# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Chemical Science' _journal_coden_Cambridge 1475 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address X.Bao ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; P.-H.Guo ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; W.Liu ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; J.Tucek ; Department of Experimental Physics Faculty of Science Palacky University Olomouc 77146 Czech Republic ; A.Bousseksou ; Laboratoire de Chimie de Coordination CNRS Toulouse 31077 France ; W.-X.Zhang ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; J.-D.Leng ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; 'Xiao-Ming Chen' ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; 'Ming-Liang Tong' ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; _publ_contact_author_name 'Dr Ming-Liang Tong' _publ_contact_author_email tongml@mail.sysu.edu.cn _publ_contact_author_address ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 PR China ; _publ_contact_author_phone 86-20-8411-0966 _publ_contact_author_fax 81-20-8411-2245 _publ_section_title ; Record high temperature spin transition exhibited by two new metal-organic frameworks ; # Attachment '- CIF_MLTong.cif' #TrackingRef '- CIF_MLTong.cif' #===================================== data_1_293K _database_code_depnum_ccdc_archive 'CCDC 824534' #TrackingRef '- CIF_MLTong.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H16 Fe N10' _chemical_formula_weight 500.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8471(12) _cell_length_b 9.1441(12) _cell_length_c 14.785(2) _cell_angle_alpha 94.125(2) _cell_angle_beta 103.444(2) _cell_angle_gamma 111.236(2) _cell_volume 1068.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 0.744 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7968 _exptl_absorpt_correction_T_max 0.8716 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5841 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4087 _reflns_number_gt 3690 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+0.7079P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4087 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.0967 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.5000 0.5000 0.02686(13) Uani 1 2 d S . . Fe2 Fe 0.5000 0.0000 0.0000 0.02672(13) Uani 1 2 d S . . N1 N 0.2861(2) 0.3663(2) 0.40544(13) 0.0302(4) Uani 1 1 d . . . N2 N 0.2252(2) 0.2309(2) 0.34128(14) 0.0336(4) Uani 1 1 d . . . N3 N 0.0360(3) 0.3474(2) 0.31544(14) 0.0360(4) Uani 1 1 d . . . N4 N 0.3764(2) 0.6459(2) 0.50028(13) 0.0308(4) Uani 1 1 d . . . N5 N -0.2702(2) 0.0009(2) 0.07049(13) 0.0321(4) Uani 1 1 d . . . N6 N 0.5596(2) 0.2134(2) 0.07353(13) 0.0299(4) Uani 1 1 d . . . N7 N 0.5463(2) 0.2746(2) 0.15663(13) 0.0323(4) Uani 1 1 d . . . N8 N 0.6899(3) 0.4778(2) 0.09069(15) 0.0441(5) Uani 1 1 d . . . N9 N 0.6027(2) 0.1407(2) -0.08782(13) 0.0333(4) Uani 1 1 d . . . N10 N 0.5956(2) 0.5886(2) 0.39616(13) 0.0303(4) Uani 1 1 d . . . C1 C 0.1718(3) 0.4309(3) 0.38822(16) 0.0309(5) Uani 1 1 d . . . C2 C 0.0775(3) 0.2258(3) 0.28866(16) 0.0321(5) Uani 1 1 d . . . C3 C 0.2157(3) 0.5848(3) 0.44427(16) 0.0324(5) Uani 1 1 d . . . C4 C 0.1075(4) 0.6638(3) 0.4405(2) 0.0504(7) Uani 1 1 d . . . H4 H -0.0018 0.6194 0.4006 0.061 Uiso 1 1 calc R . . C5 C 0.1667(4) 0.8102(4) 0.4976(2) 0.0645(9) Uani 1 1 d . . . H5 H 0.0970 0.8658 0.4974 0.077 Uiso 1 1 calc R . . C6 C 0.3296(4) 0.8728(3) 0.5549(2) 0.0554(8) Uani 1 1 d . . . H6 H 0.3711 0.9713 0.5938 0.066 Uiso 1 1 calc R . . C7 C 0.4307(3) 0.7890(3) 0.55430(18) 0.0395(6) Uani 1 1 d . . . H7 H 0.5411 0.8332 0.5929 0.047 Uiso 1 1 calc R . . C8 C -0.0224(3) 0.1068(3) 0.20280(16) 0.0330(5) Uani 1 1 d . . . C9 C 0.0415(3) 0.0043(3) 0.16731(19) 0.0421(6) Uani 1 1 d . . . H9 H 0.1464 0.0064 0.1989 0.051 Uiso 1 1 calc R . . C10 C -0.0534(3) -0.1003(3) 0.08458(19) 0.0455(6) Uani 1 1 d . . . H10 H -0.0150 -0.1726 0.0604 0.055 Uiso 1 1 calc R . . C11 C -0.2057(3) -0.0971(3) 0.03784(17) 0.0375(5) Uani 1 1 d . . . H11 H -0.2668 -0.1662 -0.0191 0.045 Uiso 1 1 calc R . . C12 C -0.1785(3) 0.0982(3) 0.15285(16) 0.0336(5) Uani 1 1 d . . . H12 H -0.2231 0.1641 0.1779 0.040 Uiso 1 1 calc R . . C13 C 0.6439(3) 0.3364(3) 0.03726(16) 0.0357(5) Uani 1 1 d . . . C14 C 0.6265(3) 0.4323(3) 0.16352(16) 0.0342(5) Uani 1 1 d . . . C15 C 0.6689(3) 0.2998(3) -0.05412(17) 0.0393(6) Uani 1 1 d . . . C16 C 0.7477(5) 0.4116(4) -0.1032(2) 0.0648(9) Uani 1 1 d . . . H16 H 0.7934 0.5195 -0.0778 0.078 Uiso 1 1 calc R . . C17 C 0.7581(5) 0.3607(4) -0.1912(2) 0.0679(10) Uani 1 1 d . . . H17 H 0.8136 0.4337 -0.2252 0.081 Uiso 1 1 calc R . . C18 C 0.6857(4) 0.2018(4) -0.2273(2) 0.0539(7) Uani 1 1 d . . . H18 H 0.6876 0.1659 -0.2874 0.065 Uiso 1 1 calc R . . C19 C 0.6096(3) 0.0948(3) -0.17449(17) 0.0410(6) Uani 1 1 d . . . H19 H 0.5613 -0.0132 -0.1998 0.049 Uiso 1 1 calc R . . C20 C 0.6465(3) 0.5456(3) 0.24540(16) 0.0346(5) Uani 1 1 d . . . C21 C 0.7412(4) 0.7074(3) 0.25513(19) 0.0457(6) Uani 1 1 d . . . H21 H 0.7895 0.7482 0.2081 0.055 Uiso 1 1 calc R . . C22 C 0.7622(4) 0.8064(3) 0.33613(19) 0.0455(6) Uani 1 1 d . . . H22 H 0.8249 0.9152 0.3441 0.055 Uiso 1 1 calc R . . C23 C 0.6905(3) 0.7440(3) 0.40467(17) 0.0364(5) Uani 1 1 d . . . H23 H 0.7083 0.8122 0.4594 0.044 Uiso 1 1 calc R . . C24 C 0.5743(3) 0.4930(3) 0.31657(16) 0.0332(5) Uani 1 1 d . . . H24 H 0.5070 0.3854 0.3091 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0313(2) 0.0240(2) 0.0238(2) -0.00201(17) 0.00413(18) 0.01254(18) Fe2 0.0289(2) 0.0265(2) 0.0215(2) -0.00253(17) 0.00538(17) 0.00932(18) N1 0.0322(10) 0.0288(9) 0.0271(9) -0.0008(7) 0.0050(8) 0.0121(8) N2 0.0345(10) 0.0292(10) 0.0313(10) -0.0036(8) 0.0019(8) 0.0120(8) N3 0.0353(11) 0.0346(10) 0.0333(10) -0.0031(8) 0.0024(8) 0.0145(9) N4 0.0354(10) 0.0279(9) 0.0279(9) 0.0000(8) 0.0059(8) 0.0135(8) N5 0.0334(10) 0.0324(10) 0.0264(9) -0.0008(8) 0.0071(8) 0.0101(8) N6 0.0319(10) 0.0315(10) 0.0246(9) -0.0009(8) 0.0063(8) 0.0123(8) N7 0.0383(11) 0.0317(10) 0.0261(9) -0.0016(8) 0.0096(8) 0.0136(8) N8 0.0647(15) 0.0296(11) 0.0361(11) 0.0009(9) 0.0211(10) 0.0127(10) N9 0.0342(10) 0.0397(11) 0.0262(9) -0.0007(8) 0.0085(8) 0.0160(9) N10 0.0353(10) 0.0286(10) 0.0273(9) 0.0006(8) 0.0065(8) 0.0147(8) C1 0.0299(11) 0.0322(12) 0.0289(11) 0.0014(9) 0.0047(9) 0.0132(9) C2 0.0342(12) 0.0291(11) 0.0299(11) 0.0011(9) 0.0062(9) 0.0115(9) C3 0.0364(12) 0.0302(12) 0.0295(11) 0.0007(9) 0.0048(9) 0.0154(10) C4 0.0430(15) 0.0483(16) 0.0556(17) -0.0096(13) -0.0030(13) 0.0266(13) C5 0.0605(19) 0.0534(18) 0.078(2) -0.0162(16) -0.0040(16) 0.0404(16) C6 0.0582(18) 0.0395(15) 0.0616(18) -0.0146(13) -0.0013(14) 0.0266(13) C7 0.0440(14) 0.0323(12) 0.0372(13) -0.0051(10) 0.0005(11) 0.0178(11) C8 0.0331(12) 0.0303(11) 0.0294(11) -0.0013(9) 0.0075(9) 0.0073(9) C9 0.0365(13) 0.0428(14) 0.0425(14) -0.0048(11) 0.0044(11) 0.0165(11) C10 0.0431(14) 0.0473(15) 0.0453(15) -0.0096(12) 0.0106(12) 0.0211(12) C11 0.0360(13) 0.0394(13) 0.0305(12) -0.0070(10) 0.0059(10) 0.0120(10) C12 0.0349(12) 0.0308(12) 0.0311(12) -0.0014(9) 0.0051(10) 0.0118(10) C13 0.0454(14) 0.0311(12) 0.0287(11) 0.0006(9) 0.0129(10) 0.0119(10) C14 0.0427(13) 0.0303(12) 0.0278(11) -0.0001(9) 0.0094(10) 0.0135(10) C15 0.0508(15) 0.0364(13) 0.0311(12) 0.0028(10) 0.0154(11) 0.0155(11) C16 0.101(3) 0.0435(16) 0.0516(18) 0.0106(14) 0.0393(18) 0.0187(17) C17 0.101(3) 0.061(2) 0.0508(18) 0.0204(16) 0.0435(19) 0.0260(19) C18 0.077(2) 0.0597(18) 0.0342(14) 0.0080(13) 0.0254(14) 0.0316(16) C19 0.0487(15) 0.0485(15) 0.0284(12) -0.0007(11) 0.0113(11) 0.0230(12) C20 0.0435(13) 0.0299(12) 0.0300(11) 0.0001(9) 0.0084(10) 0.0159(10) C21 0.0673(18) 0.0320(13) 0.0387(14) 0.0044(11) 0.0241(13) 0.0150(12) C22 0.0656(18) 0.0233(11) 0.0439(14) -0.0002(10) 0.0201(13) 0.0114(11) C23 0.0483(14) 0.0265(11) 0.0329(12) -0.0016(9) 0.0090(11) 0.0155(10) C24 0.0406(13) 0.0281(11) 0.0286(11) -0.0015(9) 0.0078(10) 0.0130(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.9695(19) . ? Fe1 N1 1.9695(19) 2_666 ? Fe1 N10 2.0040(19) 2_666 ? Fe1 N10 