Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Tomoyuki Mochida' 'Shizue Yamazaki' _publ_contact_author_name ' Dr. T. Mochida' _publ_contact_author_address ; Dept. of Chemistry, Toho University, Funabashi, Chiba 274-8510, Japan ; _publ_contact_author_email ' mochida@chem.sci.toho-u.ac.jp' _publ_contact_author_fax '+81-47-472-4406' _publ_contact_author_phone '+81-47-472-4406' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Mono- and diferrocenyl complexes with electron-accepting moieties formed by the reaction of ferrocenylalkynes with tetracyanoethylene ; _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. ; data_2,5-Dicyano-3,4-diferrocenyl-hexa-2,4-dienedinitrile _database_code_CSD 184798 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C18 H10 Fe N4 ' _chemical_formula_moiety 'C18 H10 Fe N4 ' _chemical_formula_weight 338.15 _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 9.691(3) _cell_length_b 10.043(5) _cell_length_c 8.646(4) _cell_angle_alpha 90.21(5) _cell_angle_beta 105.49(3) _cell_angle_gamma 71.15(3) _cell_volume 764.3(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.500 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.989 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.618 _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 3717 _diffrn_reflns_av_R_equivalents 0.014 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 1.0017 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.0017 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 0.10 #------------------------------------------------------------------------------ # 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 3208 _reflns_number_gt 3208 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1144 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3208 _refine_ls_number_parameters 208 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.08700(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0005 _refine_diff_density_max 0.51 _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) ; '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 0.11582(3) 0.16796(3) 0.22625(3) 0.03259(9) Uani 1.00 d . . . N(1) N 0.1098(3) 0.2769(3) -0.3231(3) 0.0722(8) Uani 1.00 d . . . N(2) N 0.5251(3) 0.3579(3) -0.1300(3) 0.0643(8) Uani 1.00 d . . . N(3) N 0.6466(3) 0.0660(3) 0.1693(3) 0.0689(8) Uani 1.00 d . . . N(4) N 0.6893(3) 0.3882(4) 0.5052(3) 0.0774(9) Uani 1.00 d . . . C(1) C 0.1270(2) 0.3417(2) 0.1148(3) 0.0346(5) Uani 1.00 d . . . C(2) C 0.1008(3) 0.3701(2) 0.2718(3) 0.0406(6) Uani 1.00 d . . . C(3) C -0.0371(3) 0.3506(3) 0.2702(3) 0.0470(6) Uani 1.00 d . . . C(4) C -0.0973(3) 0.3083(3) 0.1167(3) 0.0477(6) Uani 1.00 d . . . C(5) C 0.0017(3) 0.3012(2) 0.0213(3) 0.0409(5) Uani 1.00 d . . . C(6) C 0.3110(3) -0.0019(3) 0.2528(4) 0.0547(7) Uani 1.00 d . . . C(7) C 0.2910(3) 0.0384(3) 0.4049(3) 0.0548(7) Uani 1.00 d . . . C(8) C 0.1525(4) 0.0270(3) 0.4133(3) 0.0532(7) Uani 1.00 d . . . C(9) C 0.0859(3) -0.0207(3) 0.2669(3) 0.0505(7) Uani 1.00 d . . . C(10) C 0.1839(3) -0.0378(3) 0.1681(3) 0.0520(7) Uani 1.00 d . . . C(11) C 0.2624(2) 0.3449(2) 0.0766(2) 0.0340(5) Uani 1.00 d . . . C(12) C 0.3732(3) 0.3812(2) 0.2100(3) 0.0385(5) Uani 1.00 d . . . C(13) C 0.2912(3) 0.3266(2) -0.0697(3) 0.0386(5) Uani 1.00 d . . . C(14) C 0.1885(3) 0.2984(3) -0.2083(3) 0.0481(6) Uani 1.00 d . . . C(15) C 0.4228(3) 0.3435(3) -0.1010(3) 0.0455(6) Uani 1.00 d . . . C(16) C 0.5188(3) 0.3019(3) 0.2726(3) 0.0432(6) Uani 1.00 d . . . C(17) C 0.5902(3) 0.1694(3) 0.2155(3) 0.0473(6) Uani 1.00 d . . . C(18) C 0.6149(3) 0.3494(3) 0.4041(3) 0.0552(8) Uani 1.00 d . . . H(1) H 0.1651 0.3981 0.3597 0.0760 Uiso 1.00 calc . . . H(2) H -0.0810 0.3613 0.3575 0.0760 Uiso 1.00 calc . . . H(3) H -0.1881 0.2855 0.0851 0.0760 Uiso 1.00 calc . . . H(4) H -0.0118 0.2749 -0.0860 0.0760 Uiso 1.00 calc . . . H(5) H 0.3949 -0.0039 0.2146 0.0760 Uiso 1.00 calc . . . H(6) H 0.3597 0.0671 0.4872 0.0760 Uiso 1.00 calc . . . H(7) H 0.1113 0.0466 0.5023 0.0760 Uiso 1.00 calc . . . H(8) H -0.0083 -0.0377 0.2402 0.0760 Uiso 1.00 calc . . . H(9) H 0.1668 -0.0677 0.0623 0.0760 Uiso 1.00 calc . . . H(10) H 0.3377 0.4680 0.2546 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(1) 0.0344(2) 0.0317(2) 0.0325(2) -0.0126(1) 0.0080(1) -0.0048(1) N(1) 0.084(2) 0.084(2) 0.044(1) -0.029(2) 0.008(1) -0.022(1) N(2) 0.073(2) 0.073(2) 0.063(1) -0.032(1) 0.033(1) -0.004(1) N(3) 0.069(2) 0.060(2) 0.064(1) -0.006(1) 0.014(1) -0.005(1) N(4) 0.053(1) 0.110(2) 0.074(2) -0.037(2) 0.013(1) -0.040(2) C(1) 0.037(1) 0.0282(9) 0.037(1) -0.0110(8) 0.0064(8) -0.0028(8) C(2) 0.042(1) 0.038(1) 0.047(1) -0.0153(9) 0.0163(9) -0.0147(9) C(3) 0.042(1) 0.043(1) 0.060(1) -0.0120(10) 0.023(1) -0.013(1) C(4) 0.033(1) 0.044(1) 0.063(2) -0.0123(9) 0.008(1) -0.002(1) C(5) 0.039(1) 0.039(1) 0.039(1) -0.0137(9) 0.0004(9) 0.0009(9) C(6) 0.048(1) 0.039(1) 0.072(2) -0.004(1) 0.021(1) 0.003(1) C(7) 0.050(1) 0.050(1) 0.052(1) -0.015(1) -0.006(1) 0.008(1) C(8) 0.070(2) 0.053(1) 0.038(1) -0.023(1) 0.014(1) 0.005(1) C(9) 0.059(1) 0.041(1) 0.057(1) -0.025(1) 0.015(1) -0.003(1) C(10) 0.070(2) 0.035(1) 0.052(1) -0.015(1) 0.019(1) -0.008(1) C(11) 0.042(1) 0.0258(9) 0.0339(10) -0.0124(8) 0.0074(8) -0.0045(7) C(12) 0.045(1) 0.042(1) 0.037(1) -0.0235(9) 0.0143(9) -0.0083(9) C(13) 0.046(1) 0.0322(10) 0.037(1) -0.0125(9) 0.0111(9) -0.0029(8) C(14) 0.061(1) 0.046(1) 0.037(1) -0.015(1) 0.015(1) -0.0086(10) C(15) 0.060(1) 0.043(1) 0.037(1) -0.018(1) 0.018(1) -0.0024(9) C(16) 0.044(1) 0.057(1) 0.036(1) -0.026(1) 0.0114(9) -0.0063(10) C(17) 0.044(1) 0.053(1) 0.041(1) -0.014(1) 0.0082(10) -0.002(1) C(18) 0.043(1) 0.078(2) 0.050(1) -0.027(1) 0.014(1) -0.019(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 'DIRDIF94 (PATTY)' _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(1) 2.044(2) . . yes Fe(1) C(2) 2.033(2) . . yes Fe(1) C(3) 2.060(2) . . yes Fe(1) C(4) 2.057(2) . . yes Fe(1) C(5) 2.042(2) . . yes Fe(1) C(6) 2.056(3) . . yes Fe(1) C(7) 2.036(3) . . yes Fe(1) C(8) 2.032(3) . . yes Fe(1) C(9) 2.052(2) . . yes Fe(1) C(10) 2.061(2) . . yes N(1) C(14) 1.146(3) . . yes N(2) C(15) 1.138(4) . . yes N(3) C(17) 1.134(4) . . yes N(4) C(18) 1.130(3) . . yes C(1) C(2) 1.457(3) . . yes C(1) C(5) 1.445(3) . . yes C(1) C(11) 1.446(3) . . yes C(2) C(3) 1.409(3) . . yes C(3) C(4) 1.423(4) . . yes C(4) C(5) 1.409(4) . . yes C(6) C(7) 1.419(4) . . yes C(6) C(10) 1.410(4) . . yes C(7) C(8) 1.403(4) . . yes C(8) C(9) 1.417(4) . . yes C(9) C(10) 1.411(4) . . yes C(11) C(12) 1.485(3) . . yes C(11) C(13) 1.365(3) . . yes C(12) C(16) 1.337(3) . . yes C(13) C(14) 1.432(3) . . yes C(13) C(15) 1.432(3) . . yes C(16) C(17) 1.441(4) . . yes C(16) C(18) 1.451(3) . . 