Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof. Keith S. Murray' _publ_contact_author_address ; School of Chemistry Monash University 3800 Australia ; _publ_contact_author_phone '+61 3 9905 4512' _publ_contact_author_fax '+61 3 9905 4597' _publ_contact_author_email keith.murray@sci.monash.edu.au _publ_section_title ; Structure, Magnetism and Photomagnetism of Mixed - Ligand Tris(pyrazolyl)methane Iron(II) Spin Crossover Compounds ; loop_ _publ_author_name _publ_author_address B.Moubaraki ; School of Chemistry Monash University VIC 3800 Australia ; B.A.Leita ; School of Chemistry Monash University VIC 3800 Australia ; S.R.Batten ; School of Chemistry Monash University 3800 Australia ; P.Jensen ; School of Chemistry Monash University 3800 Australia ; K.S.Murray ; School of Chemistry Monash University VIC 3800 Australia ; ; J.P.Smith ; ; School of Chemistry Monash University VIC 3800 Australia ; J.D.Cashion ; School of Physics Monash University VIC 3800 Australia ; C.J.Kepert ; School of Chemistry University of Sydney NSW 2006 Australia ; G.J.Halder ; School of Chemistry University of Sydney NSW 2006 Australia ; J.-F.Letard ; ICMCB UPR 9048 CNRS-Universite de Bourdeaux F33608 Pessac France ; #=END data_1a _database_code_depnum_ccdc_archive 'CCDC 650142' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H32 B2 F8 Fe N12' _chemical_formula_weight 742.11 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' 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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.1814(1) _cell_length_b 10.2364(2) _cell_length_c 18.8554(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.176(1) _cell_angle_gamma 90.00 _cell_volume 1574.91(5) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular block' _exptl_crystal_colour 'light purple' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.568 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7645 _exptl_absorpt_correction_T_max 0.9454 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _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 23027 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0702 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 27.86 _reflns_number_total 7361 _reflns_number_gt 5497 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0910P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.029(18) _refine_ls_number_reflns 7361 _refine_ls_number_parameters 448 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1521 _refine_ls_wR_factor_gt 0.1336 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.092 _refine_ls_shift/su_mean 0.010 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 0.07175(6) 0.62962(5) 0.23355(3) 0.01622(14) Uani 1 1 d . . . F1 F 0.5743(6) 0.1090(7) 0.5028(5) 0.183(3) Uani 1 1 d . . . F2 F 0.8043(7) 0.1608(8) 0.5365(3) 0.160(3) Uani 1 1 d . . . F3 F 0.6575(9) 0.3055(4) 0.4732(2) 0.130(2) Uani 1 1 d . . . F4 F 0.7709(11) 0.1269(4) 0.4259(2) 0.181(4) Uani 1 1 d . . . F5 F 0.3823(4) 0.0377(3) 0.15876(14) 0.0494(8) Uani 1 1 d . . . F6 F 0.1715(3) 0.0957(3) 0.08155(15) 0.0438(8) Uani 1 1 d . . . F7 F 0.4103(3) 0.2053(3) 0.08051(14) 0.0337(6) Uani 1 1 d . . . F8 F 0.3942(3) -0.0057(3) 0.04092(13) 0.0365(6) Uani 1 1 d . . . N9 N 0.2053(3) 0.6349(4) 0.15102(15) 0.0193(6) Uani 1 1 d . . . N10 N 0.2458(4) 0.5203(4) 0.12176(18) 0.0211(8) Uani 1 1 d . . . N7 N -0.0660(4) 0.4981(4) 0.18118(19) 0.0198(8) Uani 1 1 d . . . N8 N 0.0110(4) 0.4000(3) 0.14810(16) 0.0175(7) Uani 1 1 d . . . N11 N 0.2157(4) 0.4858(3) 0.27153(18) 0.0186(7) Uani 1 1 d . . . N12 N 0.2519(4) 0.3890(3) 0.22514(17) 0.0214(7) Uani 1 1 d . . . N5 N -0.0700(5) 0.7758(4) 0.19853(19) 0.0210(8) Uani 1 1 d . . . N6 N -0.1080(4) 0.8682(3) 0.24860(16) 0.0180(7) Uani 1 1 d . . . N1 N 0.2136(4) 0.7613(4) 0.28592(19) 0.0204(8) Uani 1 1 d . . . N2 N 0.1366(4) 0.8547(3) 0.32278(17) 0.0212(7) Uani 1 1 d . . . N3 N -0.0614(3) 0.6178(4) 0.31728(15) 0.0163(6) Uani 1 1 d . . . N4 N -0.0963(4) 0.7331(3) 0.35124(17) 0.0162(7) Uani 1 1 d . . . C20 C 0.2733(5) 0.7273(5) 0.1134(2) 0.0229(9) Uani 1 1 d . . . H20 H 0.2639 0.8185 0.1215 0.028 Uiso 1 1 calc R . . C21 C 0.3612(6) 0.6705(5) 0.0600(2) 0.0314(11) Uani 1 1 d . . . H21 H 0.4220 0.7150 0.0264 0.038 Uiso 1 1 calc R . . C22 C 0.3418(5) 0.5395(5) 0.0662(2) 0.0255(10) Uani 1 1 d . . . H22 H 0.3861 0.4739 0.0375 0.031 Uiso 1 1 calc R . . C17 C -0.2243(5) 0.4748(4) 0.1677(2) 0.0255(10) Uani 1 1 d . . . H17 H -0.3095 0.5268 0.1846 0.031 Uiso 1 1 calc R . . C18 C -0.2497(5) 0.3630(4) 0.1253(2) 0.0249(10) Uani 1 1 d . . . H18 H -0.3515 0.3267 0.1076 0.030 Uiso 1 1 calc R . . C19 C -0.0966(5) 0.3179(4) 0.1150(2) 0.0246(9) Uani 1 1 d . . . H19 H -0.0709 0.2420 0.0891 0.030 Uiso 1 1 calc R . . C23 C 0.2936(5) 0.4561(5) 0.3331(2) 0.0278(10) Uani 1 1 d . . . H23 H 0.2893 0.5059 0.3754 0.033 Uiso 1 1 calc R . . C24 C 0.3828(5) 0.3417(5) 0.3272(2) 0.0296(11) Uani 1 1 d . . . H24 H 0.4501 0.3004 0.3638 0.036 Uiso 1 1 calc R . . C25 C 0.3547(5) 0.3001(5) 0.2584(2) 0.0277(10) Uani 1 1 d . . . H25 H 0.3984 0.2241 0.2379 0.033 Uiso 1 1 calc R . . C26 C 0.1887(4) 0.3998(4) 0.1520(2) 0.0199(8) Uani 1 1 d . . . H26 H 0.2277 0.3239 0.1244 0.024 Uiso 1 1 calc R . . C11 C -0.1372(6) 0.7482(5) 0.0682(2) 0.0326(11) Uani 1 1 d . . . H11A H -0.0687 0.6700 0.0752 0.049 Uiso 1 1 calc R . . H11B H -0.0903 0.8057 0.0334 0.049 Uiso 1 1 calc R . . H11C H -0.2482 0.7225 0.0506 0.049 Uiso 1 1 calc R . . C12 C -0.1436(5) 0.8187(4) 0.1371(2) 0.0209(9) Uani 1 1 d . . . C13 C -0.2251(5) 0.9372(5) 0.1481(2) 0.0261(10) Uani 1 1 d . . . H13 H -0.2863 0.9872 0.1130 0.031 Uiso 1 1 calc R . . C14 C -0.2000(5) 0.9670(4) 0.2186(2) 0.0227(9) Uani 1 1 d . . . C15 C -0.2553(6) 1.0818(5) 0.2600(2) 0.0331(10) Uani 1 1 d . . . H15A H -0.3353 1.0528 0.2929 0.050 Uiso 1 1 calc R . . H15B H -0.3062 1.1467 0.2271 0.050 Uiso 1 1 calc R . . H15C H -0.1607 1.1208 0.2869 0.050 Uiso 1 1 calc R . . C1 C 0.5017(5) 0.7075(5) 0.2658(2) 0.0333(11) Uani 1 1 d . . . H1A H 0.4527 0.6267 0.2461 0.050 Uiso 1 1 calc R . . H1B H 0.5886 0.6860 0.3024 0.050 Uiso 1 1 calc R . . H1C H 0.5481 0.7575 0.2277 0.050 Uiso 1 1 calc R . . C2 C 0.3741(5) 0.7866(4) 0.2976(2) 0.0253(10) Uani 1 1 d . . . C3 C 0.3941(6) 0.8966(5) 0.3424(2) 0.0330(12) Uani 1 1 d . . . H3 H 0.4957 0.9343 0.3592 0.040 Uiso 1 1 calc R . . C4 C 0.2446(5) 0.9392(4) 0.3572(2) 0.0251(9) Uani 1 1 d . . . C5 C 0.1902(6) 1.0490(5) 0.4009(3) 0.0365(11) Uani 1 1 d . . . H5A H 0.2852 1.0869 0.4282 0.055 Uiso 1 1 calc R . . H5B H 0.1116 1.0169 0.4336 0.055 Uiso 1 1 calc R . . H5C H 0.1379 1.1159 0.3698 0.055 Uiso 1 1 calc R . . C6 C -0.1208(5) 0.3820(4) 0.3363(2) 0.0258(9) Uani 1 1 d . . . H6A H -0.0411 0.3694 0.3006 0.039 Uiso 1 1 calc R . . H6B H -0.2287 0.3511 0.3174 0.039 Uiso 1 1 calc R . . H6C H -0.0861 0.3325 0.3793 0.039 Uiso 1 1 calc R . . C7 C -0.1308(5) 0.5242(4) 0.3543(2) 0.0205(9) Uani 1 1 d . . . C8 C -0.2086(5) 0.5780(4) 0.4109(2) 0.0209(9) Uani 1 1 d . . . H8 H -0.2682 0.5319 0.4443 0.025 Uiso 1 1 calc R . . C9 C -0.1823(5) 0.7109(4) 0.4089(2) 0.0205(9) Uani 1 1 d . . . C10 C -0.2257(5) 0.8150(4) 0.4594(2) 0.0268(9) Uani 1 1 d . . . H10A H -0.1360 0.8257 0.4964 0.040 Uiso 1 1 calc R . . H10B H -0.3260 0.7904 0.4815 0.040 Uiso 1 1 calc R . . H10C H -0.2435 0.8975 0.4336 0.040 Uiso 1 1 calc R . . C16 C -0.0401(5) 0.8532(4) 0.3213(2) 0.0201(8) Uani 1 1 d . . . H16 H -0.0771 0.9281 0.3501 0.024 Uiso 1 1 calc R . . B1 B 0.7054(8) 0.1789(6) 0.4828(3) 0.0372(13) Uani 1 1 d . . . B2 B 0.3389(6) 0.0798(5) 0.0902(2) 0.0234(10) 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 Fe1 0.0158(2) 0.0159(3) 0.0169(2) -0.0018(2) 0.00097(16) -0.0006(2) F1 0.068(3) 0.103(5) 0.380(11) -0.020(6) 0.033(4) -0.018(3) F2 0.133(4) 0.242(9) 0.095(3) -0.037(4) -0.065(3) 0.099(5) F3 0.292(8) 0.035(2) 0.073(3) 0.015(2) 0.081(4) 0.025(3) F4 0.476(11) 0.023(2) 0.058(2) -0.003(2) 0.119(4) -0.014(5) F5 0.079(2) 0.0449(19) 0.0238(14) 0.0037(13) -0.0022(13) 0.0144(16) F6 0.0255(13) 0.044(2) 0.0624(18) 0.0055(14) 0.0098(12) -0.0014(12) F7 0.0337(13) 0.0257(14) 0.0434(15) -0.0060(12) 0.0152(11) -0.0079(11) F8 0.0509(16) 0.0255(15) 0.0355(15) -0.0085(12) 0.0185(12) -0.0052(12) N9 0.0147(14) 0.0163(16) 0.0266(15) -0.0021(18) 0.0004(11) 0.0035(16) N10 0.0180(17) 0.024(2) 0.0212(18) 0.0001(15) 0.0033(13) -0.0005(14) N7 0.0149(17) 0.0199(19) 0.0246(19) -0.0043(15) 0.0004(14) 0.0017(14) N8 0.0205(16) 0.0153(18) 0.0171(15) -0.0051(13) 0.0053(12) 0.0006(13) N11 0.0202(17) 0.0156(18) 0.0203(18) 0.0011(14) 0.0035(13) -0.0013(14) N12 0.0197(16) 0.0196(19) 0.0246(17) -0.0003(15) -0.0009(13) 0.0068(14) N5 0.0248(18) 0.0155(19) 0.0231(18) -0.0034(15) 0.0055(14) 0.0007(14) N6 0.0242(16) 0.0149(18) 0.0155(15) -0.0031(13) 0.0048(12) -0.0007(13) N1 0.0189(18) 0.0193(19) 0.0228(18) -0.0011(15) 0.0017(13) -0.0029(15) N2 0.0218(17) 0.0186(19) 0.0227(17) -0.0032(14) -0.0014(13) -0.0048(14) N3 0.0196(14) 0.0139(17) 0.0159(13) -0.0062(15) 0.0044(11) -0.0002(15) N4 0.0217(17) 0.0147(18) 0.0124(16) -0.0029(14) 0.0031(13) -0.0002(14) C20 0.025(2) 0.019(2) 0.026(2) 0.0059(19) 0.0073(17) -0.0077(18) C21 0.035(3) 0.035(3) 0.024(2) 0.0050(19) 0.0080(18) -0.006(2) C22 0.0166(19) 0.037(3) 0.024(2) -0.004(2) 0.0081(16) 0.0005(19) C17 0.017(2) 0.027(2) 0.032(2) -0.0003(19) 0.0025(17) 0.0022(17) C18 0.018(2) 0.025(2) 0.032(2) -0.010(2) 0.0024(17) -0.0063(17) C19 0.031(2) 0.018(2) 0.025(2) -0.0030(18) -0.0025(17) 0.0003(18) C23 0.027(2) 0.032(3) 0.024(2) 0.0054(19) -0.0003(17) -0.0060(19) C24 0.023(2) 0.037(3) 0.029(2) 0.013(2) 0.0020(18) 0.004(2) C25 0.020(2) 0.026(3) 0.036(2) 0.009(2) 0.0018(17) 0.0076(17) C26 0.0180(19) 0.018(2) 0.024(2) -0.0033(17) 0.0067(15) 0.0003(16) C11 0.040(3) 0.038(3) 0.019(2) -0.0028(19) -0.0048(18) 0.011(2) C12 0.019(2) 0.025(2) 0.0172(19) -0.0018(17) -0.0034(15) 0.0039(17) C13 0.026(2) 0.025(2) 0.027(2) 0.0015(19) -0.0015(17) 0.0071(18) C14 0.025(2) 0.020(2) 0.023(2) -0.0004(17) 0.0031(16) 0.0020(17) C15 0.044(2) 0.021(2) 0.035(2) 0.0048(19) 0.0095(19) 0.0070(19) C1 0.021(2) 0.043(3) 0.035(2) -0.004(2) -0.0039(17) -0.003(2) C2 0.021(2) 0.026(2) 0.029(2) 0.0015(19) 0.0013(18) -0.0088(17) C3 0.030(3) 0.038(3) 0.029(2) 0.003(2) -0.0054(19) -0.015(2) C4 0.035(2) 0.023(2) 0.0164(19) -0.0025(17) -0.0022(17) -0.0115(19) C5 0.048(3) 0.026(3) 0.035(2) -0.011(2) -0.003(2) -0.011(2) C6 0.038(2) 0.017(2) 0.023(2) 0.0008(17) 0.0088(17) -0.0039(18) C7 0.026(2) 0.014(2) 0.021(2) -0.0021(17) 0.0003(17) -0.0029(17) C8 0.026(2) 0.021(2) 0.0157(19) 0.0012(16) 0.0032(15) -0.0015(17) C9 0.023(2) 0.024(2) 0.0147(19) -0.0021(17) 0.0035(15) -0.0016(17) C10 0.042(2) 0.016(2) 0.024(2) -0.0036(17) 0.0114(18) -0.0008(18) C16 0.025(2) 0.018(2) 0.0173(19) -0.0021(16) 0.0036(15) -0.0010(16) B1 0.061(4) 0.027(3) 0.023(3) 0.000(2) -0.005(2) -0.007(3) B2 0.033(2) 0.018(2) 0.020(2) -0.0011(18) 0.0084(18) -0.003(2) _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 N9 1.966(3) . ? Fe1 N7 1.974(4) . ? Fe1 N5 1.977(4) . ? Fe1 N3 1.986(3) . ? Fe1 N11 1.986(3) . ? Fe1 N1 1.993(4) . ? F1 B1 1.365(8) . ? F2 B1 1.262(7) . ? F3 B1 1.363(7) . ? F4 B1 1.344(7) . ? F5 B2 1.385(5) . ? F6 B2 1.377(6) . ? F7 B2 1.428(5) . ? F8 B2 1.376(5) . ? N9 C20 1.328(6) . ? N9 N10 1.349(5) . ? N10 C22 1.369(5) . ? N10 C26 1.450(6) . ? N7 C17 1.323(5) . ? N7 N8 1.361(5) . ? N8 C19 1.338(5) . ? N8 C26 1.451(5) . ? N11 C23 1.318(5) . ? N11 N12 1.368(5) . ? N12 C25 1.361(5) . ? N12 C26 1.442(5) . ? N5 C12 1.340(5) . ? N5 N6 1.387(5) . ? N6 C14 1.360(5) . ? N6 C16 1.449(5) . ? N1 C2 1.341(5) . ? N1 N2 1.364(5) . ? N2 C4 1.367(5) . ? N2 C16 1.444(5) . ? N3 C7 1.336(6) . ? N3 N4 1.382(5) . ? N4 C9 1.357(5) . ? N4 C16 1.441(5) . ? C20 C21 1.405(6) . ? C21 C22 1.357(7) . ? C17 C18 1.403(6) . ? C18 C19 1.362(6) . ? C23 C24 1.389(7) . ? C24 C25 1.369(6) . ? C11 C12 1.490(6) . ? C12 C13 1.408(6) . ? C13 C14 1.364(6) . ? C14 C15 1.498(6) . ? C1 C2 1.482(6) . ? C2 C3 1.410(7) . ? C3 C4 1.347(7) . ? C4 C5 1.481(6) . ? C6 C7 1.498(6) . ? C7 C8 1.395(6) . ? C8 C9 1.379(6) . ? C9 C10 1.489(6) . ? 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 N9 Fe1 N7 87.31(14) . . ? N9 Fe1 N5 93.50(14) . . ? N7 Fe1 N5 92.82(14) . . ? N9 Fe1 N3 178.05(18) . . ? N7 Fe1 N3 91.72(14) . . ? N5 Fe1 N3 88.24(15) . . ? N9 Fe1 N11 87.52(14) . . ? N7 Fe1 N11 88.68(16) . . ? N5 Fe1 N11 178.23(16) . . ? N3 Fe1 N11 90.77(14) . . ? N9 Fe1 N1 92.07(15) . . ? N7 Fe1 N1 179.21(17) . . ? N5 Fe1 N1 87.71(16) . . ? N3 Fe1 N1 88.89(14) . . ? N11 Fe1 N1 90.81(13) . . ? C20 N9 N10 106.0(3) . . ? C20 N9 Fe1 136.1(3) . . ? N10 N9 Fe1 117.8(3) . . ? N9 N10 C22 111.1(4) . . ? N9 N10 C26 118.9(3) . . ? C22 N10 C26 130.0(4) . . ? C17 N7 N8 104.9(3) . . ? C17 N7 Fe1 137.3(3) . . ? N8 N7 Fe1 117.8(2) . . ? C19 N8 N7 111.5(3) . . ? C19 N8 C26 130.2(3) . . ? N7 N8 C26 118.3(3) . . ? C23 N11 N12 106.4(3) . . ? C23 N11 Fe1 136.4(3) . . ? N12 N11 Fe1 117.2(2) . . ? C25 N12 N11 110.2(3) . . ? C25 N12 C26 131.2(4) . . ? N11 N12 C26 118.5(3) . . ? C12 N5 N6 104.9(3) . . ? C12 N5 Fe1 138.8(3) . . ? N6 N5 Fe1 116.3(3) . . ? C14 N6 N5 111.6(3) . . ? C14 N6 C16 129.4(3) . . ? N5 N6 C16 118.8(3) . . ? C2 N1 N2 105.3(3) . . ? C2 N1 Fe1 137.7(3) . . ? N2 N1 Fe1 116.9(2) . . ? N1 N2 C4 112.3(3) . . ? N1 N2 C16 118.8(3) . . ? C4 N2 C16 129.0(4) . . ? C7 N3 N4 105.1(3) . . ? C7 N3 Fe1 137.5(3) . . ? N4 N3 Fe1 117.4(2) . . ? C9 N4 N3 111.4(3) . . ? C9 N4 C16 130.9(4) . . ? N3 N4 C16 117.6(3) . . ? N9 C20 C21 110.2(4) . . ? C22 C21 C20 106.1(4) . . ? C21 C22 N10 106.6(4) . . ? N7 C17 C18 111.0(4) . . ? C19 C18 C17 104.9(4) . . ? N8 C19 C18 107.5(4) . . ? N11 C23 C24 110.4(4) . . ? C25 C24 C23 106.5(4) . . ? N12 C25 C24 106.5(4) . . ? N12 C26 N10 109.7(3) . . ? N12 C26 N8 109.7(3) . . ? N10 C26 N8 109.2(3) . . ? N5 C12 C13 110.0(4) . . ? N5 C12 C11 123.6(4) . . ? C13 C12 C11 126.4(4) . . ? C14 C13 C12 107.3(4) . . ? N6 C14 C13 106.2(4) . . ? N6 C14 C15 123.1(4) . . ? C13 C14 C15 130.8(4) . . ? N1 C2 C3 108.8(4) . . ? N1 C2 C1 122.5(4) . . ? C3 C2 C1 128.6(4) . . ? C4 C3 C2 108.4(4) . . ? C3 C4 N2 105.2(4) . . ? C3 C4 C5 132.5(4) . . ? N2 C4 C5 122.3(4) . . ? N3 C7 C8 110.6(4) . . ? N3 C7 C6 123.1(4) . . ? C8 C7 C6 126.3(4) . . ? C9 C8 C7 106.7(4) . . ? N4 C9 C8 106.1(4) . . ? N4 C9 C10 123.7(4) . . ? C8 C9 C10 130.1(4) . . ? N4 C16 N2 110.4(3) . . ? N4 C16 N6 110.5(3) . . ? N2 C16 N6 109.4(3) . . ? F2 B1 F4 108.3(6) . . ? F2 B1 F3 114.1(6) . . ? F4 B1 F3 113.4(5) . . ? F2 B1 F1 99.9(7) . . ? F4 B1 F1 112.3(6) . . ? F3 B1 F1 108.1(6) . . ? F8 B2 F6 111.6(4) . . ? F8 B2 F5 110.9(4) . . ? F6 B2 F5 109.4(3) . . ? F8 B2 F7 109.2(3) . . ? F6 B2 F7 107.0(4) . . ? F5 B2 F7 108.6(4) . . ? 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 N7 Fe1 N9 C20 136.0(4) . . . . ? N5 Fe1 N9 C20 43.4(4) . . . . ? N3 Fe1 N9 C20 -164(3) . . . . ? N11 Fe1 N9 C20 -135.2(4) . . . . ? N1 Fe1 N9 C20 -44.4(4) . . . . ? N7 Fe1 N9 N10 -44.7(3) . . . . ? N5 Fe1 N9 N10 -137.4(3) . . . . ? N3 Fe1 N9 N10 15(4) . . . . ? N11 Fe1 N9 N10 44.1(3) . . . . ? N1 Fe1 N9 N10 134.8(3) . . . . ? C20 N9 N10 C22 1.0(4) . . . . ? Fe1 N9 N10 C22 -178.5(2) . . . . ? C20 N9 N10 C26 179.8(4) . . . . ? Fe1 N9 N10 C26 0.4(4) . . . . ? N9 Fe1 N7 C17 -135.1(5) . . . . ? N5 Fe1 N7 C17 -41.7(5) . . . . ? N3 Fe1 N7 C17 46.6(5) . . . . ? N11 Fe1 N7 C17 137.3(5) . . . . ? N1 Fe1 N7 C17 -173(100) . . . . ? N9 Fe1 N7 N8 45.2(3) . . . . ? N5 Fe1 N7 N8 138.6(3) . . . . ? N3 Fe1 N7 N8 -133.1(3) . . . . ? N11 Fe1 N7 N8 -42.4(3) . . . . ? N1 Fe1 N7 N8 7(13) . . . . ? C17 N7 N8 C19 0.0(4) . . . . ? Fe1 N7 N8 C19 179.8(3) . . . . ? C17 N7 N8 C26 178.8(3) . . . . ? Fe1 N7 N8 C26 -1.4(4) . . . . ? N9 Fe1 N11 C23 133.4(4) . . . . ? N7 Fe1 N11 C23 -139.2(4) . . . . ? N5 Fe1 N11 C23 8(6) . . . . ? N3 Fe1 N11 C23 -47.5(4) . . . . ? N1 Fe1 N11 C23 41.4(4) . . . . ? N9 Fe1 N11 N12 -45.3(3) . . . . ? N7 Fe1 N11 N12 42.0(3) . . . . ? N5 Fe1 N11 N12 -170(5) . . . . ? N3 Fe1 N11 N12 133.7(3) . . . . ? N1 Fe1 N11 N12 -137.4(3) . . . . ? C23 N11 N12 C25 -0.8(4) . . . . ? Fe1 N11 N12 C25 178.3(3) . . . . ? C23 N11 N12 C26 -177.0(3) . . . . ? Fe1 N11 N12 C26 2.1(4) . . . . ? N9 Fe1 N5 C12 40.7(5) . . . . ? N7 Fe1 N5 C12 -46.8(5) . . . . ? N3 Fe1 N5 C12 -138.4(5) . . . . ? N11 Fe1 N5 C12 166(5) . . . . ? N1 Fe1 N5 C12 132.6(5) . . . . ? N9 Fe1 N5 N6 -137.3(3) . . . . ? N7 Fe1 N5 N6 135.2(3) . . . . ? N3 Fe1 N5 N6 43.6(3) . . . . ? N11 Fe1 N5 N6 -12(6) . . . . ? N1 Fe1 N5 N6 -45.4(3) . . . . ? C12 N5 N6 C14 -1.2(4) . . . . ? Fe1 N5 N6 C14 177.4(3) . . . . ? C12 N5 N6 C16 -177.4(3) . . . . ? Fe1 N5 N6 C16 1.2(4) . . . . ? N9 Fe1 N1 C2 -42.5(5) . . . . ? N7 Fe1 N1 C2 -4(13) . . . . ? N5 Fe1 N1 C2 -135.9(5) . . . . ? N3 Fe1 N1 C2 135.8(5) . . . . ? N11 Fe1 N1 C2 45.1(4) . . . . ? N9 Fe1 N1 N2 138.9(3) . . . . ? N7 Fe1 N1 N2 177(100) . . . . ? N5 Fe1 N1 N2 45.5(3) . . . . ? N3 Fe1 N1 N2 -42.8(3) . . . . ? N11 Fe1 N1 N2 -133.5(3) . . . . ? C2 N1 N2 C4 0.4(5) . . . . ? Fe1 N1 N2 C4 179.4(3) . . . . ? C2 N1 N2 C16 -179.4(3) . . . . ? Fe1 N1 N2 C16 -0.4(4) . . . . ? N9 Fe1 N3 C7 -18(4) . . . . ? N7 Fe1 N3 C7 42.4(4) . . . . ? N5 Fe1 N3 C7 135.1(4) . . . . ? N11 Fe1 N3 C7 -46.3(4) . . . . ? N1 Fe1 N3 C7 -137.1(4) . . . . ? N9 Fe1 N3 N4 161(4) . . . . ? N7 Fe1 N3 N4 -139.1(3) . . . . ? N5 Fe1 N3 N4 -46.3(3) . . . . ? N11 Fe1 N3 N4 132.2(2) . . . . ? N1 Fe1 N3 N4 41.4(2) . . . . ? C7 N3 N4 C9 1.3(4) . . . . ? Fe1 N3 N4 C9 -177.7(2) . . . . ? C7 N3 N4 C16 -178.1(3) . . . . ? Fe1 N3 N4 C16 2.9(4) . . . . ? N10 N9 C20 C21 -1.1(4) . . . . ? Fe1 N9 C20 C21 178.2(3) . . . . ? N9 C20 C21 C22 0.8(5) . . . . ? C20 C21 C22 N10 -0.2(5) . . . . ? N9 N10 C22 C21 -0.5(5) . . . . ? C26 N10 C22 C21 -179.2(4) . . . . ? N8 N7 C17 C18 -0.8(5) . . . . ? Fe1 N7 C17 C18 179.5(3) . . . . ? N7 C17 C18 C19 1.3(5) . . . . ? N7 N8 C19 C18 0.9(5) . . . . ? C26 N8 C19 C18 -177.8(4) . . . . ? C17 C18 C19 N8 -1.3(5) . . . . ? N12 N11 C23 C24 0.9(5) . . . . ? Fe1 N11 C23 C24 -177.9(3) . . . . ? N11 C23 C24 C25 -0.8(5) . . . . ? N11 N12 C25 C24 0.3(4) . . . . ? C26 N12 C25 C24 175.9(4) . . . . ? C23 C24 C25 N12 0.2(5) . . . . ? C25 N12 C26 N10 -117.0(4) . . . . ? N11 N12 C26 N10 58.3(4) . . . . ? C25 N12 C26 N8 123.0(4) . . . . ? N11 N12 C26 N8 -61.7(4) . . . . ? N9 N10 C26 N12 -60.4(4) . . . . ? C22 N10 C26 N12 118.2(4) . . . . ? N9 N10 C26 N8 59.8(4) . . . . ? C22 N10 C26 N8 -121.5(4) . . . . ? C19 N8 C26 N12 -119.9(4) . . . . ? N7 N8 C26 N12 61.5(4) . . . . ? C19 N8 C26 N10 119.8(4) . . . . ? N7 N8 C26 N10 -58.8(4) . . . . ? N6 N5 C12 C13 0.7(5) . . . . ? Fe1 N5 C12 C13 -177.4(3) . . . . ? N6 N5 C12 C11 -179.3(4) . . . . ? Fe1 N5 C12 C11 2.6(7) . . . . ? N5 C12 C13 C14 0.0(5) . . . . ? C11 C12 C13 C14 180.0(4) . . . . ? N5 N6 C14 C13 1.2(4) . . . . ? C16 N6 C14 C13 176.9(4) . . . . ? N5 N6 C14 C15 -178.5(4) . . . . ? C16 N6 C14 C15 -2.8(6) . . . . ? C12 C13 C14 N6 -0.7(5) . . . . ? C12 C13 C14 C15 179.0(4) . . . . ? N2 N1 C2 C3 0.2(5) . . . . ? Fe1 N1 C2 C3 -178.5(3) . . . . ? N2 N1 C2 C1 -179.1(4) . . . . ? Fe1 N1 C2 C1 2.2(7) . . . . ? N1 C2 C3 C4 -0.7(5) . . . . ? C1 C2 C3 C4 178.5(5) . . . . ? C2 C3 C4 N2 0.9(5) . . . . ? C2 C3 C4 C5 179.8(5) . . . . ? N1 N2 C4 C3 -0.8(5) . . . . ? C16 N2 C4 C3 179.0(4) . . . . ? N1 N2 C4 C5 -179.9(4) . . . . ? C16 N2 C4 C5 -0.1(7) . . . . ? N4 N3 C7 C8 -0.1(4) . . . . ? Fe1 N3 C7 C8 178.6(3) . . . . ? N4 N3 C7 C6 -179.0(4) . . . . ? Fe1 N3 C7 C6 -0.3(6) . . . . ? N3 C7 C8 C9 -1.2(5) . . . . ? C6 C7 C8 C9 177.7(4) . . . . ? N3 N4 C9 C8 -2.1(5) . . . . ? C16 N4 C9 C8 177.3(4) . . . . ? N3 N4 C9 C10 174.8(3) . . . . ? C16 N4 C9 C10 -5.8(7) . . . . ? C7 C8 C9 N4 1.9(5) . . . . ? C7 C8 C9 C10 -174.7(4) . . . . ? C9 N4 C16 N2 118.2(4) . . . . ? N3 N4 C16 N2 -62.5(4) . . . . ? C9 N4 C16 N6 -120.7(4) . . . . ? N3 N4 C16 N6 58.6(4) . . . . ? N1 N2 C16 N4 61.3(4) . . . . ? C4 N2 C16 N4 -118.5(4) . . . . ? N1 N2 C16 N6 -60.5(4) . . . . ? C4 N2 C16 N6 119.7(4) . . . . ? C14 N6 C16 N4 122.8(4) . . . . ? N5 N6 C16 N4 -61.7(4) . . . . ? C14 N6 C16 N2 -115.4(4) . . . . ? N5 N6 C16 N2 60.