2.0040(19) . ? Fe1 N4 2.0086(19) 2_666 ? Fe1 N4 2.0086(19) . ? Fe2 N6 1.9875(18) 2_655 ? Fe2 N6 1.9875(18) . ? Fe2 N9 2.027(2) 2_655 ? Fe2 N9 2.027(2) . ? Fe2 N5 2.055(2) 2 ? Fe2 N5 2.055(2) 1_655 ? N1 C1 1.330(3) . ? N1 N2 1.355(2) . ? N2 C2 1.339(3) . ? N3 C1 1.342(3) . ? N3 C2 1.352(3) . ? N4 C7 1.340(3) . ? N4 C3 1.353(3) . ? N5 C12 1.340(3) . ? N5 C11 1.341(3) . ? N5 Fe2 2.055(2) 1_455 ? N6 C13 1.332(3) . ? N6 N7 1.361(2) . ? N7 C14 1.341(3) . ? N8 C13 1.336(3) . ? N8 C14 1.350(3) . ? N9 C19 1.342(3) . ? N9 C15 1.361(3) . ? N10 C23 1.342(3) . ? N10 C24 1.347(3) . ? C1 C3 1.451(3) . ? C2 C8 1.469(3) . ? C3 C4 1.387(3) . ? C4 C5 1.379(4) . ? C4 H4 0.9300 . ? C5 C6 1.373(4) . ? C5 H5 0.9300 . ? C6 C7 1.374(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C12 1.377(3) . ? C8 C9 1.387(3) . ? C9 C10 1.374(3) . ? C9 H9 0.9300 . ? C10 C11 1.375(4) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C15 1.454(3) . ? C14 C20 1.469(3) . ? C15 C16 1.372(4) . ? C16 C17 1.385(4) . ? C16 H16 0.9300 . ? C17 C18 1.364(4) . ? C17 H17 0.9300 . ? C18 C19 1.378(4) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C24 1.382(3) . ? C20 C21 1.388(3) . ? C21 C22 1.381(3) . ? C21 H21 0.9300 . ? C22 C23 1.369(4) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N1 180.000(1) . 2_666 ? N1 Fe1 N10 90.45(8) . 2_666 ? N1 Fe1 N10 89.55(8) 2_666 2_666 ? N1 Fe1 N10 89.55(8) . . ? N1 Fe1 N10 90.45(8) 2_666 . ? N10 Fe1 N10 180.0 2_666 . ? N1 Fe1 N4 99.38(8) . 2_666 ? N1 Fe1 N4 80.62(8) 2_666 2_666 ? N10 Fe1 N4 92.60(8) 2_666 2_666 ? N10 Fe1 N4 87.40(8) . 2_666 ? N1 Fe1 N4 80.62(8) . . ? N1 Fe1 N4 99.38(8) 2_666 . ? N10 Fe1 N4 87.40(8) 2_666 . ? N10 Fe1 N4 92.60(8) . . ? N4 Fe1 N4 180.000(1) 2_666 . ? N6 Fe2 N6 180.00(13) 2_655 . ? N6 Fe2 N9 79.97(7) 2_655 2_655 ? N6 Fe2 N9 100.03(7) . 2_655 ? N6 Fe2 N9 100.03(7) 2_655 . ? N6 Fe2 N9 79.97(7) . . ? N9 Fe2 N9 180.00(12) 2_655 . ? N6 Fe2 N5 90.09(8) 2_655 2 ? N6 Fe2 N5 89.91(8) . 2 ? N9 Fe2 N5 92.04(8) 2_655 2 ? N9 Fe2 N5 87.96(8) . 2 ? N6 Fe2 N5 89.91(8) 2_655 1_655 ? N6 Fe2 N5 90.09(8) . 1_655 ? N9 Fe2 N5 87.96(8) 2_655 1_655 ? N9 Fe2 N5 92.04(8) . 1_655 ? N5 Fe2 N5 180.00(11) 2 1_655 ? C1 N1 N2 106.80(18) . . ? C1 N1 Fe1 114.87(15) . . ? N2 N1 Fe1 137.65(15) . . ? C2 N2 N1 104.23(18) . . ? C1 N3 C2 100.29(19) . . ? C7 N4 C3 117.5(2) . . ? C7 N4 Fe1 127.42(16) . . ? C3 N4 Fe1 114.83(15) . . ? C12 N5 C11 116.6(2) . . ? C12 N5 Fe2 121.27(16) . 1_455 ? C11 N5 Fe2 122.14(16) . 1_455 ? C13 N6 N7 106.85(18) . . ? C13 N6 Fe2 115.23(15) . . ? N7 N6 Fe2 137.82(15) . . ? C14 N7 N6 103.78(18) . . ? C13 N8 C14 100.6(2) . . ? C19 N9 C15 117.4(2) . . ? C19 N9 Fe2 127.56(18) . . ? C15 N9 Fe2 115.03(15) . . ? C23 N10 C24 117.1(2) . . ? C23 N10 Fe1 121.65(15) . . ? C24 N10 Fe1 121.21(16) . . ? N1 C1 N3 113.9(2) . . ? N1 C1 C3 116.7(2) . . ? N3 C1 C3 129.2(2) . . ? N2 C2 N3 114.7(2) . . ? N2 C2 C8 122.3(2) . . ? N3 C2 C8 122.6(2) . . ? N4 C3 C4 122.9(2) . . ? N4 C3 C1 112.7(2) . . ? C4 C3 C1 124.4(2) . . ? C5 C4 C3 118.2(3) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? C6 C5 C4 119.3(3) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C5 C6 C7 119.6(3) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? N4 C7 C6 122.6(2) . . ? N4 C7 H7 118.7 . . ? C6 C7 H7 118.7 . . ? C12 C8 C9 118.0(2) . . ? C12 C8 C2 121.3(2) . . ? C9 C8 C2 120.7(2) . . ? C10 C9 C8 118.7(2) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? C9 C10 C11 119.4(2) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? N5 C11 C10 123.1(2) . . ? N5 C11 H11 118.4 . . ? C10 C11 H11 118.4 . . ? N5 C12 C8 124.2(2) . . ? N5 C12 H12 117.9 . . ? C8 C12 H12 117.9 . . ? N6 C13 N8 113.8(2) . . ? N6 C13 C15 116.7(2) . . ? N8 C13 C15 129.4(2) . . ? N7 C14 N8 114.89(19) . . ? N7 C14 C20 122.1(2) . . ? N8 C14 C20 123.0(2) . . ? N9 C15 C16 122.6(2) . . ? N9 C15 C13 112.7(2) . . ? C16 C15 C13 124.6(2) . . ? C15 C16 C17 118.7(3) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? C18 C17 C16 119.0(3) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C17 C18 C19 119.7(3) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? N9 C19 C18 122.4(3) . . ? N9 C19 H19 118.8 . . ? C18 C19 H19 118.8 . . ? C24 C20 C21 117.9(2) . . ? C24 C20 C14 120.6(2) . . ? C21 C20 C14 121.5(2) . . ? C22 C21 C20 118.6(2) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? C23 C22 C21 119.9(2) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? N10 C23 C22 122.7(2) . . ? N10 C23 H23 118.6 . . ? C22 C23 H23 118.6 . . ? N10 C24 C20 123.8(2) . . ? N10 C24 H24 118.1 . . ? C20 C24 H24 118.1 . . ? 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 N1 Fe1 N1 C1 -121(100) 2_666 . . . ? N10 Fe1 N1 C1 87.39(17) 2_666 . . . ? N10 Fe1 N1 C1 -92.61(17) . . . . ? N4 Fe1 N1 C1 -179.90(16) 2_666 . . . ? N4 Fe1 N1 C1 0.10(16) . . . . ? N1 Fe1 N1 N2 48(100) 2_666 . . . ? N10 Fe1 N1 N2 -103.7(2) 2_666 . . . ? N10 Fe1 N1 N2 76.3(2) . . . . ? N4 Fe1 N1 N2 -10.9(2) 2_666 . . . ? N4 Fe1 N1 N2 169.1(2) . . . . ? C1 N1 N2 C2 0.9(2) . . . . ? Fe1 N1 N2 C2 -168.62(18) . . . . ? N1 Fe1 N4 C7 177.8(2) . . . . ? N1 Fe1 N4 C7 -2.2(2) 2_666 . . . ? N10 Fe1 N4 C7 86.9(2) 2_666 . . . ? N10 Fe1 N4 C7 -93.1(2) . . . . ? N4 Fe1 N4 C7 -104(100) 2_666 . . . ? N1 Fe1 N4 C3 3.28(16) . . . . ? N1 Fe1 N4 C3 -176.72(16) 2_666 . . . ? N10 Fe1 N4 C3 -87.61(17) 2_666 . . . ? N10 Fe1 N4 C3 92.39(17) . . . . ? N4 Fe1 N4 C3 82(100) 2_666 . . . ? N6 Fe2 N6 C13 7(100) 2_655 . . . ? N9 Fe2 N6 C13 175.02(17) 2_655 . . . ? N9 Fe2 N6 C13 -4.98(17) . . . . ? N5 Fe2 N6 C13 -92.92(18) 2 . . . ? N5 Fe2 N6 C13 87.08(18) 1_655 . . . ? N6 Fe2 N6 N7 -169(100) 2_655 . . . ? N9 Fe2 N6 N7 -0.8(2) 2_655 . . . ? N9 Fe2 N6 N7 179.2(2) . . . . ? N5 Fe2 N6 N7 91.3(2) 2 . . . ? N5 Fe2 N6 N7 -88.7(2) 1_655 . . . ? C13 N6 N7 C14 -0.5(2) . . . . ? Fe2 N6 N7 C14 175.59(18) . . . . ? N6 Fe2 N9 C19 5.6(2) 2_655 . . . ? N6 Fe2 N9 C19 -174.4(2) . . . . ? N9 Fe2 N9 C19 -107(100) 2_655 . . . ? N5 Fe2 N9 C19 -84.2(2) 2 . . . ? N5 Fe2 N9 C19 95.8(2) 1_655 . . . ? N6 Fe2 N9 C15 -175.66(17) 2_655 . . . ? N6 Fe2 N9 C15 4.34(17) . . . . ? N9 Fe2 N9 C15 71(100) 2_655 . . . ? N5 Fe2 N9 C15 94.62(18) 2 . . . ? N5 Fe2 N9 C15 -85.38(18) 1_655 . . . ? N1 Fe1 N10 C23 138.46(19) . . . . ? N1 Fe1 N10 C23 -41.54(19) 2_666 . . . ? N10 Fe1 N10 C23 -78(100) 2_666 . . . ? N4 Fe1 N10 C23 -122.13(19) 2_666 . . . ? N4 Fe1 N10 C23 57.87(19) . . . . ? N1 Fe1 N10 C24 -44.89(18) . . . . ? N1 Fe1 N10 C24 135.11(18) 2_666 . . . ? N10 Fe1 N10 C24 99(100) 2_666 . . . ? N4 Fe1 N10 C24 54.52(18) 2_666 . . . ? N4 Fe1 N10 C24 -125.48(18) . . . . ? N2 N1 C1 N3 -0.2(3) . . . . ? Fe1 N1 C1 N3 172.00(16) . . . . ? N2 N1 C1 C3 -175.5(2) . . . . ? Fe1 N1 C1 C3 -3.3(3) . . . . ? C2 N3 C1 N1 -0.5(3) . . . . ? C2 N3 C1 C3 174.0(2) . . . . ? N1 N2 C2 N3 -1.4(3) . . . . ? N1 N2 C2 C8 172.5(2) . . . . ? C1 N3 C2 N2 1.2(3) . . . . ? C1 N3 C2 C8 -172.7(2) . . . . ? C7 N4 C3 C4 0.4(4) . . . . ? Fe1 N4 C3 C4 175.4(2) . . . . ? C7 N4 C3 C1 179.2(2) . . . . ? Fe1 N4 C3 C1 -5.7(3) . . . . ? N1 C1 C3 N4 6.0(3) . . . . ? N3 C1 C3 N4 -168.5(2) . . . . ? N1 C1 C3 C4 -175.2(3) . . . . ? N3 C1 C3 C4 10.4(4) . . . . ? N4 C3 C4 C5 -1.0(5) . . . . ? C1 C3 C4 C5 -179.7(3) . . . . ? C3 C4 C5 C6 0.7(5) . . . . ? C4 C5 C6 C7 0.0(5) . . . . ? C3 N4 C7 C6 0.5(4) . . . . ? Fe1 N4 C7 C6 -173.9(2) . . . . ? C5 C6 C7 N4 -0.7(5) . . . . ? N2 C2 C8 C12 176.2(2) . . . . ? N3 C2 C8 C12 -10.4(4) . . . . ? N2 C2 C8 C9 -6.7(4) . . . . ? N3 C2 C8 C9 166.7(2) . . . . ? C12 C8 C9 C10 0.0(4) . . . . ? C2 C8 C9 C10 -177.2(2) . . . . ? C8 C9 C10 C11 2.1(4) . . . . ? C12 N5 C11 C10 -0.2(4) . . . . ? Fe2 N5 C11 C10 -179.0(2) 1_455 . . . ? C9 C10 C11 N5 -2.1(4) . . . . ? C11 N5 C12 C8 2.4(4) . . . . ? Fe2 N5 C12 C8 -178.77(18) 1_455 . . . ? C9 C8 C12 N5 -2.3(4) . . . . ? C2 C8 C12 N5 174.8(2) . . . . ? N7 N6 C13 N8 0.4(3) . . . . ? Fe2 N6 C13 N8 -176.69(18) . . . . ? N7 N6 C13 C15 -178.0(2) . . . . ? Fe2 N6 C13 C15 4.9(3) . . . . ? C14 N8 C13 N6 -0.1(3) . . . . ? C14 N8 C13 C15 178.1(3) . . . . ? N6 N7 C14 N8 0.4(3) . . . . ? N6 N7 C14 C20 -178.3(2) . . . . ? C13 N8 C14 N7 -0.2(3) . . . . ? C13 N8 C14 C20 178.5(2) . . . . ? C19 N9 C15 C16 -3.1(4) . . . . ? Fe2 N9 C15 C16 178.0(3) . . . . ? C19 N9 C15 C13 175.9(2) . . . . ? Fe2 N9 C15 C13 -3.0(3) . . . . ? N6 C13 C15 N9 -1.2(3) . . . . ? N8 C13 C15 N9 -179.3(3) . . . . ? N6 C13 C15 C16 177.8(3) . . . . ? N8 C13 C15 C16 -0.3(5) . . . . ? N9 C15 C16 C17 1.0(5) . . . . ? C13 C15 C16 C17 -177.8(3) . . . . ? C15 C16 C17 C18 1.8(6) . . . . ? C16 C17 C18 C19 -2.5(6) . . . . ? C15 N9 C19 C18 2.4(4) . . . . ? Fe2 N9 C19 C18 -178.9(2) . . . . ? C17 C18 C19 N9 0.4(5) . . . . ? N7 C14 C20 C24 -3.6(4) . . . . ? N8 C14 C20 C24 177.8(2) . . . . ? N7 C14 C20 C21 174.8(2) . . . . ? N8 C14 C20 C21 -3.8(4) . . . . ? C24 C20 C21 C22 1.7(4) . . . . ? C14 C20 C21 C22 -176.7(3) . . . . ? C20 C21 C22 C23 0.2(4) . . . . ? C24 N10 C23 C22 0.8(4) . . . . ? Fe1 N10 C23 C22 177.6(2) . . . . ? C21 C22 C23 N10 -1.5(4) . . . . ? C23 N10 C24 C20 1.3(3) . . . . ? Fe1 N10 C24 C20 -175.54(18) . . . . ? C21 C20 C24 N10 -2.5(4) . . . . ? C14 C20 C24 N10 175.9(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C17 H17 N3 0.93 2.62 3.544(4) 176.3 2_665 _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.428 _refine_diff_density_min -0.234 _refine_diff_density_rms 0.057 #================================END data_1_383K _database_code_depnum_ccdc_archive 'CCDC 824535' #TrackingRef '- CIF_MLTong.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H16 Fe N10' _chemical_formula_weight 500.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.966(16) _cell_length_b 9.309(16) _cell_length_c 15.08(3) _cell_angle_alpha 94.38(3) _cell_angle_beta 102.90(4) _cell_angle_gamma 110.54(5) _cell_volume 1132(4) _cell_formula_units_Z 2 _cell_measurement_temperature 383(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 0.702 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8067 _exptl_absorpt_correction_T_max 0.8782 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 383(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8308 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4335 _reflns_number_gt 3278 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4335 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1004 _refine_ls_wR_factor_gt 0.0935 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.5000 0.5000 0.03424(13) Uani 1 2 d S . . Fe2 Fe 0.5000 0.0000 0.0000 0.03707(14) Uani 1 2 d S . . N1 N 0.2897(2) 0.36795(18) 0.40642(11) 0.0389(4) Uani 1 1 d . . . N2 N 0.2307(2) 0.23352(19) 0.34339(11) 0.0427(4) Uani 1 1 d . . . N3 N 0.0435(2) 0.3490(2) 0.31703(12) 0.0454(4) Uani 1 1 d . . . N4 N 0.3754(2) 0.64458(18) 0.50040(11) 0.0397(4) Uani 1 1 d . . . N5 N -0.2520(2) 0.0031(2) 0.07583(11) 0.0454(5) Uani 1 1 d . . . N6 N 0.5579(2) 0.22092(19) 0.07620(10) 0.0404(4) Uani 1 1 d . . . N7 N 0.5479(2) 0.28177(19) 0.15959(11) 0.0421(4) Uani 1 1 d . . . N8 N 0.6896(3) 0.4830(2) 0.09462(12) 0.0557(6) Uani 1 1 d . . . N9 N 0.6085(2) 0.1610(2) -0.08950(11) 0.0461(5) Uani 1 1 d . . . N10 N 0.5978(2) 0.58975(18) 0.39821(11) 0.0390(4) Uani 1 1 d . . . C1 C 0.1757(3) 0.4312(2) 0.38893(14) 0.0394(5) Uani 1 1 d . . . C2 C 0.0863(3) 0.2288(2) 0.29123(13) 0.0398(5) Uani 1 1 d . . . C3 C 0.2180(3) 0.5848(2) 0.44431(14) 0.0410(5) Uani 1 1 d . . . C4 C 0.1105(3) 0.6622(3) 0.44013(19) 0.0655(7) Uani 1 1 d . . . H4 H 0.0040 0.6190 0.4010 0.079 Uiso 1 1 calc R . . C5 C 0.1675(4) 0.8081(3) 0.4969(2) 0.0865(10) Uani 1 1 d . . . H5 H 0.0986 0.8633 0.4962 0.104 Uiso 1 1 calc R . . C6 C 0.3270(4) 0.8685(3) 0.5537(2) 0.0745(8) Uani 1 1 d . . . H6 H 0.3663 0.9646 0.5918 0.089 Uiso 1 1 calc R . . C7 C 0.4273(3) 0.7858(2) 0.55354(16) 0.0519(6) Uani 1 1 d . . . H7 H 0.5349 0.8284 0.5914 0.062 Uiso 1 1 calc R . . C8 C -0.0108(3) 0.1096(2) 0.20654(14) 0.0416(5) Uani 1 1 d . . . C9 C 0.0521(3) 0.0048(3) 0.17364(16) 0.0562(6) Uani 1 1 d . . . H9 H 0.1544 0.0060 0.2053 0.067 Uiso 1 1 calc R . . C10 C -0.0401(3) -0.1012(3) 0.09301(17) 0.0611(7) Uani 1 1 d . . . H10 H -0.0015 -0.1733 0.0707 0.073 Uiso 1 1 calc R . . C11 C -0.1888(3) -0.0981(3) 0.04682(15) 0.0500(6) Uani 1 1 d . . . H11 H -0.2491 -0.1692 -0.0072 0.060 Uiso 1 1 calc R . . C12 C -0.1625(3) 0.1032(2) 0.15545(14) 0.0457(5) Uani 1 1 d . . . H12 H -0.2055 0.1720 0.1772 0.055 Uiso 1 1 calc R . . C13 C 0.6424(3) 0.3436(2) 0.04053(14) 0.0443(5) Uani 1 1 d . . . C14 C 0.6285(3) 0.4376(2) 0.16731(14) 0.0438(5) Uani 1 1 d . . . C15 C 0.6692(3) 0.3141(3) -0.05083(15) 0.0503(6) Uani 1 1 d . . . C16 C 0.7495(5) 0.4323(3) -0.09471(19) 0.0898(11) Uani 1 1 d . . . H16 H 0.7920 0.5360 -0.0665 0.108 Uiso 1 1 calc R . . C17 C 0.7644(5) 0.3912(4) -0.1818(2) 0.0998(13) Uani 1 1 d . . . H17 H 0.8199 0.4674 -0.2122 0.120 Uiso 1 1 calc R . . C18 C 0.6965(5) 0.2365(4) -0.22316(19) 0.0819(10) Uani 1 1 d . . . H18 H 0.7017 0.2082 -0.2825 0.098 Uiso 1 1 calc R . . C19 C 0.6207(3) 0.1243(3) -0.17498(15) 0.0597(7) Uani 1 1 d . . . H19 H 0.5767 0.0202 -0.2026 0.072 Uiso 1 1 calc R . . C20 C 0.6501(3) 0.5490(2) 0.24928(14) 0.0434(5) Uani 1 1 d . . . C21 C 0.7428(4) 0.7087(3) 0.25975(16) 0.0585(7) Uani 1 1 d . . . H21 H 0.7899 0.7490 0.2135 0.070 Uiso 1 1 calc R . . C22 C 0.7636(4) 0.8063(3) 0.33968(16) 0.0584(7) Uani 1 1 d . . . H22 H 0.8254 0.9125 0.3479 0.070 Uiso 1 1 calc R . . C23 C 0.6913(3) 0.7436(2) 0.40679(14) 0.0454(5) Uani 1 1 d . . . H23 H 0.7072 0.8096 0.4605 0.054 Uiso 1 1 calc R . . C24 C 0.5784(3) 0.4963(2) 0.31965(13) 0.0415(5) Uani 1 1 d . . . H24 H 0.5136 0.3910 0.3123 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0399(3) 0.0312(2) 0.0297(2) -0.00407(15) 0.00400(18) 0.01626(19) Fe2 0.0405(3) 0.0356(2) 0.0289(2) -0.00601(16) 0.00483(18) 0.01205(19) N1 0.0423(10) 0.0379(9) 0.0338(9) -0.0030(7) 0.0051(8) 0.0169(8) N2 0.0427(11) 0.0376(9) 0.0394(9) -0.0047(7) 0.0004(8) 0.0141(8) N3 0.0420(11) 0.0471(10) 0.0411(10) -0.0043(8) 0.0002(9) 0.0189(9) N4 0.0457(11) 0.0359(9) 0.0359(9) -0.0019(7) 0.0065(8) 0.0180(8) N5 0.0441(11) 0.0468(11) 0.0357(9) -0.0066(8) 0.0041(8) 0.0126(9) N6 0.0439(11) 0.0418(10) 0.0304(9) -0.0044(7) 0.0061(8) 0.0149(8) N7 0.0498(11) 0.0403(10) 0.0330(9) -0.0040(7) 0.0111(8) 0.0152(9) N8 0.0824(16) 0.0380(10) 0.0446(10) 0.0004(8) 0.0261(11) 0.0162(10) N9 0.0521(12) 0.0547(11) 0.0320(9) -0.0027(8) 0.0112(9) 0.0230(10) N10 0.0465(11) 0.0367(9) 0.0337(9) -0.0029(7) 0.0054(8) 0.0207(8) C1 0.0422(13) 0.0393(11) 0.0363(11) 0.0024(9) 0.0083(10) 0.0172(10) C2 0.0394(12) 0.0376(11) 0.0361(11) -0.0013(9) 0.0058(10) 0.0115(10) C3 0.0469(13) 0.0388(11) 0.0381(11) 0.0008(9) 0.0073(10) 0.0209(10) C4 0.0536(16) 0.0622(16) 0.0748(18) -0.0134(13) -0.0059(14) 0.0340(14) C5 0.076(2) 0.0711(18) 0.110(3) -0.0237(17) -0.0086(19) 0.0534(17) C6 0.079(2) 0.0522(15) 0.087(2) -0.0194(14) -0.0021(17) 0.0407(15) C7 0.0571(15) 0.0385(12) 0.0545(14) -0.0074(10) 0.0018(12) 0.0225(11) C8 0.0387(13) 0.0417(12) 0.0376(11) -0.0024(9) 0.0061(10) 0.0115(10) C9 0.0446(14) 0.0571(14) 0.0579(15) -0.0107(11) 0.0016(12) 0.0202(12) C10 0.0567(17) 0.0611(16) 0.0598(16) -0.0173(12) 0.0085(14) 0.0254(13) C11 0.0464(14) 0.0493(13) 0.0435(12) -0.0119(10) 0.0060(11) 0.0129(11) C12 0.0466(14) 0.0421(12) 0.0423(12) -0.0051(9) 0.0058(11) 0.0157(11) C13 0.0558(14) 0.0382(11) 0.0366(11) 0.0021(9) 0.0140(11) 0.0149(10) C14 0.0563(15) 0.0385(12) 0.0354(11) -0.0014(9) 0.0127(11) 0.0178(11) C15 0.0643(16) 0.0499(14) 0.0391(12) 0.0060(10) 0.0193(12) 0.0214(12) C16 0.143(3) 0.0635(18) 0.0689(18) 0.0169(15) 0.057(2) 0.0272(19) C17 0.157(4) 0.092(2) 0.073(2) 0.0344(19) 0.071(2) 0.047(2) C18 0.123(3) 0.099(2) 0.0471(15) 0.0181(16) 0.0429(19) 0.057(2) C19 0.0711(18) 0.0754(17) 0.0392(13) -0.0013(12) 0.0175(13) 0.0361(15) C20 0.0556(14) 0.0377(11) 0.0363(11) -0.0012(9) 0.0101(11) 0.0199(10) C21 0.085(2) 0.0412(13) 0.0479(13) 0.0020(10) 0.0278(14) 0.0173(13) C22 0.082(2) 0.0321(12) 0.0588(15) -0.0011(11) 0.0256(14) 0.0160(12) C23 0.0618(15) 0.0338(11) 0.0396(11) -0.0046(9) 0.0110(11) 0.0207(11) C24 0.0487(13) 0.0348(11) 0.0369(11) -0.0042(8) 0.0070(10) 0.0158(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.994(3) 2_666 ? Fe1 N1 1.994(3) . ? Fe1 