# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_publication_text _journal_name_full 'Dalton Trans.' #TrackingRef '- chandu.cif' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Rajadurai Chandrasekar' _publ_contact_author_address ;Asst.Professor, School of Chemistry, University of Hyderabad, Central University Post, Gachibowli, Hyderabad-500 046, India. ; _publ_contact_author_email chandrasekar100@yahoo.com _publ_contact_author_phone +91(40)23134824 _publ_contact_author_fax +91(40)23134824 loop_ _publ_author_name _publ_author_address C.Rajadurai ;Asst.Professor, School of Chemistry, University of Hyderabad, Central University Post, Gachibowli, Hyderabad-500 046, India. ; C.Naisa ;C/O: Dr. R. Chandrasekar, Asst.Professor, School of Chemistry, University of Hyderabad, Central University Post, Gachibowli, Hyderabad-500 046, India. ; data_chandu _database_code_depnum_ccdc_archive 'CCDC 772647' #TrackingRef '- chandu.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H46 Cl2 Fe N14 O12' _chemical_formula_sum 'C38 H46 Cl2 Fe N14 O12' _chemical_formula_weight 1017.64 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbcn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 21.3932(19) _cell_length_b 13.5171(12) _cell_length_c 15.5665(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4501.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5488 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 25.96 _exptl_crystal_description needle _exptl_crystal_colour 'wine red' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 0.531 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8237 _exptl_absorpt_correction_T_max 0.9390 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44555 _diffrn_reflns_av_R_equivalents 0.0883 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 26.09 _reflns_number_total 4472 _reflns_number_gt 4001 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0351P)^2^+12.8519P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4472 _refine_ls_number_parameters 365 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0855 _refine_ls_R_factor_gt 0.0754 _refine_ls_wR_factor_ref 0.1439 _refine_ls_wR_factor_gt 0.1397 _refine_ls_goodness_of_fit_ref 1.264 _refine_ls_restrained_S_all 1.264 _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 C1 C 0.39086(16) 0.4048(3) 0.1625(2) 0.0110(7) Uani 1 1 d . . . C2 C 0.34633(17) 0.4047(3) 0.0986(2) 0.0132(8) Uani 1 1 d . . . C3 C 0.35151(16) 0.4729(3) 0.0320(2) 0.0138(8) Uani 1 1 d . . . C4 C 0.40163(16) 0.5378(3) 0.0290(2) 0.0118(7) Uani 1 1 d . . . C5 C 0.44472(16) 0.5331(3) 0.0950(2) 0.0115(7) Uani 1 1 d . . . C6 C 0.29988(18) 0.4751(3) -0.0330(2) 0.0168(8) Uani 1 1 d . . . C7 C 0.25911(18) 0.5537(3) -0.1568(3) 0.0177(8) Uani 1 1 d . . . C8 C 0.2138(2) 0.6292(3) -0.1224(3) 0.0231(9) Uani 1 1 d . . . C13 C 0.4693(3) -0.0504(4) 0.3645(4) 0.0441(13) Uani 1 1 d . . . H13A H 0.5120 -0.0282 0.3767 0.066 Uiso 1 1 calc R . . H13B H 0.4693 -0.0911 0.3124 0.066 Uiso 1 1 calc R . . H13C H 0.4538 -0.0895 0.4130 0.066 Uiso 1 1 calc R . . C14 C 0.4273(2) 0.0393(3) 0.3512(3) 0.0365(11) Uani 1 1 d . . . H14A H 0.4439 0.0793 0.3031 0.044 Uiso 1 1 calc R . . H14B H 0.3850 0.0163 0.3350 0.044 Uiso 1 1 calc R . . C15 C 0.4224(2) 0.1033(3) 0.4295(3) 0.0288(10) Uani 1 1 d . . . C16 C 0.3752(2) 0.1859(3) 0.4230(3) 0.0206(9) Uani 1 1 d . . . C17 C 0.36114(18) 0.2719(3) 0.2794(2) 0.0142(8) Uani 1 1 d . . . C18 C 0.39493(16) 0.3454(3) 0.2401(2) 0.0118(7) Uani 1 1 d . . . C30 C 0.57728(18) 0.6933(3) 0.0925(3) 0.0162(8) Uani 1 1 d . . . C31 C 0.52345(18) 0.6642(3) 0.0536(3) 0.0139(8) Uani 1 1 d . . . C32 C 0.58306(18) 0.6349(3) 0.1669(2) 0.0155(8) Uani 1 1 d . . . C33 C 0.3727(2) 0.0887(4) 0.1080(3) 0.0295(10) Uani 1 1 d . . . C34 C 0.3349(2) 0.0051(4) 0.1364(3) 0.0327(11) Uani 1 1 d . . . H34A H 0.3616 -0.0427 0.1663 0.049 Uiso 1 1 calc R . . H34B H 0.3156 -0.0267 0.0864 0.049 Uiso 1 1 calc R . . H34C H 0.3022 0.0285 0.1755 0.049 Uiso 1 1 calc R . . Cl2 Cl 0.30198(4) 0.70607(7) 0.14811(6) 0.0184(2) Uani 1 1 d . . . Fe1 Fe 0.5000 0.47047(5) 0.2500 0.00940(18) Uani 1 2 d S . . H1 H 0.313(2) 0.362(3) 0.101(3) 0.019(11) Uiso 1 1 d . . . H2 H 0.4060(18) 0.584(3) -0.016(3) 0.015(10) Uiso 1 1 d . . . H3 H 0.2402(17) 0.493(3) -0.165(2) 0.006(9) Uiso 1 1 d . . . H4 H 0.279(2) 0.578(3) -0.210(3) 0.024(12) Uiso 1 1 d . . . H5 H 0.235(2) 0.693(3) -0.112(3) 0.020(11) Uiso 1 1 d . . . H6 H 0.185(2) 0.647(3) -0.163(3) 0.024(12) Uiso 1 1 d . . . H7 H 0.1964(19) 0.608(3) -0.068(3) 0.016(10) Uiso 1 1 d . . . H11 H 0.373(2) 0.226(3) 0.472(3) 0.028(13) Uiso 1 1 d . . . H12 H 0.335(2) 0.163(3) 0.414(3) 0.028(13) Uiso 1 1 d . . . H13 H 0.3252(19) 0.240(3) 0.262(3) 0.012(10) Uiso 1 1 d . . . H14 H 0.6135(18) 0.637(3) 0.209(3) 0.008(9) Uiso 1 1 d . . . H15 H 0.606(2) 0.739(3) 0.078(3) 0.020(11) Uiso 1 1 d . . . H16 H 0.504(2) 0.683(3) 0.006(3) 0.015(10) Uiso 1 1 d . . . H17 H 0.467(2) 0.131(3) 0.439(3) 0.017(11) Uiso 1 1 d . . . H18 H 0.407(2) 0.061(3) 0.478(3) 0.025(12) Uiso 1 1 d . . . N1 N 0.44384(13) 0.3682(2) 0.29343(19) 0.0101(6) Uani 1 1 d . . . N2 N 0.43938(13) 0.4693(2) 0.16027(19) 0.0105(6) Uani 1 1 d . . . N3 N 0.49842(14) 0.5913(2) 0.10324(19) 0.0122(6) Uani 1 1 d . . . N4 N 0.53535(14) 0.5732(2) 0.17409(19) 0.0111(6) Uani 1 1 d . . . N9 N 0.44182(14) 0.3132(2) 0.36268(19) 0.0139(7) Uani 1 1 d . . . N10 N 0.39100(15) 0.2558(2) 0.3538(2) 0.0152(7) Uani 1 1 d . . . N13 N 0.4021(2) 0.1546(3) 0.0855(3) 0.0415(11) Uani 1 1 d . . . O3 O 0.25403(13) 0.4248(2) -0.02697(18) 0.0261(7) Uani 1 1 d . . . O4 O 0.31093(12) 0.5399(2) -0.09653(16) 0.0164(6) Uani 1 1 d . . . O5 O 0.36660(14) 0.7304(3) 0.1394(2) 0.0334(8) Uani 1 1 d . . . O6 O 0.29558(18) 0.6250(3) 0.2066(3) 0.0566(12) Uani 1 1 d . . . O7 O 0.26920(15) 0.7894(3) 0.1813(2) 0.0386(9) Uani 1 1 d . . . O8 O 0.27620(15) 0.6786(2) 0.06655(19) 0.0325(8) Uani 1 1 d . . . 