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(1) Fe(1) C(2) 41.89(9) . . 0_555 yes C(1) Fe(1) C(3) 68.92(10) . . 0_555 yes C(1) Fe(1) C(4) 68.53(9) . . 0_555 yes C(1) Fe(1) C(5) 41.42(8) . . 0_555 yes C(1) Fe(1) C(6) 111.11(10) . . 0_555 yes C(1) Fe(1) C(7) 123.3(1) . . 0_555 yes C(1) Fe(1) C(8) 156.5(1) . . 0_555 yes C(1) Fe(1) C(9) 162.54(10) . . 0_555 yes C(1) Fe(1) C(10) 127.61(10) . . 0_555 yes C(2) Fe(1) C(3) 40.26(9) . . 0_555 yes C(2) Fe(1) C(4) 68.22(10) . . 0_555 yes C(2) Fe(1) C(5) 69.56(9) . . 0_555 yes C(2) Fe(1) C(6) 127.0(1) . . 0_555 yes C(2) Fe(1) C(7) 107.3(1) . . 0_555 yes C(2) Fe(1) C(8) 118.5(1) . . 0_555 yes C(2) Fe(1) C(9) 153.2(1) . . 0_555 yes C(2) Fe(1) C(10) 164.7(1) . . 0_555 yes C(3) Fe(1) C(4) 40.4(1) . . 0_555 yes C(3) Fe(1) C(5) 68.5(1) . . 0_555 yes C(3) Fe(1) C(6) 161.1(1) . . 0_555 yes C(3) Fe(1) C(7) 122.5(1) . . 0_555 yes C(3) Fe(1) C(8) 104.2(1) . . 0_555 yes C(3) Fe(1) C(9) 118.3(1) . . 0_555 yes C(3) Fe(1) C(10) 154.7(1) . . 0_555 yes C(4) Fe(1) C(5) 40.2(1) . . 0_555 yes C(4) Fe(1) C(6) 158.3(1) . . 0_555 yes C(4) Fe(1) C(7) 158.3(1) . . 0_555 yes C(4) Fe(1) C(8) 121.5(1) . . 0_555 yes C(4) Fe(1) C(9) 105.9(1) . . 0_555 yes C(4) Fe(1) C(10) 121.8(1) . . 0_555 yes C(5) Fe(1) C(6) 124.9(1) . . 0_555 yes C(5) Fe(1) C(7) 160.2(1) . . 0_555 yes C(5) Fe(1) C(8) 158.7(1) . . 0_555 yes C(5) Fe(1) C(9) 123.8(1) . . 0_555 yes C(5) Fe(1) C(10) 109.82(10) . . 0_555 yes C(6) Fe(1) C(7) 40.6(1) . . 0_555 yes C(6) Fe(1) C(8) 67.9(1) . . 0_555 yes C(6) Fe(1) C(9) 67.6(1) . . 0_555 yes C(6) Fe(1) C(10) 40.0(1) . . 0_555 yes C(7) Fe(1) C(8) 40.4(1) . . 0_555 yes C(7) Fe(1) C(9) 67.9(1) . . 0_555 yes C(7) Fe(1) C(10) 67.8(1) . . 0_555 yes C(8) Fe(1) C(9) 40.6(1) . . 0_555 yes C(8) Fe(1) C(10) 67.8(1) . . 0_555 yes C(9) Fe(1) C(10) 40.1(1) . . 0_555 yes Fe(1) C(1) C(2) 68.7(1) . . 0_555 yes Fe(1) C(1) C(5) 69.2(1) . . 0_555 yes Fe(1) C(1) C(11) 122.9(1) . . 0_555 yes C(2) C(1) C(5) 106.4(2) . . 0_555 yes C(2) C(1) C(11) 123.2(2) . . 0_555 yes C(5) C(1) C(11) 130.2(2) . . 0_555 yes Fe(1) C(2) C(1) 69.4(1) . . 0_555 yes Fe(1) C(2) C(3) 70.9(1) . . 0_555 yes C(1) C(2) C(3) 108.2(2) . . 0_555 yes Fe(1) C(3) C(2) 68.8(1) . . 0_555 yes Fe(1) C(3) C(4) 69.7(1) . . 0_555 yes C(2) C(3) C(4) 108.2(2) . . 0_555 yes Fe(1) C(4) C(3) 69.9(1) . . 0_555 yes Fe(1) C(4) C(5) 69.3(1) . . 0_555 yes C(3) C(4) C(5) 109.1(2) . . 0_555 yes Fe(1) C(5) C(1) 69.4(1) . . 0_555 yes Fe(1) C(5) C(4) 70.5(1) . . 0_555 yes C(1) C(5) C(4) 108.0(2) . . 0_555 yes Fe(1) C(6) C(7) 69.0(1) . . 0_555 yes Fe(1) C(6) C(10) 70.2(1) . . 0_555 yes C(7) C(6) C(10) 107.8(2) . . 0_555 yes Fe(1) C(7) C(6) 70.5(1) . . 0_555 yes Fe(1) C(7) C(8) 69.7(1) . . 0_555 yes C(6) C(7) C(8) 108.1(2) . . 0_555 yes Fe(1) C(8) C(7) 70.0(2) . . 0_555 yes Fe(1) C(8) C(9) 70.5(1) . . 0_555 yes C(7) C(8) C(9) 108.2(2) . . 0_555 yes Fe(1) C(9) C(8) 68.9(1) . . 0_555 yes Fe(1) C(9) C(10) 70.3(1) . . 0_555 yes C(8) C(9) C(10) 107.8(2) . . 0_555 yes Fe(1) C(10) C(6) 69.8(1) . . 0_555 yes Fe(1) C(10) C(9) 69.6(1) . . 0_555 yes C(6) C(10) C(9) 108.2(2) . . 0_555 yes C(1) C(11) C(12) 114.6(2) . . 0_555 yes C(1) C(11) C(13) 126.4(2) . . 0_555 yes C(12) C(11) C(13) 118.8(2) . . 0_555 yes C(11) C(12) C(16) 125.5(2) . . 0_555 yes C(11) C(13) C(14) 123.3(2) . . 0_555 yes C(11) C(13) C(15) 122.8(2) . . 0_555 yes C(14) C(13) C(15) 113.8(2) . . 0_555 yes N(1) C(14) C(13) 177.2(3) . . 0_555 yes N(2) C(15) C(13) 178.2(3) . . 0_555 yes C(12) C(16) C(17) 123.8(2) . . 0_555 yes C(12) C(16) C(18) 119.9(2) . . 0_555 yes C(17) C(16) C(18) 116.3(2) . . 0_555 yes N(3) C(17) C(16) 179.2(3) . . 0_555 yes N(4) C(18) C(16) 179.0(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(1) C(2) C(3) -60.6(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(1) C(5) C(4) 60.2(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(1) C(11) C(12) -85.3(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(1) C(11) C(13) 99.0(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(2) C(1) C(5) 59.2(1) 0_555 79_1 5_555 55_5 yes Fe(1) C(2) C(1) C(11) -116.2(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(2) C(3) C(4) -58.7(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(3) C(2) C(1) 59.7(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(3) C(4) C(5) -58.3(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(4) C(3) C(2) 58.2(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(4) C(5) C(1) -59.5(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(5) C(1) C(2) -58.8(1) 0_555 79_1 5_555 55_5 yes Fe(1) C(5) C(1) C(11) 116.1(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(5) C(4) C(3) 58.6(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(6) C(7) C(8) 59.8(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(6) C(10) C(9) -59.2(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(7) C(6) C(10) -59.7(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(7) C(8) C(9) 60.4(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(8) C(7) C(6) -60.3(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(8) C(9) C(10) 59.8(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(9) C(8) C(7) -60.1(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(9) C(10) C(6) 59.3(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(10) C(6) C(7) 58.9(2) 0_555 79_1 5_555 55_5 yes Fe(1) C(10) C(9) C(8) -58.9(2) 0_555 79_1 5_555 55_5 yes N(1) C(14) C(13) C(11) 167(5) 0_555 79_1 5_555 55_5 yes N(1) C(14) C(13) C(15) -8(5) 0_555 79_1 5_555 55_5 yes N(2) C(15) C(13) C(11) -151(9) 0_555 79_1 5_555 55_5 yes N(2) C(15) C(13) C(14) 24(9) 0_555 79_1 5_555 55_5 yes N(3) C(17) C(16) C(12) 84(20) 0_555 79_1 5_555 55_5 yes N(3) C(17) C(16) C(18) -94(20) 0_555 79_1 5_555 55_5 yes N(4) C(18) C(16) C(12) -56(16) 0_555 79_1 5_555 55_5 yes N(4) C(18) C(16) C(17) 122(16) 0_555 79_1 5_555 55_5 yes C(1) Fe(1) C(2) C(3) 118.9(2) 0_555 79_1 5_555 55_5 yes C(1) Fe(1) C(3) C(2) -38.8(1) 0_555 79_1 5_555 55_5 yes C(1) Fe(1) C(3) C(4) 81.2(1) 0_555 79_1 5_555 55_5 yes C(1) Fe(1) C(4) C(3) -82.3(1) 0_555 79_1 5_555 55_5 yes C(1) Fe(1) C(4) C(5) 38.5(1) 0_555 79_1 5_555 55_5 yes C(1) Fe(1) C(5) C(4) -118.9(2) 0_555 79_1 5_555 55_5 yes C(1) Fe(1) C(6) C(7) 117.0(2) 0_555 79_1 5_555 55_5 yes C(1) Fe(1) C(6) C(10) -123.9(2) 0_555 79_1 5_555 55_5 yes C(1) Fe(1) C(7) C(6) -84.0(2) 0_555 79_1 5_555 55_5 yes C(1) Fe(1) C(7) C(8) 157.2(2) 0_555 79_1 5_555 55_5 yes C(1) Fe(1) C(8) C(7) -54.5(3) 0_555 79_1 5_555 55_5 yes C(1) Fe(1) C(8) C(9) -173.2(2) 0_555 79_1 5_555 55_5 yes C(1) Fe(1) C(9) C(8) 171.0(3) 0_555 79_1 5_555 55_5 yes C(1) Fe(1) C(9) C(10) 51.9(4) 0_555 79_1 5_555 55_5 yes C(1) Fe(1) C(10) C(6) 