N10 2.027(3) 2_666 ? Fe1 N10 2.027(3) . ? Fe1 N4 2.029(3) . ? Fe1 N4 2.029(3) 2_666 ? Fe2 N6 2.108(4) . ? Fe2 N6 2.108(4) 2_655 ? Fe2 N9 2.211(3) 2_655 ? Fe2 N9 2.211(3) . ? Fe2 N5 2.251(4) 1_655 ? Fe2 N5 2.251(4) 2 ? N1 C1 1.337(3) . ? N1 N2 1.371(3) . ? N2 C2 1.340(3) . ? N3 C1 1.352(3) . ? N3 C2 1.361(3) . ? N4 C7 1.353(3) . ? N4 C3 1.364(4) . ? N5 C11 1.349(3) . ? N5 C12 1.352(3) . ? N5 Fe2 2.251(4) 1_455 ? N6 C13 1.355(3) . ? N6 N7 1.374(3) . ? N7 C14 1.357(3) . ? N8 C13 1.352(3) . ? N8 C14 1.363(3) . ? N9 C19 1.346(4) . ? N9 C15 1.362(4) . ? N10 C24 1.355(3) . ? N10 C23 1.360(3) . ? C1 C3 1.477(4) . ? C2 C8 1.493(3) . ? C3 C4 1.385(4) . ? C4 C5 1.407(4) . ? C4 H4 0.9300 . ? C5 C6 1.382(5) . ? C5 H5 0.9300 . ? C6 C7 1.374(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C12 1.384(4) . ? C8 C9 1.398(4) . ? C9 C10 1.390(4) . ? C9 H9 0.9300 . ? C10 C11 1.370(4) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C15 1.473(4) . ? C14 C20 1.483(3) . ? C15 C16 1.391(4) . ? C16 C17 1.389(4) . ? C16 H16 0.9300 . ? C17 C18 1.382(5) . ? C17 H17 0.9300 . ? C18 C19 1.386(4) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C24 1.394(3) . ? C20 C21 1.402(4) . ? C21 C22 1.388(4) . ? C21 H21 0.9300 . ? C22 C23 1.380(4) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N1 180.0 2_666 . ? N1 Fe1 N10 90.09(16) 2_666 2_666 ? N1 Fe1 N10 89.91(16) . 2_666 ? N1 Fe1 N10 89.91(16) 2_666 . ? N1 Fe1 N10 90.09(16) . . ? N10 Fe1 N10 180.000(1) 2_666 . ? N1 Fe1 N4 99.20(14) 2_666 . ? N1 Fe1 N4 80.80(14) . . ? N10 Fe1 N4 87.52(11) 2_666 . ? N10 Fe1 N4 92.48(11) . . ? N1 Fe1 N4 80.80(14) 2_666 2_666 ? N1 Fe1 N4 99.20(14) . 2_666 ? N10 Fe1 N4 92.48(11) 2_666 2_666 ? N10 Fe1 N4 87.52(11) . 2_666 ? N4 Fe1 N4 180.000(1) . 2_666 ? N6 Fe2 N6 180.00(10) . 2_655 ? N6 Fe2 N9 102.99(15) . 2_655 ? N6 Fe2 N9 77.01(15) 2_655 2_655 ? N6 Fe2 N9 77.01(15) . . ? N6 Fe2 N9 102.99(15) 2_655 . ? N9 Fe2 N9 180.00(9) 2_655 . ? N6 Fe2 N5 89.61(10) . 1_655 ? N6 Fe2 N5 90.39(10) 2_655 1_655 ? N9 Fe2 N5 87.44(13) 2_655 1_655 ? N9 Fe2 N5 92.56(13) . 1_655 ? N6 Fe2 N5 90.39(10) . 2 ? N6 Fe2 N5 89.61(10) 2_655 2 ? N9 Fe2 N5 92.56(13) 2_655 2 ? N9 Fe2 N5 87.44(13) . 2 ? N5 Fe2 N5 180.00(9) 1_655 2 ? C1 N1 N2 106.3(2) . . ? C1 N1 Fe1 115.07(18) . . ? N2 N1 Fe1 138.00(15) . . ? C2 N2 N1 104.70(19) . . ? C1 N3 C2 100.5(2) . . ? C7 N4 C3 118.0(2) . . ? C7 N4 Fe1 127.37(18) . . ? C3 N4 Fe1 114.51(17) . . ? C11 N5 C12 116.9(2) . . ? C11 N5 Fe2 122.16(17) . 1_455 ? C12 N5 Fe2 120.91(17) . 1_455 ? C13 N6 N7 106.28(19) . . ? C13 N6 Fe2 115.31(18) . . ? N7 N6 Fe2 138.10(13) . . ? C14 N7 N6 104.30(16) . . ? C13 N8 C14 100.6(2) . . ? C19 N9 C15 118.4(2) . . ? C19 N9 Fe2 127.68(19) . . ? C15 N9 Fe2 113.96(17) . . ? C24 N10 C23 117.01(19) . . ? C24 N10 Fe1 120.75(18) . . ? C23 N10 Fe1 122.17(14) . . ? N1 C1 N3 113.9(2) . . ? N1 C1 C3 116.2(2) . . ? N3 C1 C3 129.6(2) . . ? N2 C2 N3 114.51(19) . . ? N2 C2 C8 122.4(2) . . ? N3 C2 C8 122.9(2) . . ? N4 C3 C4 122.8(2) . . ? N4 C3 C1 113.2(2) . . ? C4 C3 C1 124.1(2) . . ? C3 C4 C5 118.0(3) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? C6 C5 C4 119.2(3) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C7 C6 C5 119.7(3) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? N4 C7 C6 122.5(3) . . ? N4 C7 H7 118.8 . . ? C6 C7 H7 118.8 . . ? C12 C8 C9 117.5(2) . . ? C12 C8 C2 121.5(2) . . ? C9 C8 C2 121.0(2) . . ? C10 C9 C8 119.1(3) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C11 C10 C9 119.2(2) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? N5 C11 C10 123.3(2) . . ? N5 C11 H11 118.4 . . ? C10 C11 H11 118.4 . . ? N5 C12 C8 124.1(2) . . ? N5 C12 H12 118.0 . . ? C8 C12 H12 118.0 . . ? N8 C13 N6 114.0(2) . . ? N8 C13 C15 127.4(2) . . ? N6 C13 C15 118.7(2) . . ? N7 C14 N8 114.81(18) . . ? N7 C14 C20 122.32(19) . . ? N8 C14 C20 122.9(2) . . ? N9 C15 C16 122.3(2) . . ? N9 C15 C13 114.58(18) . . ? C16 C15 C13 123.1(2) . . ? C17 C16 C15 118.2(3) . . ? C17 C16 H16 120.9 . . ? C15 C16 H16 120.9 . . ? C18 C17 C16 119.7(3) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C19 119.1(3) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? N9 C19 C18 122.2(3) . . ? N9 C19 H19 118.9 . . ? C18 C19 H19 118.9 . . ? C24 C20 C21 117.7(2) . . ? C24 C20 C14 120.2(2) . . ? C21 C20 C14 122.1(2) . . ? C22 C21 C20 119.4(2) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C23 C22 C21 119.0(2) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? N10 C23 C22 123.2(2) . . ? N10 C23 H23 118.4 . . ? C22 C23 H23 118.4 . . ? N10 C24 C20 123.7(2) . . ? N10 C24 H24 118.2 . . ? C20 C24 H24 118.2 . . ? 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 N1 Fe1 N1 C1 -147(100) 2_666 . . . ? N10 Fe1 N1 C1 87.83(17) 2_666 . . . ? N10 Fe1 N1 C1 -92.17(17) . . . . ? N4 Fe1 N1 C1 0.33(14) . . . . ? N4 Fe1 N1 C1 -179.67(14) 2_666 . . . ? N1 Fe1 N1 N2 22(100) 2_666 . . . ? N10 Fe1 N1 N2 -102.8(2) 2_666 . . . ? N10 Fe1 N1 N2 77.2(2) . . . . ? N4 Fe1 N1 N2 169.71(19) . . . . ? N4 Fe1 N1 N2 -10.29(19) 2_666 . . . ? C1 N1 N2 C2 1.5(2) . . . . ? Fe1 N1 N2 C2 -168.53(15) . . . . ? N1 Fe1 N4 C7 -2.00(19) 2_666 . . . ? N1 Fe1 N4 C7 178.00(19) . . . . ? N10 Fe1 N4 C7 87.7(2) 2_666 . . . ? N10 Fe1 N4 C7 -92.3(2) . . . . ? N4 Fe1 N4 C7 -149(100) 2_666 . . . ? N1 Fe1 N4 C3 -177.44(13) 2_666 . . . ? N1 Fe1 N4 C3 2.56(13) . . . . ? N10 Fe1 N4 C3 -87.7(2) 2_666 . . . ? N10 Fe1 N4 C3 92.3(2) . . . . ? N4 Fe1 N4 C3 36(100) 2_666 . . . ? N6 Fe2 N6 C13 -1(100) 2_655 . . . ? N9 Fe2 N6 C13 173.75(15) 2_655 . . . ? N9 Fe2 N6 C13 -6.25(15) . . . . ? N5 Fe2 N6 C13 86.5(2) 1_655 . . . ? N5 Fe2 N6 C13 -93.5(2) 2 . . . ? N6 Fe2 N6 N7 -173(100) 2_655 . . . ? N9 Fe2 N6 N7 1.3(2) 2_655 . . . ? N9 Fe2 N6 N7 -178.7(2) . . . . ? N5 Fe2 N6 N7 -86.0(2) 1_655 . . . ? N5 Fe2 N6 N7 94.0(2) 2 . . . ? C13 N6 N7 C14 -0.2(2) . . . . ? Fe2 N6 N7 C14 172.71(17) . . . . ? N6 Fe2 N9 C19 -175.0(2) . . . . ? N6 Fe2 N9 C19 5.0(2) 2_655 . . . ? N9 Fe2 N9 C19 -33(100) 2_655 . . . ? N5 Fe2 N9 C19 96.0(2) 1_655 . . . ? N5 Fe2 N9 C19 -84.0(2) 2 . . . ? N6 Fe2 N9 C15 5.20(17) . . . . ? N6 Fe2 N9 C15 -174.80(17) 2_655 . . . ? N9 Fe2 N9 C15 148(100) 2_655 . . . ? N5 Fe2 N9 C15 -83.80(19) 1_655 . . . ? N5 Fe2 N9 C15 96.20(19) 2 . . . ? N1 Fe1 N10 C24 135.75(18) 2_666 . . . ? N1 Fe1 N10 C24 -44.25(18) . . . . ? N10 Fe1 N10 C24 -26(100) 2_666 . . . ? N4 Fe1 N10 C24 -125.0(2) . . . . ? N4 Fe1 N10 C24 55.0(2) 2_666 . . . ? N1 Fe1 N10 C23 -41.23(19) 2_666 . . . ? N1 Fe1 N10 C23 138.77(19) . . . . ? N10 Fe1 N10 C23 157(100) 2_666 . . . ? N4 Fe1 N10 C23 58.0(2) . . . . ? N4 Fe1 N10 C23 -122.0(2) 2_666 . . . ? N2 N1 C1 N3 -0.8(2) . . . . ? Fe1 N1 C1 N3 171.78(13) . . . . ? N2 N1 C1 C3 -175.61(16) . . . . ? Fe1 N1 C1 C3 -3.0(2) . . . . ? C2 N3 C1 N1 -0.2(2) . . . . ? C2 N3 C1 C3 173.8(2) . . . . ? N1 N2 C2 N3 -1.7(2) . . . . ? N1 N2 C2 C8 172.72(17) . . . . ? C1 N3 C2 N2 1.2(2) . . . . ? C1 N3 C2 C8 -173.22(18) . . . . ? C7 N4 C3 C4 -0.3(3) . . . . ? Fe1 N4 C3 C4 175.63(19) . . . . ? C7 N4 C3 C1 179.40(18) . . . . ? Fe1 N4 C3 C1 -4.7(2) . . . . ? N1 C1 C3 N4 5.1(3) . . . . ? N3 C1 C3 N4 -168.69(19) . . . . ? N1 C1 C3 C4 -175.2(2) . . . . ? N3 C1 C3 C4 11.0(4) . . . . ? N4 C3 C4 C5 -0.4(4) . . . . ? C1 C3 C4 C5 -180.0(3) . . . . ? C3 C4 C5 C6 0.3(5) . . . . ? C4 C5 C6 C7 0.3(5) . . . . ? C3 N4 C7 C6 0.9(3) . . . . ? Fe1 N4 C7 C6 -174.4(2) . . . . ? C5 C6 C7 N4 -0.9(4) . . . . ? N2 C2 C8 C12 177.62(19) . . . . ? N3 C2 C8 C12 -8.4(3) . . . . ? N2 C2 C8 C9 -5.3(3) . . . . ? N3 C2 C8 C9 168.6(2) . . . . ? C12 C8 C9 C10 -0.9(3) . . . . ? C2 C8 C9 C10 -178.1(2) . . . . ? C8 C9 C10 C11 1.3(4) . . . . ? C12 N5 C11 C10 -1.1(3) . . . . ? Fe2 N5 C11 C10 -178.29(18) 1_455 . . . ? C9 C10 C11 N5 -0.3(4) . . . . ? C11 N5 C12 C8 1.5(3) . . . . ? Fe2 N5 C12 C8 178.78(15) 1_455 . . . ? C9 C8 C12 N5 -0.6(3) . . . . ? C2 C8 C12 N5 176.59(18) . . . . ? C14 N8 C13 N6 0.3(3) . . . . ? C14 N8 C13 C15 178.6(2) . . . . ? N7 N6 C13 N8 -0.1(3) . . . . ? Fe2 N6 C13 N8 -174.84(17) . . . . ? N7 N6 C13 C15 -178.6(2) . . . . ? Fe2 N6 C13 C15 6.7(3) . . . . ? N6 N7 C14 N8 