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.937 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.103 #=END data_1b-173K _database_code_depnum_ccdc_archive 'CCDC 650143' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H32 B2 F8 Fe N12' _chemical_formula_weight 742.11 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1222(2) _cell_length_b 12.0992(4) _cell_length_c 14.0078(3) _cell_angle_alpha 89.432(2) _cell_angle_beta 73.674(2) _cell_angle_gamma 79.715(1) _cell_volume 1618.44(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular block' _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.552 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Nonius KappaCCD' _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 21403 _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_sigmaI/netI 0.0831 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.87 _reflns_number_total 7474 _reflns_number_gt 4649 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0582P)^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 7474 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1015 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1278 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 0.66867(4) 0.73686(3) 0.75109(2) 0.02167(12) Uani 1 1 d . . . F1 F 0.69034(16) 0.22300(15) 0.74042(10) 0.0481(5) Uani 1 1 d . . . F2 F 0.69204(17) 0.28537(14) 0.58779(11) 0.0448(4) Uani 1 1 d . . . F3 F 0.70622(17) 0.09990(14) 0.61541(11) 0.0489(5) Uani 1 1 d . . . F4 F 0.50210(16) 0.22013(14) 0.68350(11) 0.0428(4) Uani 1 1 d . . . F5 F 0.12408(17) 0.80048(16) 1.07463(12) 0.0527(5) Uani 1 1 d . . . F6 F 0.0552(2) 0.68735(17) 0.98265(15) 0.0719(6) Uani 1 1 d . . . F7 F -0.0598(2) 0.86492(17) 1.01508(13) 0.0663(6) Uani 1 1 d . . . F8 F -0.08241(19) 0.74479(18) 1.13817(14) 0.0697(6) Uani 1 1 d . . . N1 N 0.7096(2) 0.75025(17) 0.60454(13) 0.0230(5) Uani 1 1 d . . . N2 N 0.84597(19) 0.75273(17) 0.55233(13) 0.0212(5) Uani 1 1 d . . . N3 N 0.8372(2) 0.61689(18) 0.72673(14) 0.0238(5) Uani 1 1 d . . . N4 N 0.9553(2) 0.63433(17) 0.65454(13) 0.0218(5) Uani 1 1 d . . . N5 N 0.7914(2) 0.84721(17) 0.75168(13) 0.0226(5) Uani 1 1 d . . . N6 N 0.9171(2) 0.83278(17) 0.67877(13) 0.0208(5) Uani 1 1 d . . . N7 N 0.6294(2) 0.72501(17) 0.89556(14) 0.0251(5) Uani 1 1 d . . . N8 N 0.4942(2) 0.72612(18) 0.95028(14) 0.0260(5) Uani 1 1 d . . . N9 N 0.5022(2) 0.85706(17) 0.77707(13) 0.0229(5) Uani 1 1 d . . . N10 N 0.3827(2) 0.84073(17) 0.84700(14) 0.0260(5) Uani 1 1 d . . . N11 N 0.5442(2) 0.62739(18) 0.75498(14) 0.0252(5) Uani 1 1 d . . . N12 N 0.4195(2) 0.64319(18) 0.82757(15) 0.0272(5) Uani 1 1 d . . . C1 C 0.4852(3) 0.7692(3) 0.56146(19) 0.0389(7) Uani 1 1 d . . . H1A H 0.4471 0.7652 0.6337 0.058 Uiso 1 1 calc R . . H1B H 0.4676 0.7049 0.5280 0.058 Uiso 1 1 calc R . . H1C H 0.4399 0.8392 0.5393 0.058 Uiso 1 1 calc R . . C2 C 0.6384(3) 0.7665(2) 0.53635(17) 0.0249(6) Uani 1 1 d . . . C3 C 0.7297(3) 0.7796(2) 0.44354(18) 0.0298(6) Uani 1 1 d . . . H3 H 0.7047 0.7918 0.3833 0.036 Uiso 1 1 calc R . . C4 C 0.8601(3) 0.7721(2) 0.45392(16) 0.0234(6) Uani 1 1 d . . . C5 C 0.9973(3) 0.7810(2) 0.38194(18) 0.0318(6) Uani 1 1 d . . . H5A H 0.9853 0.7924 0.3153 0.048 Uiso 1 1 calc R . . H5B H 1.0648 0.7116 0.3809 0.048 Uiso 1 1 calc R . . H5C H 1.0320 0.8449 0.4023 0.048 Uiso 1 1 calc R . . C6 C 0.7804(3) 0.4639(2) 0.84463(19) 0.0369(7) Uani 1 1 d . . . H6A H 0.6859 0.5094 0.8615 0.055 Uiso 1 1 calc R . . H6B H 0.8141 0.4578 0.9039 0.055 Uiso 1 1 calc R . . H6C H 0.7781 0.3887 0.8206 0.055 Uiso 1 1 calc R . . C7 C 0.8767(3) 0.5186(2) 0.76506(18) 0.0271(6) Uani 1 1 d . . . C8 C 1.0181(3) 0.4759(2) 0.71775(19) 0.0323(6) Uani 1 1 d . . . H8 H 1.0711 0.4077 0.7314 0.039 Uiso 1 1 calc R . . C9 C 1.0656(3) 0.5505(2) 0.64834(18) 0.0273(6) Uani 1 1 d . . . C10 C 1.2048(3) 0.5462(3) 0.5736(2) 0.0443(8) Uani 1 1 d . . . H10A H 1.1913 0.5650 0.5083 0.066 Uiso 1 1 calc R . . H10B H 1.2604 0.4704 0.5693 0.066 Uiso 1 1 calc R . . H10C H 1.2539 0.6004 0.5940 0.066 Uiso 1 1 calc R . . C11 C 0.6751(3) 0.9832(2) 0.89689(18) 0.0349(7) Uani 1 1 d . . . H11A H 0.6014 0.9378 0.9083 0.052 Uiso 1 1 calc R . . H11B H 0.6371 1.0605 0.8843 0.052 Uiso 1 1 calc R . . H11C H 0.7091 0.9831 0.9558 0.052 Uiso 1 1 calc R . . C12 C 0.7932(3) 0.9347(2) 0.80896(17) 0.0243(6) Uani 1 1 d . . . C13 C 0.9194(3) 0.9739(2) 0.77262(18) 0.0290(6) Uani 1 1 d . . . H13 H 0.9463 1.0346 0.8004 0.035 Uiso 1 1 calc R . . C14 C 0.9962(3) 0.9091(2) 0.69029(17) 0.0248(6) Uani 1 1 d . . . C15 C 1.1375(3) 0.9115(3) 0.6200(2) 0.0414(8) Uani 1 1 d . . . H15A H 1.1809 0.9668 0.6451 0.062 Uiso 1 1 calc R . . H15B H 1.1276 0.9322 0.5542 0.062 Uiso 1 1 calc R . . H15C H 1.1966 0.8369 0.6148 0.062 Uiso 1 1 calc R . . C16 C 0.9492(2) 0.7409(2) 0.60657(16) 0.0210(5) Uani 1 1 d . . . H16 H 1.0428 0.7424 0.5584 0.025 Uiso 1 1 calc R . . C17 C 0.7014(3) 0.7199(2) 0.96220(18) 0.0299(6) Uani 1 1 d . . . H17 H 0.7996 0.7172 0.9462 0.036 Uiso 1 1 calc R . . C18 C 0.6137(3) 0.7192(2) 1.05813(18) 0.0353(7) Uani 1 1 d . . . H18 H 0.6398 0.7163 1.1183 0.042 Uiso 1 1 calc R . . C19 C 0.4826(3) 0.7234(2) 1.04842(18) 0.0330(7) Uani 1 1 d . . . H19 H 0.3990 0.7242 1.1008 0.040 Uiso 1 1 calc R . . C20 C 0.4704(3) 0.9605(2) 0.74696(18) 0.0291(6) Uani 1 1 d . . . H20 H 0.5327 0.9957 0.6976 0.035 Uiso 1 1 calc R . . C21 C 0.3338(3) 1.0103(2) 0.79735(19) 0.0315(6) Uani 1 1 d . . . H21 H 0.2871 1.0836 0.7892 0.038 Uiso 1 1 calc R . . C22 C 0.2803(3) 0.9326(2) 0.86078(18) 0.0281(6) Uani 1 1 d . . . H22 H 0.1889 0.9413 0.9058 0.034 Uiso 1 1 calc R . . C23 C 0.5472(3) 0.5337(2) 0.70559(18) 0.0308(6) Uani 1 1 d . . . H23 H 0.6221 0.5010 0.6502 0.037 Uiso 1 1 calc R . . C24 C 0.4261(3) 0.4892(2) 0.74542(19) 0.0359(7) Uani 1 1 d . . . H24 H 0.4035 0.4230 0.7231 0.043 Uiso 1 1 calc R . . C25 C 0.3472(3) 0.5610(2) 0.82326(19) 0.0330(6) Uani 1 1 d . . . H25 H 0.2581 0.5543 0.8663 0.040 Uiso 1 1 calc R . . C26 C 0.3877(3) 0.7370(2) 0.89848(17) 0.0274(6) Uani 1 1 d . . . H26 H 0.2945 0.7368 0.9478 0.033 Uiso 1 1 calc R . . B1 B 0.6474(3) 0.2067(3) 0.6576(2) 0.0301(7) Uani 1 1 d . . . B2 B 0.0065(4) 0.7745(3) 1.0538(2) 0.0373(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 Fe1 0.0193(2) 0.0228(2) 0.0190(2) -0.00013(14) 0.00109(14) -0.00414(15) F1 0.0420(11) 0.0792(14) 0.0231(8) -0.0043(8) -0.0054(7) -0.0165(9) F2 0.0526(11) 0.0498(11) 0.0417(9) 0.0172(8) -0.0168(8) -0.0293(9) F3 0.0504(11) 0.0401(11) 0.0445(10) -0.0062(8) 0.0075(8) -0.0118(9) F4 0.0314(10) 0.0478(11) 0.0481(10) 0.0004(8) -0.0063(7) -0.0130(8) F5 0.0326(10) 0.0676(13) 0.0549(11) -0.0102(9) -0.0071(8) -0.0089(9) F6 0.0608(13) 0.0694(15) 0.0814(14) -0.0357(11) -0.0205(11) 0.0013(11) F7 0.0579(13) 0.0637(14) 0.0632(12) 0.0179(10) -0.0126(10) 0.0174(11) F8 0.0404(11) 0.0859(16) 0.0695(13) 0.0309(11) 0.0041(9) -0.0102(11) N1 0.0160(11) 0.0279(13) 0.0222(11) 0.0000(9) 0.0003(9) -0.0060(9) N2 0.0161(11) 0.0265(12) 0.0191(10) 0.0022(8) -0.0016(8) -0.0041(9) N3 0.0185(11) 0.0265(13) 0.0240(11) 0.0019(9) -0.0009(9) -0.0063(9) N4 0.0176(11) 0.0219(12) 0.0214(10) 0.0023(8) 0.0008(8) -0.0026(9) N5 0.0208(11) 0.0233(12) 0.0198(10) -0.0015(9) 0.0001(8) -0.0029(9) N6 0.0179(11) 0.0229(12) 0.0201(10) -0.0030(8) -0.0013(8) -0.0062(9) N7 0.0238(12) 0.0245(13) 0.0225(11) -0.0013(9) 0.0018(9) -0.0060(10) N8 0.0253(12) 0.0285(13) 0.0192(11) 0.0010(9) 0.0021(9) -0.0054(10) N9 0.0194(11) 0.0233(12) 0.0212(10) 0.0012(9) 0.0020(8) -0.0042(9) N10 0.0215(12) 0.0220(13) 0.0271(11) 0.0013(9) 0.0037(9) -0.0019(10) N11 0.0205(11) 0.0270(13) 0.0233(11) -0.0017(9) 0.0018(9) -0.0047(9) N12 0.0220(12) 0.0241(13) 0.0300(12) -0.0010(9) 0.0032(9) -0.0069(10) C1 0.0230(15) 0.062(2) 0.0316(15) 0.0019(13) -0.0065(12) -0.0079(14) C2 0.0229(14) 0.0288(16) 0.0248(13) 0.0016(11) -0.0084(11) -0.0065(12) C3 0.0281(15) 0.0400(18) 0.0238(13) 0.0047(11) -0.0095(11) -0.0097(13) C4 0.0243(14) 0.0253(15) 0.0189(13) 0.0016(10) -0.0016(10) -0.0073(11) C5 0.0286(15) 0.0431(18) 0.0232(13) 0.0023(12) -0.0028(11) -0.0127(13) C6 0.0360(17) 0.0297(17) 0.0374(16) 0.0102(12) 0.0020(12) -0.0069(13) C7 0.0304(15) 0.0215(15) 0.0265(13) 0.0020(11) -0.0035(11) -0.0044(12) C8 0.0280(15) 0.0240(16) 0.0395(16) 0.0072(12) -0.0045(12) 0.0003(12) C9 0.0231(14) 0.0251(15) 0.0287(14) 0.0018(11) -0.0019(11) -0.0005(12) C10 0.0278(16) 0.041(2) 0.0499(18) 0.0122(14) 0.0048(13) 0.0034(14) C11 0.0364(17) 0.0295(17) 0.0317(15) -0.0075(12) 0.0004(12) -0.0037(13) C12 0.0288(15) 0.0210(15) 0.0215(13) -0.0011(10) -0.0050(11) -0.0033(12) C13 0.0322(16) 0.0272(16) 0.0286(14) -0.0052(11) -0.0070(12) -0.0101(12) C14 0.0224(14) 0.0266(15) 0.0266(14) -0.0007(11) -0.0074(11) -0.0067(12) C15 0.0276(16) 0.044(2) 0.0476(18) -0.0128(14) 0.0012(13) -0.0138(14) C16 0.0148(13) 0.0237(15) 0.0222(12) -0.0003(10) -0.0015(10) -0.0034(11) C17 0.0344(16) 0.0297(16) 0.0274(14) 0.0031(11) -0.0113(12) -0.0067(13) C18 0.054(2) 0.0335(18) 0.0195(14) 0.0026(11) -0.0104(13) -0.0105(15) C19 0.0449(19) 0.0255(16) 0.0211(14) 0.0023(11) 0.0049(12) -0.0098(13) C20 0.0309(16) 0.0266(16) 0.0282(14) 0.0028(11) -0.0051(12) -0.0068(13) C21 0.0325(16) 0.0233(15) 0.0345(15) 0.0019(12) -0.0075(12) 0.0022(12) C22 0.0186(14) 0.0299(16) 0.0306(14) -0.0045(12) -0.0014(11) 0.0009(12) C23 0.0298(16) 0.0292(16) 0.0282(14) -0.0032(12) -0.0010(11) -0.0032(12) C24 0.0385(18) 0.0299(17) 0.0396(16) -0.0008(13) -0.0071(13) -0.0137(14) C25 0.0293(16) 0.0290(16) 0.0386(16) 0.0029(12) -0.0019(12) -0.0119(13) C26 0.0250(15) 0.0236(15) 0.0265(14) -0.0007(11) 0.0045(11) -0.0053(12) B1 0.0317(19) 0.034(2) 0.0231(16) 0.0012(13) -0.0022(13) -0.0113(15) B2 0.032(2) 0.037(2) 0.0379(19) -0.0006(15) -0.0050(15) 0.0007(16) _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 N7 1.9587(19) . ? Fe1 N9 1.969(2) . ? Fe1 N11 1.975(2) . ? Fe1 N5 1.981(2) . ? Fe1 N3 1.983(2) . ? Fe1 N1 1.9878(18) . ? F1 B1 1.376(3) . ? F2 B1 1.397(3) . ? F3 B1 1.385(4) . ? F4 B1 1.391(3) . ? F5 B2 1.390(4) . ? F6 B2 1.381(4) . ? F7 B2 1.368(4) . ? F8 B2 1.359(4) . ? N1 C2 1.343(3) . ? N1 N2 1.374(3) . ? N2 C4 1.368(3) . ? N2 C16 1.443(3) . ? N3 C7 1.341(3) . ? N3 N4 1.379(3) . ? N4 C9 1.352(3) . ? N4 C16 1.447(3) . ? N5 C12 1.341(3) . ? N5 N6 1.373(2) . ? N6 C14 1.363(3) . ? N6 C16 1.440(3) . ? N7 C17 1.331(3) . ? N7 N8 1.365(3) . ? N8 C19 1.347(3) . ? N8 C26 1.447(3) . ? N9 C20 1.331(3) . ? N9 N10 1.370(3) . ? N10 C22 1.352(3) . ? N10 C26 1.441(3) . ? N11 C23 1.326(3) . ? N11 N12 1.364(3) . ? N12 C25 1.347(3) . ? N12 C26 1.446(3) . ? C1 C2 1.485(3) . ? C2 C3 1.393(3) . ? C3 C4 1.355(3) . ? C4 C5 1.491(3) . ? C6 C7 1.495(3) . ? C7 C8 1.402(3) . ? C8 C9 1.366(3) . ? C9 C10 1.493(3) . ? C11 C12 1.492(3) . ? C12 C13 1.400(3) . ? C13 C14 1.358(3) . ? C14 C15 1.497(3) . ? C17 C18 1.388(3) . ? C18 C19 1.364(4) . ? C20 C21 1.391(3) . ? C21 C22 1.364(4) . ? C23 C24 1.395(4) . ? C24 C25 1.365(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 N7 Fe1 N9 87.51(8) . . ? N7 Fe1 N11 87.36(8) . . ? N9 Fe1 N11 88.10(8) . . ? N7 Fe1 N5 90.93(8) . . ? N9 Fe1 N5 91.47(8) . . ? N11 Fe1 N5 178.25(8) . . ? N7 Fe1 N3 91.79(8) . . ? N9 Fe1 N3 179.06(8) . . ? N11 Fe1 N3 92.51(8) . . ? N5 Fe1 N3 87.90(8) . . ? N7 Fe1 N1 179.38(9) . . ? N9 Fe1 N1 92.42(8) . . ? N11 Fe1 N1 93.25(8) . . ? N5 Fe1 N1 88.46(8) . . ? N3 Fe1 N1 88.27(8) . . ? C2 N1 N2 104.75(18) . . ? C2 N1 Fe1 138.12(16) . . ? N2 N1 Fe1 116.92(14) . . ? C4 N2 N1 112.00(18) . . ? C4 N2 C16 129.79(19) . . ? N1 N2 C16 118.13(17) . . ? C7 N3 N4 104.89(19) . . ? C7 N3 Fe1 137.89(17) . . ? N4 N3 Fe1 117.12(15) . . ? C9 N4 N3 111.96(19) . . ? C9 N4 C16 129.87(19) . . ? N3 N4 C16 117.72(18) . . ? C12 N5 N6 104.87(19) . . ? C12 N5 Fe1 137.97(16) . . ? N6 N5 Fe1 117.02(14) . . ? C14 N6 N5 111.80(18) . . ? C14 N6 C16 129.87(19) . . ? N5 N6 C16 118.28(19) . . ? C17 N7 N8 104.93(19) . . ? C17 N7 Fe1 136.82(18) . . ? N8 N7 Fe1 118.18(15) . . ? C19 N8 N7 111.3(2) . . ? C19 N8 C26 130.3(2) . . ? N7 N8 C26 118.21(18) . . ? C20 N9 N10 104.71(19) . . ? C20 N9 Fe1 136.93(17) . . ? N10 N9 Fe1 118.28(15) . . ? C22 N10 N9 111.5(2) . . ? C22 N10 C26 130.6(2) . . ? N9 N10 C26 117.72(19) . . ? C23 N11 N12 104.8(2) . . ? C23 N11 Fe1 137.44(17) . . ? N12 N11 Fe1 117.78(15) . . ? C25 N12 N11 111.5(2) . . ? C25 N12 C26 130.1(2) . . ? N11 N12 C26 118.3(2) . . ? N1 C2 C3 109.7(2) . . ? N1 C2 C1 122.6(2) . . ? C3 C2 C1 127.7(2) . . ? C4 C3 C2 108.4(2) . . ? C3 C4 N2 105.2(2) . . ? C3 C4 C5 132.5(2) . . ? N2 C4 C5 122.4(2) . . ? N3 C7 C8 109.8(2) . . ? N3 C7 C6 123.9(2) . . ? C8 C7 C6 126.3(2) . . ? C9 C8 C7 107.3(2) . . ? N4 C9 C8 106.0(2) . . ? N4 C9 C10 123.0(2) . . ? C8 C9 C10 130.9(2) . . ? N5 C12 C13 110.0(2) . . ? N5 C12 C11 124.0(2) . . ? C13 C12 C11 126.0(2) . . ? C14 C13 C12 107.4(2) . . ? C13 C14 N6 105.9(2) . . ? C13 C14 C15 131.9(2) . . ? N6 C14 C15 122.2(2) . . ? N6 C16 N2 110.26(19) . . ? N6 C16 N4 110.69(18) . . ? N2 C16 N4 110.08(19) . . ? N7 C17 C18 110.9(3) . . ? C19 C18 C17 106.0(2) . . ? N8 C19 C18 106.9(2) . . ? N9 C20 C21 111.0(2) . . ? C22 C21 C20 106.2(2) . . ? N10 C22 C21 106.5(2) . . ? N11 C23 C24 111.3(2) . . ? C25 C24 C23 105.4(2) . . ? N12 C25 C24 107.0(2) . . ? N10 C26 N12 109.57(19) . . ? N10 C26 N8 110.2(2) . . ? N12 C26 N8 109.3(2) . . ? F1 B1 F3 110.1(2) . . ? F1 B1 F4 110.1(2) . . ? F3 B1 F4 109.5(2) . . ? F1 B1 F2 108.9(2) . . ? F3 B1 F2 108.6(2) . . ? F4 B1 F2 109.5(2) . . ? F8 B2 F7 109.9(3) . . ? F8 B2 F6 111.8(3) . . ? F7 B2 F6 109.0(3) . . ? F8 B2 F5 109.8(3) . . ? F7 B2 F5 110.1(3) . . ? F6 B2 F5 106.1(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 N7 Fe1 N1 C2 -123(8) . . . . ? N9 Fe1 N1 C2 -39.8(3) . . . . ? N11 Fe1 N1 C2 48.4(3) . . . . ? N5 Fe1 N1 C2 -131.2(3) . . . . ? N3 Fe1 N1 C2 140.9(3) . . . . ? N7 Fe1 N1 N2 51(8) . . . . ? N9 Fe1 N1 N2 133.87(17) . . . . ? N11 Fe1 N1 N2 -137.90(17) . . . . ? N5 Fe1 N1 N2 42.46(17) . . . . ? N3 Fe1 N1 N2 -45.48(17) . . . . ? C2 N1 N2 C4 1.0(3) . . . . ? Fe1 N1 N2 C4 -174.58(15) . . . . ? C2 N1 N2 C16 178.1(2) . . . . ? Fe1 N1 N2 C16 2.5(3) . . . . ? N7 Fe1 N3 C7 38.6(3) . . . . ? N9 Fe1 N3 C7 81(5) . . . . ? N11 Fe1 N3 C7 -48.8(3) . . . . ? N5 Fe1 N3 C7 129.5(3) . . . . ? N1 Fe1 N3 C7 -142.0(3) . . . . ? N7 Fe1 N3 N4 -137.11(16) . . . . ? N9 Fe1 N3 N4 -95(5) . . . . ? N11 Fe1 N3 N4 135.46(16) . . . . ? N5 Fe1 N3 N4 -46.24(15) . . . . ? N1 Fe1 N3 N4 42.28(16) . . . . ? C7 N3 N4 C9 -0.6(3) . . . . ? Fe1 N3 N4 C9 176.45(16) . . . . ? C7 N3 N4 C16 -173.62(19) . . . . ? Fe1 N3 N4 C16 3.4(2) . . . . ? N7 Fe1 N5 C12 -39.2(3) . . . . ? N9 Fe1 N5 C12 48.3(2) . . . . ? N11 Fe1 N5 C12 -27(3) . . . . ? N3 Fe1 N5 C12 -131.0(2) . . . . ? N1 Fe1 N5 C12 140.7(2) . . . . ? N7 Fe1 N5 N6 135.64(16) . . . . ? N9 Fe1 N5 N6 -136.83(16) . . . . ? N11 Fe1 N5 N6 148(3) . . . . ? N3 Fe1 N5 N6 43.88(16) . . . . ? N1 Fe1 N5 N6 -44.45(16) . . . . ? C12 N5 N6 C14 0.3(2) . . . . ? Fe1 N5 N6 C14 -176.15(15) . . . . ? C12 N5 N6 C16 177.70(19) . . . . ? Fe1 N5 N6 C16 1.2(2) . . . . ? N9 Fe1 N7 C17 -132.4(3) . . . . ? N11 Fe1 N7 C17 139.4(3) . . . . ? N5 Fe1 N7 C17 -40.9(3) . . . . ? N3 Fe1 N7 C17 47.0(3) . . . . ? N1 Fe1 N7 C17 -49(9) . . . . ? N9 Fe1 N7 N8 44.18(17) . . . . ? N11 Fe1 N7 N8 -44.02(17) . . . . ? N5 Fe1 N7 N8 135.62(17) . . . . ? N3 Fe1 N7 N8 -136.45(17) . . . . ? N1 Fe1 N7 N8 127(8) . . . . ? C17 N7 N8 C19 0.8(3) . . . . ? Fe1 N7 N8 C19 -176.72(16) . . . . ? C17 N7 N8 C26 177.0(2) . . . . ? Fe1 N7 N8 C26 -0.6(3) . . . . ? N7 Fe1 N9 C20 131.5(2) . . . . ? N11 Fe1 N9 C20 -141.0(2) . . . . ? N5 Fe1 N9 C20 40.7(2) . . . . ? N3 Fe1 N9 C20 89(5) . . . . ? N1 Fe1 N9 C20 -47.9(2) . . . . ? N7 Fe1 N9 N10 -44.67(16) . . . . ? N11 Fe1 N9 N10 42.77(16) . . . . ? N5 Fe1 N9 N10 -135.53(16) . . . . ? N3 Fe1 N9 N10 -87(5) . . . . ? N1 Fe1 N9 N10 135.95(16) . . . . ? C20 N9 N10 C22 -0.9(3) . . . . ? Fe1 N9 N10 C22 176.43(15) . . . . ? C20 N9 N10 C26 -176.2(2) . . . . ? Fe1 N9 N10 C26 1.1(3) . . . . ? N7 Fe1 N11 C23 -132.5(3) . . . . ? N9 Fe1 N11 C23 139.9(3) . . . . ? N5 Fe1 N11 C23 -144(3) . . . . ? N3 Fe1 N11 C23 -40.8(3) . . . . ? N1 Fe1 N11 C23 47.6(3) . . . . ? N7 Fe1 N11 N12 45.17(17) . . . . ? N9 Fe1 N11 N12 -42.43(17) . . . . ? N5 Fe1 N11 N12 33(3) . . . . ? N3 Fe1 N11 N12 136.85(17) . . . . ? N1 Fe1 N11 N12 -134.74(17) . . . . ? C23 N11 N12 C25 0.1(3) . . . . ? Fe1 N11 N12 C25 -178.25(16) . . . . ? C23 N11 N12 C26 176.8(2) . . . . ? Fe1 N11 N12 C26 -1.5(3) . . . . ? N2 N1 C2 C3 -0.4(3) . . . . ? Fe1 N1 C2 C3 173.76(19) . . . . ? N2 N1 C2 C1 179.6(2) . . . . ? Fe1 N1 C2 C1 -6.2(4) . . . . ? N1 C2 C3 C4 -0.4(3) . . . . ? C1 C2 C3 C4 179.6(3) . . . . ? C2 C3 C4 N2 1.0(3) . . . . ? C2 C3 C4 C5 -179.0(3) . . . . ? N1 N2 C4 C3 -1.3(3) . . . . ? C16 N2 C4 C3 -177.9(2) . . . . ? N1 N2 C4 C5 178.7(2) . . . . ? C16 N2 C4 C5 2.0(4) . . . . ? N4 N3 C7 C8 0.5(3) . . . . ? Fe1 N3 C7 C8 -175.58(18) . . . . ? N4 N3 C7 C6 -178.2(2) . . . . ? Fe1 N3 C7 C6 5.8(4) . . . . ? N3 C7 C8 C9 -0.2(3) . . . . ? C6 C7 C8 C9 178.4(3) . . . . ? N3 N4 C9 C8 0.4(3) . . . . ? C16 N4 C9 C8 172.4(2) . . . . ? N3 N4 C9 C10 177.6(2) . . . . ? C16 N4 C9 C10 -10.5(4) . . . . ? C7 C8 C9 N4 -0.1(3) . . . . ? C7 C8 C9 C10 -176.9(3) . . . . ? N6 N5 C12 C13 -0.6(3) . . . . ? Fe1 N5 C12 C13 174.73(18) . . . . ? N6 N5 C12 C11 178.2(2) . . . . ? Fe1 N5 C12 C11 -6.5(4) . . . . ? N5 C12 C13 C14 0.6(3) . . . . ? C11 C12 C13 C14 -178.2(2) . . . . ? C12 C13 C14 N6 -0.4(3) . . . . ? C12 C13 C14 C15 179.3(3) . . . . ? N5 N6 C14 C13 0.1(3) . . . . ? C16 N6 C14 C13 -176.9(2) . . . . ? N5 N6 C14 C15 -179.7(2) . . . . ? C16 N6 C14 C15 3.3(4) . . . . ? C14 N6 C16 N2 -122.8(2) . . . . ? N5 N6 C16 N2 60.3(3) . . . . ? C14 N6 C16 N4 115.1(2) . . . . ? N5 N6 C16 N4 -61.7(2) . . . . ? C4 N2 C16 N6 113.9(3) . . . . ? N1 N2 C16 N6 -62.5(3) . . . . ? C4 N2 C16 N4 -123.7(2) . . . . ? N1 N2 C16 N4 59.9(3) . . . . ? C9 N4 C16 N6 -112.9(3) . . . . ? N3 N4 C16 N6 58.7(2) . . . . ? C9 N4 C16 N2 124.9(2) . . . . ? N3 N4 C16 N2 -63.5(2) . . . . ? N8 N7 C17 C18 -0.7(3) . . . . ? Fe1 N7 C17 C18 176.15(19) . . . . ? N7 C17 C18 C19 0.3(3) . . . . ? N7 N8 C19 C18 -0.6(3) . . . . ? C26 N8 C19 C18 -176.2(2) . . . . ? C17 C18 C19 N8 0.2(3) . . . . ? N10 N9 C20 C21 0.7(3) . . . . ? Fe1 N9 C20 C21 -175.83(18) . . . . ? N9 C20 C21 C22 -0.3(3) . . . . ? N9 N10 C22 C21 0.7(3) . . . . ? C26 N10 C22 C21 175.2(2) . . . . ? C20 C21 C22 N10 -0.3(3) . . . . ? N12 N11 C23 C24 0.0(3) . . . . ? Fe1 N11 C23 C24 177.91(19) . . . . ? N11 C23 C24 C25 -0.2(3) . . . . ? N11 N12 C25 C24 -0.2(3) . . . . ? C26 N12 C25 C24 -176.5(2) . . . . ? C23 C24 C25 N12 0.3(3) . . . . ? C22 N10 C26 N12 124.6(3) . . . . ? N9 N10 C26 N12 -61.2(3) . . . . ? C22 N10 C26 N8 -115.2(3) . . . . ? N9 N10 C26 N8 59.1(3) . . . . ? C25 N12 C26 N10 -122.4(3) . . . . ? N11 N12 C26 N10 61.6(3) . . . . ? C25 N12 C26 N8 116.9(3) . . . . ? N11 N12 C26 N8 -59.1(3) . . . . ? C19 N8 C26 N10 115.5(3) . . . . ? N7 N8 C26 N10 -59.8(3) . . . . ? C19 N8 C26 N12 -124.1(3) . . . . ? N7 N8 C26 N12 60.