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 C1 0.0075(17) 0.0116(17) 0.0138(18) -0.0022(14) 0.0007(14) 0.0013(14) C2 0.0105(19) 0.0138(18) 0.0154(19) -0.0011(15) 0.0017(14) -0.0017(15) C3 0.0094(17) 0.0165(19) 0.0156(18) -0.0048(15) 0.0002(14) 0.0024(15) C4 0.0116(18) 0.0127(18) 0.0112(17) 0.0004(15) -0.0004(14) 0.0012(15) C5 0.0115(18) 0.0115(17) 0.0116(17) -0.0012(15) 0.0003(14) 0.0033(14) C6 0.0155(19) 0.019(2) 0.0156(19) 0.0007(16) -0.0021(15) -0.0011(16) C7 0.015(2) 0.023(2) 0.0152(19) 0.0028(17) -0.0082(16) -0.0029(17) C8 0.022(2) 0.027(2) 0.021(2) 0.0051(18) -0.0037(18) 0.0055(19) C13 0.049(3) 0.025(3) 0.058(4) 0.004(2) 0.008(3) 0.008(2) C14 0.044(3) 0.028(3) 0.038(3) 0.003(2) 0.004(2) 0.000(2) C15 0.038(3) 0.023(2) 0.026(2) 0.0130(19) -0.001(2) -0.006(2) C16 0.020(2) 0.021(2) 0.020(2) 0.0037(18) 0.0078(17) -0.0079(18) C17 0.0109(18) 0.0145(19) 0.0171(19) -0.0023(15) -0.0009(15) 0.0003(15) C18 0.0095(16) 0.0134(17) 0.0126(18) 0.0001(14) -0.0008(14) 0.0016(14) C30 0.016(2) 0.0138(19) 0.019(2) 0.0000(16) 0.0008(16) -0.0048(16) C31 0.0147(18) 0.0127(18) 0.0145(19) 0.0024(15) -0.0013(15) -0.0008(15) C32 0.0140(19) 0.0171(19) 0.0155(19) -0.0032(16) -0.0038(16) -0.0023(16) C33 0.031(3) 0.036(3) 0.022(2) -0.004(2) 0.0012(19) 0.012(2) C34 0.030(2) 0.038(3) 0.030(3) 0.001(2) 0.000(2) 0.002(2) Cl2 0.0164(5) 0.0213(5) 0.0175(5) 0.0021(4) -0.0033(4) 0.0027(4) Fe1 0.0078(3) 0.0109(4) 0.0095(3) 0.000 -0.0010(3) 0.000 N1 0.0087(15) 0.0104(15) 0.0112(15) 0.0013(12) 0.0013(12) -0.0007(12) N2 0.0075(14) 0.0121(15) 0.0118(15) -0.0024(13) 0.0005(11) -0.0001(12) N3 0.0100(14) 0.0151(15) 0.0114(14) 0.0025(12) -0.0024(12) 0.0016(13) N4 0.0092(15) 0.0132(15) 0.0109(15) 0.0011(12) -0.0045(11) 0.0014(12) N9 0.0147(16) 0.0151(16) 0.0120(15) 0.0010(13) 0.0025(13) -0.0006(13) N10 0.0145(16) 0.0155(16) 0.0156(16) -0.0004(13) 0.0023(13) -0.0009(13) N13 0.049(3) 0.036(2) 0.040(3) -0.001(2) 0.003(2) 0.006(2) O3 0.0210(15) 0.0334(17) 0.0237(15) 0.0103(14) -0.0103(13) -0.0128(14) O4 0.0131(13) 0.0218(14) 0.0143(13) 0.0031(11) -0.0045(10) -0.0013(11) O5 0.0173(15) 0.046(2) 0.0367(19) -0.0072(16) 0.0029(14) 0.0023(14) O6 0.063(3) 0.053(2) 0.054(2) 0.033(2) -0.039(2) -0.031(2) O7 0.0286(18) 0.053(2) 0.0339(18) -0.0183(17) -0.0042(14) 0.0192(16) O8 0.0339(18) 0.0407(19) 0.0229(16) -0.0082(14) -0.0093(14) 0.0028(15) _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 C1 N2 1.356(4) . ? C1 C2 1.377(5) . ? C1 C18 1.454(5) . ? C2 C3 1.392(5) . ? C2 H1 0.92(4) . ? C3 C4 1.386(5) . ? C3 C6 1.498(5) . ? C4 C5 1.381(5) . ? C4 H2 0.94(4) . ? C5 N2 1.338(5) . ? C5 N3 1.398(5) . ? C6 O3 1.197(5) . ? C6 O4 1.342(4) . ? C7 O4 1.465(4) . ? C7 C8 1.505(6) . ? C7 H3 0.93(4) . ? C7 H4 0.98(5) . ? C8 H5 0.99(4) . ? C8 H6 0.91(5) . ? C8 H7 0.97(4) . ? C13 C14 1.524(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.499(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.509(6) . ? C15 H17 1.04(4) . ? C15 H18 1.00(4) . ? C16 N10 1.472(5) . ? C16 H11 0.93(5) . ? C16 H12 0.93(5) . ? C17 N10 1.342(5) . ? C17 C18 1.372(5) . ? C17 H13 0.92(4) . ? C18 N1 1.370(5) . ? C30 C31 1.359(5) . ? C30 C32 1.408(6) . ? C30 H15 0.89(4) . ? C31 N3 1.362(5) . ? C31 H16 0.89(4) . ? C32 N4 1.323(5) . ? C32 H14 0.92(4) . ? C33 N13 1.145(6) . ? C33 C34 1.458(7) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? Cl2 O7 1.424(3) . ? Cl2 O5 1.427(3) . ? Cl2 O6 1.431(3) . ? Cl2 O8 1.433(3) . ? Fe1 N2 1.906(3) . ? Fe1 N2 1.906(3) 3_655 ? Fe1 N1 1.952(3) . ? Fe1 N1 1.952(3) 3_655 ? Fe1 N4 1.974(3) . ? Fe1 N4 1.974(3) 3_655 ? N1 N9 1.310(4) . ? N3 N4 1.378(4) . ? N9 N10 1.343(4) . ? 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 N2 C1 C2 120.8(3) . . ? N2 C1 C18 109.3(3) . . ? C2 C1 C18 129.9(3) . . ? C1 C2 C3 118.8(3) . . ? C1 C2 H1 121(3) . . ? C3 C2 H1 120(3) . . ? C4 C3 C2 120.4(3) . . ? C4 C3 C6 122.4(3) . . ? C2 C3 C6 117.2(3) . . ? C5 C4 C3 117.5(3) . . ? C5 C4 H2 121(2) . . ? C3 C4 H2 121(2) . . ? N2 C5 C4 122.5(3) . . ? N2 C5 N3 111.3(3) . . ? C4 C5 N3 126.2(3) . . ? O3 C6 O4 124.9(3) . . ? O3 C6 C3 122.7(3) . . ? O4 C6 C3 112.4(3) . . ? O4 C7 C8 110.2(3) . . ? O4 C7 H3 108(2) . . ? C8 C7 H3 112(2) . . ? O4 C7 H4 105(3) . . ? C8 C7 H4 110(3) . . ? H3 C7 H4 112(3) . . ? C7 C8 H5 112(2) . . ? C7 C8 H6 111(3) . . ? H5 C8 H6 100(4) . . ? C7 C8 H7 111(2) . . ? H5 C8 H7 106(3) . . ? H6 C8 H7 116(4) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C13 112.9(4) . . ? C15 C14 H14A 109.0 . . ? C13 C14 H14A 109.0 . . ? C15 C14 H14B 109.0 . . ? C13 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C14 C15 C16 114.7(4) . . ? C14 C15 H17 105(2) . . ? C16 C15 H17 111(2) . . ? C14 C15 H18 108(3) . . ? C16 C15 H18 105(3) . . ? H17 C15 H18 113(3) . . ? N10 C16 C15 111.7(3) . . ? N10 C16 H11 104(3) . . ? C15 C16 H11 114(3) . . ? N10 C16 H12 109(3) . . ? C15 C16 H12 113(3) . . ? H11 C16 H12 105(4) . . ? N10 C17 C18 104.6(3) . . ? N10 C17 H13 125(2) . . ? C18 C17 H13 130(2) . . ? N1 C18 C17 107.2(3) . . ? N1 C18 C1 115.1(3) . . ? C17 C18 C1 137.6(3) . . ? C31 C30 C32 106.2(3) . . ? C31 C30 H15 131(3) . . ? C32 C30 H15 122(3) . . ? C30 C31 N3 106.8(3) . . ? C30 C31 H16 133(3) . . ? N3 C31 H16 120(3) . . ? N4 C32 C30 110.8(3) . . ? N4 C32 H14 120(2) . . ? C30 C32 H14 129(2) . . ? N13 C33 C34 179.7(6) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O7 Cl2 O5 109.2(2) . . ? O7 Cl2 O6 109.2(2) . . ? O5 Cl2 O6 109.2(2) . . ? O7 Cl2 O8 109.68(19) . . ? O5 Cl2 O8 110.4(2) . . ? O6 Cl2 O8 109.1(2) . . ? N2 Fe1 N2 179.09(18) . 3_655 ? N2 Fe1 N1 80.18(12) . . ? N2 Fe1 N1 99.17(12) 3_655 . ? N2 Fe1 N1 99.17(12) . 3_655 ? N2 Fe1 N1 80.17(12) 3_655 3_655 ? N1 Fe1 N1 89.85(17) . 3_655 ? N2 Fe1 N4 80.07(12) . . ? N2 Fe1 N4 100.58(12) 3_655 . ? N1 Fe1 N4 160.24(12) . . ? N1 Fe1 N4 93.15(12) 3_655 . ? N2 Fe1 N4 100.58(12) . 3_655 ? N2 Fe1 N4 80.07(12) 3_655 3_655 ? N1 Fe1 N4 93.15(12) . 3_655 ? N1 Fe1 N4 160.24(12) 3_655 3_655 ? N4 Fe1 N4 90.61(17) . 