0_555 22_1 5_555 44_5 yes C(4) Fe C(9) C(9) -162.4(7) 0_555 22_1 5_555 44_5 yes C(4) C(5) Fe C(5) 38.4(3) 0_555 22_1 5_555 44_5 yes C(4) C(5) Fe C(6) 119.7(4) 0_555 22_1 5_555 44_5 yes C(4) C(5) Fe C(6) 82.3(3) 0_555 22_1 5_555 44_5 yes C(4) C(5) Fe C(7) -78.8(4) 0_555 22_1 5_555 44_5 yes C(4) C(5) Fe C(8) -121.4(4) 0_555 22_1 5_555 44_5 yes C(4) C(5) Fe C(8) -47.2(8) 0_555 22_1 5_555 44_5 yes C(4) C(5) Fe C(9) -161.9(3) 0_555 22_1 5_555 44_5 yes C(4) C(5) Fe C(9) 166.3(6) 0_555 22_1 5_555 44_5 yes C(4) C(5) C(6) C(6) -0.2(5) 0_555 22_1 5_555 44_5 yes C(4) C(5) Fe C(5) -38.4(3) 0_555 22_1 5_555 44_5 yes C(4) C(5) Fe C(6) -82.3(3) 0_555 22_1 5_555 44_5 yes C(4) C(5) Fe C(6) -119.7(4) 0_555 22_1 5_555 44_5 yes C(4) C(5) Fe C(7) 78.8(4) 0_555 22_1 5_555 44_5 yes C(4) C(5) Fe C(8) 47.2(8) 0_555 22_1 5_555 44_5 yes C(4) C(5) Fe C(8) 121.4(4) 0_555 22_1 5_555 44_5 yes C(4) C(5) Fe C(9) -166.3(6) 0_555 22_1 5_555 44_5 yes C(4) C(5) Fe C(9) 161.9(3) 0_555 22_1 5_555 44_5 yes C(4) C(5) C(6) C(6) 0.2(5) 0_555 22_1 5_555 44_5 yes C(5) Fe C(5) C(6) 81.3(3) 0_555 22_1 5_555 44_5 yes C(5) Fe C(6) C(6) -119.5(3) 0_555 22_1 5_555 44_5 yes C(5) Fe C(6) C(6) 37.6(2) 0_555 22_1 5_555 44_5 yes C(5) Fe C(7) C(8) -79.3(5) 0_555 22_1 5_555 44_5 yes C(5) Fe C(7) C(8) 164.7(4) 0_555 22_1 5_555 44_5 yes C(5) Fe C(8) C(7) 120.4(4) 0_555 22_1 5_555 44_5 yes C(5) Fe C(8) C(9) -120.2(4) 0_555 22_1 5_555 44_5 yes C(5) Fe C(8) C(7) -41.8(9) 0_555 22_1 5_555 44_5 yes C(5) Fe C(8) C(9) -161.2(6) 0_555 22_1 5_555 44_5 yes C(5) Fe C(9) C(8) 78.3(4) 0_555 22_1 5_555 44_5 yes C(5) Fe C(9) C(9) -162.3(2) 0_555 22_1 5_555 44_5 yes C(5) Fe C(9) C(8) 163.3(5) 0_555 22_1 5_555 44_5 yes C(5) Fe C(9) C(9) 43.8(5) 0_555 22_1 5_555 44_5 yes C(5) C(4) Fe C(6) -37.4(3) 0_555 22_1 5_555 44_5 yes C(5) C(4) Fe C(6) -80.9(3) 0_555 22_1 5_555 44_5 yes C(5) C(4) Fe C(7) 120.9(3) 0_555 22_1 5_555 44_5 yes C(5) C(4) Fe C(8) 78.7(4) 0_555 22_1 5_555 44_5 yes C(5) C(4) Fe C(8) 163.0(3) 0_555 22_1 5_555 44_5 yes C(5) C(4) Fe C(9) 47.4(8) 0_555 22_1 5_555 44_5 yes C(5) C(4) Fe C(9) -165.7(6) 0_555 22_1 5_555 44_5 yes C(5) C(4) C(5) C(6) -0.4(7) 0_555 22_1 5_555 44_5 yes C(5) C(6) Fe C(6) 119.5(3) 0_555 22_1 5_555 44_5 yes C(5) C(6) Fe C(7) -48.2(9) 0_555 22_1 5_555 44_5 yes C(5) C(6) Fe C(8) -80.5(4) 0_555 22_1 5_555 44_5 yes C(5) C(6) Fe C(8) 168.7(6) 0_555 22_1 5_555 44_5 yes C(5) C(6) Fe C(9) -120.6(3) 0_555 22_1 5_555 44_5 yes C(5) C(6) Fe C(9) -161.5(3) 0_555 22_1 5_555 44_5 yes C(5) C(6) C(6) C(5) 0.0 0_555 22_1 5_555 44_5 yes C(6) Fe C(7) C(8) -43.5(10) 0_555 22_1 5_555 44_5 yes C(6) Fe C(7) C(8) -159.5(6) 0_555 22_1 5_555 44_5 yes C(6) Fe C(8) C(7) 163.2(4) 0_555 22_1 5_555 44_5 yes C(6) Fe C(8) C(9) -77.4(5) 0_555 22_1 5_555 44_5 yes C(6) Fe C(8) C(7) 161.0(5) 0_555 22_1 5_555 44_5 yes C(6) Fe C(8) C(9) 41.7(8) 0_555 22_1 5_555 44_5 yes C(6) Fe C(9) C(8) 120.4(4) 0_555 22_1 5_555 44_5 yes C(6) Fe C(9) C(9) -120.1(2) 0_555 22_1 5_555 44_5 yes C(6) Fe C(9) C(8) -162.5(4) 0_555 22_1 5_555 44_5 yes C(6) Fe C(9) C(9) 78.1(2) 0_555 22_1 5_555 44_5 yes C(6) C(5) Fe