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.517 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.082 #=END data_1b-260K _database_code_depnum_ccdc_archive 'CCDC 650144' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H32 B2 F8 Fe N12' _chemical_formula_weight 742.11 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1881(2) _cell_length_b 12.0473(3) _cell_length_c 14.3434(3) _cell_angle_alpha 94.755(1) _cell_angle_beta 72.770(2) _cell_angle_gamma 87.116(1) _cell_volume 1670.51(7) _cell_formula_units_Z 2 _cell_measurement_temperature 260(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular block' _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.535 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 260(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 'Nonius KappaCCD' _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 21576 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0706 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 27.91 _reflns_number_total 7735 _reflns_number_gt 4654 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0843P)^2^+0.2426P] 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 7735 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1067 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1687 _refine_ls_wR_factor_gt 0.1454 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 0.64859(4) 0.72052(3) 0.74442(3) 0.03511(15) Uani 1 1 d . . . F1 F 0.6865(2) 0.1848(2) 0.73955(14) 0.0847(7) Uani 1 1 d . . . F2 F 0.7001(2) 0.26764(19) 0.60243(15) 0.0729(6) Uani 1 1 d . . . F3 F 0.6853(3) 0.0833(2) 0.60403(17) 0.1030(9) Uani 1 1 d . . . F4 F 0.5005(2) 0.1993(2) 0.68654(16) 0.0804(7) Uani 1 1 d . . . F5 F 0.1008(3) 0.7723(3) 1.0842(2) 0.1171(10) Uani 1 1 d . . . F6 F 0.0043(6) 0.6665(5) 1.0082(5) 0.287(4) Uani 1 1 d . . . F7 F -0.0680(4) 0.8353(4) 1.0364(3) 0.188(2) Uani 1 1 d . . . F8 F -0.1123(4) 0.7430(5) 1.1582(3) 0.198(2) Uani 1 1 d . . . N1 N 0.7045(2) 0.7293(2) 0.59009(16) 0.0396(6) Uani 1 1 d . . . N2 N 0.8401(2) 0.74651(19) 0.54466(15) 0.0340(5) Uani 1 1 d . . . N3 N 0.8272(2) 0.6052(2) 0.70919(17) 0.0403(6) Uani 1 1 d . . . N4 N 0.9403(2) 0.63075(19) 0.63657(16) 0.0341(5) Uani 1 1 d . . . N5 N 0.7908(2) 0.84522(19) 0.74583(16) 0.0369(5) Uani 1 1 d . . . N6 N 0.9159(2) 0.82873(18) 0.67467(15) 0.0324(5) Uani 1 1 d . . . N7 N 0.5941(2) 0.7121(2) 0.89871(17) 0.0455(6) Uani 1 1 d . . . N8 N 0.4570(2) 0.7190(2) 0.94939(16) 0.0421(6) Uani 1 1 d . . . N9 N 0.4755(2) 0.8410(2) 0.77856(17) 0.0432(6) Uani 1 1 d . . . N10 N 0.3581(2) 0.8208(2) 0.84836(17) 0.0421(6) Uani 1 1 d . . . N11 N 0.4957(3) 0.5988(2) 0.75490(18) 0.0487(6) Uani 1 1 d . . . N12 N 0.3741(3) 0.6218(2) 0.82936(18) 0.0455(6) Uani 1 1 d . . . C1 C 0.4895(3) 0.7347(4) 0.5448(3) 0.0763(12) Uani 1 1 d . . . H1A H 0.4526 0.7144 0.6103 0.114 Uiso 1 1 calc R . . H1B H 0.4757 0.6773 0.4988 0.114 Uiso 1 1 calc R . . H1C H 0.4433 0.8039 0.5387 0.114 Uiso 1 1 calc R . . C2 C 0.6399(3) 0.7479(3) 0.5239(2) 0.0453(7) Uani 1 1 d . . . C3 C 0.7318(3) 0.7784(3) 0.4387(2) 0.0454(7) Uani 1 1 d . . . H3 H 0.7109 0.7957 0.3824 0.054 Uiso 1 1 calc R . . C4 C 0.8585(3) 0.7783(2) 0.45311(19) 0.0384(7) Uani 1 1 d . . . C5 C 0.9947(3) 0.8054(3) 0.3891(2) 0.0544(9) Uani 1 1 d . . . H5A H 0.9877 0.8176 0.3254 0.082 Uiso 1 1 calc R . . H5B H 1.0621 0.7444 0.3830 0.082 Uiso 1 1 calc R . . H5C H 1.0222 0.8718 0.4176 0.082 Uiso 1 1 calc R . . C6 C 0.7704(4) 0.4534(3) 0.8173(3) 0.0687(11) Uani 1 1 d . . . H6A H 0.6801 0.4917 0.8363 0.103 Uiso 1 1 calc R . . H6B H 0.8035 0.4531 0.8734 0.103 Uiso 1 1 calc R . . H6C H 0.7661 0.3779 0.7918 0.103 Uiso 1 1 calc R . . C7 C 0.8663(3) 0.5118(3) 0.7401(2) 0.0461(7) Uani 1 1 d . . . C8 C 1.0051(3) 0.4790(3) 0.6882(2) 0.0519(8) Uani 1 1 d . . . H8 H 1.0568 0.4169 0.6968 0.062 Uiso 1 1 calc R . . C9 C 1.0492(3) 0.5551(2) 0.6234(2) 0.0394(7) Uani 1 1 d . . . C10 C 1.1855(3) 0.5592(3) 0.5475(3) 0.0591(9) Uani 1 1 d . . . H10A H 1.1723 0.5601 0.4840 0.089 Uiso 1 1 calc R . . H10B H 1.2446 0.4947 0.5477 0.089 Uiso 1 1 calc R . . H10C H 1.2271 0.6256 0.5621 0.089 Uiso 1 1 calc R . . C11 C 0.6871(4) 0.9788(3) 0.8937(2) 0.0593(9) Uani 1 1 d . . . H11A H 0.6062 0.9404 0.8956 0.089 Uiso 1 1 calc R . . H11B H 0.6687 1.0568 0.8891 0.089 Uiso 1 1 calc R . . H11C H 0.7117 0.9700 0.9524 0.089 Uiso 1 1 calc R . . C12 C 0.8031(3) 0.9310(2) 0.8065(2) 0.0406(7) Uani 1 1 d . . . C13 C 0.9352(3) 0.9685(3) 0.7749(2) 0.0486(8) Uani 1 1 d . . . H13 H 0.9688 1.0271 0.8051 0.058 Uiso 1 1 calc R . . C14 C 1.0052(3) 0.9022(2) 0.6915(2) 0.0417(7) Uani 1 1 d . . . C15 C 1.1491(3) 0.9032(3) 0.6263(3) 0.0634(10) Uani 1 1 d . . . H15A H 1.1912 0.9658 0.6481 0.095 Uiso 1 1 calc R . . H15B H 1.1482 0.9093 0.5602 0.095 Uiso 1 1 calc R . . H15C H 1.2008 0.8352 0.6286 0.095 Uiso 1 1 calc R . . C16 C 0.9388(3) 0.7379(2) 0.59826(18) 0.0303(6) Uani 1 1 d . . . H16 H 1.0302 0.7434 0.5519 0.036 Uiso 1 1 calc R . . C17 C 0.6568(4) 0.7161(3) 0.9676(2) 0.0535(8) Uani 1 1 d . . . H17 H 0.7520 0.7123 0.9549 0.064 Uiso 1 1 calc R . . C18 C 0.5636(4) 0.7266(3) 1.0604(2) 0.0586(9) Uani 1 1 d . . . H18 H 0.5833 0.7311 1.1199 0.070 Uiso 1 1 calc R . . C19 C 0.4366(4) 0.7289(3) 1.0468(2) 0.0513(8) Uani 1 1 d . . . H19 H 0.3520 0.7361 1.0955 0.062 Uiso 1 1 calc R . . C20 C 0.4510(3) 0.9428(3) 0.7554(2) 0.0517(8) Uani 1 1 d . . . H20 H 0.5133 0.9788 0.7086 0.062 Uiso 1 1 calc R . . C21 C 0.3203(4) 0.9885(3) 0.8101(2) 0.0558(9) Uani 1 1 d . . . H21 H 0.2799 1.0586 0.8073 0.067 Uiso 1 1 calc R . . C22 C 0.2638(3) 0.9093(3) 0.8688(2) 0.0489(8) Uani 1 1 d . . . H22 H 0.1765 0.9151 0.9144 0.059 Uiso 1 1 calc R . . C23 C 0.4818(4) 0.4988(3) 0.7133(3) 0.0593(9) Uani 1 1 d . . . H23 H 0.5484 0.4606 0.6596 0.071 Uiso 1 1 calc R . . C24 C 0.3567(4) 0.4586(3) 0.7591(3) 0.0676(10) Uani 1 1 d . . . H24 H 0.3246 0.3911 0.7426 0.081 Uiso 1 1 calc R . . C25 C 0.2905(4) 0.5381(3) 0.8334(3) 0.0590(9) Uani 1 1 d . . . H25 H 0.2040 0.5352 0.8784 0.071 Uiso 1 1 calc R . . C26 C 0.3549(3) 0.7212(3) 0.8970(2) 0.0435(7) Uani 1 1 d . . . H26 H 0.2638 0.7219 0.9454 0.052 Uiso 1 1 calc R . . B1 B 0.6425(4) 0.1829(3) 0.6588(3) 0.0510(9) Uani 1 1 d . . . B2 B -0.0218(4) 0.7476(4) 1.0737(3) 0.0670(12) 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 Fe1 0.0271(2) 0.0408(3) 0.0329(2) 0.00278(17) -0.00242(17) -0.00237(17) F1 0.0767(15) 0.133(2) 0.0478(12) 0.0239(12) -0.0202(11) -0.0072(14) F2 0.0675(14) 0.0832(16) 0.0820(14) 0.0413(12) -0.0313(11) -0.0285(12) F3 0.125(2) 0.0708(16) 0.0769(15) -0.0134(12) 0.0216(14) -0.0204(15) F4 0.0501(13) 0.1092(19) 0.0844(15) 0.0263(13) -0.0185(11) -0.0143(12) F5 0.0574(16) 0.180(3) 0.108(2) 0.0019(19) -0.0187(14) -0.0106(17) F6 0.223(6) 0.249(6) 0.352(7) -0.214(6) -0.104(5) 0.027(4) F7 0.161(4) 0.231(5) 0.179(4) 0.068(3) -0.059(3) 0.053(3) F8 0.094(2) 0.259(5) 0.201(4) 0.085(4) 0.038(3) -0.032(3) N1 0.0234(11) 0.0535(16) 0.0411(13) 0.0040(11) -0.0079(10) -0.0069(10) N2 0.0240(11) 0.0433(14) 0.0340(12) 0.0054(10) -0.0073(9) -0.0032(10) N3 0.0304(12) 0.0396(14) 0.0459(14) 0.0104(11) -0.0022(10) -0.0037(10) N4 0.0244(11) 0.0348(13) 0.0397(13) 0.0064(10) -0.0036(10) -0.0024(10) N5 0.0297(12) 0.0383(14) 0.0383(13) -0.0005(10) -0.0047(10) -0.0033(10) N6 0.0260(11) 0.0348(13) 0.0335(12) 0.0008(9) -0.0051(9) -0.0028(10) N7 0.0367(14) 0.0542(17) 0.0423(14) 0.0038(11) -0.0070(11) -0.0029(12) N8 0.0405(14) 0.0467(15) 0.0343(14) 0.0042(10) -0.0041(11) -0.0037(11) N9 0.0377(14) 0.0437(15) 0.0423(14) 0.0066(11) -0.0028(11) -0.0012(11) N10 0.0346(13) 0.0437(15) 0.0425(14) 0.0035(11) -0.0038(11) -0.0002(11) N11 0.0435(15) 0.0504(17) 0.0454(14) -0.0030(12) -0.0054(12) -0.0011(12) N12 0.0380(14) 0.0438(15) 0.0484(15) 0.0018(11) -0.0036(11) -0.0061(11) C1 0.0345(18) 0.135(4) 0.065(2) 0.013(2) -0.0215(17) -0.011(2) C2 0.0329(16) 0.061(2) 0.0443(17) 0.0005(14) -0.0168(14) -0.0033(14) C3 0.0417(17) 0.063(2) 0.0354(16) 0.0083(14) -0.0169(13) -0.0019(15) C4 0.0389(16) 0.0420(17) 0.0342(15) 0.0044(12) -0.0110(12) -0.0025(13) C5 0.0477(19) 0.071(2) 0.0450(18) 0.0180(16) -0.0099(15) -0.0122(17) C6 0.068(2) 0.051(2) 0.078(3) 0.0291(18) -0.002(2) -0.0039(18) C7 0.0444(18) 0.0377(17) 0.0551(18) 0.0137(14) -0.0110(14) -0.0043(14) C8 0.0444(18) 0.0418(19) 0.067(2) 0.0132(15) -0.0113(16) 0.0015(15) C9 0.0310(15) 0.0353(16) 0.0502(17) 0.0037(13) -0.0105(13) 0.0015(12) C10 0.0342(17) 0.053(2) 0.079(2) 0.0091(17) -0.0013(16) 0.0075(15) C11 0.065(2) 0.053(2) 0.0469(19) -0.0133(15) -0.0027(16) -0.0018(17) C12 0.0462(17) 0.0366(16) 0.0363(15) -0.0005(12) -0.0094(13) -0.0026(13) C13 0.056(2) 0.0423(18) 0.0498(18) -0.0019(14) -0.0189(15) -0.0150(15) C14 0.0378(16) 0.0408(17) 0.0480(17) 0.0016(13) -0.0148(13) -0.0099(13) C15 0.0391(18) 0.072(3) 0.072(2) -0.0093(18) -0.0087(16) -0.0216(17) C16 0.0240(13) 0.0346(15) 0.0312(14) 0.0055(11) -0.0056(11) -0.0042(11) C17 0.056(2) 0.059(2) 0.052(2) 0.0071(15) -0.0265(17) -0.0010(16) C18 0.075(3) 0.064(2) 0.0395(19) 0.0107(15) -0.0201(17) -0.0083(19) C19 0.065(2) 0.0459(19) 0.0341(17) 0.0075(13) -0.0012(15) -0.0049(16) C20 0.055(2) 0.047(2) 0.056(2) 0.0115(15) -0.0177(16) -0.0047(16) C21 0.063(2) 0.044(2) 0.064(2) 0.0011(16) -0.0268(18) 0.0120(17) C22 0.0381(17) 0.055(2) 0.0499(18) -0.0063(15) -0.0126(14) 0.0102(15) C23 0.068(2) 0.050(2) 0.060(2) -0.0116(16) -0.0261(18) 0.0065(18) C24 0.072(3) 0.045(2) 0.092(3) 0.0016(19) -0.035(2) -0.0111(19) C25 0.050(2) 0.059(2) 0.072(2) 0.0100(18) -0.0201(18) -0.0194(18) C26 0.0325(15) 0.0479(19) 0.0422(17) 0.0027(13) 0.0004(13) -0.0034(13) B1 0.051(2) 0.063(3) 0.037(2) 0.0113(17) -0.0067(16) -0.0103(19) B2 0.044(2) 0.080(3) 0.070(3) -0.006(2) -0.012(2) 0.005(2) _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 N7 2.129(2) . ? Fe1 N1 2.129(2) . ? Fe1 N9 2.138(2) . ? Fe1 N3 2.140(2) . ? Fe1 N5 2.142(2) . ? Fe1 N11 2.175(3) . ? F1 B1 1.359(4) . ? F2 B1 1.399(4) . ? F3 B1 1.355(5) . ? F4 B1 1.381(4) . ? F5 B2 1.347(5) . ? F6 B2 1.257(5) . ? F7 B2 1.347(6) . ? F8 B2 1.295(5) . ? N1 C2 1.333(4) . ? N1 N2 1.376(3) . ? N2 C4 1.360(3) . ? N2 C16 1.440(3) . ? N3 C7 1.328(4) . ? N3 N4 1.373(3) . ? N4 C9 1.357(4) . ? N4 C16 1.445(3) . ? N5 C12 1.331(3) . ? N5 N6 1.370(3) . ? N6 C14 1.358(3) . ? N6 C16 1.441(3) . ? N7 C17 1.325(4) . ? N7 N8 1.365(3) . ? N8 C19 1.344(4) . ? N8 C26 1.453(4) . ? N9 C20 1.327(4) . ? N9 N10 1.361(3) . ? N10 C22 1.351(4) . ? N10 C26 1.435(4) . ? N11 C23 1.333(4) . ? N11 N12 1.373(3) . ? N12 C25 1.346(4) . ? N12 C26 1.444(4) . ? C1 C2 1.492(4) . ? C2 C3 1.392(4) . ? C3 C4 1.367(4) . ? C4 C5 1.489(4) . ? C6 C7 1.495(4) . ? C7 C8 1.408(4) . ? C8 C9 1.358(4) . ? C9 C10 1.495(4) . ? C11 C12 1.493(4) . ? C12 C13 1.397(4) . ? C13 C14 1.363(4) . ? C14 C15 1.489(4) . ? C17 C18 1.379(5) . ? C18 C19 1.364(5) . ? C20 C21 1.388(5) . ? C21 C22 1.361(5) . ? C23 C24 1.382(5) . ? C24 C25 1.360(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 N7 Fe1 N1 179.60(9) . . ? N7 Fe1 N9 85.16(9) . . ? N1 Fe1 N9 95.06(9) . . ? N7 Fe1 N3 95.43(9) . . ? N1 Fe1 N3 84.34(9) . . ? N9 Fe1 N3 177.72(9) . . ? N7 Fe1 N5 93.65(9) . . ? N1 Fe1 N5 86.00(9) . . ? N9 Fe1 N5 93.21(9) . . ? N3 Fe1 N5 84.56(9) . . ? N7 Fe1 N11 82.30(9) . . ? N1 Fe1 N11 98.05(9) . . ? N9 Fe1 N11 84.50(10) . . ? N3 Fe1 N11 97.76(9) . . ? N5 Fe1 N11 175.49(8) . . ? C2 N1 N2 104.8(2) . . ? C2 N1 Fe1 137.00(19) . . ? N2 N1 Fe1 116.17(16) . . ? C4 N2 N1 111.7(2) . . ? C4 N2 C16 128.7(2) . . ? N1 N2 C16 119.4(2) . . ? C7 N3 N4 105.5(2) . . ? C7 N3 Fe1 138.14(19) . . ? N4 N3 Fe1 116.30(17) . . ? C9 N4 N3 111.4(2) . . ? C9 N4 C16 128.3(2) . . ? N3 N4 C16 119.3(2) . . ? C12 N5 N6 105.2(2) . . ? C12 N5 Fe1 137.50(19) . . ? N6 N5 Fe1 116.45(16) . . ? C14 N6 N5 111.4(2) . . ? C14 N6 C16 129.2(2) . . ? N5 N6 C16 119.3(2) . . ? C17 N7 N8 104.5(2) . . ? C17 N7 Fe1 137.5(2) . . ? N8 N7 Fe1 117.37(18) . . ? C19 N8 N7 111.3(3) . . ? C19 N8 C26 128.5(3) . . ? N7 N8 C26 120.1(2) . . ? C20 N9 N10 105.0(2) . . ? C20 N9 Fe1 136.5(2) . . ? N10 N9 Fe1 118.16(18) . . ? C22 N10 N9 111.0(2) . . ? C22 N10 C26 129.1(3) . . ? N9 N10 C26 119.4(2) . . ? C23 N11 N12 103.6(3) . . ? C23 N11 Fe1 139.8(2) . . ? N12 N11 Fe1 116.49(18) . . ? C25 N12 N11 111.8(3) . . ? C25 N12 C26 128.1(3) . . ? N11 N12 C26 119.9(2) . . ? N1 C2 C3 110.6(3) . . ? N1 C2 C1 121.2(3) . . ? C3 C2 C1 128.2(3) . . ? C4 C3 C2 107.2(2) . . ? N2 C4 C3 105.7(2) . . ? N2 C4 C5 122.8(3) . . ? C3 C4 C5 131.5(3) . . ? N3 C7 C8 109.8(3) . . ? N3 C7 C6 122.5(3) . . ? C8 C7 C6 127.6(3) . . ? C9 C8 C7 107.0(3) . . ? N4 C9 C8 106.3(2) . . ? N4 C9 C10 123.6(3) . . ? C8 C9 C10 130.0(3) . . ? N5 C12 C13 110.5(3) . . ? N5 C12 C11 122.6(3) . . ? C13 C12 C11 126.9(3) . . ? C14 C13 C12 106.7(3) . . ? N6 C14 C13 106.3(2) . . ? N6 C14 C15 123.2(3) . . ? C13 C14 C15 130.5(3) . . ? N2 C16 N6 111.6(2) . . ? N2 C16 N4 111.4(2) . . ? N6 C16 N4 111.5(2) . . ? N7 C17 C18 111.7(3) . . ? C19 C18 C17 105.6(3) . . ? N8 C19 C18 106.9(3) . . ? N9 C20 C21 111.2(3) . . ? C22 C21 C20 105.6(3) . . ? N10 C22 C21 107.2(3) . . ? N11 C23 C24 112.1(3) . . ? C25 C24 C23 105.7(3) . . ? N12 C25 C24 106.9(3) . . ? N10 C26 N12 111.7(2) . . ? N10 C26 N8 110.9(2) . . ? N12 C26 N8 110.7(2) . . ? F3 B1 F1 109.3(3) . . ? F3 B1 F4 110.3(3) . . ? F1 B1 F4 110.1(3) . . ? F3 B1 F2 108.5(3) . . ? F1 B1 F2 109.3(3) . . ? F4 B1 F2 109.4(3) . . ? F6 B2 F8 121.0(6) . . ? F6 B2 F5 105.7(4) . . ? F8 B2 F5 111.0(4) . . ? F6 B2 F7 106.8(6) . . ? F8 B2 F7 105.0(4) . . ? F5 B2 F7 106.4(5) . . ? 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 N7 Fe1 N1 C2 -156(14) . . . . ? N9 Fe1 N1 C2 -31.9(3) . . . . ? N3 Fe1 N1 C2 150.3(3) . . . . ? N5 Fe1 N1 C2 -124.8(3) . . . . ? N11 Fe1 N1 C2 53.2(3) . . . . ? N7 Fe1 N1 N2 5(14) . . . . ? N9 Fe1 N1 N2 128.73(19) . . . . ? N3 Fe1 N1 N2 -49.06(19) . . . . ? N5 Fe1 N1 N2 35.86(19) . . . . ? N11 Fe1 N1 N2 -146.12(19) . . . . ? C2 N1 N2 C4 1.7(3) . . . . ? Fe1 N1 N2 C4 -164.79(19) . . . . ? C2 N1 N2 C16 177.3(2) . . . . ? Fe1 N1 N2 C16 10.8(3) . . . . ? N7 Fe1 N3 C7 36.9(3) . . . . ? N1 Fe1 N3 C7 -143.4(3) . . . . ? N9 Fe1 N3 C7 142(2) . . . . ? N5 Fe1 N3 C7 130.1(3) . . . . ? N11 Fe1 N3 C7 -46.0(3) . . . . ? N7 Fe1 N3 N4 -140.29(19) . . . . ? N1 Fe1 N3 N4 39.39(18) . . . . ? N9 Fe1 N3 N4 -36(2) . . . . ? N5 Fe1 N3 N4 -47.12(18) . . . . ? N11 Fe1 N3 N4 136.77(19) . . . . ? C7 N3 N4 C9 -0.9(3) . . . . ? Fe1 N3 N4 C9 177.18(18) . . . . ? C7 N3 N4 C16 -170.1(2) . . . . ? Fe1 N3 N4 C16 7.9(3) . . . . ? N7 Fe1 N5 C12 -32.4(3) . . . . ? N1 Fe1 N5 C12 147.8(3) . . . . ? N9 Fe1 N5 C12 52.9(3) . . . . ? N3 Fe1 N5 C12 -127.5(3) . . . . ? N11 Fe1 N5 C12 -6.3(13) . . . . ? N7 Fe1 N5 N6 134.72(18) . . . . ? N1 Fe1 N5 N6 -45.07(18) . . . . ? N9 Fe1 N5 N6 -139.93(18) . . . . ? N3 Fe1 N5 N6 39.61(18) . . . . ? N11 Fe1 N5 N6 160.8(11) . . . . ? C12 N5 N6 C14 0.7(3) . . . . ? Fe1 N5 N6 C14 -170.32(19) . . . . ? C12 N5 N6 C16 177.8(2) . . . . ? Fe1 N5 N6 C16 6.8(3) . . . . ? N1 Fe1 N7 C17 -7(14) . . . . ? N9 Fe1 N7 C17 -131.0(3) . . . . ? N3 Fe1 N7 C17 46.8(3) . . . . ? N5 Fe1 N7 C17 -38.0(3) . . . . ? N11 Fe1 N7 C17 144.0(3) . . . . ? N1 Fe1 N7 N8 161(48) . . . . ? N9 Fe1 N7 N8 37.6(2) . . . . ? N3 Fe1 N7 N8 -144.6(2) . . . . ? N5 Fe1 N7 N8 130.5(2) . . . . ? N11 Fe1 N7 N8 -47.5(2) . . . . ? C17 N7 N8 C19 1.0(3) . . . . ? Fe1 N7 N8 C19 -171.0(2) . . . . ? C17 N7 N8 C26 177.8(3) . . . . ? Fe1 N7 N8 C26 5.8(3) . . . . ? N7 Fe1 N9 C20 130.7(3) . . . . ? N1 Fe1 N9 C20 -49.0(3) . . . . ? N3 Fe1 N9 C20 26(2) . . . . ? N5 Fe1 N9 C20 37.3(3) . . . . ? N11 Fe1 N9 C20 -146.6(3) . . . . ? N7 Fe1 N9 N10 -41.5(2) . . . . ? N1 Fe1 N9 N10 138.8(2) . . . . ? N3 Fe1 N9 N10 -146(2) . . . . ? N5 Fe1 N9 N10 -134.9(2) . . . . ? N11 Fe1 N9 N10 41.2(2) . . . . ? C20 N9 N10 C22 -0.9(3) . . . . ? Fe1 N9 N10 C22 173.57(19) . . . . ? C20 N9 N10 C26 -173.7(3) . . . . ? Fe1 N9 N10 C26 0.7(3) . . . . ? N7 Fe1 N11 C23 -129.6(4) . . . . ? N1 Fe1 N11 C23 50.2(4) . . . . ? N9 Fe1 N11 C23 144.6(4) . . . . ? N3 Fe1 N11 C23 -35.1(4) . . . . ? N5 Fe1 N11 C23 -155.9(11) . . . . ? N7 Fe1 N11 N12 45.5(2) . . . . ? N1 Fe1 N11 N12 -134.7(2) . . . . ? N9 Fe1 N11 N12 -40.4(2) . . . . ? N3 Fe1 N11 N12 140.0(2) . . . . ? N5 Fe1 N11 N12 19.2(13) . . . . ? C23 N11 N12 C25 0.8(4) . . . . ? Fe1 N11 N12 C25 -175.9(2) . . . . ? C23 N11 N12 C26 175.1(3) . . . . ? Fe1 N11 N12 C26 -1.6(3) . . . . ? N2 N1 C2 C3 -1.1(3) . . . . ? Fe1 N1 C2 C3 161.0(2) . . . . ? N2 N1 C2 C1 178.5(3) . . . . ? Fe1 N1 C2 C1 -19.5(5) . . . . ? N1 C2 C3 C4 0.2(4) . . . . ? C1 C2 C3 C4 -179.3(4) . . . . ? N1 N2 C4 C3 -1.6(3) . . . . ? C16 N2 C4 C3 -176.7(3) . . . . ? N1 N2 C4 C5 178.2(3) . . . . ? C16 N2 C4 C5 3.2(5) . . . . ? C2 C3 C4 N2 0.9(3) . . . . ? C2 C3 C4 C5 -178.9(3) . . . . ? N4 N3 C7 C8 1.0(3) . . . . ? Fe1 N3 C7 C8 -176.4(2) . . . . ? N4 N3 C7 C6 -177.8(3) . . . . ? Fe1 N3 C7 C6 4.8(5) . . . . ? N3 C7 C8 C9 -0.8(4) . . . . ? C6 C7 C8 C9 177.9(3) . . . . ? N3 N4 C9 C8 0.4(3) . . . . ? C16 N4 C9 C8 168.4(3) . . . . ? N3 N4 C9 C10 178.3(3) . . . . ? C16 N4 C9 C10 -13.7(5) . . . . ? C7 C8 C9 N4 0.2(4) . . . . ? C7 C8 C9 C10 -177.5(3) . . . . ? N6 N5 C12 C13 -0.5(3) . . . . ? Fe1 N5 C12 C13 167.6(2) . . . . ? N6 N5 C12 C11 178.1(3) . . . . ? Fe1 N5 C12 C11 -13.8(5) . . . . ? N5 C12 C13 C14 0.1(4) . . . . ? C11 C12 C13 C14 -178.4(3) . . . . ? N5 N6 C14 C13 -0.7(3) . . . . ? C16 N6 C14 C13 -177.4(3) . . . . ? N5 N6 C14 C15 179.6(3) . . . . ? C16 N6 C14 C15 2.8(5) . . . . ? C12 C13 C14 N6 0.3(3) . . . . ? C12 C13 C14 C15 -179.9(3) . . . . ? C4 N2 C16 N6 105.1(3) . . . . ? N1 N2 C16 N6 -69.6(3) . . . . ? C4 N2 C16 N4 -129.5(3) . . . . ? N1 N2 C16 N4 55.7(3) . . . . ? C14 N6 C16 N2 -125.5(3) . . . . ? N5 N6 C16 N2 58.0(3) . . . . ? C14 N6 C16 N4 109.3(3) . . . . ? N5 N6 C16 N4 -67.3(3) . . . . ? C9 N4 C16 N2 125.2(3) . . . . ? N3 N4 C16 N2 -67.6(3) . . . . ? C9 N4 C16 N6 -109.4(3) . . . . ? N3 N4 C16 N6 57.8(3) . . . . ? N8 N7 C17 C18 -0.6(4) . . . . ? Fe1 N7 C17 C18 168.9(2) . . . . ? N7 C17 C18 C19 0.1(4) . . . . ? N7 N8 C19 C18 -1.0(4) . . . . ? C26 N8 C19 C18 -177.5(3) . . . . ? C17 C18 C19 N8 0.6(4) . . . . ? N10 N9 C20 C21 0.7(3) . . . . ? Fe1 N9 C20 C21 -172.2(2) . . . . ? N9 C20 C21 C22 -0.2(4) . . . . ? N9 N10 C22 C21 0.7(3) . . . . ? C26 N10 C22 C21 172.7(3) . . . . ? C20 C21 C22 N10 -0.3(4) . . . . ? N12 N11 C23 C24 -0.3(4) . . . . ? Fe1 N11 C23 C24 175.2(3) . . . . ? N11 C23 C24 C25 -0.3(4) . . . . ? N11 N12 C25 C24 -1.0(4) . . . . ? C26 N12 C25 C24 -174.7(3) . . . . ? C23 C24 C25 N12 0.8(4) . . . . ? C22 N10 C26 N12 125.5(3) . . . . ? N9 N10 C26 N12 -63.1(3) . . . . ? C22 N10 C26 N8 -110.5(3) . . . . ? N9 N10 C26 N8 60.9(3) . . . . ? C25 N12 C26 N10 -123.5(3) . . . . ? N11 N12 C26 N10 63.3(3) . . . . ? C25 N12 C26 N8 112.5(3) . . . . ? N11 N12 C26 N8 -60.8(3) . . . . ? C19 N8 C26 N10 110.7(3) . . . . ? N7 N8 C26 N10 -65.5(3) . . . . ? C19 N8 C26 N12 -124.8(3) . . . . ? N7 N8 C26 N12 59.