3_655 ? N9 N1 C18 110.2(3) . . ? N9 N1 Fe1 135.0(2) . . ? C18 N1 Fe1 114.8(2) . . ? C5 N2 C1 119.9(3) . . ? C5 N2 Fe1 119.6(2) . . ? C1 N2 Fe1 120.5(2) . . ? C31 N3 N4 110.9(3) . . ? C31 N3 C5 132.7(3) . . ? N4 N3 C5 116.4(3) . . ? C32 N4 N3 105.2(3) . . ? C32 N4 Fe1 142.1(3) . . ? N3 N4 Fe1 112.6(2) . . ? N1 N9 N10 105.7(3) . . ? C17 N10 N9 112.3(3) . . ? C17 N10 C16 128.8(3) . . ? N9 N10 C16 118.8(3) . . ? C6 O4 C7 115.0(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.09 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.619 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.090 # Attachment '- rc28.cif' data_rc28 _database_code_depnum_ccdc_archive 'CCDC 772648' #TrackingRef '- rc28.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H43 B2 F8 Fe N13 O4' _chemical_formula_sum 'C36 H43 B2 F8 Fe N13 O4' _chemical_formula_weight 951.30 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' B B 0.0013 0.0007 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.8665(11) _cell_length_b 20.8850(18) _cell_length_c 15.9996(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.515(2) _cell_angle_gamma 90.00 _cell_volume 4291.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7109 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 26.25 _exptl_crystal_description needle _exptl_crystal_colour 'wine red' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 0.442 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8500 _exptl_absorpt_correction_T_max 0.9571 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49372 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_sigmaI/netI 0.0640 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.31 _reflns_number_total 10331 _reflns_number_gt 8339 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0540P)^2^+15.1944P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10331 _refine_ls_number_parameters 618 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1114 _refine_ls_R_factor_gt 0.0901 _refine_ls_wR_factor_ref 0.1996 _refine_ls_wR_factor_gt 0.1906 _refine_ls_goodness_of_fit_ref 1.201 _refine_ls_restrained_S_all 1.201 _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 B1 B 0.4843(4) 0.9338(2) 0.6509(3) 0.0203(10) Uani 1 1 d . . . B2 B 0.9982(4) 0.9442(2) 0.3205(4) 0.0258(11) Uani 1 1 d . . . C1 C 0.1811(3) 0.6372(2) 0.3072(3) 0.0192(8) Uani 1 1 d . . . C2 C 0.1653(3) 0.68595(19) 0.3614(2) 0.0148(8) Uani 1 1 d . . . C3 C 0.0803(3) 0.72841(18) 0.3830(2) 0.0140(7) Uani 1 1 d . . . C4 C -0.0224(3) 0.72927(19) 0.3515(3) 0.0163(8) Uani 1 1 d . . . C5 C -0.0905(3) 0.77200(19) 0.3879(2) 0.0159(8) Uani 1 1 d . . . C6 C -0.0557(3) 0.81321(19) 0.4514(3) 0.0160(8) Uani 1 1 d . . . C7 C 0.0486(3) 0.80947(18) 0.4776(2) 0.0135(7) Uani 1 1 d . . . C8 C -0.2050(3) 0.7741(2) 0.3631(3) 0.0175(8) Uani 1 1 d . . . C9 C -0.3880(4) 0.6696(3) 0.3419(4) 0.0505(16) Uani 1 1 d . . . H9A H -0.3568 0.6283 0.3288 0.076 Uiso 1 1 calc R . . H9B H -0.4636 0.6674 0.3305 0.076 Uiso 1 1 calc R . . H9C H -0.3724 0.6797 0.4012 0.076 Uiso 1 1 calc R . . C10 C -0.3441(3) 0.7206(3) 0.2890(3) 0.0328(12) Uani 1 1 d . . . C11 C 0.6990(3) 0.7079(3) 0.6334(3) 0.0338(12) Uani 1 1 d . . . C12 C 0.8761(3) 0.7012(2) 0.6051(3) 0.0291(11) Uani 1 1 d . . . H12A H 0.9192 0.6986 0.5561 0.035 Uiso 1 1 calc R . . H12B H 0.8771 0.6586 0.6324 0.035 Uiso 1 1 calc R . . C13 C 0.9221(3) 0.7501(2) 0.6658(3) 0.0314(11) Uani 1 1 d . . . H13A H 0.9099 0.7931 0.6428 0.047 Uiso 1 1 calc R . . H13B H 0.9971 0.7427 0.6748 0.047 Uiso 1 1 calc R . . H13C H 0.8891 0.7462 0.7192 0.047 Uiso 1 1 calc R . . C14 C 0.7493(4) 0.9241(2) 0.5558(3) 0.0276(10) Uani 1 1 d . . . C15 C 0.7216(4) 0.9814(3) 0.5086(4) 0.0416(13) Uani 1 1 d . . . H15A H 0.7392 0.9759 0.4503 0.062 Uiso 1 1 calc R . . H15B H 0.7601 1.0180 0.5332 0.062 Uiso 1 1 calc R . . H15C H 0.6466 0.9892 0.5104 0.062 Uiso 1 1 calc R . . C16 C 0.4791(3) 0.8648(2) 0.3981(2) 0.0176(8) Uani 1 1 d . . . H16 H 0.5514 0.8743 0.4000 0.021 Uiso 1 1 calc R . . C17 C 0.4033(3) 0.8934(2) 0.3487(3) 0.0179(8) Uani 1 1 d . . . C18 C 0.3090(3) 0.86454(19) 0.3680(2) 0.0162(8) Uani 1 1 d . . . C19 C 0.4685(3) 0.77930(18) 0.5096(2) 0.0132(7) Uani 1 1 d . . . C20 C 0.5716(3) 0.7692(2) 0.5358(3) 0.0199(9) Uani 1 1 d . . . H20 H 0.6267 0.7905 0.5104 0.024 Uiso 1 1 calc R . . C21 C 0.5903(3) 0.7264(2) 0.6008(3) 0.0239(9) Uani 1 1 d . . . C22 C 0.5096(3) 0.6949(2) 0.6380(3) 0.0217(9) Uani 1 1 d . . . C23 C 0.4089(3) 0.70659(19) 0.6061(2) 0.0160(8) Uani 1 1 d . . . C24 C 0.3122(3) 0.6772(2) 0.6283(3) 0.0173(8) Uani 1 1 d . . . C25 C 0.2809(3) 0.6324(2) 0.6844(3) 0.0178(8) Uani 1 1 d . . . H25 H 0.3229 0.6098 0.7254 0.021 Uiso 1 1 calc R . . C26 C 0.1043(3) 0.5859(2) 0.7091(3) 0.0230(9) Uani 1 1 d . . . H26A H 0.0439 0.6115 0.7250 0.028 Uiso 1 1 calc R . . H26B H 0.1387 0.5679 0.7609 0.028 Uiso 1 1 calc R . . C27 C 0.0661(4) 0.5314(2) 0.6521(3) 0.0274(10) Uani 1 1 d . . . H27A H 0.0093 0.5086 0.6787 0.033 Uiso 1 1 calc R . . H27B H 0.0367 0.5497 0.5986 0.033 Uiso 1 1 calc R . . C28 C 0.1091(6) 0.4278(3) 0.5802(4) 0.0517(16) Uani 1 1 d . . . H28A H 0.0514 0.4073 0.6073 0.078 Uiso 1 1 calc R . . H28B H 0.1651 0.3966 0.5743 0.078 Uiso 1 1 calc R . . H28C H 0.0844 0.4434 0.5247 0.078 Uiso 1 1 calc R . . C29 C 0.1501(4) 0.4838(2) 0.6335(3) 0.0330(11) Uani 1 1 d . . . H29A H 0.1822 0.4672 0.6870 0.040 Uiso 1 1 calc R . . H29B H 0.2050 0.5060 0.6039 0.040 Uiso 1 1 calc R . . C30 C 0.3709(7) 0.4781(5) 0.4543(5) 0.081(3) Uani 1 1 d . . . H30A H 0.4067 0.4401 0.4345 0.122 Uiso 1 1 calc R . . H30B H 0.3566 0.4725 0.5133 0.122 Uiso 1 1 calc R . . H30C H 0.4152 0.5158 0.4484 0.122 Uiso 1 1 calc R . . C31 C 0.2741(6) 0.4869(3) 0.4051(4) 0.0560(17) Uani 1 1 d . . . H31A H 0.2359 0.5229 0.4293 0.067 Uiso 1 1 calc R . . H31B H 0.2313 0.4479 0.4104 0.067 Uiso 1 1 calc R . . C32 C 0.2837(4) 0.4999(2) 0.3146(4) 0.0362(12) Uani 1 1 d . . . H32A H 0.2130 0.4988 0.2864 0.043 Uiso 1 1 calc R . . H32B H 0.3240 0.4645 0.2911 0.043 Uiso 1 1 calc R . . C33 C 0.3344(3) 0.5623(2) 0.2921(3) 0.0233(9) Uani 1 1 d . . . H33A H 0.4078 0.5625 0.3146 0.028 Uiso 1 1 calc R . . H33B H 0.3340 