77.9(2) 0_555 79_1 5_555 55_5 yes C(1) Fe(1) C(10) C(9) -162.6(1) 0_555 79_1 5_555 55_5 yes C(1) C(2) Fe(1) C(3) -118.9(2) 0_555 79_1 5_555 55_5 yes C(1) C(2) Fe(1) C(4) -81.7(1) 0_555 79_1 5_555 55_5 yes C(1) C(2) Fe(1) C(5) -38.5(1) 0_555 79_1 5_555 55_5 yes C(1) C(2) Fe(1) C(6) 80.5(2) 0_555 79_1 5_555 55_5 yes C(1) C(2) Fe(1) C(7) 120.9(1) 0_555 79_1 5_555 55_5 yes C(1) C(2) Fe(1) C(8) 163.3(1) 0_555 79_1 5_555 55_5 yes C(1) C(2) Fe(1) C(9) -163.9(2) 0_555 79_1 5_555 55_5 yes C(1) C(2) Fe(1) C(10) 52.1(4) 0_555 79_1 5_555 55_5 yes C(1) C(2) C(3) C(4) 0.9(3) 0_555 79_1 5_555 55_5 yes C(1) C(5) Fe(1) C(2) 38.9(1) 0_555 79_1 5_555 55_5 yes C(1) C(5) Fe(1) C(3) 82.1(1) 0_555 79_1 5_555 55_5 yes C(1) C(5) Fe(1) C(4) 118.9(2) 0_555 79_1 5_555 55_5 yes C(1) C(5) Fe(1) C(6) -82.7(2) 0_555 79_1 5_555 55_5 yes C(1) C(5) Fe(1) C(7) -45.5(4) 0_555 79_1 5_555 55_5 yes C(1) C(5) Fe(1) C(8) 155.4(3) 0_555 79_1 5_555 55_5 yes C(1) C(5) Fe(1) C(9) -167.4(1) 0_555 79_1 5_555 55_5 yes C(1) C(5) Fe(1) C(10) -124.9(1) 0_555 79_1 5_555 55_5 yes C(1) C(5) C(4) C(3) -0.8(3) 0_555 79_1 5_555 55_5 yes C(1) C(11) C(12) C(16) 123.6(2) 0_555 79_1 5_555 55_5 yes C(1) C(11) C(13) C(14) -1.3(3) 0_555 79_1 5_555 55_5 yes C(1) C(11) C(13) C(15) 174.4(2) 0_555 79_1 5_555 55_5 yes C(2) Fe(1) C(1) C(5) -118.3(2) 0_555 79_1 5_555 55_5 yes C(2) Fe(1) C(1) C(11) 116.5(2) 0_555 79_1 5_555 55_5 yes C(2) Fe(1) C(3) C(4) 120.0(2) 0_555 79_1 5_555 55_5 yes C(2) Fe(1) C(4) C(3) -37.1(1) 0_555 79_1 5_555 55_5 yes C(2) Fe(1) C(4) C(5) 83.7(1) 0_555 79_1 5_555 55_5 yes C(2) Fe(1) C(5) C(4) -80.1(2) 0_555 79_1 5_555 55_5 yes C(2) Fe(1) C(6) C(7) 72.1(2) 0_555 79_1 5_555 55_5 yes C(2) Fe(1) C(6) C(10) -168.8(1) 0_555 79_1 5_555 55_5 yes C(2) Fe(1) C(7) C(6) -127.3(2) 0_555 79_1 5_555 55_5 yes C(2) Fe(1) C(7) C(8) 113.9(2) 0_555 79_1 5_555 55_5 yes C(2) Fe(1) C(8) C(7) -83.3(2) 0_555 79_1 5_555 55_5 yes C(2) Fe(1) C(8) C(9) 157.9(2) 0_555 79_1 5_555 55_5 yes C(2) Fe(1) C(9) C(8) -47.1(3) 0_555 79_1 5_555 55_5 yes C(2) Fe(1) C(9) C(10) -166.1(2) 0_555 79_1 5_555 55_5 yes C(2) Fe(1) C(10) C(6) 36.2(4) 0_555 79_1 5_555 55_5 yes C(2) Fe(1) C(10) C(9) 155.7(3) 0_555 79_1 5_555 55_5 yes C(2) C(1) Fe(1) C(3) 37.3(1) 0_555 79_1 5_555 55_5 yes C(2) C(1) Fe(1) C(4) 80.9(1) 0_555 79_1 5_555 55_5 yes C(2) C(1) Fe(1) C(5) 118.3(2) 0_555 79_1 5_555 55_5 yes C(2) C(1) Fe(1) C(6) -122.4(1) 0_555 79_1 5_555 55_5 yes C(2) C(1) Fe(1) C(7) -78.5(2) 0_555 79_1 5_555 55_5 yes C(2) C(1) Fe(1) C(8) -39.4(3) 0_555 79_1 5_555 55_5 yes C(2) C(1) Fe(1) C(9) 155.4(3) 0_555 79_1 5_555 55_5 yes C(2) C(1) Fe(1) C(10) -164.8(1) 0_555 79_1 5_555 55_5 yes C(2) C(1) C(5) C(4) 1.3(2) 0_555 79_1 5_555 55_5 yes C(2) C(1) C(11) C(12) -0.7(3) 0_555 79_1 5_555 55_5 yes C(2) C(1) C(11) C(13) -176.4(2) 0_555 79_1 5_555 55_5 yes C(2) C(3) Fe(1) C(4) -120.0(2) 0_555 79_1 5_555 55_5 yes C(2) C(3) Fe(1) C(5) -83.4(2) 0_555 79_1 5_555 55_5 yes C(2) C(3) Fe(1) C(6) 55.0(4) 0_555 79_1 5_555 55_5 yes C(2) C(3) Fe(1) C(7) 78.1(2) 0_555 79_1 5_555 55_5 yes C(2) C(3) Fe(1) C(8) 117.6(2) 0_555 79_1 5_555 55_5 yes C(2) C(3) Fe(1) C(9) 158.7(2) 0_555 79_1 5_555 55_5 yes C(2) C(3) Fe(1) C(10) -174.4(2) 0_555 79_1 5_555 55_5 yes C(2) C(3) C(4) C(5) -0.1(3) 0_555 79_1 5_555 55_5 yes C(3) Fe(1) C(1) C(5) -80.9(1) 0_555 79_1 5_555 55_5 yes C(3) Fe(1) C(1) C(11) 153.9(2) 0_555 79_1 5_555 55_5 yes C(3) Fe(1) C(4) C(5) 120.8(2) 0_555 79_1 5_555 55_5 yes C(3) Fe(1) C(5) C(4) -36.8(1) 0_555 79_1 5_555 55_5 yes C(3) Fe(1) C(6) C(7) 30.6(4) 0_555 79_1 5_555 55_5 yes C(3) Fe(1) C(6) C(10) 149.7(3) 0_555 79_1 5_555 55_5 yes C(3) Fe(1) C(7) C(6) -168.7(2) 0_555 79_1 5_555 55_5 yes C(3) Fe(1) C(7) C(8) 72.4(2) 0_555 79_1 5_555 55_5 yes C(3) Fe(1) C(8) C(7) -124.0(2) 0_555 79_1 5_555 55_5 yes C(3) Fe(1) C(8) C(9) 117.2(2) 0_555 79_1 5_555 55_5 yes C(3) Fe(1) C(9) C(8) -78.3(2) 0_555 79_1 5_555 55_5 yes C(3) Fe(1) C(9) C(10) 162.6(2) 0_555 79_1 5_555 55_5 yes C(3) Fe(1) C(10) C(6) -157.5(2) 0_555 79_1 5_555 55_5 yes C(3) Fe(1) C(10) C(9) -38.1(3) 0_555 79_1 5_555 55_5 yes C(3) C(2) Fe(1) C(4) 37.2(2) 0_555 79_1 5_555 55_5 yes C(3) C(2) Fe(1) C(5) 80.4(2) 0_555 79_1 5_555 55_5 yes C(3) C(2) Fe(1) C(6) -160.6(2) 0_555 79_1 5_555 55_5 yes C(3) C(2) Fe(1) C(7) -120.2(2) 0_555 79_1 5_555 55_5 yes C(3) C(2) Fe(1) C(8) -77.8(2) 0_555 79_1 5_555 55_5 yes C(3) C(2) Fe(1) C(9) -45.0(3) 0_555 79_1 5_555 55_5 yes C(3) C(2) Fe(1) C(10) 171.0(4) 0_555 79_1 5_555 55_5 yes C(3) C(2) C(1) C(5) -1.4(3) 0_555 79_1 5_555 55_5 yes C(3) C(2) C(1) C(11) -176.8(2) 0_555 79_1 5_555 55_5 yes C(3) C(4) Fe(1) C(5) -120.8(2) 0_555 79_1 5_555 55_5 yes C(3) C(4) Fe(1) C(6) -175.6(3) 0_555 79_1 5_555 55_5 yes C(3) C(4) Fe(1) C(7) 45.1(3) 0_555 79_1 5_555 55_5 yes C(3) C(4) Fe(1) C(8) 73.9(2) 0_555 79_1 5_555 55_5 yes C(3) C(4) Fe(1) C(9) 115.2(2) 0_555 79_1 5_555 55_5 yes C(3) C(4) Fe(1) C(10) 155.9(2) 0_555 79_1 5_555 55_5 yes C(4) Fe(1) C(1) C(5) -37.4(1) 0_555 79_1 5_555 55_5 yes C(4) Fe(1) C(1) C(11) -162.6(2) 0_555 79_1 5_555 55_5 yes C(4) Fe(1) C(6) C(7) -158.2(3) 0_555 79_1 5_555 55_5 yes C(4) Fe(1) C(6) C(10) -39.1(4) 0_555 79_1 5_555 55_5 yes C(4) Fe(1) C(7) C(6) 158.2(3) 0_555 79_1 5_555 55_5 yes C(4) Fe(1) C(7) C(8) 39.4(4) 0_555 79_1 5_555 55_5 yes C(4) Fe(1) C(8) C(7) -164.0(2) 0_555 79_1 5_555 55_5 yes C(4) Fe(1) C(8) C(9) 77.2(2) 0_555 79_1 5_555 55_5 yes C(4) Fe(1) C(9) C(8) -120.2(2) 0_555 79_1 5_555 55_5 yes C(4) Fe(1) C(9) C(10) 120.8(2) 0_555 79_1 5_555 55_5 yes C(4) Fe(1) C(10) C(6) 164.1(2) 0_555 79_1 5_555 55_5 yes C(4) Fe(1) C(10) C(9) -76.4(2) 0_555 79_1 5_555 55_5 yes C(4) C(3) Fe(1) C(5) 36.6(1) 0_555 79_1 5_555 55_5 yes C(4) C(3) Fe(1) C(6) 175.0(3) 0_555 79_1 5_555 55_5 yes C(4) C(3) Fe(1) C(7) -161.9(2) 0_555 79_1 5_555 55_5 yes C(4) C(3) Fe(1) C(8) -122.3(2) 0_555 79_1 5_555 55_5 yes C(4) C(3) Fe(1) C(9) -81.3(2) 0_555 79_1 5_555 55_5 yes C(4) C(3) Fe(1) C(10) -54.4(3) 0_555 79_1 5_555 55_5 yes C(4) C(5) Fe(1) C(6) 158.4(2) 0_555 79_1 5_555 55_5 yes C(4) C(5) Fe(1) C(7) -164.5(3) 0_555 79_1 5_555 55_5 yes C(4) C(5) Fe(1) C(8) 36.5(3) 0_555 79_1 5_555 55_5 yes C(4) C(5) Fe(1) C(9) 73.7(2) 0_555 79_1 5_555 55_5 yes C(4) C(5) Fe(1) C(10) 116.2(2) 0_555 79_1 5_555 55_5 yes C(4) C(5) C(1) C(11) 176.3(2) 0_555 79_1 5_555 55_5 yes C(5) Fe(1) C(1) C(11) -125.2(2) 0_555 79_1 5_555 55_5 yes C(5) Fe(1) C(6) C(7) 161.7(2) 0_555 79_1 5_555 55_5 yes C(5) Fe(1) C(6) C(10) -79.2(2) 0_555 79_1 5_555 55_5 yes C(5) Fe(1) C(7) C(6) -49.6(4) 0_555 79_1 5_555 55_5 yes C(5) Fe(1) C(7) C(8) -168.4(3) 0_555 79_1 5_555 55_5 yes C(5) Fe(1) C(8) C(7) 169.2(3) 0_555 79_1 5_555 55_5 yes C(5) Fe(1) C(8) C(9) 50.5(4) 0_555 79_1 5_555 55_5 yes C(5) Fe(1) C(9) C(8) -160.3(2) 