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.626 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.064 #=END data_2-123K _database_code_depnum_ccdc_archive 'CCDC 650145' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H38 Fe N12, 2(B F4), 1.5(C2 H3 N)' _chemical_formula_sum 'C32 H42.50 B2 F8 Fe N13.50' _chemical_formula_weight 845.76 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' 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 Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.172(2) _cell_length_b 12.611(3) _cell_length_c 15.108(3) _cell_angle_alpha 88.65(3) _cell_angle_beta 79.31(3) _cell_angle_gamma 64.01(3) _cell_volume 2044.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 0.448 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _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 33971 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 28.29 _reflns_number_total 9933 _reflns_number_gt 6220 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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. One of the two crystallographically distinct MeCN solvent molucules (N14, C32, C33) exhibits two-fold symmetry-related disorder, where the alternate positons are in close proximity and can not be occupied simultaneously. The occupancies of these atoms were fixed to be 0.5. Both BF4 counterions exhibit two-fold positional disorder on all atoms. Pairs of atom sites were appropriately selected and separated into parts (alternate orientations indicated by ' in atom name) to account for the disorder. Equivalent atoms were fixed to have the same ADPs. The relative occupancy of the two components was refined. The disorder of the MeCN molecule and one of the BF4 molecules are correlated, with the B2-F8 positions in close proximity to one of the MeCN orientatios which therefore cannot be occupied simultaneously. The alternate position of B2'-F8' is not in close proximity to either MeCN orientation. ; _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^)+(0.0765P)^2^+0.4451P] 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 9933 _refine_ls_number_parameters 614 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0964 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1514 _refine_ls_wR_factor_gt 0.1309 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.049 _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 0.68939(3) 0.62116(3) 0.737413(19) 0.03948(12) Uani 1 1 d . . . F1 F 0.6336(7) 0.8452(7) 0.3639(5) 0.104(2) Uani 0.504(8) 1 d PDU A 1 F2 F 0.4599(7) 0.8131(9) 0.3924(4) 0.122(3) Uani 0.504(8) 1 d PDU A 1 B1 B 0.5314(12) 0.8511(9) 0.3313(8) 0.0768(13) Uani 0.504(8) 1 d PDU A 1 F3 F 0.4627(5) 0.9684(4) 0.3251(6) 0.115(2) Uani 0.504(8) 1 d PDU A 1 F4 F 0.5531(8) 0.8041(9) 0.2468(5) 0.153(3) Uani 0.504(8) 1 d PDU A 1 F1' F 0.6425(7) 0.7822(13) 0.3486(7) 0.233(7) Uani 0.496(8) 1 d PDU A 2 F2' F 0.4994(19) 0.7776(13) 0.3511(13) 0.288(9) Uani 0.496(8) 1 d PDU A 2 B1' B 0.5390(15) 0.8517(10) 0.3306(9) 0.0768(13) Uani 0.50 1 d PDU A 2 F3' F 0.4845(12) 0.9345(8) 0.3905(8) 0.225(6) Uani 0.496(8) 1 d PDU A 2 F4' F 0.5375(16) 0.8844(12) 0.2546(7) 0.280(7) Uani 0.496(8) 1 d PDU A 2 F5 F 1.0026(11) 0.3368(8) 1.1441(10) 0.140(4) Uani 0.461(7) 1 d PDU B 1 F6 F 0.9492(10) 0.2180(11) 1.2426(4) 0.145(5) Uani 0.461(7) 1 d PDU B 1 B2 B 0.9595(17) 0.2503(10) 1.1554(9) 0.097(2) Uani 0.461(7) 1 d PDU B 1 F7 F 0.8547(11) 0.3037(10) 1.1198(7) 0.104(2) Uani 0.461(7) 1 d PDU B 1 F8 F 1.0294(12) 0.1473(7) 1.1046(6) 0.241(6) Uani 0.461(7) 1 d PDU B 1 F5' F 1.0353(11) 0.2919(17) 1.1290(8) 0.254(7) Uani 0.539(7) 1 d PDU B 2 F6' F 0.9916(12) 0.1884(9) 1.2165(10) 0.221(6) Uani 0.539(7) 1 d PDU B 2 B2' B 0.9329(11) 0.2885(13) 1.1821(6) 0.097(2) Uani 0.54 1 d PDU B 2 F7' F 0.8535(13) 0.2823(13) 1.1415(10) 0.191(6) Uani 0.539(7) 1 d PDU B 2 F8' F 0.8745(7) 0.3778(7) 1.2462(4) 0.169(3) Uani 0.539(7) 1 d PDU B 2 N11 N 0.50707(19) 0.74831(19) 0.71063(13) 0.0525(5) Uani 1 1 d . C 2 N12 N 0.50569(18) 0.78683(17) 0.62612(13) 0.0446(5) Uani 1 1 d . C 2 N7 N 0.75344(19) 0.73654(18) 0.65723(13) 0.0483(5) Uani 1 1 d . C 2 N8 N 0.71150(18) 0.76768(17) 0.57817(13) 0.0453(5) Uani 1 1 d . C 2 N9 N 0.71009(19) 0.54024(17) 0.60699(12) 0.0461(5) Uani 1 1 d . C 2 N10 N 0.66273(18) 0.61274(17) 0.54149(12) 0.0422(4) Uani 1 1 d . C 2 N3 N 0.67216(18) 0.68833(16) 0.87201(12) 0.0444(5) Uani 1 1 d . C 2 N4 N 0.72228(17) 0.60392(16) 0.93108(11) 0.0393(4) Uani 1 1 d . C 2 N1 N 0.62212(17) 0.50181(17) 0.80874(12) 0.0419(4) Uani 1 1 d . C 2 N2 N 0.67203(16) 0.45453(16) 0.88315(11) 0.0379(4) Uani 1 1 d . C 2 N5 N 0.87154(17) 0.49241(17) 0.75468(12) 0.0420(4) Uani 1 1 d . C 2 N6 N 0.87749(16) 0.43884(16) 0.83492(11) 0.0391(4) Uani 1 1 d . C 2 N13 N 0.8670(4) 0.2063(4) 0.7180(4) 0.1557(19) Uani 1 1 d . D 2 N14 N 0.2518(10) 0.9853(8) 0.9767(8) 0.137(3) Uani 0.50 1 d P E -1 C25 C 0.3910(3) 0.8128(2) 0.75499(19) 0.0612(7) Uani 1 1 d . C 2 H25 H 0.3627 0.8052 0.8167 0.073 Uiso 1 1 calc R C 2 C26 C 0.3160(2) 0.8919(2) 0.7018(2) 0.0604(7) Uani 1 1 d . C 2 C27 C 0.3927(2) 0.8731(2) 0.61983(19) 0.0537(6) Uani 1 1 d . C 2 H27 H 0.3705 0.9137 0.5674 0.064 Uiso 1 1 calc R C 2 C17 C 0.8366(3) 0.7778(2) 0.6550(2) 0.0589(7) Uani 1 1 d . C 2 H17 H 0.8822 0.7694 0.7015 0.071 Uiso 1 1 calc R C 2 C18 C 0.8498(3) 0.8352(3) 0.5764(2) 0.0620(7) Uani 1 1 d . C 2 C19 C 0.7677(2) 0.8270(2) 0.52936(18) 0.0548(6) Uani 1 1 d . C 2 H19 H 0.7530 0.8577 0.4724 0.066 Uiso 1 1 calc R C 2 C21 C 0.7369(2) 0.4333(2) 0.57556(17) 0.0511(6) Uani 1 1 d . C 2 H21 H 0.7734 0.3638 0.6067 0.061 Uiso 1 1 calc R C 2 C22 C 0.7053(2) 0.4341(2) 0.49137(17) 0.0537(6) Uani 1 1 d . C 2 C23 C 0.6586(2) 0.5507(2) 0.47226(16) 0.0514(6) Uani 1 1 d . C 2 H23 H 0.6286 0.5823 0.4191 0.062 Uiso 1 1 calc R C 2 C29 C 0.6168(2) 0.7385(2) 0.55650(15) 0.0434(5) Uani 1 1 d . C 2 H29 H 0.5942 0.7755 0.4992 0.052 Uiso 1 1 calc R C 2 C6 C 0.5801(3) 0.9041(2) 0.8733(2) 0.0766(9) Uani 1 1 d . C 2 H6A H 0.6080 0.8910 0.8076 0.115 Uiso 1 1 calc R C 2 H6B H 0.6046 0.9613 0.8957 0.115 Uiso 1 1 calc R C 2 H6C H 0.4892 0.9351 0.8884 0.115 Uiso 1 1 calc R C 2 C7 C 0.6385(2) 0.7905(2) 0.91601(17) 0.0505(6) Uani 1 1 d . C 2 C8 C 0.6659(2) 0.7721(2) 1.00249(17) 0.0539(6) Uani 1 1 d . C 2 H8 H 0.6496 0.8314 1.0473 0.065 Uiso 1 1 calc R C 2 C9 C 0.7202(2) 0.6535(2) 1.01053(14) 0.0432(5) Uani 1 1 d . C 2 C10 C 0.7717(3) 0.5821(3) 1.08662(17) 0.0594(7) Uani 1 1 d . C 2 H10A H 0.8625 0.5385 1.0690 0.089 Uiso 1 1 calc R C 2 H10B H 0.7359 0.5262 1.1006 0.089 Uiso 1 1 calc R C 2 H10C H 0.7503 0.6350 1.1401 0.089 Uiso 1 1 calc R C 2 C1 C 0.4674(3) 0.4870(3) 0.73006(19) 0.0669(8) Uani 1 1 d . C 2 H1A H 0.3788 0.5285 0.7579 0.100 Uiso 1 1 calc R C 2 H1B H 0.4829 0.4148 0.6963 0.100 Uiso 1 1 calc R C 2 H1C H 0.4902 0.5384 0.6888 0.100 Uiso 1 1 calc R C 2 C2 C 0.5439(2) 0.4554(2) 0.80192(16) 0.0459(5) Uani 1 1 d . C 2 C3 C 0.5451(2) 0.3791(2) 0.87060(17) 0.0495(6) Uani 1 1 d . C 2 H3 H 0.4981 0.3350 0.8802 0.059 Uiso 1 1 calc R C 2 C4 C 0.6266(2) 0.3800(2) 0.92116(15) 0.0427(5) Uani 1 1 d . C 2 C5 C 0.6623(3) 0.3160(3) 1.00373(18) 0.0613(7) Uani 1 1 d . C 2 H5A H 0.7509 0.2601 0.9905 0.092 Uiso 1 1 calc R C 2 H5B H 0.6124 0.2730 1.0220 0.092 Uiso 1 1 calc R C 2 H5C H 0.6471 0.3732 1.0528 0.092 Uiso 1 1 calc R C 2 C11 C 1.0189(3) 0.4670(3) 0.61135(19) 0.0724(9) Uani 1 1 d . C 2 H11A H 0.9439 0.5029 0.5849 0.109 Uiso 1 1 calc R C 2 H11B H 1.0806 0.3957 0.5745 0.109 Uiso 1 1 calc R C 2 H11C H 1.0538 0.5235 0.6132 0.109 Uiso 1 1 calc R C 2 C12 C 0.9858(2) 0.4352(2) 0.70468(16) 0.0480(6) Uani 1 1 d . C 2 C13 C 1.0628(2) 0.3467(2) 0.75240(18) 0.0538(6) Uani 1 1 d . C 2 H13 H 1.1482 0.2941 0.7316 0.065 Uiso 1 1 calc R C 2 C14 C 0.9923(2) 0.3498(2) 0.83472(16) 0.0460(6) Uani 1 1 d . C 2 C15 C 1.0242(3) 0.2739(3) 0.9119(2) 0.0704(8) Uani 1 1 d . C 2 H15A H 1.0043 0.3237 0.9668 0.106 Uiso 1 1 calc R C 2 H15B H 1.1133 0.2197 0.8992 0.106 Uiso 1 1 calc R C 2 H15C H 0.9759 0.2281 0.9204 0.106 Uiso 1 1 calc R C 2 C16 C 0.76865(19) 0.48028(18) 0.90563(14) 0.0364(5) Uani 1 1 d . C 2 H16 H 0.7945 0.4359 0.9598 0.044 Uiso 1 1 calc R C 2 C28 C 0.1817(3) 0.9787(3) 0.7274(3) 0.1029(13) Uani 1 1 d . C 2 H28A H 0.1509 1.0140 0.6732 0.154 Uiso 1 1 calc R C 2 H28B H 0.1730 1.0410 0.7696 0.154 Uiso 1 1 calc R C 2 H28C H 0.1332 0.9381 0.7563 0.154 Uiso 1 1 calc R C 2 C20 C 0.9335(4) 0.8949(4) 0.5494(3) 0.1079(13) Uani 1 1 d . C 2 H20A H 0.9885 0.8592 0.4912 0.162 Uiso 1 1 calc R C 2 H20B H 0.9838 0.8851 0.5954 0.162 Uiso 1 1 calc R C 2 H20C H 0.8824 0.9793 0.5441 0.162 Uiso 1 1 calc R C 2 C24 C 0.7174(4) 0.3303(3) 0.4367(2) 0.0891(11) Uani 1 1 d . C 2 H24A H 0.6372 0.3480 0.4203 0.134 Uiso 1 1 calc R C 2 H24B H 0.7420 0.2606 0.4724 0.134 Uiso 1 1 calc R C 2 H24C H 0.7808 0.3147 0.3818 0.134 Uiso 1 1 calc R C 2 C30 C 0.8225(4) 0.1473(4) 0.7439(3) 0.1003(13) Uani 1 1 d . D 2 C31 C 0.7654(5) 0.0733(4) 0.7763(4) 0.1404(19) Uani 1 1 d . D 2 H31A H 0.6843 0.1208 0.8152 0.211 Uiso 1 1 calc R D 2 H31B H 0.8188 0.0122 0.8110 0.211 Uiso 1 1 calc R D 2 H31C H 0.7535 0.0358 0.7251 0.211 Uiso 1 1 calc R D 2 C32 C 0.1610(15) 0.9913(11) 0.9952(10) 0.162(6) Uani 0.50 1 d P E -1 C33 C 0.034(2) 1.0053(18) 1.0289(12) 0.199(8) Uani 0.50 1 d P E -1 H33A H -0.0117 1.0758 1.0706 0.299 Uiso 0.50 1 calc PR E -1 H33B H 0.0380 0.9355 1.0606 0.299 Uiso 0.50 1 calc PR E -1 H33C H -0.0080 1.0139 0.9781 0.299 Uiso 0.50 1 calc PR E -1 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 0.0467(2) 0.0402(2) 0.03144(18) 0.00749(13) -0.01094(13) -0.01801(15) F1 0.111(5) 0.132(5) 0.097(4) 0.037(3) -0.063(4) -0.063(4) F2 0.121(4) 0.193(8) 0.080(3) 0.054(4) -0.029(3) -0.094(5) B1 0.091(3) 0.060(2) 0.072(2) 0.0137(19) -0.034(2) -0.020(2) F3 0.117(4) 0.054(3) 0.155(6) 0.033(3) -0.047(4) -0.015(2) F4 0.206(7) 0.167(7) 0.078(4) -0.050(4) 0.000(4) -0.082(6) F1' 0.081(4) 0.289(13) 0.151(7) 0.121(8) 0.037(4) 0.051(5) F2' 0.463(18) 0.179(9) 0.40(2) 0.149(12) -0.261(18) -0.241(13) B1' 0.091(3) 0.060(2) 0.072(2) 0.0137(19) -0.034(2) -0.020(2) F3' 0.282(11) 0.101(6) 0.209(9) -0.025(6) 0.070(9) -0.054(6) F4' 0.55(2) 0.205(12) 0.138(6) 0.105(7) -0.211(10) -0.159(12) F5 0.117(7) 0.116(5) 0.193(11) 0.011(5) -0.044(6) -0.051(4) F6 0.162(8) 0.247(13) 0.054(3) 0.058(4) -0.045(3) -0.111(8) B2 0.087(6) 0.147(7) 0.059(6) 0.015(4) -0.026(5) -0.048(5) F7 0.121(5) 0.111(5) 0.091(4) 0.035(4) -0.063(4) -0.046(4) F8 0.370(13) 0.111(5) 0.133(6) -0.002(4) -0.061(7) -0.003(6) F5' 0.139(8) 0.55(2) 0.100(5) -0.014(10) 0.014(5) -0.183(13) F6' 0.225(10) 0.108(5) 0.383(16) 0.078(7) -0.235(10) -0.056(6) B2' 0.087(6) 0.147(7) 0.059(6) 0.015(4) -0.026(5) -0.048(5) F7' 0.174(8) 0.255(11) 0.207(11) 0.106(7) -0.155(8) -0.110(7) F8' 0.205(6) 0.179(6) 0.114(4) -0.013(4) -0.005(4) -0.086(5) N11 0.0509(12) 0.0556(13) 0.0436(11) 0.0124(10) -0.0077(9) -0.0178(10) N12 0.0467(11) 0.0429(11) 0.0447(11) 0.0124(9) -0.0141(9) -0.0186(9) N7 0.0584(12) 0.0501(12) 0.0456(11) 0.0127(9) -0.0198(9) -0.0290(10) N8 0.0526(11) 0.0458(11) 0.0427(11) 0.0134(9) -0.0137(9) -0.0254(9) N9 0.0614(12) 0.0411(11) 0.0360(10) 0.0088(8) -0.0181(9) -0.0198(9) N10 0.0528(11) 0.0455(11) 0.0321(9) 0.0088(8) -0.0162(8) -0.0224(9) N3 0.0580(12) 0.0369(10) 0.0365(10) 0.0059(8) -0.0123(9) -0.0184(9) N4 0.0491(10) 0.0395(10) 0.0307(9) 0.0046(8) -0.0098(8) -0.0201(9) N1 0.0460(10) 0.0483(11) 0.0365(10) 0.0117(8) -0.0141(8) -0.0235(9) N2 0.0443(10) 0.0414(10) 0.0325(9) 0.0102(8) -0.0127(8) -0.0215(8) N5 0.0437(10) 0.0483(11) 0.0304(9) 0.0060(8) -0.0061(8) -0.0176(9) N6 0.0396(10) 0.0424(10) 0.0323(9) 0.0067(8) -0.0088(7) -0.0150(8) N13 0.117(3) 0.107(3) 0.253(6) 0.048(4) -0.051(3) -0.054(3) N14 0.151(8) 0.092(6) 0.149(8) 0.007(5) -0.009(7) -0.044(6) C25 0.0585(16) 0.0584(16) 0.0540(16) 0.0034(13) 0.0004(13) -0.0188(13) C26 0.0525(15) 0.0460(15) 0.0756(19) 0.0013(13) -0.0097(14) -0.0162(12) C27 0.0537(15) 0.0383(13) 0.0691(18) 0.0129(12) -0.0231(13) -0.0166(11) C17 0.0607(16) 0.0556(16) 0.0716(18) 0.0067(14) -0.0229(14) -0.0322(14) C18 0.0645(17) 0.0581(16) 0.0738(19) 0.0077(14) -0.0091(14) -0.0385(14) C19 0.0632(16) 0.0488(14) 0.0535(15) 0.0145(12) -0.0058(12) -0.0283(13) C21 0.0581(15) 0.0410(13) 0.0505(14) 0.0062(11) -0.0154(12) -0.0168(11) C22 0.0610(15) 0.0548(15) 0.0479(14) -0.0042(12) -0.0159(12) -0.0254(13) C23 0.0597(15) 0.0591(16) 0.0377(13) 0.0036(11) -0.0176(11) -0.0252(13) C29 0.0514(13) 0.0440(13) 0.0373(12) 0.0128(10) -0.0142(10) -0.0216(11) C6 0.107(2) 0.0426(15) 0.072(2) 0.0054(14) -0.0231(18) -0.0242(16) C7 0.0588(15) 0.0398(13) 0.0497(14) -0.0020(11) -0.0068(11) -0.0202(11) C8 0.0662(16) 0.0500(15) 0.0469(14) -0.0099(11) -0.0091(12) -0.0271(13) C9 0.0461(12) 0.0530(14) 0.0336(11) -0.0041(10) -0.0060(9) -0.0251(11) C10 0.0727(17) 0.0710(18) 0.0426(14) 0.0055(12) -0.0249(12) -0.0339(15) C1 0.0663(17) 0.090(2) 0.0655(18) 0.0201(16) -0.0326(14) -0.0470(16) C2 0.0428(12) 0.0532(14) 0.0462(13) 0.0070(11) -0.0116(10) -0.0244(11) C3 0.0480(13) 0.0512(14) 0.0567(15) 0.0086(12) -0.0078(11) -0.0298(12) C4 0.0433(12) 0.0418(12) 0.0410(12) 0.0058(10) -0.0036(10) -0.0189(10) C5 0.0736(18) 0.0639(17) 0.0557(16) 0.0277(13) -0.0198(13) -0.0370(15) C11 0.0603(17) 0.090(2) 0.0489(16) 0.0080(15) 0.0080(13) -0.0241(15) C12 0.0433(13) 0.0573(15) 0.0410(13) -0.0008(11) -0.0029(10) -0.0217(12) C13 0.0382(12) 0.0553(15) 0.0567(16) -0.0008(12) -0.0055(11) -0.0119(11) C14 0.0410(12) 0.0442(13) 0.0512(14) 0.0054(11) -0.0156(10) -0.0149(11) C15 0.0565(16) 0.0649(18) 0.075(2) 0.0272(15) -0.0212(14) -0.0115(14) C16 0.0430(11) 0.0370(11) 0.0299(10) 0.0070(9) -0.0106(9) -0.0173(9) C28 0.066(2) 0.084(2) 0.121(3) 0.005(2) -0.008(2) -0.0035(18) C20 0.117(3) 0.124(3) 0.123(3) 0.026(3) -0.019(3) -0.093(3) C24 0.120(3) 0.066(2) 0.081(2) -0.0124(17) -0.039(2) -0.032(2) C30 0.088(3) 0.061(2) 0.146(4) 0.013(2) -0.027(2) -0.025(2) C31 0.142(4) 0.081(3) 0.191(6) 0.001(3) -0.010(4) -0.052(3) C32 0.153(12) 0.113(9) 0.169(12) 0.064(8) 0.012(11) -0.032(9) C33 0.30(3) 0.152(11) 0.169(18) 0.004(12) -0.010(15) -0.135(14) _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 N5 2.159(2) . ? Fe1 N3 2.160(2) . ? Fe1 N9 2.162(2) . ? Fe1 N7 2.180(2) . ? Fe1 N1 2.185(2) . ? Fe1 N11 2.201(2) . ? F1 B1 1.393(11) . ? F2 B1 1.373(12) . ? B1 F3 1.354(11) . ? B1 F4 1.351(11) . ? F1' B1' 1.256(13) . ? F2' B1' 1.236(14) . ? B1' F4' 1.211(13) . ? B1' F3' 1.251(14) . ? F5 B2 1.398(17) . ? F6 B2 1.369(14) . ? B2 F8 1.355(13) . ? B2 F7 1.362(14) . ? F5' B2' 1.368(16) . ? F6' B2' 1.300(14) . ? B2' F7' 1.268(16) . ? B2' F8' 1.343(12) . ? N11 C25 1.332(3) . ? N11 N12 1.356(3) . ? N12 C27 1.348(3) . ? N12 C29 1.444(3) . ? N7 C17 1.321(3) . ? N7 N8 1.367(3) . ? N8 C19 1.344(3) . ? N8 C29 1.446(3) . ? N9 C21 1.319(3) . ? N9 N10 1.362(2) . ? N10 C23 1.342(3) . ? N10 C29 1.439(3) . ? N3 C7 1.322(3) . ? N3 N4 1.375(2) . ? N4 C9 1.357(3) . ? N4 C16 1.440(3) . ? N1 C2 1.337(3) . ? N1 N2 1.376(2) . ? N2 C4 1.354(3) . ? N2 C16 1.446(3) . ? N5 C12 1.335(3) . ? N5 N6 1.372(2) . ? N6 C14 1.356(3) . ? N6 C16 1.437(3) . ? N13 C30 1.123(5) . ? N14 C32 1.058(16) . ? C25 C26 1.382(4) . ? C26 C27 1.361(4) . ? C26 C28 1.496(4) . ? C17 C18 1.395(4) . ? C18 C19 1.368(4) . ? C18 C20 1.509(4) . ? C21 C22 1.394(3) . ? C22 C23 1.371(4) . ? C22 C24 1.501(4) . ? C6 C7 1.486(4) . ? C7 C8 1.397(4) . ? C8 C9 1.358(3) . ? C9 C10 1.500(3) . ? C1 C2 1.495(3) . ? C2 C3 1.396(3) . ? C3 C4 1.363(3) . ? C4 C5 1.498(3) . ? C11 C12 1.489(4) . ? C12 C13 1.393(4) . ? C13 C14 1.365(4) . ? C14 C15 1.488(3) . ? C30 C31 1.420(6) . ? C32 C33 1.46(2) . ? 