0.5662 0.2304 0.028 Uiso 1 1 calc R . . C34 C 0.2306(3) 0.87210(19) 0.6224(2) 0.0177(8) Uani 1 1 d . . . H34 H 0.2980 0.8728 0.6503 0.021 Uiso 1 1 calc R . . C35 C 0.1509(3) 0.9142(2) 0.6389(3) 0.0222(9) Uani 1 1 d . . . H35 H 0.1537 0.9480 0.6786 0.027 Uiso 1 1 calc R . . C36 C 0.0670(3) 0.8972(2) 0.5862(3) 0.0194(8) Uani 1 1 d . . . F1 F 0.4050(2) 0.97718(14) 0.66298(17) 0.0313(6) Uani 1 1 d . . . F2 F 0.5790(2) 0.95948(12) 0.68164(18) 0.0289(6) Uani 1 1 d . . . F3 F 0.4667(2) 0.87760(15) 0.6967(2) 0.0408(8) Uani 1 1 d . . . F4 F 0.4876(2) 0.91924(15) 0.56817(18) 0.0391(7) Uani 1 1 d . . . F5 F 0.9038(2) 0.93182(14) 0.3538(2) 0.0458(8) Uani 1 1 d . . . F6 F 1.0611(3) 0.98626(17) 0.3643(3) 0.0581(10) Uani 1 1 d . . . F7 F 0.9742(3) 0.9703(2) 0.2413(2) 0.0617(11) Uani 1 1 d . . . F8 F 1.0515(2) 0.88671(13) 0.31059(18) 0.0315(6) Uani 1 1 d . . . Fe1 Fe 0.25189(4) 0.76035(3) 0.49520(3) 0.01168(14) Uani 1 1 d . . . H1 H 0.141(4) 0.619(2) 0.265(3) 0.014(11) Uiso 1 1 d . . . H2 H 0.008(4) 0.915(2) 0.581(3) 0.009(10) Uiso 1 1 d . . . H3 H -0.095(4) 0.842(2) 0.475(3) 0.013(11) Uiso 1 1 d . . . H4 H -0.043(3) 0.701(2) 0.307(3) 0.012(11) Uiso 1 1 d . . . H5 H 0.408(4) 0.928(2) 0.315(3) 0.021(12) Uiso 1 1 d . . . H6 H 0.519(3) 0.666(2) 0.683(3) 0.016(11) Uiso 1 1 d . . . H7 H 0.239(4) 0.872(2) 0.350(3) 0.016(11) Uiso 1 1 d . . . H8 H -0.350(3) 0.707(2) 0.232(3) 0.013(11) Uiso 1 1 d . . . H9 H -0.378(4) 0.763(3) 0.303(3) 0.033(14) Uiso 1 1 d . . . N1 N 0.1781(3) 0.62783(16) 0.6683(2) 0.0174(7) Uani 1 1 d . . . N2 N 0.1434(3) 0.66625(16) 0.6056(2) 0.0173(7) Uani 1 1 d . . . N3 N 0.2253(3) 0.69675(16) 0.5813(2) 0.0153(7) Uani 1 1 d . . . N4 N 0.3902(2) 0.74906(15) 0.5429(2) 0.0138(6) Uani 1 1 d . . . N5 N 0.3251(2) 0.82033(16) 0.4265(2) 0.0137(6) Uani 1 1 d . . . N6 N 0.4319(2) 0.81978(16) 0.4444(2) 0.0143(7) Uani 1 1 d . . . N7 N 0.7719(4) 0.8792(2) 0.5921(3) 0.0406(11) Uani 1 1 d . . . N8 N 0.1140(2) 0.76796(15) 0.4457(2) 0.0136(6) Uani 1 1 d . . . N9 N 0.2008(2) 0.83094(16) 0.5630(2) 0.0145(7) Uani 1 1 d . . . N10 N 0.0981(2) 0.84650(15) 0.5411(2) 0.0149(7) Uani 1 1 d . . . N11 N 0.2557(2) 0.69357(16) 0.4105(2) 0.0147(7) Uani 1 1 d . . . N12 N 0.3256(2) 0.65217(16) 0.3898(2) 0.0166(7) Uani 1 1 d . . . N13 N 0.2794(3) 0.61762(17) 0.3262(2) 0.0174(7) Uani 1 1 d . . . O1 O 0.7691(2) 0.71743(16) 0.5770(2) 0.0257(7) Uani 1 1 d . . . O2 O 0.7172(3) 0.6868(3) 0.7017(3) 0.0699(17) Uani 1 1 d . . . O3 O -0.2630(2) 0.81338(15) 0.3887(2) 0.0233(7) Uani 1 1 d . . . O4 O -0.2329(2) 0.72657(15) 0.3109(2) 0.0264(7) Uani 1 1 d . . . 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 B1 0.017(2) 0.019(2) 0.025(2) 0.0005(19) -0.0037(19) 0.0012(18) B2 0.020(2) 0.017(2) 0.040(3) 0.003(2) -0.004(2) -0.0006(19) C1 0.0156(19) 0.021(2) 0.021(2) -0.0034(17) -0.0018(16) 0.0042(16) C2 0.0076(17) 0.019(2) 0.0178(19) 0.0016(15) -0.0017(14) -0.0005(14) C3 0.0127(17) 0.0129(19) 0.0166(18) 0.0004(14) 0.0014(14) 0.0008(14) C4 0.0156(19) 0.0130(19) 0.020(2) 0.0010(15) -0.0030(15) -0.0042(15) C5 0.0104(17) 0.017(2) 0.0196(19) 0.0043(15) -0.0017(15) -0.0020(14) C6 0.0105(18) 0.0145(19) 0.023(2) 0.0006(16) 0.0005(15) 0.0028(15) C7 0.0150(18) 0.0102(17) 0.0158(18) 0.0012(14) 0.0044(15) 0.0001(14) C8 0.0112(18) 0.023(2) 0.0178(19) 0.0031(16) 0.0009(15) 0.0005(15) C9 0.026(3) 0.068(4) 0.058(4) -0.020(3) 0.005(3) -0.014(3) C10 0.010(2) 0.045(3) 0.042(3) -0.019(2) -0.0095(19) 0.0018(19) C11 0.013(2) 0.048(3) 0.039(3) 0.021(2) -0.0072(19) -0.005(2) C12 0.0109(19) 0.028(2) 0.048(3) 0.013(2) -0.0034(19) 0.0016(17) C13 0.016(2) 0.036(3) 0.040(3) 0.004(2) -0.0054(19) 0.0002(19) C14 0.022(2) 0.033(3) 0.028(2) -0.007(2) 0.0010(19) 0.0067(19) C15 0.039(3) 0.045(3) 0.040(3) 0.010(3) -0.002(2) 0.005(2) C16 0.0152(19) 0.019(2) 0.019(2) 0.0024(16) 0.0044(16) -0.0043(15) C17 0.019(2) 0.017(2) 0.0184(19) 0.0056(16) 0.0035(16) 0.0005(16) C18 0.0162(19) 0.0157(19) 0.0166(19) -0.0032(15) -0.0004(15) 0.0009(15) C19 0.0102(17) 0.0118(17) 0.0175(18) -0.0009(14) 0.0001(14) -0.0014(13) C20 0.0110(18) 0.026(2) 0.023(2) 0.0030(17) 0.0000(15) -0.0041(16) C21 0.015(2) 0.029(2) 0.028(2) 0.0077(18) -0.0046(17) -0.0019(17) C22 0.0103(18) 0.030(2) 0.024(2) 0.0115(19) -0.0041(16) -0.0010(16) C23 0.0125(18) 0.018(2) 0.0176(19) 0.0027(15) 0.0006(15) -0.0017(15) C24 0.0123(18) 0.019(2) 0.020(2) 0.0009(16) -0.0015(15) -0.0011(15) C25 0.0115(18) 0.018(2) 0.023(2) 0.0035(16) -0.0002(15) -0.0016(15) C26 0.0148(19) 0.026(2) 0.029(2) 0.0081(18) 0.0078(17) -0.0033(17) C27 0.022(2) 0.028(2) 0.032(2) 0.007(2) -0.0002(19) -0.0100(18) C28 0.075(5) 0.032(3) 0.046(3) -0.005(3) -0.006(3) -0.018(3) C29 0.038(3) 0.031(3) 0.029(3) -0.002(2) 0.003(2) -0.010(2) C30 0.072(5) 0.120(8) 0.051(4) -0.005(5) 0.001(4) 0.030(5) C31 0.065(4) 0.037(3) 0.068(4) 0.008(3) 0.018(4) 0.009(3) C32 0.032(3) 0.025(2) 0.052(3) -0.002(2) 0.007(2) 0.009(2) C33 0.019(2) 0.024(2) 0.027(2) -0.0081(18) 0.0038(18) 0.0048(17) C34 0.0165(19) 0.019(2) 0.0175(19) -0.0007(16) -0.0034(15) -0.0043(16) C35 0.024(2) 0.017(2) 0.025(2) -0.0050(17) -0.0013(18) -0.0038(17) C36 0.016(2) 0.016(2) 0.026(2) -0.0028(17) 0.0013(17) 0.0026(16) F1 0.0248(14) 0.0359(16) 0.0321(15) -0.0102(12) -0.0067(11) 0.0122(12) F2 0.0230(13) 0.0205(13) 0.0418(16) 0.0043(11) -0.0088(12) -0.0037(11) F3 0.0210(14) 0.0404(17) 0.059(2) 0.0279(15) -0.0150(13) -0.0087(12) F4 0.0479(19) 0.0418(18) 0.0271(15) -0.0107(13) -0.0013(13) 0.0124(14) F5 0.0357(17) 0.0283(16) 0.076(2) 0.0127(16) 0.0267(16) 0.0052(13) F6 0.0414(19) 0.046(2) 0.085(3) -0.0341(19) -0.0111(18) 0.0011(16) F7 0.046(2) 0.071(3) 0.067(3) 0.033(2) -0.0036(18) 0.0058(19) F8 0.0288(15) 0.0217(14) 0.0448(17) -0.0059(12) 0.0093(12) 0.0022(11) Fe1 0.0074(2) 0.0122(3) 0.0154(3) 0.0010(2) 0.00009(19) 0.0000(2) N1 0.0140(16) 0.0187(17) 0.0200(17) 0.0030(14) 0.0046(13) 0.0010(13) N2 0.0105(15) 0.0170(17) 0.0247(18) 0.0028(14) 0.0024(13) -0.0005(13) N3 0.0114(15) 0.0151(16) 0.0195(17) 0.0018(13) 0.0013(13) -0.0011(12) N4 0.0137(15) 0.0109(16) 