0.4(3) . . . . ? N6 N7 C14 C20 -178.8(2) . . . . ? C13 N8 C14 N7 -0.4(3) . . . . ? C13 N8 C14 C20 178.8(2) . . . . ? C19 N9 C15 C16 -3.0(4) . . . . ? Fe2 N9 C15 C16 176.8(2) . . . . ? C19 N9 C15 C13 176.8(2) . . . . ? Fe2 N9 C15 C13 -3.4(3) . . . . ? N8 C13 C15 N9 179.7(2) . . . . ? N6 C13 C15 N9 -2.0(3) . . . . ? N8 C13 C15 C16 -0.4(4) . . . . ? N6 C13 C15 C16 177.8(3) . . . . ? N9 C15 C16 C17 1.3(5) . . . . ? C13 C15 C16 C17 -178.5(3) . . . . ? C15 C16 C17 C18 1.6(6) . . . . ? C16 C17 C18 C19 -2.7(6) . . . . ? C15 N9 C19 C18 1.8(4) . . . . ? Fe2 N9 C19 C18 -177.9(2) . . . . ? C17 C18 C19 N9 1.0(5) . . . . ? N7 C14 C20 C24 -3.8(4) . . . . ? N8 C14 C20 C24 177.1(2) . . . . ? N7 C14 C20 C21 175.7(2) . . . . ? N8 C14 C20 C21 -3.4(4) . . . . ? C24 C20 C21 C22 1.9(4) . . . . ? C14 C20 C21 C22 -177.6(2) . . . . ? C20 C21 C22 C23 -0.5(4) . . . . ? C24 N10 C23 C22 0.7(3) . . . . ? Fe1 N10 C23 C22 177.8(2) . . . . ? C21 C22 C23 N10 -0.9(4) . . . . ? C23 N10 C24 C20 0.9(3) . . . . ? Fe1 N10 C24 C20 -176.26(18) . . . . ? C21 C20 C24 N10 -2.1(4) . . . . ? C14 C20 C24 N10 177.3(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C17 H17 N3 0.93 2.59 3.517(5) 172.2 2_665 _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.391 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.058 #================================END data_2_293K _database_code_depnum_ccdc_archive 'CCDC 824536' #TrackingRef '- CIF_MLTong.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H20 Fe N10' _chemical_formula_weight 528.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3683(3) _cell_length_b 9.5284(4) _cell_length_c 14.3159(7) _cell_angle_alpha 93.4560(10) _cell_angle_beta 104.5000(10) _cell_angle_gamma 112.0100(10) _cell_volume 1130.00(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 0.708 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8265 _exptl_absorpt_correction_T_max 0.8714 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7847 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4295 _reflns_number_gt 3119 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0751P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4295 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.1141 _refine_ls_wR_factor_gt 0.0974 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe -0.5000 0.0000 0.0000 0.02079(15) Uani 1 2 d S . . Fe2 Fe 0.5000 0.5000 0.5000 0.02091(15) Uani 1 2 d S . . N1 N -0.2847(3) 0.1285(2) 0.08936(17) 0.0255(5) Uani 1 1 d . . . N2 N -0.2164(3) 0.2627(2) 0.15349(17) 0.0296(5) Uani 1 1 d . . . N3 N -0.0444(3) 0.1437(3) 0.17842(18) 0.0318(5) Uani 1 1 d . . . N4 N -0.3904(3) -0.1451(2) -0.00585(16) 0.0242(5) Uani 1 1 d . . . N5 N 0.2771(3) 0.4920(2) 0.42490(17) 0.0266(5) Uani 1 1 d . . . N6 N 0.4411(2) 0.2905(2) 0.43064(16) 0.0233(5) Uani 1 1 d . . . N7 N 0.4636(3) 0.2279(2) 0.35084(16) 0.0258(5) Uani 1 1 d . . . N8 N 0.3336(3) 0.0353(2) 0.42325(17) 0.0300(5) Uani 1 1 d . . . N9 N 0.3953(3) 0.3702(2) 0.59119(16) 0.0258(5) Uani 1 1 d . . . N10 N 0.4338(2) -0.0816(2) 0.11596(16) 0.0236(5) Uani 1 1 d . . . C1 C -0.1805(3) 0.0616(3) 0.1062(2) 0.0268(6) Uani 1 1 d . . . C2 C -0.0728(3) 0.2660(3) 0.2054(2) 0.0293(6) Uani 1 1 d . . . C3 C -0.2345(3) -0.0918(3) 0.0502(2) 0.0265(6) Uani 1 1 d . . . C4 C -0.1403(4) -0.1768(3) 0.0530(2) 0.0358(7) Uani 1 1 d . . . C5 C -0.2132(4) -0.3205(4) -0.0053(3) 0.0475(9) Uani 1 1 d . . . H5 H -0.1549 -0.3808 -0.0055 0.057 Uiso 1 1 calc R . . C6 C -0.3699(4) -0.3751(3) -0.0628(3) 0.0440(8) Uani 1 1 d . . . H6 H -0.4180 -0.4713 -0.1024 0.053 Uiso 1 1 calc R . . C7 C -0.4554(3) -0.2846(3) -0.0608(2) 0.0321(6) Uani 1 1 d . . . H7 H -0.5623 -0.3223 -0.0992 0.039 Uiso 1 1 calc R . . C8 C 0.0314(3) 0.3841(3) 0.2909(2) 0.0297(6) Uani 1 1 d . . . C9 C -0.0249(4) 0.4838(4) 0.3288(3) 0.0418(8) Uani 1 1 d . . . H9 H -0.1249 0.4823 0.2965 0.050 Uiso 1 1 calc R . . C10 C 0.0683(4) 0.5838(4) 0.4140(3) 0.0440(8) Uani 1 1 d . . . H10 H 0.0326 0.6517 0.4401 0.053 Uiso 1 1 calc R . . C11 C 0.2166(3) 0.5836(3) 0.4615(2) 0.0368(7) Uani 1 1 d . . . H11 H 0.2768 0.6493 0.5210 0.044 Uiso 1 1 calc R . . C12 C 0.1841(3) 0.3951(3) 0.3408(2) 0.0288(6) Uani 1 1 d . . . H12 H 0.2240 0.3315 0.3143 0.035 Uiso 1 1 calc R . . C13 C 0.0314(4) -0.1178(4) 0.1152(3) 0.0496(8) Uiso 1 1 d . . . H13A H 0.0849 -0.0107 0.1131 0.074 Uiso 1 1 calc R . . H13B H 0.0847 -0.1739 0.0908 0.074 Uiso 1 1 calc R . . H13C H 0.0347 -0.1311 0.1815 0.074 Uiso 1 1 calc R . . C14 C 0.3642(3) 0.1738(3) 0.4721(2) 0.0255(6) Uani 1 1 d . . . C15 C 0.3984(3) 0.0760(3) 0.3500(2) 0.0272(6) Uani 1 1 d . . . C16 C 0.3316(3) 0.2146(3) 0.5618(2) 0.0255(6) Uani 1 1 d . . . C17 C 0.2470(4) 0.1120(3) 0.6139(2) 0.0348(7) Uani 1 1 d . . . C18 C 0.2294(4) 0.1726(4) 0.6980(2) 0.0402(7) Uani 1 1 d . . . H18 H 0.1715 0.1074 0.7336 0.048 Uiso 1 1 calc R . . C19 C 0.2972(4) 0.3293(3) 0.7297(2) 0.0393(7) Uani 1 1 d . . . H19 H 0.2883 0.3702 0.7876 0.047 Uiso 1 1 calc R . . C20 C 0.3780(4) 0.4240(3) 0.6744(2) 0.0318(6) Uani 1 1 d . . . H20 H 0.4225 0.5297 0.6955 0.038 Uiso 1 1 calc R . . C21 C 0.3950(3) -0.0355(3) 0.2734(2) 0.0251(6) Uani 1 1 d . . . C22 C 0.3305(4) -0.1926(3) 0.2734(2) 0.0341(7) Uani 1 1 d . . . H22 H 0.2972 -0.2308 0.3261 0.041 Uiso 1 1 calc R . . C23 C 0.3170(4) -0.2910(3) 0.1940(2) 0.0369(7) Uani 1 1 d . . . H23 H 0.2747 -0.3966 0.1930 0.044 Uiso 1 1 calc R . . C24 C 0.3655(3) -0.2339(3) 0.1164(2) 0.0297(6) Uani 1 1 d . . . H24 H 0.3509 -0.3024 0.0622 0.036 Uiso 1 1 calc R . . C25 C 0.4492(3) 0.0138(3) 0.1948(2) 0.0255(6) Uani 1 1 d . . . H25 H 0.4994 0.1190 0.1964 0.031 Uiso 1 1 calc R . . C26 C 0.1734(4) -0.0593(4) 0.5793(3) 0.0501(9) Uiso 1 1 d . . . H26A H 0.1063 -0.0825 0.5128 0.075 Uiso 1 1 calc R . . H26B H 0.1096 -0.1094 0.6201 0.075 Uiso 1 1 calc R . . H26C H 0.2575 -0.0950 0.5829 0.075 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0248(3) 0.0214(3) 0.0162(3) -0.0012(2) 0.0048(2) 0.0109(2) Fe2 0.0245(3) 0.0210(3) 0.0154(3) -0.0008(2) 0.0055(2) 0.0079(2) N1 0.0261(11) 0.0255(11) 0.0236(12) -0.0001(9) 0.0056(10) 0.0108(10) N2 0.0301(12) 0.0275(11) 0.0250(13) -0.0030(10) 0.0009(10) 0.0106(10) N3 0.0327(12) 0.0329(12) 0.0270(13) -0.0013(10) 0.0048(10) 0.0137(11) N4 0.0271(11) 0.0275(11) 0.0189(11) 0.0025(9) 0.0065(9) 0.0123(10) N5 0.0286(12) 0.0245(11) 0.0243(13) 0.0013(9) 0.0088(10) 0.0079(10) N6 0.0259(11) 0.0241(11) 0.0179(11) -0.0002(9) 0.0062(9) 0.0087(9) N7 0.0322(12) 0.0249(11) 0.0182(12) -0.0024(9) 0.0074(9) 0.0102(10) N8 0.0441(14) 0.0252(11) 0.0223(13) 0.0013(9) 0.0153(11) 0.0127(11) N9 0.0305(11) 0.0278(11) 0.0187(12) -0.0006(9) 0.0053(9) 0.0135(10) N10 0.0262(11) 0.0252(11) 0.0225(12) 0.0002(9) 0.0070(9) 0.0144(10) C1 0.0290(14) 0.0311(14) 0.0224(14) 0.0032(11) 0.0069(11) 0.0151(12) C2 0.0281(14) 0.0299(14) 0.0264(15) 0.0015(12) 0.0061(12) 0.0097(12) C3 0.0305(14) 0.0298(14) 0.0205(14) 0.0028(11) 0.0067(11) 0.0142(12) C4 0.0356(15) 0.0412(16) 0.0362(18) 0.0021(13) 0.0076(13) 0.0240(14) C5 0.0505(19) 0.0487(18) 0.052(2) -0.0048(16) 0.0071(17) 0.0371(17) C6 0.0494(18) 0.0344(16) 0.046(2) -0.0096(14) 0.0039(16) 0.0239(15) C7 0.0339(15) 0.0300(14) 0.0295(16) -0.0007(12) 0.0038(13) 0.0141(13) C8 0.0293(14) 0.0266(13) 0.0277(16) 0.0009(12) 0.0061(12) 0.0072(12) C9 0.0292(15) 0.0422(17) 0.047(2) -0.0083(15) 0.0001(14) 0.0168(14) C10 0.0372(16) 0.0428(17) 0.048(2) -0.0138(15) 0.0065(15) 0.0194(15) C11 0.0351(16) 0.0372(16) 0.0316(17) -0.0072(13) 0.0062(13) 0.0118(14) C12 0.0304(14) 0.0318(14) 0.0236(15) 0.0015(11) 0.0048(12) 0.0144(12) C14 0.0301(14) 0.0260(13) 0.0215(14) 0.0026(11) 0.0096(11) 0.0115(12) C15 0.0327(14) 0.0268(13) 0.0239(15) 0.0036(11) 0.0082(12) 0.0141(12) C16 0.0295(13) 0.0289(13) 0.0185(14) 0.0026(11) 0.0079(11) 0.0120(12) C17 0.0460(17) 0.0317(15) 0.0317(17) 0.0071(12) 0.0183(14) 0.0166(14) C18 0.056(2) 0.0434(17) 0.0330(18) 0.0150(14) 0.0265(16) 0.0230(16) C19 0.0530(19) 0.0411(17) 0.0327(18) 0.0040(14) 0.0211(15) 0.0237(16) C20 0.0437(16) 0.0332(15) 0.0218(15) 0.0007(12) 0.0103(13) 0.0192(14) C21 0.0299(13) 0.0240(12) 0.0226(14) 0.0020(11) 0.0062(11) 