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 N5 Fe1 N3 84.88(8) . . ? N5 Fe1 N9 92.44(8) . . ? N3 Fe1 N9 175.42(7) . . ? N5 Fe1 N7 96.05(8) . . ? N3 Fe1 N7 100.42(8) . . ? N9 Fe1 N7 83.54(8) . . ? N5 Fe1 N1 85.34(7) . . ? N3 Fe1 N1 83.66(7) . . ? N9 Fe1 N1 92.43(8) . . ? N7 Fe1 N1 175.77(7) . . ? N5 Fe1 N11 176.32(7) . . ? N3 Fe1 N11 98.75(8) . . ? N9 Fe1 N11 83.98(8) . . ? N7 Fe1 N11 82.74(8) . . ? N1 Fe1 N11 95.63(8) . . ? F3 B1 F4 103.9(8) . . ? F3 B1 F2 107.3(10) . . ? F4 B1 F2 112.2(9) . . ? F3 B1 F1 103.6(8) . . ? F4 B1 F1 117.3(11) . . ? F2 B1 F1 111.4(8) . . ? F4' B1' F2' 117.2(13) . . ? F4' B1' F3' 113.6(11) . . ? F2' B1' F3' 107.1(16) . . ? F4' B1' F1' 117.6(16) . . ? F2' B1' F1' 89.9(12) . . ? F3' B1' F1' 108.8(11) . . ? F8 B2 F7 104.7(10) . . ? F8 B2 F6 104.9(10) . . ? F7 B2 F6 119.0(16) . . ? F8 B2 F5 116.6(16) . . ? F7 B2 F5 99.9(11) . . ? F6 B2 F5 112.1(11) . . ? F7' B2' F6' 109.8(16) . . ? F7' B2' F8' 109.1(11) . . ? F6' B2' F8' 111.4(9) . . ? F7' B2' F5' 116.5(11) . . ? F6' B2' F5' 97.0(11) . . ? F8' B2' F5' 112.5(16) . . ? C25 N11 N12 103.7(2) . . ? C25 N11 Fe1 139.60(18) . . ? N12 N11 Fe1 116.31(14) . . ? C27 N12 N11 111.3(2) . . ? C27 N12 C29 127.8(2) . . ? N11 N12 C29 120.90(18) . . ? C17 N7 N8 104.4(2) . . ? C17 N7 Fe1 138.67(18) . . ? N8 N7 Fe1 116.26(15) . . ? C19 N8 N7 111.3(2) . . ? C19 N8 C29 127.9(2) . . ? N7 N8 C29 120.82(18) . . ? C21 N9 N10 105.11(18) . . ? C21 N9 Fe1 135.48(16) . . ? N10 N9 Fe1 117.86(14) . . ? C23 N10 N9 110.60(19) . . ? C23 N10 C29 129.53(19) . . ? N9 N10 C29 119.66(18) . . ? C7 N3 N4 105.16(18) . . ? C7 N3 Fe1 138.97(16) . . ? N4 N3 Fe1 115.36(13) . . ? C9 N4 N3 111.51(18) . . ? C9 N4 C16 127.89(18) . . ? N3 N4 C16 120.59(17) . . ? C2 N1 N2 105.03(17) . . ? C2 N1 Fe1 138.90(15) . . ? N2 N1 Fe1 116.06(14) . . ? C4 N2 N1 111.43(18) . . ? C4 N2 C16 129.19(17) . . ? N1 N2 C16 119.14(17) . . ? C12 N5 N6 104.82(18) . . ? C12 N5 Fe1 138.21(15) . . ? N6 N5 Fe1 116.41(13) . . ? C14 N6 N5 111.75(18) . . ? C14 N6 C16 128.79(18) . . ? N5 N6 C16 119.45(16) . . ? N11 C25 C26 112.9(2) . . ? C27 C26 C25 104.0(2) . . ? C27 C26 C28 127.5(3) . . ? C25 C26 C28 128.5(3) . . ? N12 C27 C26 108.0(2) . . ? N7 C17 C18 112.2(3) . . ? C19 C18 C17 104.4(2) . . ? C19 C18 C20 127.3(3) . . ? C17 C18 C20 128.3(3) . . ? N8 C19 C18 107.7(2) . . ? N9 C21 C22 112.1(2) . . ? C23 C22 C21 103.9(2) . . ? C23 C22 C24 128.8(2) . . ? C21 C22 C24 127.2(3) . . ? N10 C23 C22 108.2(2) . . ? N10 C29 N12 111.12(19) . . ? N10 C29 N8 111.21(19) . . ? N12 C29 N8 110.87(19) . . ? N3 C7 C8 110.3(2) . . ? N3 C7 C6 121.1(2) . . ? C8 C7 C6 128.7(2) . . ? C9 C8 C7 107.2(2) . . ? N4 C9 C8 105.8(2) . . ? N4 C9 C10 123.0(2) . . ? C8 C9 C10 131.2(2) . . ? N1 C2 C3 110.2(2) . . ? N1 C2 C1 122.1(2) . . ? C3 C2 C1 127.7(2) . . ? C4 C3 C2 106.9(2) . . ? N2 C4 C3 106.41(19) . . ? N2 C4 C5 123.9(2) . . ? C3 C4 C5 129.7(2) . . ? N5 C12 C13 110.5(2) . . ? N5 C12 C11 121.9(2) . . ? C13 C12 C11 127.7(2) . . ? C14 C13 C12 106.9(2) . . ? N6 C14 C13 106.0(2) . . ? N6 C14 C15 123.3(2) . . ? C13 C14 C15 130.6(2) . . ? N6 C16 N4 112.04(18) . . ? N6 C16 N2 112.13(17) . . ? N4 C16 N2 111.40(17) . . ? N13 C30 C31 179.6(6) . . ? N14 C32 C33 175(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 N5 Fe1 N11 C25 158.3(11) . . . . ? N3 Fe1 N11 C25 -31.2(3) . . . . ? N9 Fe1 N11 C25 145.0(3) . . . . ? N7 Fe1 N11 C25 -130.7(3) . . . . ? N1 Fe1 N11 C25 53.2(3) . . . . ? N5 Fe1 N11 N12 -30.2(13) . . . . ? N3 Fe1 N11 N12 140.22(17) . . . . ? N9 Fe1 N11 N12 -43.49(18) . . . . ? N7 Fe1 N11 N12 40.73(18) . . . . ? N1 Fe1 N11 N12 -135.35(17) . . . . ? C25 N11 N12 C27 0.8(3) . . . . ? Fe1 N11 N12 C27 -173.51(16) . . . . ? C25 N11 N12 C29 179.3(2) . . . . ? Fe1 N11 N12 C29 5.0(3) . . . . ? N5 Fe1 N7 C17 -39.7(3) . . . . ? N3 Fe1 N7 C17 46.2(3) . . . . ? N9 Fe1 N7 C17 -131.4(3) . . . . ? N1 Fe1 N7 C17 -148.7(9) . . . . ? N11 Fe1 N7 C17 143.8(3) . . . . ? N5 Fe1 N7 N8 129.28(16) . . . . ? N3 Fe1 N7 N8 -144.84(16) . . . . ? N9 Fe1 N7 N8 37.50(16) . . . . ? N1 Fe1 N7 N8 20.2(11) . . . . ? N11 Fe1 N7 N8 -47.22(16) . . . . ? C17 N7 N8 C19 -0.3(3) . . . . ? Fe1 N7 N8 C19 -172.78(16) . . . . ? C17 N7 N8 C29 -179.3(2) . . . . ? Fe1 N7 N8 C29 8.3(3) . . . . ? N5 Fe1 N9 C21 54.3(3) . . . . ? N3 Fe1 N9 C21 0.3(11) . . . . ? N7 Fe1 N9 C21 150.1(3) . . . . ? N1 Fe1 N9 C21 -31.1(2) . . . . ? N11 Fe1 N9 C21 -126.5(3) . . . . ? N5 Fe1 N9 N10 -142.33(17) . . . . ? N3 Fe1 N9 N10 163.6(9) . . . . ? N7 Fe1 N9 N10 -46.51(16) . . . . ? N1 Fe1 N9 N10 132.23(17) . . . . ? N11 Fe1 N9 N10 36.83(17) . . . . ? C21 N9 N10 C23 1.2(3) . . . . ? Fe1 N9 N10 C23 -166.76(16) . . . . ? C21 N9 N10 C29 176.4(2) . . . . ? Fe1 N9 N10 C29 8.4(3) . . . . ? N5 Fe1 N3 C7 131.7(3) . . . . ? N9 Fe1 N3 C7 -174.0(8) . . . . ? N7 Fe1 N3 C7 36.4(3) . . . . ? N1 Fe1 N3 C7 -142.5(3) . . . . ? N11 Fe1 N3 C7 -47.7(3) . . . . ? N5 Fe1 N3 N4 -38.58(15) . . . . ? N9 Fe1 N3 N4 15.7(10) . . . . ? N7 Fe1 N3 N4 -133.81(15) . . . . ? N1 Fe1 N3 N4 47.29(15) . . . . ? N11 Fe1 N3 N4 142.03(15) . . . . ? C7 N3 N4 C9 -0.3(3) . . . . ? Fe1 N3 N4 C9 173.04(15) . . . . ? C7 N3 N4 C16 179.5(2) . . . . ? Fe1 N3 N4 C16 -7.1(2) . . . . ? N5 Fe1 N1 C2 -135.3(3) . . . . ? N3 Fe1 N1 C2 139.3(3) . . . . ? N9 Fe1 N1 C2 -43.1(2) . . . . ? N7 Fe1 N1 C2 -25.9(11) . . . . ? N11 Fe1 N1 C2 41.1(3) . . . . ? N5 Fe1 N1 N2 43.28(15) . . . . ? N3 Fe1 N1 N2 -42.07(15) . . . . ? N9 Fe1 N1 N2 135.53(15) . . . . ? N7 Fe1 N1 N2 152.7(9) . . . . ? N11 Fe1 N1 N2 -140.28(15) . . . . ? C2 N1 N2 C4 0.5(2) . . . . ? Fe1 N1 N2 C4 -178.59(14) . . . . ? C2 N1 N2 C16 175.40(19) . . . . ? Fe1 N1 N2 C16 -3.7(2) . . . . ? N3 Fe1 N5 C12 -143.8(3) . . . . ? N9 Fe1 N5 C12 39.9(3) . . . . ? N7 Fe1 N5 C12 -43.8(3) . . . . ? N1 Fe1 N5 C12 132.2(3) . . . . ? N11 Fe1 N5 C12 26.7(13) . . . . ? N3 Fe1 N5 N6 46.46(16) . . . . ? N9 Fe1 N5 N6 -129.82(16) . . . . ? N7 Fe1 N5 N6 146.43(16) . . . . ? N1 Fe1 N5 N6 -37.58(16) . . . . ? N11 Fe1 N5 N6 -143.0(11) . . . . ? C12 N5 N6 C14 -0.5(3) . . . . ? Fe1 N5 N6 C14 172.44(15) . . . . ? C12 N5 N6 C16 179.5(2) . . . . ? Fe1 N5 N6 C16 -7.6(3) . . . . ? N12 N11 C25 C26 -0.5(3) . . . . ? Fe1 N11 C25 C26 171.6(2) . . . . ? N11 C25 C26 C27 0.1(4) . . . . ? N11 C25 C26 C28 -179.7(3) . . . . ? N11 N12 C27 C26 -0.8(3) . . . . ? C29 N12 C27 C26 -179.1(2) . . . . ? C25 C26 C27 N12 0.4(3) . . . . ? C28 C26 C27 N12 -179.8(3) . . . . ? N8 N7 C17 C18 0.1(3) . . . . ? Fe1 N7 C17 C18 169.8(2) . . . . ? N7 C17 C18 C19 0.2(3) . . . . ? N7 C17 C18 C20 179.2(3) . . . . ? N7 N8 C19 C18 0.4(3) . . . . ? C29 N8 C19 C18 179.3(2) . . . . ? C17 C18 C19 N8 -0.3(3) . . . . ? C20 C18 C19 N8 -179.4(3) . . . . ? N10 N9 C21 C22 -1.4(3) . . . . ? Fe1 N9 C21 C22 163.37(19) . . . . ? N9 C21 C22 C23 1.1(3) . . . . ? N9 C21 C22 C24 -177.4(3) . . . . ? N9 N10 C23 C22 -0.6(3) . . . . ? C29 N10 C23 C22 -175.2(2) . . . . ? C21 C22 C23 N10 -0.3(3) . . . . ? C24 C22 C23 N10 178.2(3) . . . . ? C23 N10 C29 N12 106.5(3) . . . . ? N9 N10 C29 N12 -67.7(3) . . . . ? C23 N10 C29 N8 -129.5(2) . . . . ? N9 N10 C29 N8 56.4(3) . . . . ? C27 N12 C29 N10 -122.9(2) . . . . ? N11 N12 C29 N10 58.9(3) . . . . ? C27 N12 C29 N8 112.9(3) . . . . ? N11 N12 C29 N8 -65.3(3) . . . . ? C19 N8 C29 N10 114.1(3) . . . . ? N7 N8 C29 N10 -67.2(3) . . . . ? C19 N8 C29 N12 -121.8(2) . . . . ? N7 N8 C29 N12 57.0(3) . . . . ? N4 N3 C7 C8 -0.4(3) . . . . ? Fe1 N3 C7 C8 -171.23(19) . . . . ? N4 N3 C7 C6 179.7(3) . . . . ? Fe1 N3 C7 C6 8.9(4) . . . . ? N3 C7 C8 C9 0.9(3) . . . . ? C6 C7 C8 C9 -179.2(3) . . . . ? N3 N4 C9 C8 0.9(3) . . . . ? C16 N4 C9 C8 -179.0(2) . . . . ? N3 N4 C9 C10 -178.5(2) . . . . ? C16 N4 C9 C10 1.6(4) . . . . ? C7 C8 C9 N4 -1.1(3) . . . . ? C7 C8 C9 C10 178.3(3) . . . . ? N2 N1 C2 C3 -0.5(3) . . . . ? Fe1 N1 C2 C3 178.18(18) . . . . ? N2 N1 C2 C1 178.5(2) . . . . ? Fe1 N1 C2 C1 -2.8(4) . . . . ? N1 C2 C3 C4 0.4(3) . . . . ? C1 C2 C3 C4 -178.5(3) . . . . ? N1 N2 C4 C3 -0.2(2) . . . . ? C16 N2 C4 C3 -174.5(2) . . . . ? N1 N2 C4 C5 -179.3(2) . . . . ? C16 N2 C4 C5 6.4(4) . . . . ? C2 C3 C4 N2 -0.1(3) . . . . ? C2 C3 C4 C5 178.9(3) . . . . ? N6 N5 C12 C13 0.1(3) . . . . ? Fe1 N5 C12 C13 -170.39(19) . . . . ? N6 N5 C12 C11 -179.9(3) . . . . ? Fe1 N5 C12 C11 9.6(4) . . . . ? N5 C12 C13 C14 0.3(3) . . . . ? C11 C12 C13 C14 -179.7(3) . . . . ? N5 N6 C14 C13 0.7(3) . . . . ? C16 N6 C14 C13 -179.3(2) . . . . ? N5 N6 C14 C15 -178.0(2) . . . . ? C16 N6 C14 C15 2.0(4) . . . . ? C12 C13 C14 N6 -0.6(3) . . . . ? C12 C13 C14 C15 177.9(3) . . . . ? C14 N6 C16 N4 122.6(2) . . . . ? N5 N6 C16 N4 -57.4(2) . . . . ? C14 N6 C16 N2 -111.2(2) . . . . ? N5 N6 C16 N2 68.8(2) . . . . ? C9 N4 C16 N6 -112.9(2) . . . . ? N3 N4 C16 N6 67.2(2) . . . . ? C9 N4 C16 N2 120.6(2) . . . . ? N3 N4 C16 N2 -59.3(2) . . . . ? C4 N2 C16 N6 112.9(2) . . . . ? N1 N2 C16 N6 -61.0(2) . . . . ? C4 N2 C16 N4 -120.6(2) . . . . ? N1 N2 C16 N4 65.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.413 _refine_diff_density_min -0.241 _refine_diff_density_rms 0.050 #=END data_2-25qs _database_code_depnum_ccdc_archive 'CCDC 650146' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Fe(picpzpz)()(BF!4$)!2$.MeOH _chemical_melting_point ? _chemical_formula_moiety 'C29 H38 Fe N12, 2(B F4), 1.5(C2 H3 N)' _chemical_formula_sum 'C32 H42.50 B2 F8 Fe N13.50' _chemical_formula_weight 845.76 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' 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 Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.931(10) _cell_length_b 12.370(11) _cell_length_c 15.070(13) _cell_angle_alpha 88.648(13) _cell_angle_beta 78.824(13) _cell_angle_gamma 64.001(12) _cell_volume 1956(3) _cell_formula_units_Z 2 _cell_measurement_temperature 25(2) _cell_measurement_reflns_used 4331 _cell_measurement_theta_min 2.576 _cell_measurement_theta_max 25.458 _exptl_crystal_description block-shaped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 0.468 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 0.900 _exptl_absorpt_process_details 'SADABS (Bruker, 1996)' _exptl_special_details ; In a thin film of perfluorpolyether oil on a mohair fibre ; _diffrn_ambient_temperature 25(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 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 183 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 15552 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.69 _reflns_number_total 7182 _reflns_number_gt 6429 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXTL (BrukerAXS, 2000)' _computing_structure_refinement 'SHELXTL (BrukerAXS, 2000)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material XCIF _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. One of the two crystallographically distinct MeCN solvent molucules (N14, C32, C33) exhibits two-fold symmetry-related disorder, where the alternate positons are in close proximity and can not be occupied simultaneously. The occupancies of these atoms were fixed to be 0.5. One BF4 counterions exhibits two-fold positional disorder on all atoms. Pairs of atom sites were appropriately selected and separated into parts (A & B) to account for the disorder. Equivalent atoms were fixed to have the same ADPs. The relative occupancy of the two components was refined. The disorder of the MeCN molecule and the BF4 molecules are correlated, with the B2A-F8A positions in close proximity to one of the MeCN orientatios which therefore cannot be occupied simultaneously. The alternate position of B2B-F8B is not in close proximity to either MeCN orientation. ; _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^)+(0.0663P)^2^+3.9739P] 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 7182 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1364 _refine_ls_wR_factor_gt 0.1294 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 0.68736(3) 0.61881(3) 0.73757(2) 0.01239(12) Uani 1 1 d . . . N1 N 0.61848(19) 0.49937(18) 0.80704(14) 0.0143(4) Uani 1 1 d . . . N2 N 0.66689(19) 0.45211(18) 0.88260(14) 0.0132(4) Uani 1 1 d . . . N3 N 0.6666(2) 0.68885(19) 0.87106(15) 0.0166(4) Uani 1 1 d . . . N4 N 0.71917(19) 0.60433(18) 0.93089(14) 0.0141(4) Uani 1 1 d . . . N5 N 0.8716(2) 0.48940(19) 0.75408(14) 0.0157(4) Uani 1 1 d . . . N6 N 0.87829(19) 0.43450(18) 0.83437(14) 0.0135(4) Uani 1 1 d . . . N7 N 0.7555(2) 0.7340(2) 0.66063(15) 0.0187(5) Uani 1 1 d . . . N8 N 0.7174(2) 0.76585(19) 0.58027(15) 0.0172(4) Uani 1 1 d . . . N9 N 0.7126(2) 0.53644(19) 0.60732(15) 0.0173(4) Uani 1 1 d . . . N10 N 0.6651(2) 0.60972(19) 0.54157(14) 0.0160(4) Uani 1 1 d . . . N11 N 0.5042(2) 0.7471(2) 0.71090(16) 0.0208(5) Uani 1 1 d . . . N12 N 0.5047(2) 0.78923(19) 0.62621(16) 0.0187(5) Uani 1 1 d . . . C1 C 0.4633(3) 0.4819(3) 0.7258(2) 0.0260(6) Uani 1 1 d . . . H1A H 0.4914 0.5293 0.6820 0.039 Uiso 1 1 calc R . . H1B H 0.3728 0.5289 0.7527 0.039 Uiso 1 1 calc R . . H1C H 0.4761 0.4073 0.6949 0.039 Uiso 1 1 calc R . . C2 C 0.5392(2) 0.4516(2) 0.79882(17) 0.0176(5) Uani 1 1 d . . . C3 C 0.5382(2) 0.3735(2) 0.86814(18) 0.0182(5) Uani 1 1 d . . . H3 H 0.4904 0.3283 0.8769 0.022 Uiso 1 1 calc R . . C4 C 0.6197(2) 0.3752(2) 0.92073(17) 0.0151(5) Uani 1 1 d . . . C5 C 0.6541(3) 0.3119(2) 1.00393(18) 0.0206(5) Uani 1 1 d . . . H5A H 0.7461 0.2602 0.9928 0.031 Uiso 1 1 calc R . . H5B H 0.6085 0.2624 1.0193 0.031 Uiso 1 1 calc R . . H5C H 0.6302 0.3716 1.0543 0.031 Uiso 1 1 calc R . . C6 C 0.5688(3) 0.9114(2) 0.8723(2) 0.0250(6) Uani 1 1 d . . . H6A H 0.5993 0.8995 0.8064 0.037 Uiso 1 1 calc R . . H6B H 0.5883 0.9727 0.8965 0.037 Uiso 1 1 calc R . . H6C H 0.4765 0.9383 0.8866 0.037 Uiso 1 1 calc R . . C7 C 0.6335(2) 0.7948(2) 0.91452(19) 0.0199(5) Uani 1 1 d . . . C8 C 0.6648(2) 0.7779(2) 1.00098(19) 0.0202(5) Uani 1 1 d . . . H8 H 0.6500 0.8391 1.0448 0.024 Uiso 1 1 calc R . . C9 C 0.7209(2) 0.6558(2) 1.00941(17) 0.0166(5) Uani 1 1 d . . . C10 C 0.7771(3) 0.5836(2) 1.08440(18) 0.0206(5) Uani 1 1 d . . . H10A H 0.7443 0.5238 1.0984 0.031 Uiso 1 1 calc R . . H10B H 0.7538 0.6375 1.1385 0.031 Uiso 1 1 calc R . . H10C H 0.8701 0.5424 1.0654 0.031 Uiso 1 1 calc R . . C11 C 1.0233(3) 0.4672(3) 0.61028(19) 0.0264(6) Uani 1 1 d . . . H11A H 0.9454 0.5166 0.5883 0.040 Uiso 1 1 calc R . . H11B H 1.0751 0.3944 0.5696 0.040 Uiso 1 1 calc R . . H11C H 1.0719 0.5135 0.6117 0.040 Uiso 1 1 calc R . . C12 C 0.9893(2) 0.4324(2) 0.70345(17) 0.0184(5) Uani 1 1 d . . . C13 C 1.0701(2) 0.3415(2) 0.75103(18) 0.0194(5) Uani 1 1 d . . . H13 H 1.1577 0.2888 0.7298 0.023 Uiso 1 1 calc R . . C14 C 0.9970(2) 0.3440(2) 0.83415(18) 0.0166(5) Uani 1 1 d . . . C15 C 1.0290(3) 0.2676(2) 0.91178(19) 0.0224(6) Uani 1 1 d . . . H15A H 1.1194 0.2099 0.8977 0.034 Uiso 1 1 calc R . . H15B H 0.9769 0.2238 0.9226 0.034 Uiso 1 1 calc R . . H15C H 1.0119 0.3188 0.9661 0.034 Uiso 1 1 calc R . . C16 C 0.7664(2) 0.4770(2) 0.90657(16) 0.0136(5) Uani 1 1 d . . . H16 H 0.7915 0.4320 0.9610 0.016 Uiso 1 1 calc R . . C17 C 0.8424(3) 0.7753(2) 0.6609(2) 0.0229(6) Uani 1 1 d . . . H17 H 0.8866 0.7665 0.7087 0.028 Uiso 1 1 calc R . . C18 C 0.8599(3) 0.8331(2) 0.5819(2) 0.0240(6) Uani 1 1 d . . . C19 C 0.7780(3) 0.8256(2) 0.5318(2) 0.0214(6) Uani 1 1 d . . . H19 H 0.7663 0.8565 0.4743 0.026 Uiso 1 1 calc R . . C20 C 0.9466(3) 0.8933(3) 0.5571(2) 0.0334(7) Uani 1 1 d . . . H20A H 0.9967 0.8819 0.6039 0.050 Uiso 1 1 calc R . . H20B H 0.8953 0.9797 0.5526 0.050 Uiso 1 1 calc R . . H20C H 1.0041 0.8575 0.4986 0.050 Uiso 1 1 calc R . . C21 C 0.7381(2) 0.4265(2) 0.57608(18) 0.0182(5) Uani 1 1 d . . . H21 H 0.7745 0.3556 0.6071 0.022 Uiso 1 1 calc R . . C22 C 0.7042(2) 0.4284(2) 0.49130(18) 0.0182(5) Uani 1 1 d . . . C23 C 0.6578(2) 0.5481(2) 0.47148(18) 0.0183(5) Uani 1 1 d . . . H23 H 0.6267 0.5809 0.4187 0.022 Uiso 1 1 calc R . . C24 C 0.7140(3) 0.3225(2) 0.43705(19) 0.0235(6) Uani 1 1 d . . . H24A H 0.7389 0.2516 0.4728 0.035 Uiso 1 1 calc R . . H24B H 0.7782 0.3056 0.3810 0.035 Uiso 1 1 calc R . . H24C H 0.6313 0.3416 0.4221 0.035 Uiso 1 1 calc R . . C25 C 0.3843(3) 0.8130(3) 0.7558(2) 0.0271(6) Uani 1 1 d . . . H25 H 0.3535 0.8037 0.8172 0.033 Uiso 1 1 calc R . . C26 C 0.3094(3) 0.8972(3) 0.7020(2) 0.0288(7) Uani 1 1 d . . . C27 C 0.3894(3) 0.8794(2) 0.6194(2) 0.0244(6) Uani 1 1 d . . . H27 H 0.3684 0.9221 0.5672 0.029 Uiso 1 1 calc R . . C28 C 0.1708(3) 0.9871(3) 0.7274(3) 0.0438(9) Uani 1 1 d . . . H28A H 0.1593 1.0436 0.7767 0.066 Uiso 1 1 calc R . . H28B H 0.1189 0.9444 0.7474 0.066 Uiso 1 1 calc R . . H28C H 0.1443 1.0316 0.6747 0.066 Uiso 1 1 calc R . . C29 C 0.6192(2) 0.7394(2) 0.55667(18) 0.0179(5) Uani 1 1 d . . . H29 H 0.5985 0.7774 0.4990 0.021 Uiso 1 1 calc R . . N13 N 0.8626(2) 0.2099(2) 0.7239(2) 0.0341(6) Uani 1 1 d . . . C30 C 0.8170(3) 0.1478(2) 0.74703(19) 0.0227(6) Uani 1 1 d . . . C31 C 0.7575(3) 0.0680(3) 0.7761(3) 0.0384(8) Uani 1 1 d . . . H31A H 0.7261 0.0496 0.7258 0.058 Uiso 1 1 calc R . . H31B H 0.6862 0.1080 0.8274 0.058 Uiso 1 1 calc R . . H31C H 0.8204 -0.0070 0.7947 0.058 Uiso 1 1 calc R . . N14 N 1.2548(6) -0.0104(5) 0.9852(5) 0.0447(15) Uani 0.50 1 d P . . C32 C 1.1579(11) -0.0029(7) 1.0113(7) 0.065(3) Uani 0.50 1 d P . . C33 C 1.0245(11) 0.0108(10) 1.0433(7) 0.070(3) Uani 0.50 1 d P . . H33A H 0.9907 0.0019 0.9911 0.105 Uiso 0.50 1 calc PR . . H33B H 0.9704 0.0908 1.0745 0.105 Uiso 0.50 1 calc PR . . H33C H 1.0256 -0.0513 1.0851 0.105 Uiso 0.50 1 calc PR . . B1 B 0.5310(3) 0.8575(3) 0.3338(2) 0.0218(6) Uani 1 1 d . . . F1 F 0.64080(15) 0.84122(15) 0.36600(11) 0.0258(4) Uani 1 1 d . . . F2 F 0.46934(17) 0.79975(16) 0.39114(12) 0.0333(4) Uani 1 1 d . . . F3 F 0.56587(19) 0.80613(18) 0.24551(13) 0.0412(5) Uani 1 1 d . . . F4 F 0.45064(16) 0.97861(14) 0.33638(12) 0.0287(4) Uani 1 1 d . . . B2A B 0.9617(8) 0.2418(9) 1.1502(6) 0.0373(14) Uani 0.472(3) 1 d P A 1 F5A F 1.0491(4) 0.1400(4) 1.1030(3) 0.0463(7) Uani 0.472(3) 1 d P A 1 F6A F 1.02043(18) 0.33008(19) 1.13270(14) 0.0429(5) Uani 0.472(3) 1 d P A 1 F7A F 0.84890(17) 0.30150(17) 1.12151(13) 0.0364(4) Uani 0.472(3) 1 d P A 1 F8A F 0.9591(3) 0.2079(3) 1.2310(2) 0.0758(9) Uani 0.472(3) 1 d P A 1 B2B B 0.9286(7) 0.3059(8) 1.1800(5) 0.0373(14) Uani 0.528(3) 1 d P A 2 F5B F 0.8572(4) 0.3952(4) 1.2504(3) 0.0463(7) Uani 0.528(3) 1 d P A 2 F6B F 1.02043(18) 0.33008(19) 1.13270(14) 0.0429(5) Uani 0.528(3) 1 d P A 2 F7B F 0.84890(17) 0.30150(17) 1.12151(13) 0.0364(4) Uani 0.528(3) 1 d P A 2 F8B F 0.9591(3) 0.2079(3) 1.2310(2) 0.0758(9) Uani 0.528(3) 1 d P A 2 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 0.01415(19) 0.01111(19) 0.01335(19) 0.00135(13) -0.00329(13) -0.00672(14) N1 0.0152(10) 0.0157(10) 0.0135(10) 0.0009(8) -0.0042(8) -0.0076(8) N2 0.0145(10) 0.0130(10) 0.0143(10) 0.0015(8) -0.0042(8) -0.0075(8) N3 0.0185(11) 0.0121(10) 0.0200(11) 0.0026(8) -0.0044(9) -0.0074(9) N4 0.0151(10) 0.0125(10) 0.0158(10) 0.0006(8) -0.0035(8) -0.0070(8) N5 0.0186(11) 0.0155(10) 0.0144(10) 0.0017(8) -0.0011(8) -0.0099(9) N6 0.0148(10) 0.0132(10) 0.0141(10) 0.0014(8) -0.0024(8) -0.0078(8) N7 0.0177(11) 0.0190(11) 0.0210(11) -0.0021(9) -0.0052(9) -0.0089(9) N8 0.0182(11) 0.0143(10) 0.0219(11) 0.0018(8) -0.0051(9) -0.0094(9) N9 0.0182(11) 0.0141(10) 0.0219(11) 0.0042(8) -0.0090(9) -0.0073(9) N10 0.0184(11) 0.0142(10) 0.0184(11) 0.0045(8) -0.0066(9) -0.0089(9) N11 0.0234(12) 0.0159(11) 0.0242(12) 0.0001(9) -0.0001(9) -0.0116(9) N12 0.0169(11) 0.0136(10) 0.0275(12) 0.0041(9) -0.0052(9) -0.0081(9) C1 0.0283(15) 0.0332(16) 0.0278(15) 0.0072(12) -0.0137(12) -0.0207(13) C2 0.0150(12) 0.0196(13) 0.0195(13) -0.0026(10) -0.0024(10) -0.0090(10) C3 0.0173(12) 0.0181(12) 0.0220(13) -0.0021(10) -0.0020(10) -0.0108(10) C4 0.0152(12) 0.0126(11) 0.0178(12) -0.0008(9) 0.0001(9) -0.0078(10) C5 0.0251(14) 0.0204(13) 0.0221(13) 0.0048(11) -0.0059(11) -0.0149(11) C6 0.0301(15) 0.0146(13) 0.0311(15) 0.0002(11) -0.0068(12) -0.0105(12) C7 0.0181(13) 0.0152(12) 0.0273(14) -0.0026(10) -0.0010(11) -0.0096(11) C8 0.0185(13) 0.0186(13) 0.0247(14) -0.0061(10) 0.0002(10) -0.0107(11) C9 0.0135(12) 0.0203(13) 0.0177(12) -0.0042(10) 0.0005(10) -0.0103(10) C10 0.0207(13) 0.0257(14) 0.0177(13) -0.0028(11) -0.0045(10) -0.0119(11) C11 0.0236(14) 0.0274(15) 0.0214(14) 0.0003(11) 0.0059(11) -0.0093(12) C12 0.0205(13) 0.0173(12) 0.0183(13) -0.0027(10) 0.0014(10) -0.0112(11) C13 0.0153(12) 0.0177(12) 0.0244(14) -0.0048(10) -0.0006(10) -0.0076(10) C14 0.0145(12) 0.0139(12) 0.0221(13) -0.0025(10) -0.0048(10) -0.0063(10) C15 0.0178(13) 0.0195(13) 0.0286(14) 0.0031(11) -0.0064(11) -0.0063(11) C16 0.0135(11) 0.0147(12) 0.0146(12) 0.0001(9) -0.0025(9) -0.0081(10) C17 0.0177(13) 0.0222(13) 0.0304(15) -0.0071(11) -0.0043(11) -0.0099(11) C18 0.0193(13) 0.0178(13) 0.0359(16) -0.0033(11) -0.0010(11) -0.0106(11) C19 0.0219(13) 0.0143(12) 0.0290(14) 0.0020(11) -0.0010(11) -0.0106(11) C20 0.0274(15) 0.0308(16) 0.0494(19) 0.0013(14) -0.0037(14) -0.0212(14) C21 0.0172(12) 0.0136(12) 0.0259(14) 0.0021(10) -0.0059(10) -0.0081(10) C22 0.0165(12) 0.0193(13) 0.0210(13) 0.0001(10) -0.0022(10) -0.0105(10) C23 0.0203(13) 0.0202(13) 0.0187(13) 0.0019(10) -0.0045(10) -0.0127(11) C24 0.0267(14) 0.0209(13) 0.0259(14) -0.0002(11) -0.0065(11) -0.0126(12) C25 0.0225(14) 0.0224(14) 0.0349(16) -0.0079(12) 0.0057(12) -0.0129(12) C26 0.0191(14) 0.0167(13) 0.0507(19) -0.0087(13) -0.0033(13) -0.0091(11) C27 0.0201(13) 0.0135(12) 0.0424(17) 0.0022(11) -0.0112(12) -0.0079(11) C28 0.0215(16) 0.0319(18) 0.071(3) -0.0153(17) -0.0030(16) -0.0076(14) C29 0.0181(12) 0.0140(12) 0.0245(13) 0.0033(10) -0.0062(10) -0.0092(10) N13 0.0259(13) 0.0246(13) 0.0519(17) 0.0035(12) -0.0103(12) -0.0102(11) C30 0.0212(13) 0.0164(13) 0.0282(14) 0.0008(11) -0.0077(11) -0.0049(11) C31 0.0400(18) 0.0231(15) 0.049(2) 0.0043(14) 0.0005(15) -0.0151(14) N14 0.039(3) 0.029(3) 0.055(4) 0.007(3) 0.006(3) -0.011(3) C32 0.090(8) 0.031(4) 0.071(6) 0.009(4) -0.038(6) -0.016(5) C33 0.088(7) 0.053(5) 0.071(6) 0.005(5) 0.006(5) -0.042(5) B1 0.0221(15) 0.0151(14) 0.0254(16) 0.0005(12) -0.0044(12) -0.0058(12) F1 0.0205(8) 0.0261(8) 0.0285(9) 0.0057(7) -0.0045(7) -0.0088(7) F2 0.0392(10) 0.0353(10) 0.0388(10) 0.0166(8) -0.0153(8) -0.0261(8) F3 0.0418(11) 0.0456(11) 0.0306(10) -0.0145(8) -0.0010(8) -0.0160(9) F4 0.0263(9) 0.0185(8) 0.0405(10) 0.0043(7) -0.0101(7) -0.0080(7) B2A 0.027(3) 0.050(4) 0.030(4) 0.002(3) -0.009(3) -0.011(3) F5A 0.0413(16) 0.0544(18) 0.0354(15) 0.0058(13) -0.0085(12) -0.0139(14) F6A 0.0345(10) 0.0547(13) 0.0417(11) -0.0040(9) -0.0066(9) -0.0218(10) F7A 0.0278(9) 0.0423(11) 0.0399(10) 0.0067(8) -0.0141(8) -0.0136(8) F8A 0.107(2) 0.0850(19) 0.0827(19) 0.0454(16) -0.0720(18) -0.0659(18) B2B 0.027(3) 0.050(4) 0.030(4) 0.002(3) -0.009(3) -0.011(3) F5B 0.0413(16) 0.0544(18) 0.0354(15) 0.0058(13) -0.0085(12) -0.0139(14) F6B 0.0345(10) 0.0547(13) 0.0417(11) -0.0040(9) -0.0066(9) -0.0218(10) F7B 0.0278(9) 0.0423(11) 0.0399(10) 0.0067(8) -0.0141(8) -0.0136(8) F8B 0.107(2) 0.0850(19) 0.0827(19) 0.0454(16) -0.0720(18) -0.0659(18) _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 N3 2.135(3) . ? Fe1 N5 2.137(3) . ? Fe1 N9 2.140(3) . ? Fe1 N7 2.147(3) . ? Fe1 N1 2.148(2) . ? Fe1 N11 2.174(3) . ? N1 C2 1.341(3) . ? N1 N2 1.378(3) . ? N2 C4 1.367(3) . ? N2 C16 1.457(3) . ? N3 C7 1.338(3) . ? N3 N4 1.378(3) . ? N4 C9 1.365(3) . ? N4 C16 1.450(3) . ? N5 C12 1.339(3) . ? N5 N6 1.372(3) . ? N6 C14 1.367(3) . ? N6 C16 1.446(3) . ? N7 C17 1.342(4) . ? N7 N8 1.364(3) . ? N8 C19 1.357(3) . ? N8 C29 1.453(3) . ? N9 C21 1.332(4) . ? N9 N10 1.360(3) . ? N10 C23 1.355(3) . ? N10 C29 1.457(3) . ? N11 C25 1.341(4) . ? N11 N12 1.367(3) . ? N12 C27 1.360(4) . ? N12 C29 1.443(4) . ? C1 C2 1.496(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.408(4) . ? C3 C4 1.376(4) . ? C3 H3 0.9500 . ? C4 C5 1.492(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.501(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.410(4) . ? C8 C9 1.372(4) . ? C8 H8 0.9500 . ? C9 C10 1.498(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.492(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.410(4) . ? C13 C14 1.373(4) . ? C13 H13 0.9500 . ? C14 C15 1.487(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16 1.0000 . ? C17 C18 1.402(4) . ? C17 H17 0.9500 . ? C18 C19 1.378(4) . ? C18 C20 1.510(4) . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.409(4) . ? C21 H21 0.9500 . ? C22 C23 1.382(4) . ? C22 C24 1.509(4) . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.403(5) . ? C25 H25 0.9500 . ? C26 C27 1.370(5) . ? C26 C28 1.510(4) . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29 1.0000 . ? N13 C30 1.134(4) . ? C30 C31 1.464(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? N14 C32 1.109(13) . ? C32 C33 1.504(16) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? B1 F4 1.376(4) . ? B1 F3 1.393(4) . ? B1 F2 1.409(4) . ? B1 F1 1.415(4) . ? B2A F8A 1.277(9) . ? B2A F5A 1.335(11) . ? B2A F7A 1.372(9) . ? B2A F6A 1.530(10) . ? B2B F5B 1.397(9) . ? 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 N3 Fe1 N5 85.57(9) . . ? N3 Fe1 N9 176.02(8) . . ? N5 Fe1 N9 91.78(9) . . ? N3 Fe1 N7 99.15(10) . . ? N5 Fe1 N7 94.78(10) . . ? N9 Fe1 N7 84.02(10) . . ? N3 Fe1 N1 84.26(9) . . ? N5 Fe1 N1 85.88(10) . . ? N9 Fe1 N1 92.60(10) . . ? N7 Fe1 N1 176.56(8) . . ? N3 Fe1 N11 98.18(9) . . ? N5 Fe1 N11 176.09(8) . . ? N9 Fe1 N11 84.53(9) . . ? N7 Fe1 N11 83.57(10) . . ? N1 Fe1 N11 95.55(10) . . ? C2 N1 N2 105.3(2) . . ? C2 N1 Fe1 138.69(18) . . ? N2 N1 Fe1 116.04(15) . . ? C4 N2 N1 111.6(2) . . ? C4 N2 C16 128.3(2) . . ? N1 N2 C16 119.74(19) . . ? C7 N3 N4 104.6(2) . . ? C7 N3 Fe1 138.79(18) . . ? N4 N3 Fe1 115.67(16) . . ? C9 N4 N3 112.2(2) . . ? C9 N4 C16 127.5(2) . . ? N3 N4 C16 120.3(2) . . ? C12 N5 N6 104.7(2) . . ? C12 N5 Fe1 138.05(18) . . ? N6 N5 Fe1 116.80(15) . . ? C14 N6 N5 112.2(2) . . ? C14 N6 C16 128.5(2) . . ? N5 N6 C16 119.3(2) . . ? C17 N7 N8 104.4(2) . . ? C17 N7 Fe1 138.2(2) . . ? N8 N7 Fe1 116.62(16) . . ? C19 N8 N7 111.9(2) . . ? C19 N8 C29 127.4(2) . . ? N7 N8 C29 120.6(2) . . ? C21 N9 N10 104.8(2) . . ? C21 N9 Fe1 135.04(18) . . ? N10 N9 Fe1 117.93(17) . . ? C23 N10 N9 111.9(2) . . ? C23 N10 C29 128.5(2) . . ? N9 N10 C29 119.3(2) . . ? C25 N11 N12 103.7(2) . . ? C25 N11 Fe1 139.4(2) . . ? N12 N11 Fe1 116.35(16) . . ? C27 N12 N11 112.0(2) . . ? C27 N12 C29 127.5(2) . . ? N11 N12 C29 120.5(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 110.2(2) . . ? N1 C2 C1 122.9(2) . . ? C3 C2 C1 126.9(2) . . ? C4 C3 C2 106.8(2) . . ? C4 C3 H3 126.6 . . ? C2 C3 H3 126.6 . . ? N2 C4 C3 106.0(2) . . ? N2 C4 C5 123.5(2) . . ? C3 C4 C5 130.4(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 110.7(2) . . ? N3 C7 C6 121.2(3) . . ? C8 C7 C6 128.1(2) . . ? C9 C8 C7 106.6(2) . . ? C9 C8 H8 126.7 . . ? C7 C8 H8 126.7 . . ? N4 C9 C8 105.8(2) . . ? N4 C9 C10 123.0(2) . . ? C8 C9 C10 131.2(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 110.8(2) . . ? N5 C12 C11 121.8(2) . . ? C13 C12 C11 127.5(2) . . ? C14 C13 C12 106.4(2) . . ? C14 C13 H13 126.8 . . ? C12 C13 H13 126.8 . . ? N6 C14 C13 105.9(2) . . ? N6 C14 C15 123.1(2) . . ? C13 C14 C15 130.9(2) . . ? 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 . . ? N6 C16 N4 111.16(19) . . ? N6 C16 N2 111.4(2) . . ? N4 C16 N2 110.88(19) . . ? N6 C16 H16 107.7 . . ? N4 C16 H16 107.7 . . ? N2 C16 H16 107.7 . . ? N7 C17 C18 111.6(3) . . ? N7 C17 H17 124.2 . . ? C18 C17 H17 124.2 . . ? C19 C18 C17 105.0(2) . . ? C19 C18 C20 127.0(3) . . ? C17 C18 C20 128.0(3) . . ? N8 C19 C18 107.0(3) . . ? N8 C19 H19 126.5 . . ? C18 C19 H19 126.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N9 C21 C22 111.7(2) . . ? N9 C21 H21 124.2 . . ? C22 C21 H21 124.2 . . ? C23 C22 C21 104.5(2) . . ? C23 C22 C24 128.7(3) . . ? C21 C22 C24 126.8(2) . . ? N10 C23 C22 107.1(2) . . ? N10 C23 H23 126.5 . . ? C22 C23 H23 126.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N11 C25 C26 112.3(3) . . ? N11 C25 H25 123.8 . . ? C26 C25 H25 123.8 . . ? C27 C26 C25 104.7(3) . . ? C27 C26 C28 126.9(3) . . ? C25 C26 C28 128.4(3) . . ? N12 C27 C26 107.2(3) . . ? N12 C27 H27 126.4 . . ? C26 C27 H27 126.4 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N12 C29 N8 110.9(2) . . ? N12 C29 N10 110.6(2) . . ? N8 C29 N10 110.4(2) . . ? N12 C29 H29 108.3 . . ? N8 C29 H29 108.3 . . ? N10 C29 H29 108.3 . . ? N13 C30 C31 179.5(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N14 C32 C33 177.4(10) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? F4 B1 F3 110.1(2) . . ? F4 B1 F2 109.6(2) . . ? F3 B1 F2 109.6(2) . . ? F4 B1 F1 109.7(2) . . ? F3 B1 F1 110.0(2) . . ? F2 B1 F1 107.8(2) . . ? F8A B2A F5A 100.9(7) . . ? F8A B2A F7A 118.9(7) . . ? F5A B2A F7A 117.5(7) . . ? F8A B2A F6A 112.4(7) . . ? F5A B2A F6A 104.3(6) . . ? F7A B2A F6A 102.2(6) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.69 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.705 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.079 #=END data_2-25ss _database_code_depnum_ccdc_archive 'CCDC 650147' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Fe(4-Metpm)(dmtpm))(BF!4$)!2$.3/2(MeCN) _chemical_melting_point ? _chemical_formula_moiety 'C29 H38 Fe N12, 2(B F4), 1.5(C2 H3 N)' _chemical_formula_sum 'C32 H42.50 B2 F8 Fe N13.50' _chemical_formula_weight 845.76 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' 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 Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.939(9) _cell_length_b 12.345(10) _cell_length_c 15.054(12) _cell_angle_alpha 88.730(12) _cell_angle_beta 80.016(12) _cell_angle_gamma 63.535(11) _cell_volume 1952(3) _cell_formula_units_Z 2 _cell_measurement_temperature 25(2) _cell_measurement_reflns_used 968 _cell_measurement_theta_min 3.219 _cell_measurement_theta_max 25.477 _exptl_crystal_description block-shaped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 0.469 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.776 _exptl_absorpt_correction_T_max 0.870 _exptl_absorpt_process_details 'SADABS (Bruker, 1996)' _exptl_special_details ; In a thin film of perfluorpolyether oil on a mohair fibre ; _diffrn_ambient_temperature 25(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 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 213 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 15533 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0259 _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 18 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.56 _reflns_number_total 7171 _reflns_number_gt 6387 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXTL (BrukerAXS, 2000)' _computing_structure_refinement 'SHELXTL (BrukerAXS, 2000)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material XCIF _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. One of the two crystallographically distinct MeCN solvent molucules (N14, C32, C33) exhibits two-fold symmetry-related disorder, where the alternate positons are in close proximity and can not be occupied simultaneously. The occupancies of these atoms were fixed to be 0.5. One BF4 counterions exhibits two-fold positional disorder on the F5 & F8 atoms. Pairs of atom sites were appropriately selected and separated into parts (A & B) to account for the disorder. Equivalent atoms were fixed to have the same ADPs. The relative occupancy of the two components was refined. The disorder of the MeCN molecule and the BF4 molecules are correlated, with the F5A position in close proximity to one of the MeCN orientatios which therefore cannot be occupied simultaneously. The alternate position of F5B is not in close proximity to either MeCN orientation. ; _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^)+(0.0556P)^2^+3.1932P] 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 7171 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.1141 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 0.68856(3) 0.61415(3) 0.73892(2) 0.01382(10) Uani 1 1 d . . . N1 N 0.61804(17) 0.50582(17) 0.80359(12) 0.0154(4) Uani 1 1 d . . . N2 N 0.66549(17) 0.45479(16) 0.87983(12) 0.0141(4) Uani 1 1 d . . . N3 N 0.66985(18) 0.68667(17) 0.86338(13) 0.0163(4) Uani 1 1 d . . . N4 N 0.71964(17) 0.60493(16) 0.92708(12) 0.0149(4) Uani 1 1 d . . . N5 N 0.86413(18) 0.48847(17) 0.75326(12) 0.0158(4) Uani 1 1 d . . . N6 N 0.87585(17) 0.43350(16) 0.83398(12) 0.0141(4) Uani 1 1 d . . . N7 N 0.75793(19) 0.71989(18) 0.67139(14) 0.0213(4) Uani 1 1 d . . . N8 N 0.72100(19) 0.75858(18) 0.59077(14) 0.0205(4) Uani 1 1 d . . . N9 N 0.70755(18) 0.53460(17) 0.61936(13) 0.0188(4) Uani 1 1 d . . . N10 N 0.66649(19) 0.60616(17) 0.54996(13) 0.0187(4) Uani 1 1 d . . . N11 N 0.51608(19) 0.73929(18) 0.71803(14) 0.0208(4) Uani 1 1 d . . . N12 N 0.50988(19) 0.78469(18) 0.63426(15) 0.0222(4) Uani 1 1 d . . . C1 C 0.4582(2) 0.4970(2) 0.71962(17) 0.0251(5) Uani 1 1 d . . . H1A H 0.4822 0.5496 0.6792 0.038 Uiso 1 1 calc R . . H1B H 0.3677 0.5403 0.7465 0.038 Uiso 1 1 calc R . . H1C H 0.4740 0.4236 0.6851 0.038 Uiso 1 1 calc R . . C2 C 0.5359(2) 0.4626(2) 0.79305(16) 0.0181(5) Uani 1 1 d . . . C3 C 0.5331(2) 0.3831(2) 0.86124(15) 0.0182(5) Uani 1 1 d . . . H3 H 0.4835 0.3399 0.8682 0.022 Uiso 1 1 calc R . . C4 C 0.6158(2) 0.3797(2) 0.91576(15) 0.0164(4) Uani 1 1 d . . . C5 C 0.6495(2) 0.3122(2) 0.99836(16) 0.0209(5) Uani 1 1 d . . . H5A H 0.7409 0.2572 0.9878 0.031 Uiso 1 1 calc R . . H5B H 0.6014 0.2651 1.0120 0.031 Uiso 1 1 calc R . . H5C H 0.6284 0.3699 1.0495 0.031 Uiso 1 1 calc R . . C6 C 0.5673(2) 0.9117(2) 0.85961(18) 0.0244(5) Uani 1 1 d . . . H6A H 0.6009 0.8988 0.7945 0.037 Uiso 1 1 calc R . . H6B H 0.5836 0.9746 0.8850 0.037 Uiso 1 1 calc R . . H6C H 0.4754 0.9375 0.8700 0.037 Uiso 1 1 calc R . . C7 C 0.6315(2) 0.7958(2) 0.90438(16) 0.0196(5) Uani 1 1 d . . . C8 C 0.6582(2) 0.7826(2) 0.99291(16) 0.0205(5) Uani 1 1 d . . . H8 H 0.6398 0.8464 1.0358 0.025 Uiso 1 1 calc R . . C9 C 0.7156(2) 0.6608(2) 1.00552(15) 0.0172(5) Uani 1 1 d . . . C10 C 0.7711(2) 0.5917(2) 1.08285(15) 0.0210(5) Uani 1 1 d . . . H10A H 0.7398 0.5311 1.0972 0.031 Uiso 1 1 calc R . . H10B H 0.7457 0.6479 1.1358 0.031 Uiso 1 1 calc R . . H10C H 0.8641 0.5511 1.0662 0.031 Uiso 1 1 calc R . . C11 C 1.0114(2) 0.4659(2) 0.60778(17) 0.0261(5) Uani 1 1 d . . . H11A H 0.9324 0.5150 0.5856 0.039 Uiso 1 1 calc R . . H11B H 1.0622 0.3918 0.5685 0.039 Uiso 1 1 calc R . . H11C H 1.0599 0.5124 0.6075 0.039 Uiso 1 1 calc R . . C12 C 0.9804(2) 0.4331(2) 0.70230(15) 0.0191(5) Uani 1 1 d . . . C13 C 1.0650(2) 0.3434(2) 0.75023(16) 0.0199(5) Uani 1 1 d . . . H13 H 1.1527 0.2919 0.7289 0.024 Uiso 1 1 calc R . . C14 C 0.9964(2) 0.3447(2) 0.83354(15) 0.0168(5) Uani 1 1 d . . . C15 C 1.0332(2) 0.2676(2) 0.91187(16) 0.0218(5) Uani 1 1 d . . . H15A H 1.1243 0.2118 0.8983 0.033 Uiso 1 1 calc R . . H15B H 0.9843 0.2210 0.9225 0.033 Uiso 1 1 calc R . . H15C H 1.0151 0.3196 0.9660 0.033 Uiso 1 1 calc R . . C16 C 0.7659(2) 0.47668(19) 0.90528(15) 0.0142(4) Uani 1 1 d . . . H16 H 0.7911 0.4318 0.9602 0.017 Uiso 1 1 calc R . . C17 C 0.8440(2) 0.7589(2) 0.67914(18) 0.0263(5) Uani 1 1 d . . . H17 H 0.8874 0.7451 0.7286 0.032 Uiso 1 1 calc R . . C18 C 0.8615(2) 0.8232(2) 0.6042(2) 0.0294(6) Uani 1 1 d . . . C19 C 0.7810(2) 0.8216(2) 0.54886(19) 0.0257(5) Uani 1 1 d . . . H19 H 0.7700 0.8576 0.4926 0.031 Uiso 1 1 calc R . . C20 C 0.9477(3) 0.8843(3) 0.5874(2) 0.0386(7) Uani 1 1 d . . . H20A H 1.0014 0.8633 0.6336 0.058 Uiso 1 1 calc R . . H20B H 0.8959 0.9724 0.5901 0.058 Uiso 1 1 calc R . . H20C H 1.0016 0.8567 0.5275 0.058 Uiso 1 1 calc R . . C21 C 0.7345(2) 0.4234(2) 0.58990(16) 0.0196(5) Uani 1 1 d . . . H21 H 0.7675 0.3535 0.6235 0.023 Uiso 1 1 calc R . . C22 C 0.7077(2) 0.4225(2) 0.50215(16) 0.0206(5) Uani 1 1 d . . . C23 C 0.6645(2) 0.5416(2) 0.47897(16) 0.0202(5) Uani 1 1 d . . . H23 H 0.6384 0.5724 0.4238 0.024 Uiso 1 1 calc R . . C24 C 0.7161(3) 0.3162(2) 0.44957(17) 0.0247(5) Uani 1 1 d . . . H24A H 0.7581 0.2420 0.4805 0.037 Uiso 1 1 calc R . . H24B H 0.7654 0.3085 0.3888 0.037 Uiso 1 1 calc R . . H24C H 0.6302 0.3288 0.4451 0.037 Uiso 1 1 calc R . . C25 C 0.3985(2) 0.8005(2) 0.76610(19) 0.0267(6) Uani 1 1 d . . . H25 H 0.3735 0.7879 0.8273 0.032 Uiso 1 1 calc R . . C26 C 0.3167(2) 0.8858(2) 0.7145(2) 0.0317(6) Uani 1 1 d . . . C27 C 0.3906(2) 0.8737(2) 0.6310(2) 0.0288(6) Uani 1 1 d . . . H27 H 0.3637 0.9189 0.5804 0.035 Uiso 1 1 calc R . . C28 C 0.1783(3) 0.9717(3) 0.7444(3) 0.0420(8) Uani 1 1 d . . . H28A H 0.1681 1.0215 0.7978 0.063 Uiso 1 1 calc R . . H28B H 0.1296 0.9255 0.7593 0.063 Uiso 1 1 calc R . . H28C H 0.1470 1.0243 0.6955 0.063 Uiso 1 1 calc R . . C29 C 0.6222(2) 0.7360(2) 0.56417(17) 0.0209(5) Uani 1 1 d . . . H29 H 0.6007 0.7759 0.5068 0.025 Uiso 1 1 calc R . . N13 N 0.8629(2) 0.2034(2) 0.73979(18) 0.0345(6) Uani 1 1 d . . . C30 C 0.8114(2) 0.1458(2) 0.75847(18) 0.0241(5) Uani 1 1 d . . . C31 C 0.7442(3) 0.0723(3) 0.7833(2) 0.0407(7) Uani 1 1 d . . . H31A H 0.7052 0.0653 0.7330 0.061 Uiso 1 1 calc R . . H31B H 0.6778 0.1110 0.8367 0.061 Uiso 1 1 calc R . . H31C H 0.8046 -0.0086 0.7970 0.061 Uiso 1 1 calc R . . N14 N 1.2615(5) -0.0097(5) 0.9889(4) 0.0374(11) Uani 0.50 1 d P . . C32 C 1.1613(8) -0.0063(6) 1.0081(5) 0.0565(19) Uani 0.50 1 d P . . C33 C 1.0357(8) -0.0014(7) 1.0301(6) 0.060(2) Uani 0.50 1 d P . . H33A H 1.0246 -0.0470 0.9827 0.089 Uiso 0.50 1 calc PR . . H33B H 0.9708 0.0832 1.0343 0.089 Uiso 0.50 1 calc PR . . H33C H 1.0271 -0.0372 1.0881 0.089 Uiso 0.50 1 calc PR . . B1 B 0.5396(3) 0.8530(3) 0.3405(2) 0.0244(6) Uani 1 1 d . . . F1 F 0.64824(14) 0.83797(14) 0.37483(10) 0.0296(3) Uani 1 1 d . . . F2 F 0.48313(17) 0.78914(16) 0.39353(13) 0.0417(4) Uani 1 1 d . . . F3 F 0.57434(18) 0.80832(19) 0.25124(12) 0.0527(5) Uani 1 1 d . . . F4 F 0.45404(14) 0.97415(13) 0.34694(11) 0.0313(4) Uani 1 1 d . . . B2 B 0.9390(4) 0.2848(5) 1.1615(3) 0.0573(12) Uani 1 1 d . . . F6 F 1.01341(15) 0.34144(15) 1.13094(10) 0.0326(4) Uani 1 1 d . A . F7 F 0.84727(14) 0.30767(15) 1.10920(11) 0.0340(4) Uani 1 1 d . A . F5A F 1.0325(4) 0.1513(3) 1.1228(3) 0.0512(7) Uani 0.520(2) 1 d P A 1 F8A F 0.9016(4) 0.2713(5) 1.2421(2) 0.0542(9) Uani 0.520(2) 1 d P A 1 F5B F 0.9994(4) 0.1812(4) 1.1957(3) 0.0512(7) Uani 0.480(2) 1 d P A 2 F8B F 0.8604(4) 0.3740(5) 1.2504(2) 0.0542(9) Uani 0.480(2) 1 d P A 2 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 0.01453(17) 0.01249(17) 0.01451(17) 0.00110(12) -0.00481(12) -0.00539(13) N1 0.0147(9) 0.0174(9) 0.0140(9) 0.0021(7) -0.0059(7) -0.0061(8) N2 0.0142(9) 0.0139(9) 0.0149(9) 0.0018(7) -0.0048(7) -0.0063(7) N3 0.0156(9) 0.0138(9) 0.0196(10) 0.0027(7) -0.0045(7) -0.0062(8) N4 0.0154(9) 0.0146(9) 0.0154(9) 0.0004(7) -0.0039(7) -0.0070(8) N5 0.0198(10) 0.0140(9) 0.0139(9) 0.0007(7) -0.0019(7) -0.0083(8) N6 0.0141(9) 0.0150(9) 0.0128(9) 0.0013(7) -0.0032(7) -0.0060(8) N7 0.0175(10) 0.0195(10) 0.0252(11) -0.0053(8) -0.0075(8) -0.0053(8) N8 0.0195(10) 0.0167(10) 0.0280(11) 0.0014(8) -0.0069(8) -0.0097(8) N9 0.0195(10) 0.0158(10) 0.0234(10) 0.0054(8) -0.0110(8) -0.0077(8) N10 0.0204(10) 0.0163(10) 0.0229(10) 0.0055(8) -0.0097(8) -0.0094(8) N11 0.0209(10) 0.0163(10) 0.0271(11) 0.0004(8) -0.0019(8) -0.0109(8) N12 0.0180(10) 0.0139(10) 0.0361(12) 0.0029(8) -0.0086(9) -0.0071(8) C1 0.0254(13) 0.0296(13) 0.0280(13) 0.0051(10) -0.0133(11) -0.0163(11) C2 0.0147(11) 0.0187(11) 0.0200(11) -0.0020(9) -0.0039(9) -0.0062(9) C3 0.0171(11) 0.0193(11) 0.0208(11) -0.0008(9) -0.0024(9) -0.0106(9) C4 0.0150(11) 0.0147(11) 0.0185(11) -0.0009(9) -0.0005(9) -0.0066(9) C5 0.0249(12) 0.0222(12) 0.0208(12) 0.0050(9) -0.0064(10) -0.0144(10) C6 0.0251(13) 0.0141(11) 0.0335(14) 0.0001(10) -0.0072(11) -0.0076(10) C7 0.0152(11) 0.0161(11) 0.0275(12) -0.0010(9) -0.0017(9) -0.0076(9) C8 0.0172(11) 0.0191(12) 0.0247(12) -0.0066(9) -0.0004(9) -0.0084(10) C9 0.0139(10) 0.0220(12) 0.0175(11) -0.0043(9) -0.0003(9) -0.0104(9) C10 0.0199(12) 0.0268(13) 0.0175(11) -0.0020(9) -0.0050(9) -0.0108(10) C11 0.0262(13) 0.0244(13) 0.0219(13) -0.0001(10) 0.0055(10) -0.0098(11) C12 0.0219(12) 0.0184(11) 0.0180(11) -0.0035(9) 0.0005(9) -0.0111(10) C13 0.0150(11) 0.0193(12) 0.0245(12) -0.0032(9) -0.0010(9) -0.0078(9) C14 0.0146(11) 0.0156(11) 0.0217(11) -0.0013(9) -0.0056(9) -0.0072(9) C15 0.0186(12) 0.0193(12) 0.0260(12) 0.0039(10) -0.0088(10) -0.0055(10) C16 0.0137(10) 0.0139(10) 0.0162(10) -0.0003(8) -0.0038(8) -0.0069(9) C17 0.0190(12) 0.0264(13) 0.0330(14) -0.0088(11) -0.0054(10) -0.0090(10) C18 0.0176(12) 0.0230(13) 0.0466(16) -0.0106(12) -0.0017(11) -0.0091(10) C19 0.0221(12) 0.0166(12) 0.0378(15) -0.0006(10) -0.0015(11) -0.0095(10) C20 0.0303(15) 0.0371(16) 0.0546(19) -0.0026(14) -0.0035(13) -0.0221(13) C21 0.0190(11) 0.0161(11) 0.0253(12) 0.0032(9) -0.0084(9) -0.0080(9) C22 0.0188(11) 0.0214(12) 0.0232(12) 0.0014(9) -0.0055(9) -0.0098(10) C23 0.0207(12) 0.0223(12) 0.0213(12) 0.0029(9) -0.0074(9) -0.0119(10) C24 0.0305(13) 0.0215(12) 0.0244(12) 0.0011(10) -0.0095(10) -0.0120(11) C25 0.0206(12) 0.0206(12) 0.0377(15) -0.0069(11) 0.0010(11) -0.0100(10) C26 0.0212(13) 0.0201(13) 0.0547(18) -0.0088(12) -0.0049(12) -0.0102(11) C27 0.0232(13) 0.0137(12) 0.0533(17) 0.0036(11) -0.0172(12) -0.0082(10) C28 0.0234(14) 0.0263(15) 0.070(2) -0.0096(14) -0.0094(14) -0.0050(12) C29 0.0210(12) 0.0157(11) 0.0294(13) 0.0044(9) -0.0097(10) -0.0095(10) N13 0.0248(12) 0.0244(12) 0.0531(16) -0.0006(11) -0.0112(11) -0.0085(10) C30 0.0217(12) 0.0159(12) 0.0313(13) -0.0008(10) -0.0093(10) -0.0037(10) C31 0.0389(17) 0.0233(14) 0.058(2) 0.0004(13) -0.0020(14) -0.0142(13) N14 0.028(3) 0.036(3) 0.050(3) 0.004(2) -0.005(2) -0.015(2) C32 0.072(5) 0.032(4) 0.055(4) 0.002(3) -0.014(4) -0.012(4) C33 0.064(5) 0.049(4) 0.067(5) 0.029(4) -0.008(4) -0.029(4) B1 0.0238(14) 0.0171(13) 0.0274(14) 0.0010(11) -0.0039(11) -0.0053(11) F1 0.0207(7) 0.0303(8) 0.0332(8) 0.0056(6) -0.0036(6) -0.0081(6) F2 0.0483(10) 0.0414(10) 0.0543(11) 0.0262(8) -0.0268(9) -0.0317(9) F3 0.0454(11) 0.0606(12) 0.0370(10) -0.0242(9) -0.0006(8) -0.0117(9) F4 0.0278(8) 0.0180(7) 0.0450(9) 0.0038(6) -0.0099(7) -0.0065(6) B2 0.0323(19) 0.086(3) 0.064(3) 0.049(2) -0.0279(19) -0.032(2) F6 0.0289(8) 0.0408(9) 0.0313(8) 0.0006(7) -0.0083(7) -0.0172(7) F7 0.0246(8) 0.0405(9) 0.0387(9) 0.0047(7) -0.0112(7) -0.0143(7) F5A 0.0439(16) 0.0457(16) 0.0677(18) 0.0206(16) -0.0310(17) -0.0168(13) F8A 0.0437(18) 0.109(3) 0.0203(11) 0.0031(19) -0.0057(12) -0.043(2) F5B 0.0439(16) 0.0457(16) 0.0677(18) 0.0206(16) -0.0310(17) -0.0168(13) F8B 0.0437(18) 0.109(3) 0.0203(11) 0.0031(19) -0.0057(12) -0.043(2) _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 N9 1.998(2) . ? Fe1 N7 2.009(2) . ? Fe1 N5 2.023(2) . ? Fe1 N11 2.023(2) . ? Fe1 N1 2.026(2) . ? Fe1 N3 2.028(2) . ? N1 C2 1.339(3) . ? N1 N2 1.382(3) . ? N2 C4 1.364(3) . ? N2 C16 1.452(3) . ? N3 C7 1.339(3) . ? N3 N4 1.382(3) . ? N4 C9 1.363(3) . ? N4 C16 1.449(3) . ? N5 C12 1.338(3) . ? N5 N6 1.376(3) . ? N6 C14 1.366(3) . ? N6 C16 1.440(3) . ? N7 C17 1.337(3) . ? N7 N8 1.367(3) . ? N8 C19 1.355(3) . ? N8 C29 1.446(3) . ? N9 C21 1.330(3) . ? N9 N10 1.365(3) . ? N10 C23 1.357(3) . ? N10 C29 1.454(3) . ? N11 C25 1.338(3) . ? N11 N12 1.369(3) . ? N12 C27 1.366(3) . ? N12 C29 1.447(3) . ? C1 C2 1.499(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.412(3) . ? C3 C4 1.376(3) . ? C3 H3 0.9500 . ? C4 C5 1.494(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.500(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.413(4) . ? C8 C9 1.372(4) . ? C8 H8 0.9500 . ? C9 C10 1.497(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.501(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.410(3) . ? C13 C14 1.370(3) . ? C13 H13 0.9500 . ? C14 C15 1.499(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16 1.0000 . ? C17 C18 1.404(4) . ? C17 H17 0.9500 . ? C18 C19 1.383(4) . ? C18 C20 1.511(4) . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.414(3) . ? C21 H21 0.9500 . ? C22 C23 1.383(4) . ? C22 C24 1.503(3) . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.406(4) . ? C25 H25 0.9500 . ? C26 C27 1.374(4) . ? C26 C28 1.503(4) . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29 1.0000 . ? N13 C30 1.133(4) . ? C30 C31 1.461(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? N14 C32 1.163(10) . ? C32 C33 1.452(12) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? B1 F4 1.378(3) . ? B1 F3 1.385(4) . ? B1 F2 1.404(3) . ? B1 F1 1.413(3) . ? B2 F8A 1.253(5) . ? B2 F5B 1.303(6) . ? B2 F6 1.373(4) . ? B2 F7 1.383(4) . ? B2 F5A 1.574(7) . ? B2 F8B 1.610(7) . ? 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 N9 Fe1 N7 87.48(9) . . ? N9 Fe1 N5 90.74(8) . . ? N7 Fe1 N5 92.25(10) . . ? N9 Fe1 N11 86.95(9) . . ? N7 Fe1 N11 86.09(10) . . ? N5 Fe1 N11 177.21(8) . . ? N9 Fe1 N1 90.90(9) . . ? N7 Fe1 N1 178.34(7) . . ? N5 Fe1 N1 88.11(9) . . ? N11 Fe1 N1 93.49(9) . . ? N9 Fe1 N3 176.93(8) . . ? N7 Fe1 N3 95.33(9) . . ? N5 Fe1 N3 87.90(8) . . ? N11 Fe1 N3 94.48(8) . . ? N1 Fe1 N3 86.31(9) . . ? C2 N1 N2 105.12(18) . . ? C2 N1 Fe1 138.06(16) . . ? N2 N1 Fe1 116.78(14) . . ? C4 N2 N1 111.96(18) . . ? C4 N2 C16 129.23(19) . . ? N1 N2 C16 118.50(17) . . ? C7 N3 N4 104.83(19) . . ? C7 N3 Fe1 138.79(16) . . ? N4 N3 Fe1 116.05(14) . . ? C9 N4 N3 112.27(19) . . ? C9 N4 C16 128.60(19) . . ? N3 N4 C16 119.12(18) . . ? C12 N5 N6 104.78(18) . . ? C12 N5 Fe1 137.71(16) . . ? N6 N5 Fe1 117.36(14) . . ? C14 N6 N5 112.11(18) . . ? C14 N6 C16 129.66(19) . . ? N5 N6 C16 118.22(18) . . ? C17 N7 N8 105.1(2) . . ? C17 N7 Fe1 137.04(18) . . ? N8 N7 Fe1 117.54(15) . . ? C19 N8 N7 111.9(2) . . ? C19 N8 C29 128.9(2) . . ? N7 N8 C29 119.02(19) . . ? C21 N9 N10 105.27(19) . . ? C21 N9 Fe1 135.21(16) . . ? N10 N9 Fe1 118.59(15) . . ? C23 N10 N9 111.59(19) . . ? C23 N10 C29 130.0(2) . . ? N9 N10 C29 118.19(19) . . ? C25 N11 N12 105.0(2) . . ? C25 N11 Fe1 137.86(19) . . ? N12 N11 Fe1 116.98(15) . . ? C27 N12 N11 111.0(2) . . ? C27 N12 C29 129.5(2) . . ? N11 N12 C29 119.44(19) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 110.1(2) . . ? N1 C2 C1 123.9(2) . . ? C3 C2 C1 126.1(2) . . ? C4 C3 C2 107.1(2) . . ? C4 C3 H3 126.5 . . ? C2 C3 H3 126.5 . . ? N2 C4 C3 105.7(2) . . ? N2 C4 C5 123.8(2) . . ? C3 C4 C5 130.4(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 110.1(2) . . ? N3 C7 C6 122.6(2) . . ? C8 C7 C6 127.4(2) . . ? C9 C8 C7 107.3(2) . . ? C9 C8 H8 126.4 . . ? C7 C8 H8 126.4 . . ? N4 C9 C8 105.5(2) . . ? N4 C9 C10 122.6(2) . . ? C8 C9 C10 131.9(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 110.5(2) . . ? N5 C12 C11 122.9(2) . . ? C13 C12 C11 126.7(2) . . ? C14 C13 C12 106.8(2) . . ? C14 C13 H13 126.6 . . ? C12 C13 H13 126.6 . . ? N6 C14 C13 105.8(2) . . ? N6 C14 C15 122.8(2) . . ? C13 C14 C15 131.4(2) . . ? 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 . . ? N6 C16 N4 110.41(17) . . ? N6 C16 N2 110.87(18) . . ? N4 C16 N2 109.94(17) . . ? N6 C16 H16 108.5 . . ? N4 C16 H16 108.5 . . ? N2 C16 H16 108.5 . . ? N7 C17 C18 110.8(2) . . ? N7 C17 H17 124.6 . . ? C18 C17 H17 124.6 . . ? C19 C18 C17 105.7(2) . . ? C19 C18 C20 126.5(3) . . ? C17 C18 C20 127.8(3) . . ? N8 C19 C18 106.4(2) . . ? N8 C19 H19 126.8 . . ? C18 C19 H19 126.8 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N9 C21 C22 111.3(2) . . ? N9 C21 H21 124.3 . . ? C22 C21 H21 124.3 . . ? C23 C22 C21 104.7(2) . . ? C23 C22 C24 128.3(2) . . ? C21 C22 C24 126.9(2) . . ? N10 C23 C22 107.1(2) . . ? N10 C23 H23 126.5 . . ? C22 C23 H23 126.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N11 C25 C26 111.4(3) . . ? N11 C25 H25 124.3 . . ? C26 C25 H25 124.3 . . ? C27 C26 C25 105.1(2) . . ? C27 C26 C28 127.5(3) . . ? C25 C26 C28 127.4(3) . . ? N12 C27 C26 107.4(2) . . ? N12 C27 H27 126.3 . . ? C26 C27 H27 126.3 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N8 C29 N12 109.8(2) . . ? N8 C29 N10 109.69(19) . . ? N12 C29 N10 109.21(19) . . ? N8 C29 H29 109.4 . . ? N12 C29 H29 109.4 . . ? N10 C29 H29 109.4 . . ? N13 C30 C31 179.4(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N14 C32 C33 178.7(8) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? F4 B1 F3 110.0(2) . . ? F4 B1 F2 109.1(2) . . ? F3 B1 F2 110.1(2) . . ? F4 B1 F1 109.7(2) . . ? F3 B1 F1 110.1(2) . . ? F2 B1 F1 107.9(2) . . ? F8A B2 F6 127.0(4) . . ? F5B B2 F6 114.1(3) . . ? F8A B2 F7 111.9(3) . . ? F5B B2 F7 124.1(4) . . ? F6 B2 F7 111.4(3) . . ? F8A B2 F5A 103.1(4) . . ? F6 B2 F5A 99.8(3) . . ? F7 B2 F5A 97.9(4) . . ? F5B B2 F8B 102.4(4) . . ? F6 B2 F8B 96.4(4) . . ? F7 B2 F8B 103.1(3) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.56 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.213 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.070 #=END data_2-96K _database_code_depnum_ccdc_archive 'CCDC 650148' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Fe(4-Metpm)(dmtpm))(BF!4$)!2$.3/2(MeCN) _chemical_melting_point ? _chemical_formula_moiety 'C29 H38 Fe N12, 2(B F4), 1.5(C2 H3 N)' _chemical_formula_sum 'C32 H42.50 B2 F8 Fe N13.50' _chemical_formula_weight 845.76 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' 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 Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.918(2) _cell_length_b 12.367(2) _cell_length_c 15.048(3) _cell_angle_alpha 88.760(3) _cell_angle_beta 79.423(3) _cell_angle_gamma 63.765(3) _cell_volume 1951.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 96(2) _cell_measurement_reflns_used 4439 _cell_measurement_theta_min 2.374 _cell_measurement_theta_max 27.989 _exptl_crystal_description block-shaped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 0.469 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.848 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details 'SADABS (Bruker, 1996)' _exptl_special_details ; In a thin film of perfluorpolyether oil on a mohair fibre ; _diffrn_ambient_temperature 96(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 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 194 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 18851 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 28.04 _reflns_number_total 8860 _reflns_number_gt 7652 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXTL (BrukerAXS, 2000)' _computing_structure_refinement 'SHELXTL (BrukerAXS, 2000)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material XCIF _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. One of the two crystallographically distinct MeCN solvent molucules (N14, C32, C33) exhibits two-fold symmetry-related disorder, where the alternate positons are in close proximity and can not be occupied simultaneously. The occupancies of these atoms were fixed to be 0.5. One BF4 counterions exhibits two-fold positional disorder in the B2, F5 & F8 atom sites. Pairs of atom sites were appropriately selected and separated into parts (A & B) to account for the disorder. Equivalent atoms were fixed to have the same ADPs. The relative occupancy of the two components was refined. The disorder of the MeCN molecule and the BF4 molecules are correlated, with the B2A-F5A-F8A positions in close proximity to one of the MeCN orientatios which therefore cannot be occupied simultaneously. The alternate position of B2-F5B-F8B is not in close proximity to either MeCN orientation. ; _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^)+(0.0810P)^2^+2.9356P] 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 8860 _refine_ls_number_parameters 544 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1592 _refine_ls_wR_factor_gt 0.1480 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.037 _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 0.68869(3) 0.61714(3) 0.73794(2) 0.01969(11) Uani 1 1 d . . . N1 N 0.61872(18) 0.50330(18) 0.80549(12) 0.0219(4) Uani 1 1 d . . . N2 N 0.66702(18) 0.45403(17) 0.88093(12) 0.0194(4) Uani 1 1 d . . . N3 N 0.66926(19) 0.68774(17) 0.86764(14) 0.0236(4) Uani 1 1 d . . . N4 N 0.72022(18) 0.60449(17) 0.92857(13) 0.0211(4) Uani 1 1 d . . . N5 N 0.8687(2) 0.48911(18) 0.75323(13) 0.0255(4) Uani 1 1 d . . . N6 N 0.87758(18) 0.43472(17) 0.83350(13) 0.0214(4) Uani 1 1 d . . . N7 N 0.7570(2) 0.7281(2) 0.66428(16) 0.0312(5) Uani 1 1 d . . . N8 N 0.7176(2) 0.76383(19) 0.58477(16) 0.0295(4) Uani 1 1 d . . . N9 N 0.7100(2) 0.53674(19) 0.61249(15) 0.0296(5) Uani 1 1 d . . . N10 N 0.6647(2) 0.60953(19) 0.54567(14) 0.0272(4) Uani 1 1 d . . . N11 N 0.5101(2) 0.74416(19) 0.71490(16) 0.0322(5) Uani 1 1 d . . . N12 N 0.5064(2) 0.78714(19) 0.63074(17) 0.0318(5) Uani 1 1 d . . . C1 C 0.4603(3) 0.4911(3) 0.72402(19) 0.0388(6) Uani 1 1 d . . . H1A H 0.4876 0.5395 0.6811 0.058 Uiso 1 1 calc R . . H1B H 0.3700 0.5381 0.7514 0.058 Uiso 1 1 calc R . . H1C H 0.4723 0.4174 0.6921 0.058 Uiso 1 1 calc R . . C2 C 0.5380(2) 0.4579(2) 0.79661(16) 0.0259(5) Uani 1 1 d . . . C3 C 0.5367(2) 0.3793(2) 0.86471(17) 0.0272(5) Uani 1 1 d . . . H3 H 0.4879 0.3351 0.8726 0.033 Uiso 1 1 calc R . . C4 C 0.6189(2) 0.3782(2) 0.91775(16) 0.0234(4) Uani 1 1 d . . . C5 C 0.6537(3) 0.3125(2) 1.00014(18) 0.0307(5) Uani 1 1 d . . . H5A H 0.6326 0.3708 1.0509 0.046 Uiso 1 1 calc R . . H5B H 0.7453 0.2583 0.9886 0.046 Uiso 1 1 calc R . . H5C H 0.6059 0.2651 1.0152 0.046 Uiso 1 1 calc R . . C6 C 0.5698(3) 0.9107(2) 0.8672(2) 0.0385(6) Uani 1 1 d . . . H6A H 0.5986 0.8976 0.8013 0.058 Uiso 1 1 calc R . . H6B H 0.5918 0.9710 0.8900 0.058 Uiso 1 1 calc R . . H6C H 0.4772 0.9396 0.8822 0.058 Uiso 1 1 calc R . . C7 C 0.6335(2) 0.7948(2) 0.91002(18) 0.0283(5) Uani 1 1 d . . . C8 C 0.6624(2) 0.7788(2) 0.99745(18) 0.0301(5) Uani 1 1 d . . . H8 H 0.6457 0.8409 1.0413 0.036 Uiso 1 1 calc R . . C9 C 0.7189(2) 0.6575(2) 1.00741(16) 0.0245(5) Uani 1 1 d . . . C10 C 0.7738(3) 0.5863(3) 1.08344(17) 0.0307(5) Uani 1 1 d . . . H10A H 0.7416 0.5261 1.0967 0.046 Uiso 1 1 calc R . . H10B H 0.7488 0.6408 1.1374 0.046 Uiso 1 1 calc R . . H10C H 0.8670 0.5454 1.0660 0.046 Uiso 1 1 calc R . . C11 C 1.0176(4) 0.4652(3) 0.6083(2) 0.0524(9) Uani 1 1 d . . . H11A H 0.9390 0.5102 0.5851 0.079 Uiso 1 1 calc R . . H11B H 1.0728 0.3915 0.5692 0.079 Uiso 1 1 calc R . . H11C H 1.0620 0.5155 0.6089 0.079 Uiso 1 1 calc R . . C12 C 0.9856(3) 0.4324(3) 0.70212(18) 0.0342(6) Uani 1 1 d . . . C13 C 1.0675(3) 0.3422(3) 0.7497(2) 0.0358(6) Uani 1 1 d . . . H13 H 1.1552 0.2896 0.7283 0.043 Uiso 1 1 calc R . . C14 C 0.9967(2) 0.3446(2) 0.83310(18) 0.0282(5) Uani 1 1 d . . . C15 C 1.0308(3) 0.2684(3) 0.9102(2) 0.0380(6) Uani 1 1 d . . . H15A H 1.0121 0.3199 0.9648 0.057 Uiso 1 1 calc R . . H15B H 1.1219 0.2124 0.8966 0.057 Uiso 1 1 calc R . . H15C H 0.9809 0.2225 0.9202 0.057 Uiso 1 1 calc R . . C16 C 0.7669(2) 0.4773(2) 0.90517(15) 0.0194(4) Uani 1 1 d . . . H16 H 0.7924 0.4323 0.9598 0.023 Uiso 1 1 calc R . . C17 C 0.8432(3) 0.7688(3) 0.6668(2) 0.0411(7) Uani 1 1 d . . . H17 H 0.8883 0.7575 0.7148 0.049 Uiso 1 1 calc R . . C18 C 0.8588(3) 0.8305(3) 0.5894(3) 0.0441(7) Uani 1 1 d . . . C19 C 0.7766(3) 0.8256(2) 0.5384(2) 0.0377(6) Uani 1 1 d . . . H19 H 0.7635 0.8590 0.4816 0.045 Uiso 1 1 calc R . . C20 C 0.9442(4) 0.8918(4) 0.5669(3) 0.0657(11) Uani 1 1 d . . . H20A H 0.9940 0.8799 0.6145 0.098 Uiso 1 1 calc R . . H20B H 0.8920 0.9785 0.5629 0.098 Uiso 1 1 calc R . . H20C H 1.0022 0.8570 0.5087 0.098 Uiso 1 1 calc R . . C21 C 0.7364(2) 0.4266(2) 0.58192(18) 0.0289(5) Uani 1 1 d . . . H21 H 0.7715 0.3562 0.6141 0.035 Uiso 1 1 calc R . . C22 C 0.7060(2) 0.4274(2) 0.49601(17) 0.0287(5) Uani 1 1 d . . . C23 C 0.6603(2) 0.5466(2) 0.47508(17) 0.0290(5) Uani 1 1 d . . . H23 H 0.6311 0.5785 0.4212 0.035 Uiso 1 1 calc R . . C24 C 0.7159(3) 0.3217(3) 0.4424(2) 0.0397(6) Uani 1 1 d . . . H24A H 0.7456 0.2498 0.4773 0.060 Uiso 1 1 calc R . . H24B H 0.7767 0.3071 0.3852 0.060 Uiso 1 1 calc R . . H24C H 0.6321 0.3390 0.4298 0.060 Uiso 1 1 calc R . . C25 C 0.3915(3) 0.8072(3) 0.7615(3) 0.0459(8) Uani 1 1 d . . . H25 H 0.3637 0.7965 0.8229 0.055 Uiso 1 1 calc R . . C26 C 0.3129(3) 0.8914(3) 0.7082(3) 0.0545(10) Uani 1 1 d . . . C27 C 0.3895(3) 0.8757(2) 0.6261(3) 0.0457(8) Uani 1 1 d . . . H27 H 0.3654 0.9192 0.5744 0.055 Uiso 1 1 calc R . . C28 C 0.1742(4) 0.9785(4) 0.7365(4) 0.0899(18) Uani 1 1 d . . . H28A H 0.1636 1.0334 0.7868 0.135 Uiso 1 1 calc R . . H28B H 0.1248 0.9335 0.7560 0.135 Uiso 1 1 calc R . . H28C H 0.1438 1.0254 0.6852 0.135 Uiso 1 1 calc R . . C29 C 0.6192(3) 0.7382(2) 0.56054(18) 0.0290(5) Uani 1 1 d . . . H29 H 0.5971 0.7772 0.5032 0.035 Uiso 1 1 calc R . . N13 N 0.8642(3) 0.2063(3) 0.7278(3) 0.0600(8) Uani 1 1 d . . . C30 C 0.8162(3) 0.1466(3) 0.7504(2) 0.0402(7) Uani 1 1 d . . . C31 C 0.7539(4) 0.0710(3) 0.7799(3) 0.0611(10) Uani 1 1 d . . . H31A H 0.8171 -0.0078 0.7937 0.092 Uiso 1 1 calc R . . H31B H 0.7140 0.0600 0.7316 0.092 Uiso 1 1 calc R . . H31C H 0.6885 0.1097 0.8343 0.092 Uiso 1 1 calc R . . N14 N 1.2588(8) -0.0091(6) 0.9885(6) 0.0672(18) Uani 0.50 1 d P . . C32 C 1.1586(13) -0.0065(8) 1.0098(9) 0.090(3) Uani 0.50 1 d P . . C33 C 1.0318(12) 0.0002(12) 1.0360(9) 0.101(4) Uani 0.50 1 d P . . H33A H 1.0292 -0.0471 1.0888 0.151 Uiso 0.50 1 calc PR . . H33B H 1.0119 -0.0324 0.9855 0.151 Uiso 0.50 1 calc PR . . H33C H 0.9690 0.0847 1.0514 0.151 Uiso 0.50 1 calc PR . . B1 B 0.5334(3) 0.8546(3) 0.3378(2) 0.0370(7) Uani 1 1 d . . . F2 F 0.4704(3) 0.7986(2) 0.39279(18) 0.0758(8) Uani 1 1 d . . . F1 F 0.64272(18) 0.8376(2) 0.36972(14) 0.0528(5) Uani 1 1 d . . . F3 F 0.5668(3) 0.8075(3) 0.24888(18) 0.0945(10) Uani 1 1 d . . . F4 F 0.4543(2) 0.97390(18) 0.33969(18) 0.0622(6) Uani 1 1 d . . . B2A B 0.9597(8) 0.2553(9) 1.1480(7) 0.0551(19) Uani 0.498(4) 1 d PD A 1 F5A F 1.0457(5) 0.1496(6) 1.1104(4) 0.0790(10) Uani 0.498(4) 1 d P A 1 F8A F 0.9244(9) 0.2430(11) 1.2407(9) 0.098(3) Uani 0.498(4) 1 d P A 1 B2B B 0.9280(8) 0.3032(10) 1.1766(7) 0.0551(19) Uani 0.502(4) 1 d PD A 2 F5B F 0.8619(5) 0.3826(6) 1.2498(4) 0.0790(10) Uani 0.502(4) 1 d P A 2 F8B F 0.9833(9) 0.1902(11) 1.2163(9) 0.098(3) Uani 0.502(4) 1 d P A 2 F6 F 1.0173(2) 0.3356(2) 1.13055(16) 0.0659(6) Uani 1 1 d D . . F7 F 0.8498(2) 0.3032(2) 1.11601(16) 0.0608(6) Uani 1 1 d 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 Fe1 0.02388(18) 0.01838(17) 0.01795(17) 0.00236(11) -0.00615(12) -0.00968(13) N1 0.0225(9) 0.0263(10) 0.0184(9) 0.0011(7) -0.0065(7) -0.0113(8) N2 0.0207(9) 0.0212(9) 0.0188(8) 0.0015(7) -0.0056(7) -0.0108(7) N3 0.0263(10) 0.0175(9) 0.0274(10) 0.0027(7) -0.0068(8) -0.0097(8) N4 0.0238(9) 0.0201(9) 0.0210(9) -0.0010(7) -0.0051(7) -0.0109(8) N5 0.0305(10) 0.0251(10) 0.0205(9) -0.0021(7) 0.0031(8) -0.0149(9) N6 0.0208(9) 0.0215(9) 0.0219(9) -0.0007(7) -0.0026(7) -0.0100(8) N7 0.0303(11) 0.0271(11) 0.0373(12) -0.0038(9) -0.0132(9) -0.0110(9) N8 0.0309(11) 0.0246(10) 0.0394(12) 0.0063(9) -0.0143(9) -0.0156(9) N9 0.0380(12) 0.0239(10) 0.0350(11) 0.0107(8) -0.0207(9) -0.0162(9) N10 0.0339(11) 0.0265(10) 0.0301(10) 0.0090(8) -0.0166(9) -0.0177(9) N11 0.0284(11) 0.0236(10) 0.0435(13) 0.0012(9) -0.0021(9) -0.0125(9) N12 0.0279(11) 0.0207(10) 0.0507(13) 0.0085(9) -0.0154(10) -0.0116(9) C1 0.0416(15) 0.0592(19) 0.0335(14) 0.0101(12) -0.0181(12) -0.0347(15) C2 0.0233(11) 0.0329(13) 0.0246(11) -0.0024(9) -0.0052(9) -0.0148(10) C3 0.0247(11) 0.0326(13) 0.0286(12) -0.0017(9) -0.0024(9) -0.0176(10) C4 0.0244(11) 0.0230(11) 0.0241(11) -0.0009(8) -0.0025(9) -0.0124(9) C5 0.0366(14) 0.0309(13) 0.0322(13) 0.0091(10) -0.0095(10) -0.0209(11) C6 0.0438(16) 0.0195(12) 0.0497(16) -0.0009(11) -0.0086(13) -0.0121(11) C7 0.0259(12) 0.0212(11) 0.0368(13) -0.0045(9) -0.0004(10) -0.0114(9) C8 0.0280(12) 0.0266(12) 0.0357(13) -0.0101(10) -0.0005(10) -0.0138(10) C9 0.0219(11) 0.0296(12) 0.0240(11) -0.0071(9) -0.0005(9) -0.0145(10) C10 0.0321(13) 0.0386(14) 0.0246(11) -0.0051(10) -0.0076(10) -0.0174(11) C11 0.057(2) 0.0509(19) 0.0395(16) -0.0084(14) 0.0236(15) -0.0278(16) C12 0.0351(14) 0.0350(14) 0.0324(13) -0.0111(11) 0.0100(11) -0.0212(12) C13 0.0226(12) 0.0359(14) 0.0459(15) -0.0161(12) 0.0046(11) -0.0139(11) C14 0.0198(11) 0.0245(11) 0.0392(13) -0.0071(10) -0.0061(10) -0.0084(9) C15 0.0266(13) 0.0310(14) 