0.0165(15) -0.0017(12) -0.0003(12) -0.0021(12) N5 0.0082(15) 0.0187(17) 0.0141(15) 0.0001(13) 0.0005(12) 0.0005(12) N6 0.0075(15) 0.0178(17) 0.0177(16) 0.0025(13) 0.0001(12) -0.0016(12) N7 0.041(3) 0.036(3) 0.044(3) -0.002(2) -0.004(2) 0.012(2) N8 0.0108(14) 0.0137(16) 0.0162(16) 0.0040(13) 0.0011(12) -0.0013(12) N9 0.0083(15) 0.0157(16) 0.0194(16) 0.0028(13) -0.0001(12) -0.0019(12) N10 0.0095(15) 0.0137(16) 0.0215(17) -0.0006(13) 0.0003(13) 0.0015(12) N11 0.0093(15) 0.0151(16) 0.0197(17) 0.0003(13) 0.0015(13) -0.0003(12) N12 0.0097(15) 0.0201(18) 0.0201(17) -0.0042(14) 0.0006(13) 0.0004(13) N13 0.0104(15) 0.0199(17) 0.0218(17) -0.0044(14) 0.0000(13) -0.0008(13) O1 0.0114(14) 0.0307(17) 0.0346(18) 0.0097(14) -0.0022(13) 0.0010(12) O2 0.0137(17) 0.133(5) 0.062(3) 0.071(3) -0.0075(18) -0.007(2) O3 0.0109(13) 0.0262(16) 0.0324(17) -0.0050(13) -0.0016(12) 0.0008(12) O4 0.0107(14) 0.0307(18) 0.0369(18) -0.0114(14) -0.0069(13) 0.0033(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 B1 F4 1.361(6) . ? B1 F1 1.386(5) . ? B1 F2 1.393(5) . ? B1 F3 1.410(6) . ? B2 F6 1.360(6) . ? B2 F5 1.380(6) . ? B2 F7 1.397(6) . ? B2 F8 1.397(6) . ? C1 N13 1.346(5) . ? C1 C2 1.361(6) . ? C1 H1 0.90(5) . ? C2 N11 1.372(5) . ? C2 C3 1.467(5) . ? C3 N8 1.350(5) . ? C3 C4 1.384(5) . ? C4 C5 1.402(6) . ? C4 H4 0.95(4) . ? C5 C6 1.384(6) . ? C5 C8 1.503(5) . ? C6 C7 1.383(5) . ? C6 H3 0.89(5) . ? C7 N8 1.331(5) . ? C7 N10 1.399(5) . ? C8 O3 1.198(5) . ? C8 O4 1.334(5) . ? C9 C10 1.492(9) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 O4 1.457(5) . ? C10 H8 0.95(5) . ? C10 H9 1.01(6) . ? C11 O2 1.188(6) . ? C11 O1 1.329(6) . ? C11 C21 1.512(6) . ? C12 O1 1.462(5) . ? C12 C13 1.504(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 N7 1.131(6) . ? C14 C15 1.448(7) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.356(6) . ? C16 N6 1.362(5) . ? C16 H16 0.9500 . ? C17 C18 1.406(6) . ? C17 H5 0.90(5) . ? C18 N5 1.322(5) . ? C18 H7 0.95(5) . ? C19 N4 1.328(5) . ? C19 C20 1.383(5) . ? C19 N6 1.401(5) . ? C20 C21 1.381(6) . ? C20 H20 0.9500 . ? C21 C22 1.393(6) . ? C22 C23 1.385(5) . ? C22 H6 0.93(5) . ? C23 N4 1.355(5) . ? C23 C24 1.451(5) . ? C24 N3 1.370(5) . ? C24 C25 1.374(6) . ? C25 N1 1.335(5) . ? C25 H25 0.9500 . ? C26 N1 1.474(5) . ? C26 C27 1.520(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C29 1.512(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.523(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.444(10) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.487(9) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.511(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 N13 1.476(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 N9 1.321(5) . ? C34 C35 1.389(6) . ? C34 H34 0.9500 . ? C35 C36 1.374(6) . ? C35 H35 0.9500 . ? C36 N10 1.356(5) . ? C36 H2 0.84(5) . ? Fe1 N8 1.905(3) . ? Fe1 N4 1.907(3) . ? Fe1 N11 1.947(3) . ? Fe1 N5 1.947(3) . ? Fe1 N3 1.959(3) . ? Fe1 N9 1.967(3) . ? N1 N2 1.340(5) . ? N2 N3 1.310(5) . ? N5 N6 1.386(4) . ? N9 N10 1.385(4) . ? N11 N12 1.306(5) . ? N12 N13 1.355(5) . ? 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 F4 B1 F1 110.4(4) . . ? F4 B1 F2 110.5(4) . . ? F1 B1 F2 109.5(4) . . ? F4 B1 F3 109.6(4) . . ? F1 B1 F3 109.2(4) . . ? F2 B1 F3 107.6(3) . . ? F6 B2 F5 115.6(5) . . ? F6 B2 F7 107.9(4) . . ? F5 B2 F7 105.9(4) . . ? F6 B2 F8 109.4(4) . . ? F5 B2 F8 109.4(4) . . ? F7 B2 F8 108.4(4) . . ? N13 C1 C2 104.9(4) . . ? N13 C1 H1 122(3) . . ? C2 C1 H1 133(3) . . ? C1 C2 N11 107.3(3) . . ? C1 C2 C3 138.2(4) . . ? N11 C2 C3 114.4(3) . . ? N8 C3 C4 121.2(4) . . ? N8 C3 C2 109.6(3) . . ? C4 C3 C2 129.1(4) . . ? C3 C4 C5 117.6(4) . . ? C3 C4 H4 119(3) . . ? C5 C4 H4 123(3) . . ? C6 C5 C4 121.2(4) . . ? C6 C5 C8 116.3(4) . . ? C4 C5 C8 122.5(4) . . ? C7 C6 C5 116.9(4) . . ? C7 C6 H3 118(3) . . ? C5 C6 H3 125(3) . . ? N8 C7 C6 123.0(4) . . ? N8 C7 N10 111.6(3) . . ? C6 C7 N10 125.4(4) . . ? O3 C8 O4 125.1(4) . . ? O3 C8 C5 123.5(4) . . ? O4 C8 C5 111.4(3) . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O4 C10 C9 109.0(4) . . ? O4 C10 H8 106(3) . . ? C9 C10 H8 108(3) . . ? O4 C10 H9 108(3) . . ? C9 C10 H9 108(3) . . ? H8 C10 H9 118(4) . . ? O2 C11 O1 125.2(4) . . ? O2 C11 C21 122.5(5) . . ? O1 C11 C21 112.3(4) . . ? O1 C12 C13 111.5(4) . . ? O1 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? O1 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N7 C14 C15 179.3(6) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N6 107.1(4) . . ? C17 C16 H16 126.5 . . ? N6 C16 H16 126.5 . . ? C16 C17 C18 106.4(4) . . ? C16 C17 H5 129(3) . . ? C18 C17 H5 124(3) . . ? N5 C18 C17 110.8(4) . . ? N5 C18 H7 117(3) . . ? C17 C18 H7 133(3) . . ? N4 C19 C20 122.9(4) . . ? N4 C19 N6 110.9(3) . . ? C20 C19 N6 126.2(4) . . ? C21 C20 C19 116.6(4) . . ? C21 C20 H20 121.7 . . ? C19 C20 H20 121.7 . . ? C20 C21 C22 121.8(4) . . ? C20 C21 C11 122.6(4) . . ? C22 C21 C11 115.5(4) . . ? C23 C22 C21 117.7(4) . . ? C23 C22 H6 118(3) . . ? C21 C22 H6 124(3) . . ? N4 C23 C22 120.6(4) . . ? N4 C23 C24 110.1(3) . . ? C22 C23 C24 129.2(4) . . ? N3 C24 C25 107.4(3) . . ? N3 C24 C23 115.0(4) . . ? C25 C24 C23 137.5(4) . . ? N1 C25 C24 104.4(4) . . ? N1 C25 H25 127.8 . . ? C24 C25 H25 127.8 . . ? N1 C26 C27 111.9(4) . . ? N1 C26 H26A 109.2 . . ? C27 C26 H26A 109.2 . . ? N1 C26 H26B 109.2 . . ? C27 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C29 C27 C26 113.7(4) . . ? C29 C27 H27A 108.8 . . ? C26 C27 H27A 108.8 . . ? C29 C27 H27B 108.8 . . ? C26 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 C28 112.9(5) . . ? C27 C29 H29A 109.0 . . ? C28 C29 H29A 109.0 . . ? C27 C29 H29B 109.0 . . ? C28 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C30 C31 C32 115.7(6) . . ? C30 C31 H31A 108.4 . . ? C32 C31 H31A 108.4 . . ? C30 C31 H31B 108.4 . . ? C32 C31 H31B 108.4 . . ? H31A C31 H31B 107.4 . . ? C31 C32 C33 116.9(5) . . ? C31 C32 H32A 108.1 . . ? C33 C32 H32A 108.1 . . ? C31 C32 H32B 108.1 . . ? C33 C32 