0_555 79_1 5_555 55_5 yes C(5) Fe(1) C(9) C(10) 80.7(2) 0_555 79_1 5_555 55_5 yes C(5) Fe(1) C(10) C(6) 121.1(2) 0_555 79_1 5_555 55_5 yes C(5) Fe(1) C(10) C(9) -119.4(2) 0_555 79_1 5_555 55_5 yes C(5) C(1) Fe(1) C(6) 119.3(2) 0_555 79_1 5_555 55_5 yes C(5) C(1) Fe(1) C(7) 163.2(2) 0_555 79_1 5_555 55_5 yes C(5) C(1) Fe(1) C(8) -157.7(3) 0_555 79_1 5_555 55_5 yes C(5) C(1) Fe(1) C(9) 37.1(4) 0_555 79_1 5_555 55_5 yes C(5) C(1) Fe(1) C(10) 76.9(2) 0_555 79_1 5_555 55_5 yes C(5) C(1) C(11) C(12) -174.9(2) 0_555 79_1 5_555 55_5 yes C(5) C(1) C(11) C(13) 9.4(4) 0_555 79_1 5_555 55_5 yes C(5) C(4) Fe(1) C(6) -54.9(3) 0_555 79_1 5_555 55_5 yes C(5) C(4) Fe(1) C(7) 165.8(3) 0_555 79_1 5_555 55_5 yes C(5) C(4) Fe(1) C(8) -165.3(1) 0_555 79_1 5_555 55_5 yes C(5) C(4) Fe(1) C(9) -124.0(2) 0_555 79_1 5_555 55_5 yes C(5) C(4) Fe(1) C(10) -83.4(2) 0_555 79_1 5_555 55_5 yes C(6) Fe(1) C(1) C(11) -5.9(2) 0_555 79_1 5_555 55_5 yes C(6) Fe(1) C(7) C(8) -118.8(2) 0_555 79_1 5_555 55_5 yes C(6) Fe(1) C(8) C(7) 37.9(2) 0_555 79_1 5_555 55_5 yes C(6) Fe(1) C(8) C(9) -80.8(2) 0_555 79_1 5_555 55_5 yes C(6) Fe(1) C(9) C(8) 81.8(2) 0_555 79_1 5_555 55_5 yes C(6) Fe(1) C(9) C(10) -37.3(2) 0_555 79_1 5_555 55_5 yes C(6) Fe(1) C(10) C(9) 119.5(2) 0_555 79_1 5_555 55_5 yes C(6) C(7) Fe(1) C(8) 118.8(2) 0_555 79_1 5_555 55_5 yes C(6) C(7) Fe(1) C(9) 80.8(2) 0_555 79_1 5_555 55_5 yes C(6) C(7) Fe(1) C(10) 37.4(2) 0_555 79_1 5_555 55_5 yes C(6) C(7) C(8) C(9) 0.1(3) 0_555 79_1 5_555 55_5 yes C(6) C(10) Fe(1) C(7) -37.9(2) 0_555 79_1 5_555 55_5 yes C(6) C(10) Fe(1) C(8) -81.6(2) 0_555 79_1 5_555 55_5 yes C(6) C(10) Fe(1) C(9) -119.5(2) 0_555 79_1 5_555 55_5 yes C(6) C(10) C(9) C(8) 0.4(3) 0_555 79_1 5_555 55_5 yes C(7) Fe(1) C(1) C(11) 38.0(2) 0_555 79_1 5_555 55_5 yes C(7) Fe(1) C(6) C(10) 119.1(2) 0_555 79_1 5_555 55_5 yes C(7) Fe(1) C(8) C(9) -118.8(2) 0_555 79_1 5_555 55_5 yes C(7) Fe(1) C(9) C(8) 37.8(2) 0_555 79_1 5_555 55_5 yes C(7) Fe(1) C(9) C(10) -81.3(2) 0_555 79_1 5_555 55_5 yes C(7) Fe(1) C(10) C(9) 81.6(2) 0_555 79_1 5_555 55_5 yes C(7) C(6) Fe(1) C(8) -37.7(2) 0_555 79_1 5_555 55_5 yes C(7) C(6) Fe(1) C(9) -81.8(2) 0_555 79_1 5_555 55_5 yes C(7) C(6) Fe(1) C(10) -119.1(2) 0_555 79_1 5_555 55_5 yes C(7) C(6) C(10) C(9) -0.3(3) 0_555 79_1 5_555 55_5 yes C(7) C(8) Fe(1) C(9) 118.8(2) 0_555 79_1 5_555 55_5 yes C(7) C(8) Fe(1) C(10) 81.3(2) 0_555 79_1 5_555 55_5 yes C(7) C(8) C(9) C(10) -0.3(3) 0_555 79_1 5_555 55_5 yes C(8) Fe(1) C(1) C(11) 77.1(3) 0_555 79_1 5_555 55_5 yes C(8) Fe(1) C(6) C(10) 81.4(2) 0_555 79_1 5_555 55_5 yes C(8) Fe(1) C(9) C(10) -119.1(2) 0_555 79_1 5_555 55_5 yes C(8) Fe(1) C(10) C(9) 37.9(2) 0_555 79_1 5_555 55_5 yes C(8) C(7) Fe(1) C(9) -38.0(2) 0_555 79_1 5_555 55_5 yes C(8) C(7) Fe(1) C(10) -81.5(2) 0_555 79_1 5_555 55_5 yes C(8) C(7) C(6) C(10) 0.1(3) 0_555 79_1 5_555 55_5 yes C(8) C(9) Fe(1) C(10) 119.1(2) 0_555 79_1 5_555 55_5 yes C(9) Fe(1) C(1) C(11) -88.1(3) 0_555 79_1 5_555 55_5 yes C(9) Fe(1) C(6) C(10) 37.4(2) 0_555 79_1 5_555 55_5 yes C(9) C(8) Fe(1) C(10) -37.4(2) 0_555 79_1 5_555 55_5 yes C(10) Fe(1) C(1) C(11) -48.3(2) 0_555 79_1 5_555 55_5 yes C(11) C(12) C(16) C(17) 1.5(4) 0_555 79_1 5_555 55_5 yes C(11) C(12) C(16) C(18) -179.5(2) 0_555 79_1 5_555 55_5 yes C(12) C(11) C(13) C(14) -176.8(2) 0_555 79_1 5_555 55_5 yes C(12) C(11) C(13) C(15) -1.1(3) 0_555 79_1 5_555 55_5 yes C(13) C(11) C(12) C(16) -60.4(3) 0_555 79_1 5_555 55_5 yes C(13) C(11) C(12) C(16) -60.4(3) 0_555 79_1 5_555 55_5 yes #------------------------------------------------------------------------------ #===END data_2,5-Dicyano-3-ferrocenyl-hexa-2,4-dienedinitrile _database_code_CSD 184799 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C28.50 H18.50 Cl1.50 Fe2 N4' _chemical_formula_moiety '?' _chemical_formula_weight 569.92 _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 11.755(3) _cell_length_b 12.482(3) _cell_length_c 16.933(2) _cell_angle_alpha 90 _cell_angle_beta 98.47(1) _cell_angle_gamma 90 _cell_volume 2457.5(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.1 _cell_measurement_theta_max 12.5 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'red-black' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.368 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.749 _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 6197 _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9995 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 11.24 #------------------------------------------------------------------------------ # 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 5648 _reflns_number_gt 3486 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1261 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3486 _refine_ls_number_parameters 308 _refine_ls_goodness_of_fit_ref 1.317 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.06200(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0009 _refine_diff_density_max 0.44 _refine_diff_density_min -0.45 _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) ; 'Fe' 'Fe' 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;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 Fe1 Fe 1.32743(6) 0.24676(6) 0.21521(4) 0.0459(2) Uani 1.00 d . . . Fe2 Fe 0.76783(5) 0.36074(5) 0.04404(3) 0.0325(2) Uani 1.00 d . . . Cl1 Cl 0.4351 0.0404 0.9253 0.1698 Uani 1.00 d . . . N1 N 1.1360(5) 0.2930(4) 0.3998(2) 0.072(2) Uani 1.00 d . . . N2 N 0.8177(4) 0.1854(5) 0.2713(3) 0.074(2) Uani 1.00 d . . . N3 N 1.0658(5) -0.0142(4) 0.2003(3) 0.071(2) Uani 1.00 d . . . N4 N 0.8392(4) 0.0453(4) -0.0198(3) 0.069(2) Uani 1.00 d . . . C1 C 1.1702(4) 0.3115(4) 0.1781(2) 0.038(1) Uani 1.00 d . . . C2 C 1.2263(4) 0.2870(4) 0.1103(3) 0.046(1) Uani 1.00 d . . . C3 C 1.3317(4) 0.3450(5) 0.1186(3) 0.057(2) Uani 1.00 d . . . C4 C 1.3401(4) 0.4054(4) 0.1899(3) 0.059(2) Uani 1.00 d . . . C5 C 1.2423(4) 0.3850(4) 0.2273(3) 0.048(1) Uani 1.00 d . . . C6 C 1.3092(5) 0.1146(5) 0.2834(4) 0.065(2) Uani 1.00 d . . . C7 C 1.3564(6) 0.0847(5) 0.2145(4) 0.078(2) Uani 1.00 d . . . C8 C 1.4618(6) 0.1436(6) 0.2179(5) 0.088(2) Uani 1.00 d . . . C9 C 1.4774(5) 0.2073(7) 0.2857(5) 0.089(2) Uani 1.00 d . . . C10 C 1.3827(6) 0.1900(6) 0.3272(3) 0.077(2) Uani 1.00 d . . . C11 C 0.9369(3) 0.3194(3) 0.0650(2) 0.031(1) Uani 1.00 d . . . C12 C 0.9216(3) 0.4259(3) 0.0938(2) 0.035(1) Uani 1.00 d . . . C13 C 0.8703(4) 0.4886(4) 0.0280(3) 0.043(1) Uani 1.00 d . . . C14 C 0.8551(4) 0.4238(4) -0.0402(3) 0.048(1) Uani 1.00 d . . . C15 C 0.8938(4) 0.3189(4) -0.0198(2) 0.038(1) Uani 1.00 d . . . C16 C 0.6703(4) 0.2493(4) 0.0918(3) 0.056(2) Uani 1.00 d . . . C17 C 0.6595(4) 0.3507(5) 0.1280(3) 0.056(2) Uani 1.00 d . . . C18 C 0.6165(4) 0.4235(4) 0.0674(3) 0.056(2) Uani 1.00 d . . . C19 C 0.5996(4) 0.3669(5) -0.0060(3) 0.058(2) Uani 1.00 d . . . C20 C 0.6339(4) 0.2594(4) 0.0096(3) 0.056(2) Uani 1.00 d . . . C21 C 1.0604(4) 0.2657(3) 0.1908(2) 0.033(1) Uani 1.00 d . . . C22 C 0.9846(3) 0.2321(3) 0.1154(2) 0.031(1) Uani 1.00 d . . . C23 C 1.0198(4) 0.2555(3) 0.2611(2) 0.038(1) Uani 1.00 d . . . C24 C 1.0869(4) 0.2792(4) 0.3378(3) 0.049(1) Uani 1.00 d . . . C25 C 0.9064(5) 0.2170(4) 0.2658(2) 0.049(1) Uani 1.00 d . . . C26 C 0.9707(4) 0.1250(3) 0.1006(2) 0.039(1) Uani 1.00 d . . . C27 C 1.0250(4) 0.0476(4) 0.1558(3) 0.047(1) Uani 1.00 d . . . C28 C 0.8983(4) 0.0816(4) 0.0329(3) 0.047(1) Uani 1.00 d . . . C29 C 0.4257 0.0516 1.0122 0.1765 Uani 1.00 d . . . H1 H 1.1987 0.2393 0.0681 0.0760 Uiso 1.00 calc . . . H2 H 1.3870 0.3429 0.0829 0.0760 Uiso 1.00 calc . . . H3 H 1.4025 0.4507 0.2102 0.0760 Uiso 1.00 calc . . . H4 H 1.2269 0.4153 0.2761 0.0760 Uiso 1.00 calc . . . H5 H 1.2388 0.0890 0.2975 0.0760 Uiso 1.00 calc . . . H6 H 1.3254 0.0349 0.1746 0.0760 Uiso 1.00 calc . . . H7 H 1.5125 0.1403 0.1792 0.0760 Uiso 1.00 calc . . . H8 H 1.5405 0.2539 0.3016 0.0760 Uiso 1.00 calc . . . H9 H 1.3710 0.2230 0.3759 0.0760 Uiso 1.00 calc . . . H10 H 0.9409 0.4497 0.1474 0.0760 Uiso 1.00 calc . . . H11 H 0.8491 0.5618 0.0301 0.0760 Uiso 1.00 calc . . . H12 H 0.8212 0.4463 -0.0920 0.0760 Uiso 1.00 calc . . . H13 H 0.8930 0.2596 -0.0550 0.0760 Uiso 1.00 calc . . . H14 H 0.6982 0.1857 0.1188 0.0760 Uiso 1.00 calc . . . H15 H 0.6788 0.3667 0.1832 0.0760 Uiso 1.00 calc . . . H16 H 0.6008 0.4972 0.0745 0.0760 Uiso 1.00 calc . . . H17 H 0.5707 0.3961 -0.0568 0.0760 Uiso 1.00 calc . . . H18 H 0.6322 0.2038 -0.0289 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 Fe1 0.0334(4) 0.0511(4) 0.0503(4) 0.0018(3) -0.0031(3) 0.0190(3) Fe2 0.0243(3) 0.0385(3) 0.0333(3) -0.0001(3) -0.0009(2) -0.0013(3) Cl1 0.2050 0.1261 0.1740 -0.0507 0.0138 -0.0343 N1 0.081(4) 0.098(4) 0.033(2) -0.007(3) -0.005(2) 0.002(2) N2 0.061(3) 0.116(4) 0.046(3) -0.020(3) 0.011(2) 0.017(3) N3 0.100(4) 0.044(3) 0.062(3) -0.004(3) -0.007(3) 0.009(2) N4 0.073(3) 0.066(3) 0.064(3) -0.005(3) -0.008(3) -0.019(2) C1 0.034(2) 0.039(2) 0.038(2) 0.001(2) -0.006(2) 0.013(2) C2 0.037(2) 0.062(3) 0.038(2) 0.001(2) 0.000(2) 0.016(2) C3 0.035(3) 0.072(4) 0.063(3) -0.005(2) 0.000(2) 0.031(3) C4 0.043(3) 0.054(3) 0.072(3) -0.013(2) -0.014(3) 0.022(3) C5 0.043(3) 0.041(3) 0.054(3) -0.006(2) -0.011(2) 0.008(2) C6 0.049(3) 0.066(4) 0.078(4) 0.008(3) -0.001(3) 0.042(3) C7 0.074(4) 0.052(3) 0.109(5) 0.014(3) 0.015(4) 0.020(3) C8 0.058(4) 0.094(5) 0.116(6) 0.038(4) 0.027(4) 0.047(5) C9 0.043(3) 0.106(6) 0.108(6) 0.008(4) -0.018(4) 0.055(5) C10 0.068(4) 0.091(5) 0.064(4) 0.016(4) -0.018(3) 0.043(3) C11 0.025(2) 0.040(2) 0.028(2) 0.000(2) 0.002(2) 0.004(2) C12 0.028(2) 0.037(2) 0.039(2) -0.003(2) -0.001(2) 0.003(2) C13 0.036(2) 0.041(2) 0.050(3) -0.001(2) 0.000(2) 0.011(2) C14 0.041(3) 0.065(3) 0.037(2) 0.002(2) 0.002(2) 0.015(2) C15 0.032(2) 0.055(3) 0.027(2) 0.004(2) 0.003(2) 0.004(2) C16 0.038(3) 0.060(3) 0.071(3) -0.012(2) 0.012(2) 0.005(3) C17 0.034(2) 0.079(4) 0.058(3) -0.007(3) 0.018(2) -0.013(3) C18 0.025(2) 0.067(3) 0.075(3) 0.008(2) 0.003(2) -0.022(3) C19 0.025(2) 0.070(4) 0.072(3) 0.003(2) -0.011(2) -0.009(3) C20 0.035(3) 0.058(3) 0.072(3) -0.009(2) -0.002(2) -0.017(3) C21 0.034(2) 0.031(2) 0.032(2) 0.003(2) 0.000(2) 0.006(2) C22 0.026(2) 0.041(2) 0.025(2) 0.004(2) 0.005(2) 0.003(2) C23 0.038(2) 0.043(2) 0.029(2) 0.003(2) -0.002(2) 0.004(2) C24 0.053(3) 0.060(3) 0.033(2) 0.002(2) 0.004(2) 0.001(2) C25 0.052(3) 0.066(3) 0.028(2) -0.006(3) 0.006(2) 0.005(2) C26 0.040(2) 0.039(2) 0.036(2) -0.001(2) 0.004(2) 0.000(2) C27 0.061(3) 0.035(2) 0.045(3) -0.008(2) 0.003(2) 0.002(2) C28 0.052(3) 0.044(3) 0.045(3) -0.001(2) 0.005(2) -0.006(2) C29 0.1168 0.1666 0.2381 -0.0033 -0.0002 0.0118 #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution DirectMethod _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 FE1 C1 2.031(4) . . yes FE1 C2 2.050(4) . . yes FE1 C3 2.051(5) . . yes FE1 C4 2.036(5) . . yes FE1 C5 2.020(5) . . yes FE1 C6 2.043(5) . . yes FE1 C7 2.052(6) . . yes FE1 C8 2.033(6) . . yes FE1 C9 2.039(6) . . yes FE1 C10 2.039(5) . . yes FE2 C11 2.033(4) . . yes FE2 C12 2.047(4) . . yes FE2 C13 2.042(4) . . yes FE2 C14 2.034(4) . . yes FE2 C15 2.026(4) . . yes FE2 C16 2.044(5) . . yes FE2 C17 2.047(5) . . yes FE2 C18 2.035(5) . . yes FE2 C19 2.034(4) . . yes FE2 C20 2.036(5) . . yes CL1 C29 1.499 . . yes N1 C24 1.134(6) . . yes N2 C25 1.132(6) . . yes N3 C27 1.134(6) . . yes N4 C28 1.141(6) . . yes C1 C2 1.438(6) . . yes C1 C5 1.431(6) . . yes C1 C21 1.457(6) . . yes C2 C3 1.425(7) . . yes C3 C4 1.415(8) . . yes C4 C5 1.415(7) . . yes C6 C7 1.415(9) . . yes C6 C10 1.412(9) . . yes C7 C8 1.434(10) . . yes C8 C9 1.39(1) . . yes C9 C10 1.419(9) . . yes C11 C12 1.436(6) . . yes C11 C15 1.450(5) . . yes C11 C22 1.445(5) . . yes C12 C13 1.422(6) . . yes C13 C14 1.400(6) . . yes C14 C15 1.413(7) . . yes C16 C17 1.420(7) . . yes C16 C20 1.401(7) . . yes C17 C18 1.407(8) . . yes C18 C19 1.417(7) . . yes C19 C20 1.415(7) . . yes C21 C22 1.505(5) . . yes C21 C23 1.352(6) . . yes C22 C26 1.366(6) . . yes C23 C24 1.447(6) . . yes C23 C25 1.430(7) . . yes C26 C27 1.428(6) . . yes C26 C28 1.430(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 C1 FE1 C2 41.3(2) . . 0_555 yes C1 FE1 C3 69.1(2) . . 0_555 yes C1 FE1 C4 68.8(2) . . 0_555 yes C1 FE1 C5 41.4(2) . . 0_555 yes C1 FE1 C6 109.3(2) . . 0_555 yes C1 FE1 C7 122.3(2) . . 0_555 yes C1 FE1 C8 158.1(3) . . 0_555 yes C1 FE1 C9 161.3(3) . . 0_555 yes C1 FE1 C10 125.3(2) . . 0_555 yes C2 FE1 C3 40.7(2) . . 0_555 yes C2 FE1 C4 68.3(2) . . 0_555 yes C2 FE1 C5 69.3(2) . . 0_555 yes C2 FE1 C6 126.3(2) . . 0_555 yes C2 FE1 C7 108.2(3) . . 0_555 yes C2 FE1 C8 121.6(3) . . 0_555 yes C2 FE1 C9 155.2(3) . . 0_555 yes C2 FE1 C10 163.0(2) . . 0_555 yes C3 FE1 C4 40.5(2) . . 0_555 yes C3 FE1 C5 69.0(2) . . 0_555 yes C3 FE1 C6 161.9(3) . . 0_555 yes C3 FE1 C7 124.1(3) . . 0_555 yes C3 FE1 C8 106.6(3) . . 0_555 yes C3 FE1 C9 119.4(2) . . 0_555 yes C3 FE1 C10 155.2(3) . . 0_555 yes C4 FE1 C5 40.8(2) . . 0_555 yes C4 FE1 C6 157.1(3) . . 0_555 yes C4 FE1 C7 160.1(3) . . 0_555 yes C4 FE1 C8 122.7(3) . . 0_555 yes C4 FE1 C9 105.9(3) . . 0_555 yes C4 FE1 C10 120.7(3) . . 0_555 yes C5 FE1 C6 122.5(2) . . 0_555 yes C5 FE1 C7 158.1(2) . . 0_555 yes C5 FE1 C8 159.0(3) . . 0_555 yes C5 FE1 C9 123.1(3) . . 0_555 yes C5 FE1 C10 107.3(2) . . 0_555 yes C6 FE1 C7 40.4(2) . . 0_555 yes C6 FE1 C8 67.8(3) . . 0_555 yes C6 FE1 C9 68.1(2) . . 0_555 yes C6 FE1 C10 40.5(2) . . 