0.0133(11) C22 0.0504(18) 0.0304(14) 0.0290(16) 0.0091(12) 0.0184(14) 0.0194(14) C23 0.0542(19) 0.0236(13) 0.0410(18) 0.0061(12) 0.0216(15) 0.0195(14) C24 0.0396(15) 0.0244(13) 0.0305(16) 0.0014(11) 0.0138(13) 0.0170(12) C25 0.0311(14) 0.0244(13) 0.0213(14) 0.0003(11) 0.0066(11) 0.0129(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.968(2) 2_455 ? Fe1 N1 1.968(2) . ? Fe1 N10 2.013(2) 1_455 ? Fe1 N10 2.014(2) 2 ? Fe1 N4 2.016(2) . ? Fe1 N4 2.016(2) 2_455 ? Fe2 N6 1.984(2) . ? Fe2 N6 1.984(2) 2_666 ? Fe2 N9 2.031(2) . ? Fe2 N9 2.031(2) 2_666 ? Fe2 N5 2.066(2) 2_666 ? Fe2 N5 2.066(2) . ? N1 C1 1.336(3) . ? N1 N2 1.356(3) . ? N2 C2 1.351(3) . ? N3 C1 1.342(4) . ? N3 C2 1.344(3) . ? N4 C7 1.335(3) . ? N4 C3 1.357(3) . ? N5 C12 1.341(4) . ? N5 C11 1.350(4) . ? N6 C14 1.342(3) . ? N6 N7 1.355(3) . ? N7 C15 1.342(3) . ? N8 C15 1.345(4) . ? N8 C14 1.348(3) . ? N9 C20 1.338(4) . ? N9 C16 1.366(3) . ? N10 C25 1.347(3) . ? N10 C24 1.350(3) . ? N10 Fe1 2.014(2) 1_655 ? C1 C3 1.461(4) . ? C2 C8 1.459(4) . ? C3 C4 1.399(4) . ? C4 C5 1.383(4) . ? C4 C13 1.498(4) . ? C5 C6 1.369(5) . ? C5 H5 0.9300 . ? C6 C7 1.383(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.389(4) . ? C8 C12 1.391(4) . ? C9 C10 1.364(5) . ? C9 H9 0.9300 . ? C10 C11 1.386(4) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C16 1.456(4) . ? C15 C21 1.466(4) . ? C16 C17 1.394(4) . ? C17 C18 1.377(4) . ? C17 C26 1.508(4) . ? C18 C19 1.379(4) . ? C18 H18 0.9300 . ? C19 C20 1.375(4) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C25 1.385(4) . ? C21 C22 1.389(4) . ? C22 C23 1.378(4) . ? C22 H22 0.9300 . ? C23 C24 1.370(4) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N1 180.00(19) 2_455 . ? N1 Fe1 N10 91.31(9) 2_455 1_455 ? N1 Fe1 N10 88.69(9) . 1_455 ? N1 Fe1 N10 88.69(9) 2_455 2 ? N1 Fe1 N10 91.31(9) . 2 ? N10 Fe1 N10 180.00(12) 1_455 2 ? N1 Fe1 N4 99.75(9) 2_455 . ? N1 Fe1 N4 80.25(9) . . ? N10 Fe1 N4 90.40(8) 1_455 . ? N10 Fe1 N4 89.60(8) 2 . ? N1 Fe1 N4 80.25(9) 2_455 2_455 ? N1 Fe1 N4 99.75(9) . 2_455 ? N10 Fe1 N4 89.60(8) 1_455 2_455 ? N10 Fe1 N4 90.40(8) 2 2_455 ? N4 Fe1 N4 180.00(14) . 2_455 ? N6 Fe2 N6 180.00(6) . 2_666 ? N6 Fe2 N9 79.36(9) . . ? N6 Fe2 N9 100.64(9) 2_666 . ? N6 Fe2 N9 100.64(9) . 2_666 ? N6 Fe2 N9 79.36(9) 2_666 2_666 ? N9 Fe2 N9 180.0 . 2_666 ? N6 Fe2 N5 89.89(9) . 2_666 ? N6 Fe2 N5 90.11(9) 2_666 2_666 ? N9 Fe2 N5 91.20(9) . 2_666 ? N9 Fe2 N5 88.80(9) 2_666 2_666 ? N6 Fe2 N5 90.11(9) . . ? N6 Fe2 N5 89.89(9) 2_666 . ? N9 Fe2 N5 88.80(9) . . ? N9 Fe2 N5 91.20(9) 2_666 . ? N5 Fe2 N5 180.0 2_666 . ? C1 N1 N2 107.0(2) . . ? C1 N1 Fe1 115.40(18) . . ? N2 N1 Fe1 136.50(17) . . ? C2 N2 N1 104.0(2) . . ? C1 N3 C2 101.1(2) . . ? C7 N4 C3 118.1(2) . . ? C7 N4 Fe1 126.22(18) . . ? C3 N4 Fe1 115.67(17) . . ? C12 N5 C11 116.8(2) . . ? C12 N5 Fe2 122.99(18) . . ? C11 N5 Fe2 120.15(19) . . ? C14 N6 N7 107.1(2) . . ? C14 N6 Fe2 115.97(17) . . ? N7 N6 Fe2 136.89(17) . . ? C15 N7 N6 104.3(2) . . ? C15 N8 C14 101.2(2) . . ? C20 N9 C16 118.0(2) . . ? C20 N9 Fe2 125.70(19) . . ? C16 N9 Fe2 116.20(18) . . ? C25 N10 C24 117.1(2) . . ? C25 N10 Fe1 121.25(17) . 1_655 ? C24 N10 Fe1 121.58(17) . 1_655 ? N1 C1 N3 113.4(2) . . ? N1 C1 C3 116.6(2) . . ? N3 C1 C3 129.8(2) . . ? N3 C2 N2 114.4(2) . . ? N3 C2 C8 123.6(3) . . ? N2 C2 C8 121.6(2) . . ? N4 C3 C4 122.9(2) . . ? N4 C3 C1 111.8(2) . . ? C4 C3 C1 125.3(2) . . ? C5 C4 C3 116.8(3) . . ? C5 C4 C13 120.5(3) . . ? C3 C4 C13 122.7(3) . . ? C6 C5 C4 120.9(3) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 118.8(3) . . ? C5 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? N4 C7 C6 122.5(3) . . ? N4 C7 H7 118.7 . . ? C6 C7 H7 118.7 . . ? C9 C8 C12 117.7(3) . . ? C9 C8 C2 120.1(3) . . ? C12 C8 C2 122.1(2) . . ? C10 C9 C8 119.3(3) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 C10 C11 119.5(3) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? N5 C11 C10 122.6(3) . . ? N5 C11 H11 118.7 . . ? C10 C11 H11 118.7 . . ? N5 C12 C8 123.9(3) . . ? N5 C12 H12 118.0 . . ? C8 C12 H12 118.0 . . ? C4 C13 H13A 109.5 . . ? C4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N6 C14 N8 112.7(2) . . ? N6 C14 C16 116.7(2) . . ? N8 C14 C16 130.5(2) . . ? N7 C15 N8 114.6(2) . . ? N7 C15 C21 122.1(2) . . ? N8 C15 C21 123.3(2) . . ? N9 C16 C17 122.3(3) . . ? N9 C16 C14 111.6(2) . . ? C17 C16 C14 126.0(2) . . ? C18 C17 C16 117.6(3) . . ? C18 C17 C26 120.5(3) . . ? C16 C17 C26 121.8(3) . . ? C17 C18 C19 120.5(3) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C20 C19 C18 118.8(3) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? N9 C20 C19 122.6(3) . . ? N9 C20 H20 118.7 . . ? C19 C20 H20 118.7 . . ? C25 C21 C22 117.5(2) . . ? C25 C21 C15 120.1(2) . . ? C22 C21 C15 122.3(3) . . ? C23 C22 C21 118.9(3) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C24 C23 C22 120.2(3) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? N10 C24 C23 122.2(3) . . ? N10 C24 H24 118.9 . . ? C23 C24 H24 118.9 . . ? N10 C25 C21 124.0(2) . . ? N10 C25 H25 118.0 . . ? C21 C25 H25 118.0 . . ? C17 C26 H26A 109.5 . . ? C17 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C17 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.671 _refine_diff_density_min -0.571 _refine_diff_density_rms 0.096 #================================END data_2_383K _database_code_depnum_ccdc_archive 'CCDC 824537' #TrackingRef '- CIF_MLTong.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H20 Fe N10' _chemical_formula_weight 528.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5062(9) _cell_length_b 9.6419(11) _cell_length_c 14.3420(19) _cell_angle_alpha 93.661(4) _cell_angle_beta 104.415(3) _cell_angle_gamma 111.004(3) _cell_volume 1171.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 383(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 0.683 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8112 _exptl_absorpt_correction_T_max 0.8588 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 383(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8053 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4371 _reflns_number_gt 3390 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0814P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4371 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1294 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe -0.5000 0.0000 0.0000 0.02287(16) Uani 1 2 d S . . Fe2 Fe 0.5000 0.5000 0.5000 0.02599(17) Uani 1 2 d S . . N1 N -0.2907(2) 0.1251(2) 0.08976(16) 0.0286(5) Uani 1 1 d . . . N2 N -0.2258(2) 0.2574(3) 0.15286(16) 0.0317(5) Uani 1 1 d . . . N3 N -0.0528(3) 0.1425(3) 0.17749(17) 0.0353(5) Uani 1 1 d . . . N4 N -0.3888(2) -0.1425(2) -0.00505(15) 0.0276(5) Uani 1 1 d . . . N5 N 0.2604(3) 0.4899(3) 0.41896(17) 0.0341(5) Uani 1 1 d . . . N6 N 0.4430(2) 0.2853(2) 0.43055(15) 0.0289(5) Uani 1 1 d . . . N7 N 0.4642(3) 0.2218(3) 0.34972(16) 0.0312(5) Uani 1 1 d . . . N8 N 0.3354(3) 0.0341(3) 0.42280(17) 0.0348(5) Uani 1 1 d . . . N9 N 0.3918(3) 0.3586(3) 0.59449(16) 0.0307(5) Uani 1 1 d . . . N10 N 0.4326(2) -0.0825(2) 0.11460(15) 0.0267(5) Uani 1 1 d . . . C1 C -0.1856(3) 0.0603(3) 0.10633(19) 0.0282(6) Uani 1 1 d . . . C2 C -0.0837(3) 0.2616(3) 0.2039(2) 0.0330(6) Uani 1 1 d . . . C3 C -0.2362(3) -0.0898(3) 0.05065(19) 0.0281(6) Uani 1 1 d . . . C4 C -0.1421(3) -0.1743(4) 0.0533(2) 0.0403(7) Uani 1 1 d . . . C5 C -0.2109(4) -0.3150(4) -0.0037(3) 0.0528(9) Uani 1 1 d . . . H5A H -0.1522 -0.3742 -0.0039 0.063 Uiso 1 1 calc R . . C6 C -0.3663(4) -0.3696(4) -0.0609(3) 0.0499(8) Uani 1 1 d . . . H6A H -0.4125 -0.4646 -0.0996 0.060 Uiso 1 1 calc R . . C7 C -0.4510(3) -0.2801(3) -0.0592(2) 0.0365(6) Uani 1 1 d . . . H7A H -0.5557 -0.3168 -0.0972 0.044 Uiso 1 1 calc R . . C8 C 0.0178(3) 0.3807(3) 0.2876(2) 0.0335(6) Uani 1 1 d . . . C9 C -0.0352(4) 0.4825(4) 0.3243(3) 0.0512(9) Uani 1 1 d . . . H9A H -0.1337 0.4813 0.2924 0.061 Uiso 1 1 calc R . . C10 C 0.0563(4) 0.5844(4) 0.4068(3) 0.0543(9) Uani 1 1 d . . . H10A H 0.0207 0.6525 0.4319 0.065 Uiso 1 1 calc R . . C11 C 0.2035(4) 0.5854(4) 0.4531(2) 0.0445(7) Uani 1 1 d . . . H11A H 0.2652 0.6547 0.5099 0.053 Uiso 1 1 calc R . . C12 C 0.1684(3) 0.3910(3) 0.3380(2) 0.0336(6) Uani 1 1 d . . . H12A H 0.2067 0.3247 0.3136 0.040 Uiso 1 1 calc R . . C13 C 0.0267(4) -0.1157(4) 0.1148(3) 0.0574(9) Uiso 1 1 d . . . H13A H 0.0702 -0.1896 0.1060 0.086 Uiso 1 1 calc R . . H13B H 0.0322 -0.0954 0.1823 0.086 Uiso 1 1 calc R . . H13C H 0.0857 -0.0244 0.0954 0.086 Uiso 1 1 calc R . . C14 C 0.3663(3) 0.1700(3) 0.47146(19) 0.0293(6) Uani 1 1 d . . . C15 C 0.3992(3) 0.0723(3) 0.34897(19) 0.0298(6) Uani 1 1 d . . . C16 C 0.3317(3) 0.2081(3) 0.56224(19) 0.0298(6) Uani 1 1 d . . . C17 C 0.2469(4) 0.1044(4) 0.6119(2) 0.0399(7) Uani 1 1 d . . . C18 C 0.2290(4) 0.1620(4) 0.6968(2) 0.0506(9) Uani 1 1 d . . . H18A H 0.1720 0.0965 0.7313 0.061 Uiso 1 1 calc R . . C19 C 0.2934(4) 0.3137(4) 0.7312(2) 0.0501(9) Uani 1 1 d . . . H19A H 0.2839 0.3513 0.7896 0.060 Uiso 1 1 calc R . . C20 C 0.3729(4) 0.4099(4) 0.6774(2) 0.0394(7) Uani 1 1 d . . . H20A H 0.4144 0.5132 0.6995 0.047 Uiso 1 1 calc R . . C21 C 0.3936(3) -0.0379(3) 0.27143(19) 0.0284(6) Uani 1 1 d . . . C22 C 0.3298(4) -0.1919(3) 0.2711(2) 0.0386(7) Uani 1 1 d . . . H22A H 0.2970 -0.2292 0.3236 0.046 Uiso 1 1 calc R . . C23 C 0.3159(4) -0.2885(3) 0.1912(2) 0.0415(7) Uani 1 1 d . . . H23A H 0.2735 -0.3921 0.1895 0.050 Uiso 1 1 calc R . . C24 C 0.3648(3) -0.2316(3) 0.1139(2) 0.0332(6) Uani 1 1 d . . . H24A H 0.3506 -0.2984 0.0594 0.040 Uiso 1 1 calc R . . C25 C 0.4484(3) 0.0110(3) 0.19340(19) 0.0289(6) Uani 1 1 d . . . H25A H 0.4987 0.1141 0.1959 0.035 Uiso 1 1 calc R . . C26 C 0.1766(5) -0.0638(4) 0.5763(3) 0.0634(10) Uiso 1 1 d . . . H26A H 0.1992 -0.0844 0.5165 0.095 Uiso 1 1 calc R . . H26B H 0.0645 -0.1012 0.5650 0.095 Uiso 1 1 calc R . . H26C H 0.2212 -0.1125 0.6247 0.095 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0263(3) 0.0231(3) 0.0187(3) -0.0023(2) 0.0041(2) 0.0116(2) Fe2 0.0286(3) 0.0241(3) 0.0205(3) -0.0023(2) 0.0056(2) 0.0069(2) N1 0.0308(11) 0.0281(13) 0.0255(12) -0.0010(9) 0.0062(9) 0.0119(10) N2 0.0306(11) 0.0272(13) 0.0298(13) -0.0059(10) 0.0008(9) 0.0099(10) N3 0.0306(12) 0.0382(14) 0.0322(14) -0.0031(11) 0.0023(10) 0.0139(11) N4 0.0303(11) 0.0290(13) 0.0231(12) 0.0013(9) 0.0065(9) 0.0126(10) N5 0.0368(12) 0.0292(13) 0.0299(13) -0.0005(10) 0.0069(10) 0.0082(10) N6 0.0326(11) 0.0293(13) 0.0210(12) -0.0031(9) 0.0075(9) 0.0089(10) N7 0.0383(12) 0.0307(14) 0.0220(12) -0.0026(10) 0.0104(10) 0.0106(10) N8 0.0465(14) 0.0307(14) 0.0277(13) 0.0014(10) 0.0160(11) 0.0128(11) N9 0.0346(12) 0.0341(14) 0.0217(12) -0.0018(10) 0.0065(9) 0.0137(10) N10 0.0277(10) 0.0304(13) 0.0223(12) -0.0001(9) 0.0059(9) 0.0132(9) C1 0.0308(13) 0.0297(15) 0.0243(14) 0.0022(11) 0.0066(11) 0.0132(12) C2 0.0300(14) 0.0338(16) 0.0297(16) 0.0006(12) 0.0053(11) 0.0090(12) C3 0.0324(14) 0.0306(15) 0.0231(14) 0.0012(11) 0.0084(11) 0.0145(12) C4 0.0403(16) 0.0455(19) 0.0402(18) 0.0027(14) 0.0081(13) 0.0259(14) C5 0.059(2) 0.050(2) 0.057(2) -0.0077(17) 0.0079(17) 0.0380(18) C6 0.0527(19) 0.043(2) 0.055(2) -0.0093(16) 0.0055(16) 0.0286(16) C7 0.0406(15) 0.0280(16) 0.0368(17) -0.0054(12) 0.0049(12) 0.0147(13) C8 0.0325(14) 0.0271(15) 0.0327(16) -0.0019(12) 0.0055(11) 0.0060(12) C9 0.0335(16) 0.050(2) 0.061(2) -0.0125(17) 0.0002(15) 0.0181(15) C10 0.0428(18) 0.049(2) 0.063(2) -0.0211(17) 0.0032(16) 0.0219(16) C11 0.0396(16) 0.0392(19) 0.0413(19) -0.0142(14) 0.0057(13) 0.0075(14) C12 0.0342(14) 0.0307(16) 0.0305(16) -0.0014(12) 0.0046(12) 0.0107(12) C14 0.0330(13) 0.0315(15) 0.0225(14) -0.0001(11) 0.0075(11) 0.0125(12) C15 0.0359(14) 0.0307(16) 0.0229(14) 0.0007(11) 0.0079(11) 0.0142(12) C16 0.0352(14) 0.0324(16) 0.0222(14) -0.0001(11) 0.0079(11) 0.0146(12) C17 0.0524(17) 0.0376(17) 0.0332(17) 0.0055(13) 0.0188(14) 0.0173(14) C18 0.074(2) 0.051(2) 0.042(2) 0.0175(17) 0.0353(18) 0.0279(19) C19 0.076(2) 0.055(2) 0.0318(18) 0.0043(16) 0.0277(17) 0.0323(19) C20 0.0541(18) 0.0407(18) 0.0280(16) -0.0009(13) 0.0137(13) 0.0235(15) C21 0.0329(13) 0.0301(15) 0.0229(14) 0.0007(11) 0.0072(11) 0.0142(12) C22 0.0546(18) 0.0338(17) 0.0351(17) 0.0095(13) 0.0219(14) 0.0193(14) C23 0.0619(19) 0.0254(16) 0.0460(19) 0.0056(14) 0.0257(16) 0.0203(15) C24 0.0441(15) 0.0240(15) 0.0343(16) -0.0011(12) 0.0139(12) 0.0159(12) C25 0.0334(13) 0.0273(15) 0.0243(14) -0.0001(11) 0.0067(11) 0.0115(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.969(2) 2_455 ? Fe1 N1 1.969(2) . ? Fe1 N10 2.017(2) 1_455 ? Fe1 N10 2.017(2) 2 ? Fe1 N4 2.019(2) 2_455 ? Fe1 N4 2.019(2) . ? Fe2 N6 2.058(2) . ? Fe2 N6 2.058(2) 2_666 ? Fe2 N9 2.163(2) . ? Fe2 N9 2.163(2) 2_666 ? Fe2 N5 2.249(2) . ? Fe2 N5 2.249(2) 2_666 ? N1 C1 1.339(3) . ? N1 N2 1.355(3) . ? N2 C2 1.351(3) . ? N3 C2 1.338(4) . ? N3 C1 1.342(3) . ? N4 C7 1.339(4) . ? N4 C3 1.357(3) . ? N5 C12 1.333(4) . ? N5 C11 1.346(4) . ? N6 C14 1.352(3) . ? N6 N7 1.369(3) . ? N7 C15 1.348(3) . ? N8 C14 1.340(3) . ? N8 C15 1.354(3) . ? N9 C20 1.336(3) . ? N9 C16 1.354(4) . ? N10 C25 1.342(3) . ? N10 C24 1.346(3) . ? N10 Fe1 2.017(2) 1_655 ? C1 C3 1.457(4) . ? C2 C8 1.464(4) . ? C3 C4 1.405(4) . ? C4 C5 1.376(4) . ? C4 C13 1.502(5) . ? C5 C6 1.384(4) . ? C5 H5A 0.9300 . ? C6 C7 1.378(4) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.384(4) . ? C8 C12 1.398(4) . ? C9 C10 1.359(4) . ? C9 H9A 0.9300 . ? C10 C11 1.388(5) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C16 1.475(3) . ? C15 C21 1.465(4) . ? C16 C17 1.399(4) . ? C17 C18 1.380(4) . ? C17 C26 1.511(5) . ? C18 C19 1.369(5) . ? C18 H18A 0.9300 . ? C19 C20 1.380(4) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.388(4) . ? C21 C25 1.388(4) . ? C22 C23 1.377(4) . ? C22 H22A 0.9300 . ? C23 C24 1.378(4) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N1 180.00(19) 2_455 . ? N1 Fe1 N10 90.81(8) 2_455 1_455 ? N1 Fe1 N10 89.19(8) . 1_455 ? N1 Fe1 N10 89.19(8) 2_455 2 ? N1 Fe1 N10 90.81(8) . 2 ? N10 Fe1 N10 180.0(2) 1_455 2 ? N1 Fe1 N4 79.97(9) 2_455 2_455 ? N1 Fe1 N4 100.03(9) . 2_455 ? N10 Fe1 N4 89.70(8) 1_455 2_455 ? N10 Fe1 N4 90.30(8) 2 2_455 ? N1 Fe1 N4 100.03(9) 2_455 . ? N1 Fe1 N4 79.97(9) . . ? N10 Fe1 N4 90.30(8) 1_455 . ? N10 Fe1 N4 89.70(8) 2 . ? N4 Fe1 N4 180.00(12) 2_455 . ? N6 Fe2 N6 180.00(6) . 2_666 ? N6 Fe2 N9 76.73(8) . . ? N6 Fe2 N9 103.27(8) 2_666 . ? N6 Fe2 N9 103.27(8) . 2_666 ? N6 Fe2 N9 76.73(8) 2_666 2_666 ? N9 Fe2 N9 180.000(1) . 2_666 ? N6 Fe2 N5 89.95(9) . . ? N6 Fe2 N5 90.05(9) 2_666 . ? N9 Fe2 N5 88.47(8) . . ? N9 Fe2 N5 91.53(8) 2_666 . ? N6 Fe2 N5 90.05(9) . 2_666 ? N6 Fe2 N5 89.95(9) 2_666 2_666 ? N9 Fe2 N5 91.53(8) . 2_666 ? N9 Fe2 N5 88.47(8) 2_666 2_666 ? N5 Fe2 N5 180.0 . 2_666 ? C1 N1 N2 106.9(2) . . ? C1 N1 Fe1 115.84(18) . . ? N2 N1 Fe1 136.43(16) . . ? C2 N2 N1 104.0(2) . . ? C2 N3 C1 101.3(2) . . ? C7 N4 C3 118.4(2) . . ? C7 N4 Fe1 125.89(18) . . ? C3 N4 Fe1 115.67(17) . . ? C12 N5 C11 117.2(2) . . ? C12 N5 Fe2 123.08(19) . . ? C11 N5 Fe2 119.7(2) . . ? C14 N6 N7 106.5(2) . . ? C14 N6 Fe2 116.94(17) . . ? N7 N6 Fe2 136.55(17) . . ? C15 N7 N6 104.2(2) . . ? C14 N8 C15 101.4(2) . . ? C20 N9 C16 119.2(2) . . ? C20 N9 Fe2 124.7(2) . . ? C16 N9 Fe2 116.00(17) . . ? C25 N10 C24 117.4(2) . . ? C25 N10 Fe1 120.55(18) . 1_655 ? C24 N10 Fe1 121.95(18) . 