H32B 108.1 . . ? H32A C32 H32B 107.3 . . ? N13 C33 C32 111.3(4) . . ? N13 C33 H33A 109.4 . . ? C32 C33 H33A 109.4 . . ? N13 C33 H33B 109.4 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? N9 C34 C35 111.3(4) . . ? N9 C34 H34 124.4 . . ? C35 C34 H34 124.4 . . ? C36 C35 C34 106.4(4) . . ? C36 C35 H35 126.8 . . ? C34 C35 H35 126.8 . . ? N10 C36 C35 106.3(4) . . ? N10 C36 H2 125(3) . . ? C35 C36 H2 128(3) . . ? N8 Fe1 N4 177.53(14) . . ? N8 Fe1 N11 80.38(14) . . ? N4 Fe1 N11 97.32(13) . . ? N8 Fe1 N5 100.53(13) . . ? N4 Fe1 N5 80.40(14) . . ? N11 Fe1 N5 91.99(14) . . ? N8 Fe1 N3 98.65(14) . . ? N4 Fe1 N3 80.42(14) . . ? N11 Fe1 N3 90.94(14) . . ? N5 Fe1 N3 160.82(14) . . ? N8 Fe1 N9 80.37(14) . . ? N4 Fe1 N9 101.94(13) . . ? N11 Fe1 N9 160.74(13) . . ? N5 Fe1 N9 91.07(14) . . ? N3 Fe1 N9 92.38(14) . . ? C25 N1 N2 112.5(3) . . ? C25 N1 C26 127.9(4) . . ? N2 N1 C26 119.6(3) . . ? N3 N2 N1 106.0(3) . . ? N2 N3 C24 109.7(3) . . ? N2 N3 Fe1 135.8(3) . . ? C24 N3 Fe1 114.6(3) . . ? C19 N4 C23 120.4(3) . . ? C19 N4 Fe1 119.5(3) . . ? C23 N4 Fe1 119.9(3) . . ? C18 N5 N6 105.2(3) . . ? C18 N5 Fe1 142.0(3) . . ? N6 N5 Fe1 112.7(2) . . ? C16 N6 N5 110.5(3) . . ? C16 N6 C19 132.9(3) . . ? N5 N6 C19 116.2(3) . . ? C7 N8 C3 120.1(3) . . ? C7 N8 Fe1 119.3(3) . . ? C3 N8 Fe1 120.4(3) . . ? C34 N9 N10 105.1(3) . . ? C34 N9 Fe1 142.4(3) . . ? N10 N9 Fe1 112.5(2) . . ? C36 N10 N9 110.9(3) . . ? C36 N10 C7 133.0(3) . . ? N9 N10 C7 116.1(3) . . ? N12 N11 C2 110.5(3) . . ? N12 N11 Fe1 134.3(3) . . ? C2 N11 Fe1 115.2(3) . . ? N11 N12 N13 105.4(3) . . ? C1 N13 N12 111.8(3) . . ? C1 N13 C33 128.2(4) . . ? N12 N13 C33 119.7(3) . . ? C11 O1 C12 114.9(4) . . ? C8 O4 C10 115.9(3) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.144 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.106 # Attachment '- rc35.cif' data_rc35 _database_code_depnum_ccdc_archive 'CCDC 772649' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H34 Cl2 Fe N14 O8' _chemical_formula_sum 'C28 H34 Cl2 Fe N14 O8' _chemical_formula_weight 821.44 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9124(13) _cell_length_b 12.0189(13) _cell_length_c 14.8282(16) _cell_angle_alpha 66.581(2) _cell_angle_beta 76.138(2) _cell_angle_gamma 62.629(2) _cell_volume 1725.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3991 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 25.98 _exptl_crystal_description trigonal _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 0.663 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8158 _exptl_absorpt_correction_T_max 0.9740 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13450 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0936 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6680 _reflns_number_gt 4736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0800P)^2^+2.3942P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6680 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1241 _refine_ls_R_factor_gt 0.0873 _refine_ls_wR_factor_ref 0.1948 _refine_ls_wR_factor_gt 0.1783 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _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 C1 C 0.4986(6) 0.6533(6) 0.4611(4) 0.0252(13) Uani 1 1 d . . . H1 H 0.4430 0.6613 0.5164 0.030 Uiso 1 1 calc R . . C2 C 0.6286(6) 0.5785(6) 0.4640(4) 0.0273(14) Uani 1 1 d . . . H2 H 0.6750 0.5293 0.5196 0.033 Uiso 1 1 calc R . . C3 C 0.6737(5) 0.5920(6) 0.3691(4) 0.0253(13) Uani 1 1 d . . . H3 H 0.7578 0.5529 0.3468 0.030 Uiso 1 1 calc R . . C4 C 0.6712(5) 0.6895(5) 0.1468(4) 0.0197(12) Uani 1 1 d . . . H4 H 0.7508 0.6311 0.1703 0.024 Uiso 1 1 calc R . . C5 C 0.6533(5) 0.7462(6) 0.0445(4) 0.0228(13) Uani 1 1 d . . . C6 C 0.5302(5) 0.8349(6) 0.0138(4) 0.0212(12) Uani 1 1 d . . . H6 H 0.5149 0.8737 -0.0527 0.025 Uiso 1 1 calc R . . C7 C 0.4334(5) 0.8623(5) 0.0849(4) 0.0190(12) Uani 1 1 d . . . C8 C 0.5665(5) 0.7242(5) 0.2093(4) 0.0196(12) Uani 1 1 d . . . C9 C 0.2365(5) 1.0276(6) -0.0179(4) 0.0232(13) Uani 1 1 d . . . H9 H 0.2690 1.0373 -0.0829 0.028 Uiso 1 1 calc R . . C10 C 0.3010(5) 0.9517(5) 0.0649(4) 0.0188(12) Uani 1 1 d . . . C11 C -0.1165(5) 1.2162(6) 0.0185(4) 0.0290(14) Uani 1 1 d . . . H11A H -0.1126 1.2684 0.0526 0.035 Uiso 1 1 calc R . . H11B H -0.1259 1.1379 0.0675 0.035 Uiso 1 1 calc R . . C12 C 0.0046(5) 1.1745(6) -0.0451(4) 0.0303(14) Uani 1 1 d . . . H12A H -0.0026 1.1293 -0.0835 0.036 Uiso 1 1 calc R . . H12B H 0.0171 1.2530 -0.0905 0.036 Uiso 1 1 calc R . . C13 C -0.2306(5) 1.2984(6) -0.0446(4) 0.0308(14) Uani 1 1 d . . . H13A H -0.2234 1.3791 -0.0910 0.037 Uiso 1 1 calc R . . H13B H -0.2310 1.2481 -0.0820 0.037 Uiso 1 1 calc R . . C14 C -0.3543(6) 1.3341(8) 0.0185(5) 0.0484(19) Uani 1 1 d . . . H14C H -0.3583 1.2547 0.0681 0.073 Uiso 1 1 calc R . . H14D H -0.4242 1.3778 -0.0221 0.073 Uiso 1 1 calc R . . H14E H -0.3583 1.3925 0.0496 0.073 Uiso 1 1 calc R . . C15 C 0.0522(5) 0.6648(6) 0.4631(4) 0.0274(14) Uani 1 1 d . . . H15 H 0.0041 0.6488 0.5224 0.033 Uiso 1 1 calc R . . C16 C 0.0664(5) 0.6195(6) 0.3884(4) 0.0260(13) Uani 1 1 d . . . H16 H 0.0304 0.5664 0.3862 0.031 Uiso 1 1 calc R . . C17 C 0.1455(5) 0.6691(6) 0.3165(4) 0.0231(13) Uani 1 1 d . . . H17 H 0.1710 0.6535 0.2567 0.028 Uiso 1 1 calc R . . C18 C 0.1372(5) 0.8118(5) 0.4809(4) 0.0196(12) Uani 1 1 d . . . C19 C 0.0893(5) 0.8090(6) 0.5752(4) 0.0225(13) Uani 1 1 d . . . H19 H 0.0461 0.7558 0.6126 0.027 Uiso 1 1 calc R . . C20 C 0.1070(5) 0.8876(6) 0.6133(4) 0.0238(13) Uani 1 1 d . . . C21 C 0.1745(5) 0.9664(6) 0.5529(4) 0.0228(13) Uani 1 1 d . . . H21 H 0.1883 1.0202 0.5760 0.027 Uiso 1 1 calc R . . C22 C 0.2187(5) 0.9610(5) 0.4594(4) 0.0209(12) Uani 1 1 d . . . C23 C 0.2853(5) 1.0398(5) 0.3872(4) 0.0214(12) Uani 1 1 d . . . C24 C 0.3250(5) 1.1279(6) 0.3876(4) 0.0239(13) Uani 1 1 d . . . H24 H 0.3190 1.1549 0.4399 0.029 Uiso 1 1 calc R . . C25 C 0.4394(6) 1.2587(6) 0.2523(4) 0.0273(14) Uani 1 1 d . . . H25A H 0.4073 1.3197 0.1886 0.033 Uiso 1 1 calc R . . H25B H 0.5294 