C(7) 161.5(3) 0_555 22_1 5_555 44_5 yes C(6) C(5) Fe C(8) 118.9(4) 0_555 22_1 5_555 44_5 yes C(6) C(5) Fe C(8) -166.9(7) 0_555 22_1 5_555 44_5 yes C(6) C(5) Fe C(9) 78.4(4) 0_555 22_1 5_555 44_5 yes C(6) C(5) Fe C(9) 46.6(7) 0_555 22_1 5_555 44_5 yes C(6) C(6) Fe C(7) 167.8(8) 0_555 22_1 5_555 44_5 yes C(6) C(6) Fe C(8) -49.2(6) 0_555 22_1 5_555 44_5 yes C(6) C(6) Fe C(8) -159.9(3) 0_555 22_1 5_555 44_5 yes C(6) C(6) Fe C(9) -79.0(3) 0_555 22_1 5_555 44_5 yes C(6) C(6) Fe C(9) -119.8(2) 0_555 22_1 5_555 44_5 yes C(7) Fe C(8) C(9) 119.4(6) 0_555 22_1 5_555 44_5 yes C(7) Fe C(8) C(9) -119.4(6) 0_555 22_1 5_555 44_5 yes C(7) Fe C(9) C(8) -38.1(4) 0_555 22_1 5_555 44_5 yes C(7) Fe C(9) C(9) 81.3(1) 0_555 22_1 5_555 44_5 yes C(7) Fe C(9) C(8) 38.1(4) 0_555 22_1 5_555 44_5 yes C(7) Fe C(9) C(9) -81.3(1) 0_555 22_1 5_555 44_5 yes C(7) C(8) Fe C(8) -39.5(4) 0_555 22_1 5_555 44_5 yes C(7) C(8) Fe C(9) -119.4(6) 0_555 22_1 5_555 44_5 yes C(7) C(8) Fe C(9) -82.1(4) 0_555 22_1 5_555 44_5 yes C(7) C(8) C(9) C(9) -0.9(6) 0_555 22_1 5_555 44_5 yes C(7) C(8) Fe C(8) 39.5(4) 0_555 22_1 5_555 44_5 yes C(7) C(8) Fe C(9) 82.1(4) 0_555 22_1 5_555 44_5 yes C(7) C(8) Fe C(9) 119.4(6) 0_555 22_1 5_555 44_5 yes C(7) C(8) C(9) C(9) 0.9(6) 0_555 22_1 5_555 44_5 yes C(8) Fe C(8) C(9) -79.8(4) 0_555 22_1 5_555 44_5 yes C(8) Fe C(9) C(9) 119.5(4) 0_555 22_1 5_555 44_5 yes C(8) Fe C(9) C(9) -36.7(3) 0_555 22_1 5_555 44_5 yes C(8) C(7) Fe C(9) 36.5(4) 0_555 22_1 5_555 44_5 yes C(8) C(7) Fe C(9) 79.5(5) 0_555 22_1 5_555 44_5 yes C(8) C(7) C(8) C(9) -1.4(9) 0_555 22_1 5_555 44_5 yes C(8) C(9) Fe C(9) -119.5(4) 0_555 22_1 5_555 44_5 yes C(8) C(9) C(9) C(8) 0.0 0_555 22_1 5_555 44_5 yes C(10) C(11) C(12) C(13) -1.4(5) 0_555 22_1 5_555 44_5 yes C(10) C(11) C(12) C(13) -1.4(5) 0_555 22_1 5_555 44_5 yes C(11) C(10) C(11) C(12) 0.7(3) 0_555 22_1 5_555 44_5 yes C(11) C(12) C(13) C(12) 0.7(3) 0_555 22_1 5_555 44_5 yes C(11) C(12) C(13) C(12) 0.7(3) 0_555 22_1 5_555 44_5 yes #------------------------------------------------------------------------------ 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 2.742(5) . 7_545 ? O(1) O(3) 2.787(4) . 1_455 ? O(1) C(1) 3.479(4) . 4_543 ? O(2) O(3) 2.715(4) . . ? O(2) O(3) 2.715(4) . 3_544 ? O(2) C(5) 3.523(5) . . ? O(2) C(5) 3.523(5) . 3_544 ? O(3) O(3) 2.671(7) . 5_544 ? O(3) C(12) 3.542(5) . . ? O(3) C(13) 3.557(5) . . ? O(3) C(10) 3.579(5) . 1_655 ? N C(8) 3.385(7) . 1_655 ? N C(11) 3.487(5) . 7_555 ? N C(12) 3.514(6) . 7_555 ? C(1) C(7) 3.398(10) . 1_655 ? C(1) C(8) 3.584(8) . 1_655 ? C(1) C(8) 3.584(8) . 6_653 ? C(2) C(9) 3.427(7) . 1_655 ? C(3) C(9) 3.554(8) . 1_655 ? C(3) C(9) 3.554(8) . 6_653 ? #------------------------------------------------------------------------------ loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_site_distance_DH _geom_hbond_site_distance_HA _geom_hbond_site_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O(1) H(10) O(3) . . 1_455 0.951 1.922 2.787(4) 150.080 no #------------------------------------------------------------------------------ #-----------END