0_555 yes C7 FE1 C8 41.1(3) . . 0_555 yes C7 FE1 C9 68.6(3) . . 0_555 yes C7 FE1 C10 68.5(3) . . 0_555 yes C8 FE1 C9 39.8(3) . . 0_555 yes C8 FE1 C10 67.6(3) . . 0_555 yes C9 FE1 C10 40.7(3) . . 0_555 yes C11 FE2 C12 41.2(2) . . 0_555 yes C11 FE2 C13 68.9(2) . . 0_555 yes C11 FE2 C14 68.9(2) . . 0_555 yes C11 FE2 C15 41.9(2) . . 0_555 yes C11 FE2 C16 110.4(2) . . 0_555 yes C11 FE2 C17 123.7(2) . . 0_555 yes C11 FE2 C18 157.5(2) . . 0_555 yes C11 FE2 C19 161.3(2) . . 0_555 yes C11 FE2 C20 125.9(2) . . 0_555 yes C12 FE2 C13 40.7(2) . . 0_555 yes C12 FE2 C14 68.3(2) . . 0_555 yes C12 FE2 C15 69.6(2) . . 0_555 yes C12 FE2 C16 128.3(2) . . 0_555 yes C12 FE2 C17 109.9(2) . . 0_555 yes C12 FE2 C18 120.7(2) . . 0_555 yes C12 FE2 C19 154.4(2) . . 0_555 yes C12 FE2 C20 164.4(2) . . 0_555 yes C13 FE2 C14 40.2(2) . . 0_555 yes C13 FE2 C15 68.8(2) . . 0_555 yes C13 FE2 C16 163.9(2) . . 0_555 yes C13 FE2 C17 125.4(2) . . 0_555 yes C13 FE2 C18 106.0(2) . . 0_555 yes C13 FE2 C19 118.1(2) . . 0_555 yes C13 FE2 C20 153.4(2) . . 0_555 yes C14 FE2 C15 40.7(2) . . 0_555 yes C14 FE2 C16 155.7(2) . . 0_555 yes C14 FE2 C17 160.1(2) . . 0_555 yes C14 FE2 C18 122.2(2) . . 0_555 yes C14 FE2 C19 104.6(2) . . 0_555 yes C14 FE2 C20 119.2(2) . . 0_555 yes C15 FE2 C16 122.2(2) . . 0_555 yes C15 FE2 C17 158.9(2) . . 0_555 yes C15 FE2 C18 158.7(2) . . 0_555 yes C15 FE2 C19 122.0(2) . . 0_555 yes C15 FE2 C20 106.4(2) . . 0_555 yes C16 FE2 C17 40.6(2) . . 0_555 yes C16 FE2 C18 68.1(2) . . 0_555 yes C16 FE2 C19 67.9(2) . . 0_555 yes C16 FE2 C20 40.2(2) . . 0_555 yes C17 FE2 C18 40.3(2) . . 0_555 yes C17 FE2 C19 68.0(2) . . 0_555 yes C17 FE2 C20 68.1(2) . . 0_555 yes C18 FE2 C19 40.8(2) . . 0_555 yes C18 FE2 C20 68.5(2) . . 0_555 yes C19 FE2 C20 40.7(2) . . 0_555 yes FE1 C1 C2 70.1(2) . . 0_555 yes FE1 C1 C5 68.9(3) . . 0_555 yes FE1 C1 C21 125.8(3) . . 0_555 yes C2 C1 C5 107.4(4) . . 0_555 yes C2 C1 C21 123.7(4) . . 0_555 yes C5 C1 C21 128.8(4) . . 0_555 yes FE1 C2 C1 68.7(2) . . 0_555 yes FE1 C2 C3 69.7(3) . . 0_555 yes C1 C2 C3 107.9(4) . . 0_555 yes FE1 C3 C2 69.6(3) . . 0_555 yes FE1 C3 C4 69.2(3) . . 0_555 yes C2 C3 C4 107.7(5) . . 0_555 yes FE1 C4 C3 70.3(3) . . 0_555 yes FE1 C4 C5 69.0(3) . . 0_555 yes C3 C4 C5 109.1(4) . . 0_555 yes FE1 C5 C1 69.7(3) . . 0_555 yes FE1 C5 C4 70.2(3) . . 0_555 yes C1 C5 C4 107.7(4) . . 0_555 yes FE1 C6 C7 70.1(3) . . 0_555 yes FE1 C6 C10 69.6(3) . . 0_555 yes C7 C6 C10 109.0(6) . . 0_555 yes FE1 C7 C6 69.5(3) . . 0_555 yes FE1 C7 C8 68.7(3) . . 0_555 yes C6 C7 C8 105.8(6) . . 0_555 yes FE1 C8 C7 70.2(3) . . 0_555 yes FE1 C8 C9 70.3(4) . . 0_555 yes C7 C8 C9 109.7(6) . . 0_555 yes FE1 C9 C8 69.9(4) . . 0_555 yes FE1 C9 C10 69.7(3) . . 0_555 yes C8 C9 C10 107.7(7) . . 0_555 yes FE1 C10 C6 69.9(3) . . 0_555 yes FE1 C10 C9 69.6(3) . . 0_555 yes C6 C10 C9 107.8(7) . . 0_555 yes FE2 C11 C12 69.9(2) . . 0_555 yes FE2 C11 C15 68.8(2) . . 0_555 yes FE2 C11 C22 125.4(3) . . 0_555 yes C12 C11 C15 107.3(4) . . 0_555 yes C12 C11 C22 123.6(3) . . 0_555 yes C15 C11 C22 129.0(4) . . 0_555 yes FE2 C12 C11 68.9(2) . . 0_555 yes FE2 C12 C13 69.5(2) . . 0_555 yes C11 C12 C13 107.6(4) . . 0_555 yes FE2 C13 C12 69.8(2) . . 0_555 yes FE2 C13 C14 69.6(3) . . 0_555 yes C12 C13 C14 108.5(4) . . 0_555 yes FE2 C14 C13 70.2(3) . . 0_555 yes FE2 C14 C15 69.3(2) . . 0_555 yes C13 C14 C15 109.6(4) . . 0_555 yes FE2 C15 C11 69.3(2) . . 0_555 yes FE2 C15 C14 69.9(3) . . 0_555 yes C11 C15 C14 106.9(4) . . 0_555 yes FE2 C16 C17 69.8(3) . . 0_555 yes FE2 C16 C20 69.6(3) . . 0_555 yes C17 C16 C20 108.3(5) . . 0_555 yes FE2 C17 C16 69.6(3) . . 0_555 yes FE2 C17 C18 69.4(3) . . 0_555 yes C16 C17 C18 107.9(4) . . 0_555 yes FE2 C18 C17 70.3(3) . . 0_555 yes FE2 C18 C19 69.6(3) . . 0_555 yes C17 C18 C19 107.8(5) . . 0_555 yes FE2 C19 C18 69.6(3) . . 0_555 yes FE2 C19 C20 69.7(3) . . 0_555 yes C18 C19 C20 108.1(5) . . 0_555 yes FE2 C20 C16 70.2(3) . . 0_555 yes FE2 C20 C19 69.6(3) . . 0_555 yes C16 C20 C19 107.9(5) . . 0_555 yes C1 C21 C22 114.2(3) . . 0_555 yes C1 C21 C23 127.1(4) . . 0_555 yes C22 C21 C23 118.7(4) . . 0_555 yes C11 C22 C21 114.9(3) . . 0_555 yes C11 C22 C26 127.2(4) . . 0_555 yes C21 C22 C26 117.9(4) . . 0_555 yes C21 C23 C24 123.7(4) . . 0_555 yes C21 C23 C25 122.2(4) . . 0_555 yes C24 C23 C25 114.1(4) . . 0_555 yes N1 C24 C23 175.9(6) . . 0_555 yes N2 C25 C23 178.3(5) . . 0_555 yes C22 C26 C27 120.9(4) . . 0_555 yes C22 C26 C28 124.0(4) . . 0_555 yes C27 C26 C28 115.1(4) . . 0_555 yes N3 C27 C26 178.5(6) . . 0_555 yes N4 C28 C26 178.2(5) . . 0_555 yes #------------------------------------------------------------------------------ #===END data__Dicyano-ferrocenyl-ferrocenylethynyl-hexa-dienedinitrile _database_code_CSD 184800 #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C33 H18 Fe2 N6 ' _chemical_formula_moiety 'C33 H18 Fe2 N6 ' _chemical_formula_weight 610.24 _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 7.570(4) _cell_length_b 13.463(7) _cell_length_c 13.906(8) _cell_angle_alpha 106.062(12) _cell_angle_beta 99.238(12) _cell_angle_gamma 91.081(10) _cell_volume 1341.2(12) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4806 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 13.7 _cell_measurement_temperature 93.1 #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'blue-black' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 620.00 _exptl_absorpt_coefficient_mu 1.116 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.724 _exptl_absorpt_correction_T_max 0.925 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 14598 _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9759 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9759 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -3.0 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 5993 _reflns_number_gt 4445 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.2440 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 5994 _refine_ls_number_parameters 389 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.007Fo^2^ + 1.000\s^2^(Fo)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0090 _refine_diff_density_max 2.22 _refine_diff_density_min -1.73 _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_extinction_coef 157.2(48) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.006 0.003 ; 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' 0.349 0.972 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'N' 'N' 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 Fe1 Fe 0.50800(9) 0.37468(5) 0.79137(5) 0.0180(2) Uani 1.00 1 d . . . Fe2 Fe 0.95695(10) 0.30278(6) 0.34795(7) 0.0284(2) Uani 1.00 1 d . . . N1 N 0.9641(7) 0.3601(4) 1.0268(4) 0.0306(12) Uani 