1.2077 0.2420 0.033 Uiso 1 1 calc R . . C26 C 0.4201(6) 1.3376(6) 0.3168(4) 0.0316(14) Uani 1 1 d . . . H26A H 0.4557 1.2774 0.3796 0.038 Uiso 1 1 calc R . . H26B H 0.3301 1.3865 0.3294 0.038 Uiso 1 1 calc R . . C27 C 0.4844(6) 1.4358(6) 0.2664(4) 0.0319(15) Uani 1 1 d . . . H27A H 0.4590 1.4857 0.1995 0.038 Uiso 1 1 calc R . . H27B H 0.4555 1.4984 0.3014 0.038 Uiso 1 1 calc R . . C28 C 0.6273(6) 1.3658(6) 0.2644(5) 0.0358(16) Uani 1 1 d . . . H28A H 0.6531 1.3200 0.3307 0.054 Uiso 1 1 calc R . . H28B H 0.6632 1.4300 0.2308 0.054 Uiso 1 1 calc R . . H28C H 0.6563 1.3030 0.2305 0.054 Uiso 1 1 calc R . . Cl1 Cl 0.95420(13) 0.57166(14) 0.79778(10) 0.0269(4) Uani 1 1 d . . . Cl3 Cl 0.75722(16) 0.87959(16) 0.28945(11) 0.0375(4) Uani 1 1 d . . . Fe1 Fe 0.29441(7) 0.86020(8) 0.28709(5) 0.0171(2) Uani 1 1 d . . . N5 N 0.7514(5) 0.7150(5) -0.0208(3) 0.0310(12) Uani 1 1 d . . . H1A H 0.7401 0.7490 -0.0828 0.037 Uiso 1 1 calc R . . H1B H 0.8259 0.6607 -0.0009 0.037 Uiso 1 1 calc R . . N2 N 0.4488(4) 0.8064(4) 0.1825(3) 0.0179(10) Uani 1 1 d . . . N3 N 0.5738(4) 0.6728(4) 0.3126(3) 0.0196(10) Uani 1 1 d . . . N4 N 0.4639(4) 0.7122(4) 0.3686(3) 0.0207(10) Uani 1 1 d . . . N1 N 0.2160(4) 0.9681(5) 0.1437(3) 0.0213(10) Uani 1 1 d . . . N6 N 0.1029(4) 1.0492(5) 0.1128(3) 0.0259(11) Uani 1 1 d . . . N7 N 0.1156(4) 1.0855(5) 0.0146(3) 0.0236(11) Uani 1 1 d . . . N9 N 0.1812(4) 0.7412(5) 0.3420(3) 0.0222(10) Uani 1 1 d . . . N10 N 0.1225(4) 0.7384(5) 0.4335(3) 0.0212(10) Uani 1 1 d . . . N11 N 0.3149(4) 1.0271(4) 0.2961(3) 0.0203(10) Uani 1 1 d . . . N12 N 0.3683(4) 1.1077(4) 0.2397(3) 0.0208(10) Uani 1 1 d . . . N13 N 0.3755(4) 1.1684(5) 0.2952(3) 0.0220(10) Uani 1 1 d . . . N8 N 0.2000(4) 0.8855(4) 0.4230(3) 0.0191(10) Uani 1 1 d . . . N14 N 0.0611(4) 0.8917(5) 0.7046(3) 0.0282(12) Uani 1 1 d . . . H14A H 0.0196 0.8448 0.7409 0.034 Uiso 1 1 calc R . . H14B H 0.0733 0.9412 0.7267 0.034 Uiso 1 1 calc R . . O1 O 0.7465(5) 0.8354(5) 0.3940(3) 0.0460(13) Uani 1 1 d . . . O2 O 0.6354(6) 0.9456(7) 0.2513(4) 0.090(2) Uani 1 1 d . . . O3 O 0.8245(4) 0.7694(5) 0.2546(3) 0.0445(12) Uani 1 1 d . . . O4 O 0.8204(8) 0.9625(7) 0.2523(4) 0.094(3) Uani 1 1 d . . . O5 O 0.9192(4) 0.7050(4) 0.7907(3) 0.0376(11) Uani 1 1 d . . . O6 O 1.0414(4) 0.5436(4) 0.7172(3) 0.0468(13) Uani 1 1 d . . . O7 O 1.0097(5) 0.4815(5) 0.8888(3) 0.0516(13) Uani 1 1 d . . . O8 O 0.8440(4) 0.5565(5) 0.7934(4) 0.0530(14) Uani 1 1 d . . . 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 C1 0.031(3) 0.031(3) 0.009(3) -0.003(2) 0.000(2) -0.013(3) C2 0.028(3) 0.033(4) 0.015(3) -0.006(3) -0.001(2) -0.009(3) C3 0.020(3) 0.027(3) 0.019(3) -0.005(3) 0.004(2) -0.007(3) C4 0.016(3) 0.020(3) 0.016(3) -0.005(2) 0.003(2) -0.005(2) C5 0.022(3) 0.025(3) 0.022(3) -0.010(2) 0.008(2) -0.013(3) C6 0.027(3) 0.028(3) 0.009(3) -0.005(2) -0.001(2) -0.013(3) C7 0.019(3) 0.017(3) 0.015(3) -0.002(2) 0.001(2) -0.006(2) C8 0.026(3) 0.015(3) 0.013(3) -0.001(2) 0.002(2) -0.010(2) C9 0.025(3) 0.032(3) 0.008(3) -0.004(2) 0.006(2) -0.014(3) C10 0.021(3) 0.024(3) 0.009(2) -0.003(2) 0.004(2) -0.011(2) C11 0.029(3) 0.029(3) 0.021(3) -0.004(3) -0.004(3) -0.009(3) C12 0.029(3) 0.032(4) 0.014(3) 0.000(3) -0.004(2) -0.005(3) C13 0.027(3) 0.030(4) 0.024(3) -0.003(3) -0.001(3) -0.008(3) C14 0.030(4) 0.065(5) 0.039(4) -0.022(4) -0.002(3) -0.007(4) C15 0.026(3) 0.029(3) 0.024(3) -0.003(3) -0.002(2) -0.014(3) C16 0.028(3) 0.029(3) 0.022(3) -0.004(3) -0.004(2) -0.017(3) C17 0.024(3) 0.029(3) 0.017(3) -0.011(3) 0.000(2) -0.009(3) C18 0.016(3) 0.021(3) 0.015(3) -0.004(2) 0.000(2) -0.003(2) C19 0.020(3) 0.027(3) 0.018(3) -0.007(2) 0.004(2) -0.010(3) C20 0.017(3) 0.027(3) 0.020(3) -0.008(3) 0.005(2) -0.006(3) C21 0.021(3) 0.026(3) 0.018(3) -0.011(2) 0.004(2) -0.006(3) C22 0.016(3) 0.022(3) 0.018(3) -0.008(2) 0.004(2) -0.004(2) C23 0.021(3) 0.020(3) 0.016(3) -0.004(2) -0.001(2) -0.004(2) C24 0.023(3) 0.029(3) 0.019(3) -0.012(3) 0.003(2) -0.009(3) C25 0.028(3) 0.030(3) 0.021(3) -0.006(3) 0.007(2) -0.016(3) C26 0.035(4) 0.036(4) 0.025(3) -0.007(3) -0.002(3) -0.018(3) C27 0.042(4) 0.027(3) 0.028(3) -0.009(3) -0.001(3) -0.015(3) C28 0.042(4) 0.037(4) 0.029(3) -0.009(3) -0.002(3) -0.017(3) Cl1 0.0232(8) 0.0258(8) 0.0207(7) -0.0048(6) 0.0056(6) -0.0069(6) Cl3 0.0494(11) 0.0386(10) 0.0221(8) -0.0089(7) -0.0032(7) -0.0167(8) Fe1 0.0152(4) 0.0209(4) 0.0092(4) -0.0045(3) 0.0034(3) -0.0050(3) N5 0.024(3) 0.038(3) 0.015(2) -0.008(2) 0.007(2) -0.004(2) N2 0.015(2) 0.026(3) 0.009(2) -0.0040(19) 0.0039(17) -0.010(2) N3 0.017(2) 0.022(3) 0.015(2) -0.0023(19) 0.0003(18) -0.007(2) N4 0.018(2) 0.023(3) 0.017(2) -0.010(2) 0.0051(19) -0.005(2) N1 0.016(2) 0.027(3) 0.013(2) -0.007(2) 0.0016(18) -0.003(2) N6 0.023(3) 0.030(3) 0.015(2) -0.001(2) -0.001(2) -0.008(2) N7 0.027(3) 0.027(3) 0.009(2) 0.003(2) -0.0022(19) -0.011(2) N9 0.021(2) 0.026(3) 0.013(2) -0.005(2) -0.0011(19) -0.006(2) N10 0.013(2) 0.027(3) 0.014(2) -0.004(2) 0.0019(18) -0.005(2) N11 0.020(2) 0.023(3) 0.014(2) -0.006(2) 0.0045(19) -0.008(2) N12 0.017(2) 0.022(3) 0.017(2) -0.009(2) 0.0024(19) -0.003(2) N13 0.024(3) 0.024(3) 0.016(2) -0.006(2) 0.0034(19) -0.012(2) N8 0.016(2) 0.020(3) 0.014(2) -0.006(2) 0.0013(18) -0.003(2) N14 0.026(3) 0.041(3) 0.015(2) -0.012(2) 0.010(2) -0.015(2) O1 0.066(3) 0.065(3) 0.021(2) -0.016(2) 0.008(2) -0.042(3) O2 0.053(4) 0.106(5) 0.062(4) -0.039(4) -0.017(3) 0.021(4) O3 0.051(3) 0.048(3) 0.033(3) -0.022(2) 0.007(2) -0.016(3) O4 0.202(8) 0.112(5) 0.032(3) -0.032(3) 0.032(4) -0.127(6) O5 0.041(3) 0.032(3) 0.038(3) -0.017(2) 0.018(2) -0.019(2) O6 0.052(3) 0.032(3) 0.036(3) -0.013(2) 0.022(2) -0.013(2) O7 0.050(3) 0.052(3) 0.032(3) 0.002(2) -0.014(2) -0.012(3) O8 0.042(3) 0.057(3) 0.060(3) -0.009(3) -0.010(3) -0.025(3) _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 C1 N4 1.335(7) . ? C1 C2 1.389(8) . ? C1 H1 0.9300 . ? C2 C3 1.353(7) . ? C2 H2 0.9300 . ? C3 N3 1.353(7) . ? C3 H3 0.9300 . ? C4 C8 1.365(7) . ? C4 C5 1.418(7) . ? C4 H4 0.9300 . ? C5 N5 1.338(7) . ? C5 