1_655 ? N1 C1 N3 113.2(2) . . ? N1 C1 C3 116.2(2) . . ? N3 C1 C3 130.5(2) . . ? N3 C2 N2 114.6(3) . . ? N3 C2 C8 124.0(2) . . ? N2 C2 C8 121.1(2) . . ? N4 C3 C4 122.4(3) . . ? N4 C3 C1 112.2(2) . . ? C4 C3 C1 125.3(2) . . ? C5 C4 C3 117.2(3) . . ? C5 C4 C13 120.5(3) . . ? C3 C4 C13 122.4(3) . . ? C4 C5 C6 120.8(3) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C7 C6 C5 118.5(3) . . ? C7 C6 H6A 120.7 . . ? C5 C6 H6A 120.7 . . ? N4 C7 C6 122.6(3) . . ? N4 C7 H7A 118.7 . . ? C6 C7 H7A 118.7 . . ? C9 C8 C12 116.9(3) . . ? C9 C8 C2 121.3(2) . . ? C12 C8 C2 121.7(3) . . ? C10 C9 C8 120.3(3) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C9 C10 C11 119.1(3) . . ? C9 C10 H10A 120.4 . . ? C11 C10 H10A 120.4 . . ? N5 C11 C10 122.5(3) . . ? N5 C11 H11A 118.8 . . ? C10 C11 H11A 118.8 . . ? N5 C12 C8 124.0(3) . . ? N5 C12 H12A 118.0 . . ? C8 C12 H12A 118.0 . . ? C4 C13 H13A 109.5 . . ? C4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N8 C14 N6 113.4(2) . . ? N8 C14 C16 129.1(2) . . ? N6 C14 C16 117.6(2) . . ? N7 C15 N8 114.5(2) . . ? N7 C15 C21 121.7(2) . . ? N8 C15 C21 123.7(2) . . ? N9 C16 C17 122.0(2) . . ? N9 C16 C14 112.5(2) . . ? C17 C16 C14 125.5(3) . . ? C18 C17 C16 117.0(3) . . ? C18 C17 C26 120.2(3) . . ? C16 C17 C26 122.8(3) . . ? C19 C18 C17 121.2(3) . . ? C19 C18 H18A 119.4 . . ? C17 C18 H18A 119.4 . . ? C18 C19 C20 118.7(3) . . ? C18 C19 H19A 120.7 . . ? C20 C19 H19A 120.7 . . ? N9 C20 C19 121.9(3) . . ? N9 C20 H20A 119.1 . . ? C19 C20 H20A 119.1 . . ? C22 C21 C25 118.0(3) . . ? C22 C21 C15 122.2(2) . . ? C25 C21 C15 119.8(2) . . ? C23 C22 C21 118.6(3) . . ? C23 C22 H22A 120.7 . . ? C21 C22 H22A 120.7 . . ? C22 C23 C24 120.0(3) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? N10 C24 C23 122.2(3) . . ? N10 C24 H24A 118.9 . . ? C23 C24 H24A 118.9 . . ? N10 C25 C21 123.6(3) . . ? N10 C25 H25A 118.2 . . ? C21 C25 H25A 118.2 . . ? C17 C26 H26A 109.5 . . ? C17 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C17 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C7 H7A N2 0.93 2.32 3.124(4) 144.8 2_455 C11 H11A N7 0.93 2.65 3.479(4) 149.1 2_666 C20 H20A N7 0.93 2.62 3.420(4) 144.1 2_666 _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.768 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.072 #================================END data_2_600K _database_code_depnum_ccdc_archive 'CCDC 824538' _audit_creation_date 2011-04-13 _audit_creation_method 'Materials Studio' _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 _symmetry_cell_setting triclinic loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 9.5368 _cell_length_b 9.7585 _cell_length_c 14.5674 _cell_angle_alpha 94.9888 _cell_angle_beta 103.1962 _cell_angle_gamma 112.1438 _cell_measurement_temperature 600(2) _diffrn_ambient_temperature 600(2) _diffrn_radiation_wavelength 1.5418 _pd_calc_method 'Rietveld Refinement' _chemical_formula_sum 'C26 H20 Fe N10' _chemical_formula_weight 528.37 _pd_meas_2theta_range_min 5.000 _pd_meas_2theta_range_max 60.000 _pd_meas_2theta_range_inc 0.019695 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 N6 N 0.42531 0.26939 0.43748 0.02324 Uani 1.00 N7 N 0.45402 0.20903 0.35840 0.02572 Uani 1.00 N8 N 0.33758 0.01567 0.43340 0.02990 Uani 1.00 N9 N 0.36754 0.34642 0.59583 0.02570 Uani 1.00 N10 N 0.46590 -0.09333 0.13182 0.02355 Uani 1.00 C14 C 0.35669 0.15236 0.48052 0.02541 Uani 1.00 C15 C 0.40055 0.05796 0.35956 0.02718 Uani 1.00 C16 C 0.31951 0.19135 0.56978 0.02540 Uani 1.00 C17 C 0.24495 0.08775 0.62450 0.03467 Uani 1.00 C18 C 0.22095 0.14678 0.70764 0.04008 Uani 1.00 H18 H 0.16923 0.08057 0.74494 0.05653 Uiso 1.00 C19 C 0.27305 0.30343 0.73604 0.03918 Uani 1.00 H19 H 0.26000 0.34367 0.79329 0.05608 Uiso 1.00 C20 C 0.34466 0.39907 0.67822 0.03177 Uani 1.00 H20 H 0.37854 0.50457 0.69713 0.04527 Uiso 1.00 C21 C 0.40697 -0.05143 0.28429 0.02508 Uani 1.00 C22 C 0.34217 -0.20899 0.28151 0.03405 Uani 1.00 H22 H 0.30196 -0.24863 0.33166 0.04800 Uiso 1.00 C23 C 0.33849 -0.30554 0.20321 0.03680 Uani 1.00 H23 H 0.29614 -0.41128 0.20047 0.05172 Uiso 1.00 C24 C 0.39704 -0.24621 0.12936 0.02963 Uani 1.00 H24 H 0.38910 -0.31348 0.07573 0.04212 Uiso 1.00 C25 C 0.47156 0.00020 0.20957 0.02541 Uani 1.00 H25 H 0.52187 0.10582 0.21330 0.03531 Uiso 1.00 C26 C 0.18844 -0.08343 0.59356 0.05011 Uiso 1.00 H26A H 0.12052 -0.11556 0.52762 0.07517 Uiso 1.00 H26B H 0.12896 -0.13577 0.63580 0.07517 Uiso 1.00 H26C H 0.27986 -0.10795 0.59755 0.07517 Uiso 1.00 N1 N -0.26094 0.13664 0.08270 0.02547 Uani 1.00 N2 N -0.19814 0.27090 0.14763 0.02953 Uani 1.00 N3 N -0.03475 0.14671 0.18378 0.03172 Uani 1.00 N4 N -0.36505 -0.14079 -0.00978 0.02419 Uani 1.00 N5 N 0.25871 0.49226 0.43852 0.02651 Uani 1.00 C1 C -0.16206 0.06658 0.10621 0.02674 Uani 1.00 C2 C -0.06303 0.27109 0.20682 0.02922 Uani 1.00 C3 C -0.21286 -0.08733 0.05018 0.02646 Uani 1.00 C4 C -0.11937 -0.17270 0.05655 0.03574 Uani 1.00 C5 C -0.18879 -0.31696 -0.00239 0.04738 Uani 1.00 H5 H -0.13082 -0.37756 -0.00028 0.07038 Uiso 1.00 C6 C -0.34168 -0.37173 -0.06379 0.04392 Uani 1.00 H6 H -0.38742 -0.46830 -0.10382 0.06185 Uiso 1.00 C7 C -0.42686 -0.28081 -0.06519 0.03204 Uani 1.00 H7 H -0.53119 -0.31862 -0.10631 0.04363 Uiso 1.00 C8 C 0.03123 0.38841 0.29473 0.02962 Uani 1.00 C9 C -0.02837 0.49051 0.32680 0.04163 Uani 1.00 H9 H -0.12335 0.49115 0.28931 0.05641 Uiso 1.00 C10 C 0.05397 0.58983 0.41390 0.04384 Uani 1.00 H10 H 0.01596 0.65934 0.43609 0.06063 Uiso 1.00 C11 C 0.19471 0.58642 0.46909 0.03674 Uani 1.00 H11 H 0.24716 0.65159 0.52961 0.04902 Uiso 1.00 C12 C 0.17643 0.39618 0.35248 0.02877 Uani 1.00 H12 H 0.21896 0.33085 0.33008 0.03969 Uiso 1.00 C13 C 0.04823 -0.11356 0.12311 0.04963 Uiso 1.00 H13A H 0.10434 -0.00651 0.12246 0.07445 Uiso 1.00 H13B H 0.10397 -0.17011 0.10130 0.07445 Uiso 1.00 H13C H 0.04383 -0.12614 0.18822 0.07445 Uiso 1.00 FE2 Fe 0.50000 0.50000 0.50000 0.05000 Uiso 1.00 FE1 Fe -0.50000 0.00000 0.00000 0.05000 Uiso 1.00 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N6 0.02594 0.02408 0.01748 0.00886 0.00575 0.00030 N7 0.03217 0.02490 0.01768 0.01046 0.00689 -0.00192 N8 0.04411 0.02525 0.02153 0.01304 0.01450 0.00178 N9 0.03055 0.02787 0.01832 0.01367 0.00492 -0.00010 N10 0.02616 0.02532 0.02210 0.01457 0.00676 0.00058 C14 0.03008 0.02603 0.02108 0.01171 0.00915 0.00308 C15 0.03273 0.02689 0.02361 0.01428 0.00780 0.00404 C16 0.02947 0.02892 0.01817 0.01222 0.00745 0.00310 C17 0.04601 0.03177 0.03107 0.01691 0.01757 0.00762 C18 0.05592 0.04355 0.03237 0.02342 0.02563 0.01569 C19 0.05300 0.04125 0.03179 0.02408 0.02036 0.00468 C20 0.04371 0.03331 0.02124 0.01952 0.00968 0.00113 C21 0.02989 0.02407 0.02229 0.01345 0.00583 0.00237 C22 0.05037 0.03054 0.02851 0.01976 0.01767 0.00950 C23 0.05419 0.02382 0.04008 0.01989 0.02072 0.00637 C24 0.03961 0.02455 0.02976 0.01731 0.01322 0.00170 C25 0.03113 0.02445 0.02088 0.01310 0.00612 0.00068 N1 0.02614 0.02553 0.02326 0.01096 0.00518 0.00032 N2 0.03012 0.02746 0.02473 0.01086 0.00045 -0.00251 N3 0.03272 0.03291 0.02654 0.01393 0.00440 -0.00077 N4 0.02707 0.02756 0.01865 0.01245 0.00614 0.00292 N5 0.02858 0.02445 0.02379 0.00807 0.00827 0.00180 C1 0.02903 0.03115 0.02219 0.01527 0.00661 0.00367 C2 0.02811 0.02991 0.02604 0.00986 0.00569 0.00205 C3 0.03053 0.02984 0.02021 0.01444 0.00633 0.00331 C4 0.03564 0.04133 0.03574 0.02424 0.00738 0.00262 C5 0.05046 0.04906 0.05161 0.03735 0.00684 -0.00431 C6 0.04936 0.03461 0.04552 0.02423 0.00326 -0.00922 C7 0.03388 0.03007 0.02915 0.01437 0.00329 -0.00024 C8 0.02928 0.02655 0.02729 0.00746 0.00559 0.00143 C9 0.02919 0.04224 0.04660 0.01701 -0.00017 -0.00758 C10 0.03716 0.04289 0.04708 0.01964 0.00612 -0.01305 C11 0.03514 0.03719 0.03079 0.01206 0.00568 -0.00641 C12 0.03044 0.03184 0.02339 0.01456 0.00446 0.00202 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _ccdc_geom_bond_type N6 N7 1.377 . S N6 C14 1.369 . S N7 C15 1.369 . D N8 C14 1.373 . D N8 C15 1.369 . S N9 C16 1.394 . D N9 C20 1.360 . S N10 C24 1.378 . D N10 C25 1.369 . S C14 C16 1.479 . S C15 C21 1.491 . S C16 C17 1.421 . S C17 C18 1.399 . D C17 C26 1.537 . S C18 H18 0.948 . S C18 C19 1.407 . S C19 H19 0.945 . S C19 C20 1.402 . D C20 H20 0.948 . S C21 C22 1.417 . S C21 C25 1.409 . D C22 H22 0.946 . S C22 C23 1.400 . D C23 H23 0.949 . S C23 C24 1.394 . S C24 H24 0.945 . S C25 H25 0.949 . S C26 H26A 0.975 . S C26 H26B 0.978 . S C26 H26C 0.978 . S N1 N2 1.380 . S N1 C1 1.361 . S N2 C2 1.376 . D N3 C1 1.366 . D N3 C2 1.370 . S N4 C3 1.383 . D N4 C7 1.360 . S N5 C11 1.375 . S N5 C12 1.363 . D C1 C3 1.488 . S C2 C8 1.484 . S C3 C4 1.426 . S C4 C5 1.409 . D C4 C13 1.526 . S C5 H5 0.948 . S C5 C6 1.395 . S C6 H6 0.947 . S C6 C7 1.409 . D C7 H7 0.947 . S C8 C9 1.415 . D C8 C12 1.417 . S C9 H9 0.947 . S C9 C10 1.387 . S C10 H10 0.947 . S C10 C11 1.412 . D C11 H11 0.945 . S C12 H12 0.947 . S C13 H13A 0.980 . S C13 H13B 0.978 . S C13 H13C 0.975 . S #_eof #End of Crystallographic Information File