1.00 1 d . . . N2 N 1.1081(6) 0.0659(3) 0.8454(4) 0.0283(12) Uani 1.00 1 d . . . N4 N 0.6858(8) -0.0657(5) 0.4688(4) 0.045(2) Uani 1.00 1 d . . . N3 N 0.5750(7) 0.0153(4) 0.7809(4) 0.0347(13) Uani 1.00 1 d . . . N5 N 0.6286(7) -0.2093(4) 0.9117(4) 0.0348(13) Uani 1.00 1 d . . . N6 N 0.8517(7) 0.1169(4) 1.0273(5) 0.038(2) Uani 1.00 1 d . . . C5 C 0.6286(7) 0.3462(4) 0.6668(4) 0.0225(12) Uani 1.00 1 d . . . C9 C 0.2373(7) 0.3529(4) 0.7668(4) 0.0251(13) Uani 1.00 1 d . . . C31 C 0.5797(8) -0.0155(4) 0.9893(4) 0.0258(13) Uani 1.00 1 d . . . C6 C 0.4234(7) 0.2671(4) 0.8597(4) 0.0241(13) Uani 1.00 1 d . . . C21 C 0.8353(7) 0.2443(4) 0.7623(4) 0.0208(12) Uani 1.00 1 d . . . C26 C 0.9508(7) 0.3023(4) 0.9469(4) 0.0224(12) Uani 1.00 1 d . . . C7 C 0.4132(7) 0.3698(4) 0.9224(4) 0.0244(13) Uani 1.00 1 d . . . C3 C 0.6526(7) 0.5058(4) 0.7875(5) 0.0269(13) Uani 1.00 1 d . . . C24 C 0.9695(7) 0.1999(4) 0.5197(4) 0.0262(13) Uani 1.00 1 d . . . C1 C 0.7523(6) 0.3396(4) 0.7538(4) 0.0197(12) Uani 1.00 1 d . . . C15 C 1.0086(8) 0.1518(4) 0.3366(4) 0.029(1) Uani 1.00 1 d . . . C8 C 0.2959(7) 0.4225(4) 0.8647(4) 0.0266(13) Uani 1.00 1 d . . . C12 C 1.1850(7) 0.2950(5) 0.4452(5) 0.032(2) Uani 1.00 1 d . . . C30 C 0.7067(8) -0.0061(5) 0.5492(5) 0.031(1) Uani 1.00 1 d . . . C19 C 0.7766(8) 0.3310(5) 0.2315(5) 0.037(2) Uani 1.00 1 d . . . C25 C 0.9305(6) 0.2285(4) 0.8477(4) 0.0196(11) Uani 1.00 1 d . . . C10 C 0.3143(7) 0.2574(4) 0.7624(4) 0.0245(13) Uani 1.00 1 d . . . C2 C 0.7674(7) 0.4397(4) 0.8292(4) 0.0231(12) Uani 1.00 1 d . . . C28 C 0.7289(7) 0.0682(4) 0.6473(4) 0.0255(13) Uani 1.00 1 d . . . C4 C 0.5670(7) 0.4489(4) 0.6884(4) 0.0263(13) Uani 1.00 1 d . . . C22 C 0.8204(7) 0.1618(4) 0.6635(4) 0.0212(12) Uani 1.00 1 d . . . C32 C 0.6083(7) -0.1234(4) 0.9464(4) 0.0253(13) Uani 1.00 1 d . . . C11 C 1.0523(7) 0.2143(4) 0.4388(4) 0.0260(13) Uani 1.00 1 d . . . C29 C 0.6426(7) 0.0402(4) 0.7227(4) 0.0263(13) Uani 1.00 1 d . . . C23 C 0.8982(7) 0.1842(4) 0.5867(4) 0.0275(13) Uani 1.00 1 d . . . C27 C 1.0274(7) 0.1366(4) 0.8460(4) 0.0224(12) Uani 1.00 1 d . . . C14 C 1.1162(8) 0.1926(5) 0.2790(5) 0.036(2) Uani 1.00 1 d . . . C33 C 0.7319(8) 0.0574(4) 1.0108(4) 0.029(1) Uani 1.00 1 d . . . C20 C 0.6897(9) 0.3088(7) 0.3042(6) 0.049(2) Uani 1.00 1 d . . . C18 C 0.8970(10) 0.4138(5) 0.2703(6) 0.045(2) Uani 1.00 1 d . . . C13 C 1.2222(8) 0.2784(6) 0.3441(6) 0.040(2) Uani 1.00 1 d . . . C16 C 0.7609(12) 0.3920(9) 0.4013(6) 0.073(3) Uani 1.00 1 d . . . C17 C 0.8877(10) 0.4522(6) 0.3703(6) 0.047(2) Uani 1.00 1 d . . . H6 H 0.4727(7) 0.3976(4) 0.9906(4) 0.029(2) Uiso 1.00 1 c . . . H7 H 0.2637(7) 0.4919(4) 0.8882(4) 0.032(2) Uiso 1.00 1 c . . . H5 H 0.4917(7) 0.2151(4) 0.8789(4) 0.031(2) Uiso 1.00 1 c . . . H9 H 0.2978(7) 0.1972(4) 0.7059(4) 0.028(2) Uiso 1.00 1 c . . . H1 H 0.8397(7) 0.4582(4) 0.8948(4) 0.027(2) Uiso 1.00 1 c . . . H2 H 0.6382(7) 0.5764(4) 0.8202(5) 0.033(2) Uiso 1.00 1 c . . . H8 H 0.1589(7) 0.3685(4) 0.7131(4) 0.030(2) Uiso 1.00 1 c . . . H3 H 0.4817(7) 0.4744(4) 0.6447(4) 0.033(2) Uiso 1.00 1 c . . . H4 H 0.5949(7) 0.2926(4) 0.6052(4) 0.028(2) Uiso 1.00 1 c . . . H14 H 0.7306(12) 0.4031(9) 0.4670(6) 0.098(5) Uiso 1.00 1 c . . . H15 H 0.9576(10) 0.5119(6) 0.4135(6) 0.057(3) Uiso 1.00 1 c . . . H16 H 0.9741(10) 0.4396(5) 0.2339(6) 0.056(2) Uiso 1.00 1 c . . . H17 H 0.7546(8) 0.2927(5) 0.1617(5) 0.045(2) Uiso 1.00 1 c . . . H18 H 0.6038(9) 0.2531(7) 0.2950(6) 0.062(3) Uiso 1.00 1 c . . . H13 H 0.9242(8) 0.0936(4) 0.3111(4) 0.036(2) Uiso 1.00 1 c . . . H12 H 1.1142(8) 0.1670(5) 0.2079(5) 0.049(2) Uiso 1.00 1 c . . . H11 H 1.3077(8) 0.3182(6) 0.3247(6) 0.055(3) Uiso 1.00 1 c . . . H10 H 1.2367(7) 0.3487(5) 0.5039(5) 0.038(2) 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 Fe1 0.0199(4) 0.0157(4) 0.0187(4) 0.0041(3) 0.0075(3) 0.0027(3) Fe2 0.0247(5) 0.0252(4) 0.0338(5) 0.0098(3) 0.0050(3) 0.0055(3) N1 0.043(3) 0.025(2) 0.020(2) 0.004(2) 0.005(2) 0.001(2) N2 0.031(2) 0.020(2) 0.029(3) 0.005(2) 0.001(2) 0.003(2) N4 0.040(3) 0.048(3) 0.029(3) 0.014(3) -0.001(2) -0.016(3) N3 0.043(3) 0.026(2) 0.033(3) 0.002(2) 0.005(2) 0.006(2) N5 0.035(3) 0.030(3) 0.036(3) 0.002(2) 0.011(2) 0.001(2) N6 0.036(3) 0.035(3) 0.047(3) 0.003(2) 0.011(2) 0.014(3) C5 0.019(2) 0.029(3) 0.022(3) 0.009(2) 0.009(2) 0.008(2) C9 0.026(3) 0.025(3) 0.025(3) 0.009(2) 0.010(2) 0.004(2) C31 0.031(3) 0.026(3) 0.020(3) 0.002(2) 0.001(2) 0.008(2) C6 0.031(3) 0.018(2) 0.027(3) 0.001(2) 0.017(2) 0.007(2) C21 0.022(2) 0.021(2) 0.020(2) 0.005(2) 0.008(2) 0.004(2) C26 0.029(3) 0.018(2) 0.023(3) 0.003(2) 0.009(2) 0.007(2) C7 0.023(3) 0.027(3) 0.022(3) 0.004(2) 0.008(2) 0.003(2) C3 0.031(3) 0.017(2) 0.033(3) -0.000(2) 0.003(2) 0.009(2) C24 0.025(3) 0.030(3) 0.021(3) 0.008(2) 0.004(2) 0.003(2) C1 0.013(2) 0.023(2) 0.026(3) 0.005(2) 0.007(2) 0.009(2) C15 0.041(3) 0.022(3) 0.025(3) 0.010(2) 0.012(2) 0.005(2) C8 0.030(3) 0.023(3) 0.027(3) 0.008(2) 0.014(2) 0.001(2) C12 0.021(3) 0.029(3) 0.046(4) 0.008(2) 0.003(2) 0.012(3) C30 0.031(3) 0.030(3) 0.026(3) 0.014(2) 0.002(2) -0.001(2) C19 0.035(3) 0.038(3) 0.040(4) 0.014(3) 0.008(3) 0.012(3) C25 0.017(2) 0.021(2) 0.019(2) 0.002(2) 0.005(2) 0.004(2) C10 0.022(2) 0.018(2) 0.031(3) -0.002(2) 0.007(2) 0.001(2) C2 0.021(2) 0.019(2) 0.027(3) -0.001(2) 0.002(2) 0.004(2) C28 0.025(3) 0.031(3) 0.016(2) 0.010(2) 0.003(2) -0.002(2) C4 0.024(3) 0.031(3) 0.028(3) 0.005(2) 0.005(2) 0.016(2) C22 0.021(2) 0.027(3) 0.016(2) 0.013(2) 0.005(2) 0.005(2) C32 0.025(3) 0.026(3) 0.029(3) 0.006(2) 0.010(2) 0.010(2) C11 0.025(3) 0.027(3) 0.025(3) 0.009(2) 0.008(2) 0.003(2) C29 0.029(3) 0.023(3) 0.019(3) 0.003(2) -0.001(2) -0.004(2) C23 0.024(3) 0.032(3) 0.022(3) 0.010(2) 0.004(2) -0.000(2) C27 0.025(3) 0.023(3) 0.016(2) 0.003(2) 0.004(2) 0.001(2) C14 0.030(3) 0.055(4) 0.038(3) 0.028(3) 0.023(3) 0.025(3) C33 0.031(3) 0.026(3) 0.032(3) 0.002(2) 0.012(2) 0.008(2) C20 0.030(3) 0.065(5) 0.061(5) 0.006(3) 0.011(3) 0.033(4) C18 0.051(4) 0.040(4) 0.050(4) 0.017(3) 0.007(3) 0.022(3) C13 0.021(3) 0.052(4) 0.064(5) 0.017(3) 0.015(3) 0.041(4) C16 0.071(5) 0.132(8) 0.043(4) 0.089(6) 0.037(4) 0.048(5) C17 0.047(4) 0.037(4) 0.058(5) 0.023(3) 0.004(3) 0.018(3) #============================================================================== _computing_data_collection 'CrystalClear' _computing_cell_refinement 'CrystalClear' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SIR97' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure Ver. 2.00' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . C5 . 2.033(5) yes Fe1 . C9 . 2.025(6) yes Fe1 . C6 . 2.081(5) yes Fe1 . C7 . 2.080(6) yes Fe1 . C3 . 2.078(5) yes Fe1 . C1 . 2.031(5) yes Fe1 . C8 . 2.057(5) yes Fe1 . C10 . 