C6 1.411(8) . ? C6 C7 1.377(7) . ? C6 H6 0.9300 . ? C7 N2 1.349(6) . ? C7 C10 1.464(7) . ? C8 N2 1.335(7) . ? C8 N3 1.414(6) . ? C9 N7 1.343(7) . ? C9 C10 1.359(7) . ? C9 H9 0.9300 . ? C10 N1 1.365(6) . ? C11 C12 1.510(8) . ? C11 C13 1.530(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N7 1.478(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.519(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14C 0.9600 . ? C14 H14D 0.9600 . ? C14 H14E 0.9600 . ? C15 C16 1.362(8) . ? C15 N10 1.369(7) . ? C15 H15 0.9300 . ? C16 C17 1.382(7) . ? C16 H16 0.9300 . ? C17 N9 1.323(7) . ? C17 H17 0.9300 . ? C18 N8 1.333(7) . ? C18 C19 1.371(7) . ? C18 N10 1.413(7) . ? C19 C20 1.386(8) . ? C19 H19 0.9300 . ? C20 N14 1.345(6) . ? C20 C21 1.423(7) . ? C21 C22 1.375(7) . ? C21 H21 0.9300 . ? C22 N8 1.342(7) . ? C22 C23 1.466(7) . ? C23 C24 1.346(8) . ? C23 N11 1.363(6) . ? C24 N13 1.349(7) . ? C24 H24 0.9300 . ? C25 N13 1.463(7) . ? C25 C26 1.511(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.548(8) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.511(9) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? Cl1 O6 1.422(4) . ? Cl1 O8 1.426(5) . ? Cl1 O5 1.424(4) . ? Cl1 O7 1.428(5) . ? Cl3 O4 1.385(5) . ? Cl3 O1 1.419(4) . ? Cl3 O3 1.426(5) . ? Cl3 O2 1.426(6) . ? Fe1 N8 2.122(4) . ? Fe1 N2 2.131(4) . ? Fe1 N1 2.173(4) . ? Fe1 N11 2.186(4) . ? Fe1 N9 2.202(5) . ? Fe1 N4 2.204(5) . ? N5 H1A 0.8600 . ? N5 H1B 0.8600 . ? N3 N4 1.360(6) . ? N1 N6 1.307(6) . ? N6 N7 1.335(6) . ? N9 N10 1.365(6) . ? N11 N12 1.308(6) . ? N12 N13 1.336(6) . ? N14 H14A 0.8600 . ? N14 H14B 0.8600 . ? 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 N4 C1 C2 111.3(5) . . ? N4 C1 H1 124.4 . . ? C2 C1 H1 124.4 . . ? C3 C2 C1 105.7(5) . . ? C3 C2 H2 127.2 . . ? C1 C2 H2 127.2 . . ? N3 C3 C2 107.3(5) . . ? N3 C3 H3 126.4 . . ? C2 C3 H3 126.4 . . ? C8 C4 C5 117.1(5) . . ? C8 C4 H4 121.5 . . ? C5 C4 H4 121.5 . . ? N5 C5 C6 121.2(5) . . ? N5 C5 C4 120.3(5) . . ? C6 C5 C4 118.6(5) . . ? C7 C6 C5 118.1(5) . . ? C7 C6 H6 120.9 . . ? C5 C6 H6 120.9 . . ? N2 C7 C6 123.8(5) . . ? N2 C7 C10 111.6(4) . . ? C6 C7 C10 124.6(5) . . ? N2 C8 C4 125.7(5) . . ? N2 C8 N3 112.6(4) . . ? C4 C8 N3 121.6(5) . . ? N7 C9 C10 105.0(4) . . ? N7 C9 H9 127.5 . . ? C10 C9 H9 127.5 . . ? C9 C10 N1 107.6(5) . . ? C9 C10 C7 134.9(5) . . ? N1 C10 C7 117.6(4) . . ? C12 C11 C13 110.5(5) . . ? C12 C11 H11A 109.6 . . ? C13 C11 H11A 109.6 . . ? C12 C11 H11B 109.6 . . ? C13 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? N7 C12 C11 111.8(4) . . ? N7 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? N7 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C11 111.4(5) . . ? C14 C13 H13A 109.4 . . ? C11 C13 H13A 109.4 . . ? C14 C13 H13B 109.4 . . ? C11 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C13 C14 H14C 109.5 . . ? C13 C14 H14D 109.5 . . ? H14C C14 H14D 109.5 . . ? C13 C14 H14E 109.5 . . ? H14C C14 H14E 109.5 . . ? H14D C14 H14E 109.5 . . ? C16 C15 N10 106.5(5) . . ? C16 C15 H15 126.7 . . ? N10 C15 H15 126.7 . . ? C15 C16 C17 105.4(5) . . ? C15 C16 H16 127.3 . . ? C17 C16 H16 127.3 . . ? N9 C17 C16 112.7(5) . . ? N9 C17 H17 123.6 . . ? C16 C17 H17 123.6 . . ? N8 C18 C19 124.3(5) . . ? N8 C18 N10 112.5(4) . . ? C19 C18 N10 123.2(5) . . ? C18 C19 C20 118.2(5) . . ? C18 C19 H19 120.9 . . ? C20 C19 H19 120.9 . . ? N14 C20 C19 121.6(5) . . ? N14 C20 C21 120.0(5) . . ? C19 C20 C21 118.4(5) . . ? C22 C21 C20 118.4(5) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? N8 C22 C21 122.7(5) . . ? N8 C22 C23 112.3(4) . . ? C21 C22 C23 124.9(5) . . ? C24 C23 N11 108.6(5) . . ? C24 C23 C22 135.0(5) . . ? N11 C23 C22 116.4(5) . . ? C23 C24 N13 104.7(5) . . ? C23 C24 H24 127.6 . . ? N13 C24 H24 127.6 . . ? N13 C25 C26 112.5(4) . . ? N13 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? N13 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? C25 C26 C27 110.6(5) . . ? C25 C26 H26A 109.5 . . ? C27 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C28 C27 C26 112.3(5) . . ? C28 C27 H27A 109.1 . . ? C26 C27 H27A 109.1 . . ? C28 C27 H27B 109.1 . . ? C26 C27 H27B 109.1 . . ? H27A C27 H27B 107.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O6 Cl1 O8 108.8(3) . . ? O6 Cl1 O5 109.4(3) . . ? O8 Cl1 O5 109.2(3) . . ? O6 Cl1 O7 110.1(3) . . ? O8 Cl1 O7 109.1(3) . . ? O5 Cl1 O7 110.3(3) . . ? O4 Cl3 O1 110.7(3) . . ? O4 Cl3 O3 108.8(4) . . ? O1 Cl3 O3 110.6(3) . . ? O4 Cl3 O2 110.4(5) . . ? O1 Cl3 O2 110.8(3) . . ? O3 Cl3 O2 105.4(3) . . ? N8 Fe1 N2 158.14(17) . . ? N8 Fe1 N1 126.42(16) . . ? N2 Fe1 N1 74.04(16) . . ? N8 Fe1 N11 73.64(16) . . ? N2 Fe1 N11 99.09(16) . . ? N1 Fe1 N11 94.91(17) . . ? N8 Fe1 N9 73.14(17) . . ? N2 Fe1 N9 116.48(17) . . ? N1 Fe1 N9 94.59(17) . . ? N11 Fe1 N9 144.42(16) . . ? N8 Fe1 N4 87.58(16) . . ? N2 Fe1 N4 72.00(16) . . ? N1 Fe1 N4 145.94(16) . . ? N11 Fe1 N4 92.95(17) . . ? N9 Fe1 N4 98.03(16) . . ? C5 N5 H1A 120.0 . . ? C5 N5 H1B 120.0 . . ? H1A N5 H1B 120.0 . . ? C8 N2 C7 116.6(4) . . ? C8 N2 Fe1 122.1(3) . . ? C7 N2 Fe1 121.1(4) . . ? C3 N3 N4 111.3(4) . . ? C3 N3 C8 131.5(4) . . ? N4 N3 C8 117.2(4) . . ? C1 N4 N3 104.5(4) . . ? C1 N4 Fe1 139.3(4) . . ? N3 N4 Fe1 115.9(3) . . ? N6 N1 C10 109.5(4) . . ? N6 N1 Fe1 134.9(3) . . ? C10 N1 Fe1 115.6(3) . . ? N1 N6 N7 106.5(4) . . ? N6 N7 C9 111.4(4) . . ? N6 N7 C12 121.2(4) . . ? C9 N7 C12 127.3(4) . . ? C17 N9 N10 104.0(4) . . ? C17 N9 Fe1 142.0(4) . . ? N10 N9 Fe1 113.9(3) . . ? N9 N10 C15 111.3(4) . . ? N9 N10 C18 118.5(4) . . ? C15 N10 C18 130.1(4) . . ? N12 N11 C23 108.7(4) . . ? N12 N11 Fe1 135.5(3) . . ? C23 N11 Fe1 114.7(3) . . ? N11 N12 N13 106.9(4) . . ? N12 N13 C24 111.0(4) . . ? N12 N13 C25 118.7(4) . . ? C24 N13 C25 130.2(5) . . ? C18 N8 C22 118.0(4) . . ? C18 N8 Fe1 121.0(4) . . ? C22 N8 Fe1 120.2(3) . . ? C20 N14 H14A 120.0 . . ? C20 N14 H14B 120.0 . . ? H14A N14 H14B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.235 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.118