2.043(5) yes Fe1 . C2 . 2.061(5) yes Fe1 . C4 . 2.056(6) yes Fe2 . C15 . 2.045(6) yes Fe2 . C12 . 2.039(6) yes Fe2 . C19 . 2.069(7) yes Fe2 . C11 . 2.027(6) yes Fe2 . C14 . 2.055(6) yes Fe2 . C20 . 2.027(7) yes Fe2 . C18 . 2.090(7) yes Fe2 . C13 . 2.047(6) yes Fe2 . C16 . 2.031(6) yes Fe2 . C17 . 2.040(7) yes N1 . C26 . 1.155(7) yes N2 . C27 . 1.140(7) yes N4 . C30 . 1.166(7) yes N3 . C29 . 1.143(8) yes N5 . C32 . 1.147(7) yes N6 . C33 . 1.150(8) yes C5 . C1 . 1.430(7) yes C5 . C4 . 1.434(7) yes C9 . C8 . 1.419(7) yes C9 . C10 . 1.412(7) yes C31 . C32 . 1.445(8) yes C31 . C33 . 1.436(8) yes C6 . C7 . 1.427(7) yes C6 . C10 . 1.438(8) yes C21 . C1 . 1.464(7) yes C21 . C25 . 1.358(7) yes C21 . C22 . 1.495(7) yes C26 . C25 . 1.442(7) yes C7 . C8 . 1.431(8) yes C3 . C2 . 1.427(7) yes C3 . C4 . 1.420(8) yes C24 . C11 . 1.427(8) yes C24 . C23 . 1.213(8) yes C1 . C2 . 1.450(7) yes C15 . C11 . 1.419(8) yes C15 . C14 . 1.430(8) yes C12 . C11 . 1.440(8) yes C12 . C13 . 1.44(1) yes C30 . C28 . 1.434(7) yes C19 . C20 . 1.38(1) yes C19 . C18 . 1.35(1) yes C25 . C27 . 1.447(7) yes C28 . C22 . 1.371(8) yes C28 . C29 . 1.448(8) yes C22 . C23 . 1.398(8) yes C14 . C13 . 1.40(1) yes C20 . C16 . 1.509(13) yes C18 . C17 . 1.356(11) yes C16 . C17 . 1.435(13) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C5 . Fe1 . C9 . 117.1(2) yes C5 . Fe1 . C6 . 127.3(2) yes C9 . Fe1 . C6 . 68.1(2) yes C5 . Fe1 . C7 . 165.6(2) yes C9 . Fe1 . C7 . 68.2(2) yes C6 . Fe1 . C7 . 40.1(2) yes C5 . Fe1 . C3 . 68.5(2) yes C9 . Fe1 . C3 . 125.8(2) yes C6 . Fe1 . C3 . 154.9(2) yes C7 . Fe1 . C3 . 120.5(2) yes C5 . Fe1 . C1 . 41.2(2) yes C9 . Fe1 . C1 . 152.2(2) yes C6 . Fe1 . C1 . 108.9(2) yes C7 . Fe1 . C1 . 128.4(2) yes C3 . Fe1 . C1 . 68.8(2) yes C5 . Fe1 . C8 . 151.6(2) yes C9 . Fe1 . C8 . 40.7(2) yes C6 . Fe1 . C8 . 67.8(2) yes C7 . Fe1 . C8 . 40.5(2) yes C3 . Fe1 . C8 . 107.9(2) yes C5 . Fe1 . C10 . 106.3(2) yes C9 . Fe1 . C10 . 40.6(2) yes C6 . Fe1 . C10 . 40.8(2) yes C7 . Fe1 . C10 . 68.3(2) yes C3 . Fe1 . C10 . 162.9(2) yes C5 . Fe1 . C2 . 69.2(2) yes C9 . Fe1 . C2 . 163.9(2) yes C6 . Fe1 . C2 . 121.3(2) yes C7 . Fe1 . C2 . 109.6(2) yes C3 . Fe1 . C2 . 40.3(2) yes C5 . Fe1 . C4 . 41.1(2) yes C9 . Fe1 . C4 . 106.0(2) yes C6 . Fe1 . C4 . 164.3(2) yes C7 . Fe1 . C4 . 152.9(2) yes C3 . Fe1 . C4 . 40.2(2) yes C1 . Fe1 . C8 . 166.0(2) yes C1 . Fe1 . C10 . 118.8(2) yes C8 . Fe1 . C10 . 68.4(2) yes C1 . Fe1 . C2 . 41.5(2) yes C8 . Fe1 . C2 . 127.4(2) yes C10 . Fe1 . C2 . 154.8(2) yes C1 . Fe1 . C4 . 69.1(2) yes C8 . Fe1 . C4 . 117.9(2) yes C10 . Fe1 . C4 . 125.4(2) yes C2 . Fe1 . C4 . 68.3(2) yes C15 . Fe2 . C12 . 69.5(2) yes C15 . Fe2 . C19 . 117.2(2) yes C12 . Fe2 . C19 . 163.6(3) yes C15 . Fe2 . C11 . 40.8(2) yes C12 . Fe2 . C11 . 41.5(2) yes C19 . Fe2 . C11 . 152.6(3) yes C15 . Fe2 . C14 . 40.8(2) yes C12 . Fe2 . C14 . 68.7(3) yes C19 . Fe2 . C14 . 105.9(3) yes C11 . Fe2 . C14 . 68.3(2) yes C15 . Fe2 . C20 . 108.1(3) yes C12 . Fe2 . C20 . 155.9(3) yes C19 . Fe2 . C20 . 39.5(3) yes C11 . Fe2 . C20 . 121.1(3) yes C14 . Fe2 . C20 . 126.1(3) yes C15 . Fe2 . C18 . 146.4(3) yes C12 . Fe2 . C18 . 128.3(3) yes C19 . Fe2 . C18 . 38.0(3) yes C11 . Fe2 . C18 . 169.4(3) yes C14 . Fe2 . C18 . 113.1(3) yes C15 . Fe2 . C13 . 68.3(3) yes C12 . Fe2 . C13 . 41.1(3) yes C19 . Fe2 . C13 . 125.1(3) yes C11 . Fe2 . C13 . 68.5(2) yes C14 . Fe2 . C13 . 39.8(3) yes C15 . Fe2 . C16 . 132.7(4) yes C12 . Fe2 . C16 . 119.5(3) yes C19 . Fe2 . C16 . 68.2(3) yes C11 . Fe2 . C16 . 112.5(3) yes C14 . Fe2 . C16 . 169.2(4) yes C15 . Fe2 . C17 . 173.7(3) yes C12 . Fe2 . C17 . 110.8(3) yes C19 . Fe2 . C17 . 64.3(3) yes C11 . Fe2 . C17 . 135.5(3) yes C14 . Fe2 . C17 . 145.4(3) yes C20 . Fe2 . C18 . 67.3(3) yes C20 . Fe2 . C13 . 162.0(3) yes C18 . Fe2 . C13 . 105.4(3) yes C20 . Fe2 . C16 . 43.7(4) yes C18 . Fe2 . C16 . 68.3(3) yes C13 . Fe2 . C16 . 151.0(4) yes C20 . Fe2 . C17 . 68.8(3) yes C18 . Fe2 . C17 . 38.3(3) yes C13 . Fe2 . C17 . 116.4(3) yes C16 . Fe2 . C17 . 41.3(4) yes Fe1 . C5 . C1 . 69.3(3) yes Fe1 . C5 . C4 . 70.3(3) yes C1 . C5 . C4 . 108.0(5) yes Fe1 . C9 . C8 . 70.9(3) yes Fe1 . C9 . C10 . 70.4(3) yes C8 . C9 . C10 . 109.0(5) yes C32 . C31 . C33 . 117.1(5) yes Fe1 . C6 . C7 . 69.9(3) yes Fe1 . C6 . C10 . 68.2(3) yes C7 . C6 . C10 . 107.8(5) yes C1 . C21 . C25 . 126.5(5) yes C1 . C21 . C22 . 114.0(4) yes C25 . C21 . C22 . 119.4(4) yes N1 . C26 . C25 . 178.5(6) yes Fe1 . C7 . C6 . 70.0(3) yes Fe1 . C7 . C8 . 68.9(3) yes C6 . C7 . C8 . 107.8(5) yes Fe1 . C3 . C2 . 69.2(3) yes Fe1 . C3 . C4 . 69.1(3) yes C2 . C3 . C4 . 108.5(5) yes C11 . C24 . C23 . 177.8(6) yes Fe1 . C1 . C5 . 69.5(3) yes Fe1 . C1 . C21 . 122.6(4) yes C5 . C1 . C21 . 123.8(5) yes Fe1 . C1 . C2 . 70.3(3) yes C5 . C1 . C2 . 107.5(4) yes C21 . C1 . C2 . 128.6(5) yes Fe2 . C15 . C11 . 68.9(3) yes Fe2 . C15 . C14 . 69.9(3) yes C11 . C15 . C14 . 107.0(5) yes Fe1 . C8 . C9 . 68.4(3) yes Fe1 . C8 . C7 . 70.6(3) yes C9 . C8 . C7 . 107.8(5) yes Fe2 . C12 . C11 . 68.8(3) yes Fe2 . C12 . C13 . 69.7(3) yes C11 . C12 . C13 . 105.8(5) yes N4 . C30 . C28 . 178.7(6) yes Fe2 . C19 . C20 . 68.6(4) yes Fe2 . C19 . C18 . 71.8(4) yes C20 . C19 . C18 . 112.8(7) yes C21 . C25 . C26 . 123.8(5) yes C21 . C25 . C27 . 122.3(5) yes C26 . C25 . C27 . 113.8(4) yes Fe1 . C10 . C9 . 69.0(3) yes Fe1 . C10 . C6 . 71.0(3) yes C9 . C10 . C6 . 107.6(5) yes Fe1 . C2 . C3 . 70.5(3) yes Fe1 . C2 . C1 . 68.1(3) yes C3 . C2 . C1 . 107.7(5) yes C30 . C28 . C22 . 119.7(5) yes C30 . C28 . C29 . 116.4(5) yes C22 . C28 . C29 . 123.8(5) yes Fe1 . C4 . C5 . 68.6(3) yes Fe1 . C4 . C3 . 70.7(3) yes C5 . C4 . C3 . 108.4(5) yes C21 . C22 . C28 . 121.3(5) yes C21 . C22 . C23 . 117.9(5) yes C28 . C22 . C23 . 120.7(5) yes N5 . C32 . C31 . 179.1(6) yes Fe2 . C11 . C24 . 124.1(4) yes Fe2 . C11 . C15 . 70.3(3) yes C24 . C11 . C15 . 124.1(5) yes Fe2 . C11 . C12 . 69.7(3) yes C24 . C11 . C12 . 126.7(5) yes C15 . C11 . C12 . 109.1(5) yes N3 . C29 . C28 . 178.1(6) yes C24 . C23 . C22 . 177.3(6) yes N2 . C27 . C25 . 178.0(5) yes Fe2 . C14 . C15 . 69.2(3) yes Fe2 . C14 . C13 . 69.8(4) yes C15 . C14 . C13 . 108.7(6) yes N6 . C33 . C31 . 178.7(6) yes Fe2 . C20 . C19 . 71.9(4) yes Fe2 . C20 . C16 . 68.3(4) yes C19 . C20 . C16 . 105.1(7) yes Fe2 . C18 . C19 . 70.2(4) yes Fe2 . C18 . C17 . 68.9(4) yes C19 . C18 . C17 . 107.5(7) yes Fe2 . C13 . C12 . 69.1(3) yes Fe2 . C13 . C14 . 70.4(3) yes C12 . C13 . C14 . 109.3(5) yes Fe2 . C16 . C20 . 68.0(4) yes Fe2 . C16 . C17 . 69.7(4) yes C20 . C16 . C17 . 102.7(6) yes Fe2 . C17 . C18 . 72.8(4) yes Fe2 . C17 . C16 . 69.0(4) yes C18 . C17 . C16 . 111.9(7) yes #============================================================================== #===END