0.0509(17) -0.0010(12) -0.0145(12) -0.0052(11) C16 0.0197(10) 0.0192(10) 0.0203(10) -0.0005(8) -0.0041(8) -0.0095(8) C17 0.0290(13) 0.0382(15) 0.0563(18) -0.0141(13) -0.0119(12) -0.0131(12) C18 0.0310(14) 0.0345(15) 0.070(2) -0.0092(14) -0.0053(14) -0.0182(12) C19 0.0357(14) 0.0260(13) 0.0559(18) 0.0045(12) -0.0089(13) -0.0177(11) C20 0.0458(19) 0.063(2) 0.101(3) -0.010(2) -0.004(2) -0.0380(19) C21 0.0315(12) 0.0231(11) 0.0367(13) 0.0057(10) -0.0148(10) -0.0133(10) C22 0.0292(12) 0.0285(12) 0.0316(12) 0.0016(10) -0.0073(10) -0.0151(10) C23 0.0319(13) 0.0330(13) 0.0274(12) 0.0047(10) -0.0109(10) -0.0175(11) C24 0.0498(17) 0.0333(14) 0.0380(15) -0.0013(11) -0.0121(13) -0.0187(13) C25 0.0289(14) 0.0308(14) 0.072(2) -0.0175(14) 0.0064(14) -0.0128(12) C26 0.0273(14) 0.0276(14) 0.105(3) -0.0200(16) -0.0112(17) -0.0088(12) C27 0.0349(15) 0.0188(12) 0.090(3) 0.0033(13) -0.0318(16) -0.0102(11) C28 0.0308(18) 0.050(2) 0.170(5) -0.043(3) -0.015(2) -0.0009(16) C29 0.0337(13) 0.0247(12) 0.0376(13) 0.0100(10) -0.0166(11) -0.0177(10) N13 0.0421(15) 0.0389(15) 0.101(3) 0.0101(16) -0.0239(16) -0.0165(13) C30 0.0370(15) 0.0264(13) 0.0563(18) 0.0041(12) -0.0190(13) -0.0097(12) C31 0.064(2) 0.0327(16) 0.084(3) 0.0040(17) -0.004(2) -0.0228(16) N14 0.062(4) 0.051(4) 0.087(5) 0.012(3) -0.012(4) -0.025(3) C32 0.109(9) 0.036(4) 0.111(9) 0.009(5) -0.039(7) -0.013(5) C33 0.092(9) 0.088(8) 0.123(11) 0.033(8) -0.008(7) -0.047(7) B1 0.0379(16) 0.0264(14) 0.0416(17) 0.0011(12) -0.0090(13) -0.0091(13) F2 0.0920(18) 0.0872(18) 0.0874(17) 0.0503(14) -0.0470(15) -0.0657(16) F1 0.0368(9) 0.0649(13) 0.0504(11) 0.0117(9) -0.0081(8) -0.0176(9) F3 0.092(2) 0.109(2) 0.0621(16) -0.0406(15) -0.0049(14) -0.0285(17) F4 0.0551(12) 0.0345(10) 0.0920(17) 0.0079(10) -0.0238(11) -0.0121(9) B2A 0.036(4) 0.061(6) 0.055(5) 0.006(4) -0.019(3) -0.006(4) F5A 0.062(2) 0.101(3) 0.065(2) 0.019(2) -0.0196(17) -0.026(2) F8A 0.099(7) 0.126(9) 0.101(6) 0.030(5) -0.065(6) -0.063(6) B2B 0.036(4) 0.061(6) 0.055(5) 0.006(4) -0.019(3) -0.006(4) F5B 0.062(2) 0.101(3) 0.065(2) 0.019(2) -0.0196(17) -0.026(2) F8B 0.099(7) 0.126(9) 0.101(6) 0.030(5) -0.065(6) -0.063(6) F6 0.0493(12) 0.0911(17) 0.0609(13) -0.0100(12) -0.0111(10) -0.0336(12) F7 0.0469(11) 0.0626(13) 0.0769(15) 0.0055(11) -0.0304(10) -0.0212(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 N9 2.073(2) . ? Fe1 N5 2.079(2) . ? Fe1 N3 2.087(2) . ? Fe1 N7 2.089(2) . ? Fe1 N1 2.092(2) . ? Fe1 N11 2.100(2) . ? N1 C2 1.336(3) . ? N1 N2 1.375(3) . ? N2 C4 1.361(3) . ? N2 C16 1.449(3) . ? N3 C7 1.334(3) . ? N3 N4 1.371(3) . ? N4 C9 1.362(3) . ? N4 C16 1.445(3) . ? N5 C12 1.339(3) . ? N5 N6 1.368(3) . ? N6 C14 1.362(3) . ? N6 C16 1.438(3) . ? N7 C17 1.335(4) . ? N7 N8 1.359(3) . ? N8 C19 1.355(4) . ? N8 C29 1.449(3) . ? N9 C21 1.327(3) . ? N9 N10 1.358(3) . ? N10 C23 1.353(3) . ? N10 C29 1.444(3) . ? N11 C25 1.335(4) . ? N11 N12 1.363(3) . ? N12 C27 1.353(4) . ? N12 C29 1.441(4) . ? C1 C2 1.495(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.401(4) . ? C3 C4 1.369(3) . ? C3 H3 0.9500 . ? C4 C5 1.488(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.491(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.408(4) . ? C8 C9 1.364(4) . ? C8 H8 0.9500 . ? C9 C10 1.495(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.489(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.404(4) . ? C13 C14 1.370(4) . ? C13 H13 0.9500 . ? C14 C15 1.478(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16 1.0000 . ? C17 C18 1.407(5) . ? C17 H17 0.9500 . ? C18 C19 1.373(4) . ? C18 C20 1.507(4) . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.404(4) . ? C21 H21 0.9500 . ? C22 C23 1.379(4) . ? C22 C24 1.499(4) . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.408(5) . ? C25 H25 0.9500 . ? C26 C27 1.356(6) . ? C26 C28 1.504(5) . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29 1.0000 . ? N13 C30 1.130(4) . ? C30 C31 1.449(5) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? N14 C32 1.163(14) . ? C32 C33 1.456(18) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? B1 F4 1.352(4) . ? B1 F3 1.386(4) . ? B1 F2 1.391(4) . ? B1 F1 1.398(4) . ? B2A F5A 1.309(11) . ? B2A F7 1.354(8) . ? B2A F8A 1.406(18) . ? B2A F6 1.433(10) . ? B2B F5B 1.358(11) . ? B2B F6 1.367(10) . ? B2B F7 1.419(9) . ? B2B F8B 1.428(17) . ? 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 N9 Fe1 N5 91.45(8) . . ? N9 Fe1 N3 176.42(8) . . ? N5 Fe1 N3 86.62(8) . . ? N9 Fe1 N7 85.17(8) . . ? N5 Fe1 N7 94.06(8) . . ? N3 Fe1 N7 97.96(8) . . ? N9 Fe1 N1 91.98(8) . . ? N5 Fe1 N1 86.76(8) . . ? N3 Fe1 N1 84.91(7) . . ? N7 Fe1 N1 177.05(8) . . ? N9 Fe1 N11 85.67(9) . . ? N5 Fe1 N11 176.90(8) . . ? N3 Fe1 N11 96.32(9) . . ? N7 Fe1 N11 84.58(9) . . ? N1 Fe1 N11 94.46(8) . . ? C2 N1 N2 104.94(19) . . ? C2 N1 Fe1 138.54(16) . . ? N2 N1 Fe1 116.50(14) . . ? C4 N2 N1 111.81(18) . . ? C4 N2 C16 128.88(19) . . ? N1 N2 C16 118.99(18) . . ? C7 N3 N4 105.09(19) . . ? C7 N3 Fe1 138.60(17) . . ? N4 N3 Fe1 115.73(14) . . ? C9 N4 N3 112.08(19) . . ? C9 N4 C16 127.9(2) . . ? N3 N4 C16 119.98(18) . . ? C12 N5 N6 104.9(2) . . ? C12 N5 Fe1 137.80(19) . . ? N6 N5 Fe1 117.05(14) . . ? C14 N6 N5 112.2(2) . . ? C14 N6 C16 128.9(2) . . ? N5 N6 C16 118.93(18) . . ? C17 N7 N8 104.4(2) . . ? C17 N7 Fe1 138.1(2) . . ? N8 N7 Fe1 117.15(16) . . ? C19 N8 N7 112.4(2) . . ? C19 N8 C29 127.8(2) . . ? N7 N8 C29 119.8(2) . . ? C21 N9 N10 105.3(2) . . ? C21 N9 Fe1 135.04(18) . . ? N10 N9 Fe1 118.18(16) . . ? C23 N10 N9 111.4(2) . . ? C23 N10 C29 129.3(2) . . ? N9 N10 C29 119.1(2) . . ? C25 N11 N12 104.3(3) . . ? C25 N11 Fe1 138.8(2) . . ? N12 N11 Fe1 116.71(16) . . ? C27 N12 N11 111.6(3) . . ? C27 N12 C29 128.3(3) . . ? N11 N12 C29 120.1(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 110.4(2) . . ? N1 C2 C1 123.1(2) . . ? C3 C2 C1 126.5(2) . . ? C4 C3 C2 106.9(2) . . ? C4 C3 H3 126.5 . . ? C2 C3 H3 126.5 . . ? N2 C4 C3 105.9(2) . . ? N2 C4 C5 123.7(2) . . ? C3 C4 C5 130.4(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 110.0(2) . . ? N3 C7 C6 122.2(2) . . ? C8 C7 C6 127.8(2) . . ? C9 C8 C7 107.2(2) . . ? C9 C8 H8 126.4 . . ? C7 C8 H8 126.4 . . ? N4 C9 C8 105.7(2) . . ? N4 C9 C10 122.6(2) . . ? C8 C9 C10 131.7(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 110.4(2) . . ? N5 C12 C11 122.2(3) . . ? C13 C12 C11 127.3(3) . . ? C14 C13 C12 106.7(2) . . ? C14 C13 H13 126.6 . . ? C12 C13 H13 126.6 . . ? N6 C14 C13 105.8(2) . . ? N6 C14 C15 123.2(2) . . ? C13 C14 C15 131.0(2) . . ? 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 . . ? N6 C16 N4 110.87(18) . . ? N6 C16 N2 111.33(17) . . ? N4 C16 N2 110.43(18) . . ? N6 C16 H16 108.0 . . ? N4 C16 H16 108.0 . . ? N2 C16 H16 108.0 . . ? N7 C17 C18 111.5(3) . . ? N7 C17 H17 124.2 . . ? C18 C17 H17 124.2 . . ? C19 C18 C17 105.0(3) . . ? C19 C18 C20 126.6(4) . . ? C17 C18 C20 128.3(3) . . ? N8 C19 C18 106.7(3) . . ? N8 C19 H19 126.7 . . ? C18 C19 H19 126.7 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N9 C21 C22 111.5(2) . . ? N9 C21 H21 124.3 . . ? C22 C21 H21 124.3 . . ? C23 C22 C21 104.6(2) . . ? C23 C22 C24 128.6(2) . . ? C21 C22 C24 126.7(2) . . ? N10 C23 C22 107.2(2) . . ? N10 C23 H23 126.4 . . ? C22 C23 H23 126.4 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N11 C25 C26 111.5(3) . . ? N11 C25 H25 124.2 . . ? C26 C25 H25 124.2 . . ? C27 C26 C25 104.8(3) . . ? C27 C26 C28 127.9(4) . . ? C25 C26 C28 127.3(4) . . ? N12 C27 C26 107.8(3) . . ? N12 C27 H27 126.1 . . ? C26 C27 H27 126.1 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N12 C29 N10 110.1(2) . . ? N12 C29 N8 110.3(2) . . ? N10 C29 N8 110.3(2) . . ? N12 C29 H29 108.7 . . ? N10 C29 H29 108.7 . . ? N8 C29 H29 108.7 . . ? N13 C30 C31 179.5(4) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N14 C32 C33 178.5(10) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? F4 B1 F3 108.0(3) . . ? F4 B1 F2 109.0(3) . . ? F3 B1 F2 110.5(3) . . ? F4 B1 F1 110.1(3) . . ? F3 B1 F1 109.9(3) . . ? F2 B1 F1 109.3(3) . . ? F5A B2A F7 115.6(8) . . ? F5A B2A F8A 108.3(8) . . ? F7 B2A F8A 105.6(8) . . ? F5A B2A F6 106.1(7) . . ? F7 B2A F6 107.8(7) . . ? F8A B2A F6 113.7(9) . . ? F5B B2B F6 108.1(8) . . ? F5B B2B F7 113.0(7) . . ? F6 B2B F7 107.9(7) . . ? F5B B2B F8B 102.9(8) . . ? F6 B2B F8B 112.7(8) . . ? F7 B2B F8B 112.3(9) . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 28.04 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 1.117 _refine_diff_density_min -0.990 _refine_diff_density_rms 0.078 #=END data_2-200K _database_code_depnum_ccdc_archive 'CCDC 650149' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Fe(4-Metpm)(dmtpm))(BF!4$)!2$.3/2(MeCN) _chemical_melting_point ? _chemical_formula_moiety 'C29 H38 Fe N12, 2(B F4), 1.5(C2 H3 N)' _chemical_formula_sum 'C32 H42.50 B2 F8 Fe N13.50' _chemical_formula_weight 845.76 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' 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 Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.064(5) _cell_length_b 12.530(6) _cell_length_c 15.084(7) _cell_angle_alpha 88.711(7) _cell_angle_beta 78.965(7) _cell_angle_gamma 63.981(7) _cell_volume 2006.3(15) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 4079 _cell_measurement_theta_min 2.353 _cell_measurement_theta_max 27.584 _exptl_crystal_description block-shaped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 0.456 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.839 _exptl_absorpt_correction_T_max 0.951 _exptl_absorpt_process_details 'SADABS (Bruker, 1996)' _exptl_special_details ; In a thin film of perfluorpolyether oil on a mohair fibre ; _diffrn_ambient_temperature 200(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 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 187 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 19671 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _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 1.38 _diffrn_reflns_theta_max 28.07 _reflns_number_total 9182 _reflns_number_gt 7582 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXTL (BrukerAXS, 2000)' _computing_structure_refinement 'SHELXTL (BrukerAXS, 2000)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material XCIF _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. One of the two crystallographically distinct MeCN solvent molucules (N14, C32, C33) exhibits two-fold symmetry-related disorder, where the alternate positons are in close proximity and can not be occupied simultaneously. The occupancies of these atoms were fixed to be 0.5. The BF4 counterion comprised of B1-F4 exhibits two-fold postitional disorder at the F2, F3 & F4 atom sites. The 2nd BF4 counterion (B2-F8) exhibits two-fold positional disorder on all atoms. In both instances, pairs of atom sites were appropriately selected and separated into parts (A & B) to account for the disorder. Equivalent atoms were fixed to have the same ADPs. The relative occupancies of the components were refined. The disorder of the MeCN molecule and the 2nd BF4 counterion are correlated, with the B2A-F8A positions in close proximity to one of the MeCN orientatios which therefore cannot be occupied simultaneously. The alternate position of B2B-F8B is not in close proximity to either MeCN orientation. ; _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^)+(0.0860P)^2^+2.1462P] 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 9182 _refine_ls_number_parameters 554 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1679 _refine_ls_wR_factor_gt 0.1524 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.046 _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 0.68819(3) 0.62068(3) 0.73762(2) 0.02847(12) Uani 1 1 d . . . N1 N 0.62028(19) 0.50054(18) 0.80837(13) 0.0304(4) Uani 1 1 d . . . N2 N 0.66975(18) 0.45334(17) 0.88285(12) 0.0280(4) Uani 1 1 d . . . N3 N 0.6695(2) 0.68871(17) 0.87278(13) 0.0323(4) Uani 1 1 d . . . N4 N 0.72091(19) 0.60424(17) 0.93149(13) 0.0291(4) Uani 1 1 d . . . N5 N 0.87183(19) 0.49094(18) 0.75426(13) 0.0303(4) Uani 1 1 d . . . N6 N 0.87783(18) 0.43720(17) 0.83455(12) 0.0281(4) Uani 1 1 d . . . N7 N 0.7537(2) 0.73689(19) 0.65811(14) 0.0353(4) Uani 1 1 d . . . N8 N 0.7129(2) 0.76793(19) 0.57906(14) 0.0330(4) Uani 1 1 d . . . N9 N 0.7107(2) 0.53963(18) 0.60641(13) 0.0337(4) Uani 1 1 d . . . N10 N 0.6630(2) 0.61224(18) 0.54141(13) 0.0308(4) Uani 1 1 d . . . N11 N 0.5043(2) 0.7486(2) 0.71103(15) 0.0382(5) Uani 1 1 d . . . N12 N 0.5040(2) 0.78842(18) 0.62640(14) 0.0330(4) Uani 1 1 d . . . C1 C 0.4660(3) 0.4843(3) 0.7287(2) 0.0495(7) Uani 1 1 d . . . H1A H 0.4960 0.5285 0.6838 0.074 Uiso 1 1 calc R . . H1B H 0.3771 0.5337 0.7556 0.074 Uiso 1 1 calc R . . H1C H 0.4753 0.4112 0.6992 0.074 Uiso 1 1 calc R . . C2 C 0.5418(2) 0.4533(2) 0.80127(17) 0.0344(5) Uani 1 1 d . . . C3 C 0.5420(2) 0.3763(2) 0.87011(18) 0.0365(5) Uani 1 1 d . . . H3 H 0.4947 0.3318 0.8795 0.044 Uiso 1 1 calc R . . C4 C 0.6238(2) 0.3777(2) 0.92123(16) 0.0311(5) Uani 1 1 d . . . C5 C 0.6590(3) 0.3144(3) 1.00379(19) 0.0428(6) Uani 1 1 d . . . H5A H 0.6444 0.3722 1.0526 0.064 Uiso 1 1 calc R . . H5B H 0.7482 0.2570 0.9902 0.064 Uiso 1 1 calc R . . H5C H 0.6075 0.2722 1.0229 0.064 Uiso 1 1 calc R . . C6 C 0.5757(4) 0.9075(3) 0.8748(2) 0.0546(8) Uani 1 1 d . . . H6A H 0.5997 0.8941 0.8087 0.082 Uiso 1 1 calc R . . H6B H 0.6034 0.9641 0.8947 0.082 Uiso 1 1 calc R . . H6C H 0.4840 0.9399 0.8935 0.082 Uiso 1 1 calc R . . C7 C 0.6367(3) 0.7924(2) 0.91655(18) 0.0368(5) Uani 1 1 d . . . C8 C 0.6664(3) 0.7743(2) 1.00329(18) 0.0386(6) Uani 1 1 d . . . H8 H 0.6513 0.8341 1.0479 0.046 Uiso 1 1 calc R . . C9 C 0.7212(2) 0.6539(2) 1.01077(16) 0.0322(5) Uani 1 1 d . . . C10 C 0.7746(3) 0.5820(3) 1.08593(18) 0.0430(6) Uani 1 1 d . . . H10A H 0.7404 0.5241 1.0993 0.064 Uiso 1 1 calc R . . H10B H 0.7517 0.6350 1.1401 0.064 Uiso 1 1 calc R . . H10C H 0.8665 0.5399 1.0677 0.064 Uiso 1 1 calc R . . C11 C 1.0211(3) 0.4666(3) 0.61039(19) 0.0515(7) Uani 1 1 d . . . H11A H 0.9450 0.5267 0.5926 0.077 Uiso 1 1 calc R . . H11B H 1.0581 0.3958 0.5682 0.077 Uiso 1 1 calc R . . H11C H 1.0821 0.4989 0.6088 0.077 Uiso 1 1 calc R . . C12 C 0.9877(2) 0.4336(2) 0.70401(17) 0.0353(5) Uani 1 1 d . . . C13 C 1.0665(2) 0.3443(2) 0.75138(18) 0.0388(6) Uani 1 1 d . . . H13 H 1.1530 0.2919 0.7302 0.047 Uiso 1 1 calc R . . C14 C 0.9945(2) 0.3474(2) 0.83424(17) 0.0335(5) Uani 1 1 d . . . C15 C 1.0260(3) 0.2712(3) 0.9114(2) 0.0487(7) Uani 1 1 d . . . H15A H 1.0087 0.3213 0.9661 0.073 Uiso 1 1 calc R . . H15B H 1.1153 0.2143 0.8975 0.073 Uiso 1 1 calc R . . H15C H 0.9746 0.2277 0.9215 0.073 Uiso 1 1 calc R . . C16 C 0.7679(2) 0.4785(2) 0.90629(15) 0.0270(4) Uani 1 1 d . . . H16 H 0.7936 0.4338 0.9604 0.032 Uiso 1 1 calc R . . C17 C 0.8388(3) 0.7778(2) 0.6568(2) 0.0412(6) Uani 1 1 d . . . H17 H 0.8840 0.7691 0.7038 0.049 Uiso 1 1 calc R . . C18 C 0.8536(3) 0.8354(3) 0.5776(2) 0.0457(6) Uani 1 1 d . . . C19 C 0.7713(3) 0.8272(2) 0.52953(19) 0.0397(6) Uani 1 1 d . . . H19 H 0.7579 0.8575 0.4722 0.048 Uiso 1 1 calc R . . C20 C 0.9392(4) 0.8946(4) 0.5512(3) 0.0733(11) Uani 1 1 d . . . H20A H 0.9888 0.8848 0.5978 0.110 Uiso 1 1 calc R . . H20B H 0.8884 0.9796 0.5456 0.110 Uiso 1 1 calc R . . H20C H 0.9959 0.8579 0.4931 0.110 Uiso 1 1 calc R . . C21 C 0.7372(3) 0.4308(2) 0.57495(17) 0.0366(5) Uani 1 1 d . . . H21 H 0.7738 0.3608 0.6059 0.044 Uiso 1 1 calc R . . C22 C 0.7043(3) 0.4326(2) 0.49038(18) 0.0390(6) Uani 1 1 d . . . C23 C 0.6571(3) 0.5505(2) 0.47126(17) 0.0371(5) Uani 1 1 d . . . H23 H 0.6261 0.5827 0.4185 0.045 Uiso 1 1 calc R . . C24 C 0.7153(4) 0.3276(3) 0.4361(2) 0.0598(9) Uani 1 1 d . . . H24A H 0.7318 0.2599 0.4740 0.090 Uiso 1 1 calc R . . H24B H 0.7847 0.3061 0.3835 0.090 Uiso 1 1 calc R . . H24C H 0.6364 0.3486 0.4155 0.090 Uiso 1 1 calc R . . C25 C 0.3870(3) 0.8134(3) 0.7559(2) 0.0448(6) Uani 1 1 d . . . H25 H 0.3576 0.8052 0.8176 0.054 Uiso 1 1 calc R . . C26 C 0.3119(3) 0.8947(2) 0.7023(2) 0.0449(6) Uani 1 1 d . . . C27 C 0.3902(3) 0.8760(2) 0.6200(2) 0.0395(6) Uani 1 1 d . . . H27 H 0.3685 0.9173 0.5676 0.047 Uiso 1 1 calc R . . C28 C 0.1751(3) 0.9826(4) 0.7285(3) 0.0727(11) Uani 1 1 d . . . H28A H 0.1639 1.0373 0.7785 0.109 Uiso 1 1 calc R . . H28B H 0.1243 0.9399 0.7476 0.109 Uiso 1 1 calc R . . H28C H 0.1482 1.0280 0.6764 0.109 Uiso 1 1 calc R . . C29 C 0.6167(2) 0.7399(2) 0.55675(16) 0.0314(5) Uani 1 1 d . . . H29 H 0.5949 0.7773 0.4993 0.038 Uiso 1 1 calc R . . N13 N 0.8643(4) 0.2089(4) 0.7189(4) 0.1026(15) Uani 1 1 d . . . C30 C 0.8203(4) 0.1489(3) 0.7444(3) 0.0669(10) Uani 1 1 d . . . C31 C 0.7625(5) 0.0720(4) 0.7772(4) 0.0949(15) Uani 1 1 d . . . H31A H 0.8282 -0.0076 0.7830 0.142 Uiso 1 1 calc R . . H31B H 0.7130 0.0669 0.7344 0.142 Uiso 1 1 calc R . . H31C H 0.7071 0.1047 0.8364 0.142 Uiso 1 1 calc R . . N14 N 1.2526(11) -0.0106(8) 0.9798(8) 0.110(3) Uani 0.50 1 d P . . C32 C 1.1594(19) -0.0081(12) 1.0015(12) 0.136(4) Uani 0.50 1 d PU . . C33 C 1.0271(17) 0.0101(13) 1.0349(11) 0.137(4) Uani 0.50 1 d PU . . H33A H 1.0275 -0.0573 1.0694 0.205 Uiso 0.50 1 calc PR . . H33B H 0.9869 0.0156 0.9832 0.205 Uiso 0.50 1 calc PR . . H33C H 0.9801 0.0838 1.0740 0.205 Uiso 0.50 1 calc PR . . B1 B 0.5318(4) 0.8550(3) 0.3333(3) 0.0537(9) Uani 1 1 d . . . F2 F 0.4641(4) 0.8035(3) 0.3875(2) 0.1194(12) Uani 1 1 d . A . F1A F 0.6400(3) 0.8372(3) 0.36388(19) 0.0761(9) Uani 0.817(3) 1 d P A 1 F3A F 0.5605(5) 0.8094(5) 0.2455(3) 0.1391(18) Uani 0.817(3) 1 d P A 1 F4A F 0.4574(3) 0.9716(3) 0.3324(3) 0.1002(12) Uani 0.817(3) 1 d P A 1 F1B F 0.6303(12) 0.7605(15) 0.3411(9) 0.0761(9) Uani 0.183(3) 1 d P A 2 F3B F 0.509(2) 0.902(2) 0.2671(12) 0.1391(18) Uani 0.183(3) 1 d P A 2 F4B F 0.5042(14) 0.9372(12) 0.4092(13) 0.1002(12) Uani 0.183(3) 1 d P A 2 B2A B 0.9647(9) 0.2450(12) 1.1528(8) 0.076(3) Uani 0.461(5) 1 d PD B 3 F5A F 1.0491(8) 0.1487(8) 1.1070(5) 0.1296(17) Uani 0.461(5) 1 d P B 3 F8A F 0.9409(15) 0.2267(14) 1.2449(13) 0.100(2) Uani 0.461(5) 1 d PD B 3 B2B B 0.9297(9) 0.2972(12) 1.1807(6) 0.076(3) Uani 0.539(5) 1 d PD B 4 F5B F 0.8657(7) 0.3865(7) 1.2484(4) 0.1296(17) Uani 0.539(5) 1 d P B 4 F8B F 0.9824(13) 0.1868(11) 1.2251(11) 0.100(2) Uani 0.539(5) 1 d PD B 4 F6 F 1.0191(3) 0.3257(4) 1.1335(2) 0.1232(12) Uani 1 1 d D . . F7 F 0.8522(3) 0.2982(3) 1.1264(2) 0.0974(9) Uani 1 1 d 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 Fe1 0.03258(19) 0.02854(19) 0.02406(18) 0.00485(12) -0.00779(13) -0.01263(14) N1 0.0336(10) 0.0347(10) 0.0260(9) 0.0075(8) -0.0110(8) -0.0162(8) N2 0.0321(10) 0.0308(10) 0.0236(9) 0.0053(7) -0.0088(7) -0.0151(8) N3 0.0399(11) 0.0270(10) 0.0281(10) 0.0037(7) -0.0080(8) -0.0126(8) N4 0.0346(10) 0.0300(10) 0.0239(9) 0.0024(7) -0.0078(7) -0.0146(8) N5 0.0318(10) 0.0334(10) 0.0235(9) 0.0051(7) -0.0057(7) -0.0125(8) N6 0.0295(9) 0.0291(9) 0.0243(9) 0.0038(7) -0.0071(7) -0.0112(8) N7 0.0411(11) 0.0358(11) 0.0346(11) 0.0081(8) -0.0149(9) -0.0196(9) N8 0.0377(11) 0.0338(10) 0.0312(10) 0.0093(8) -0.0107(8) -0.0181(9) N9 0.0430(12) 0.0309(10) 0.0275(10) 0.0065(8) -0.0123(8) -0.0147(9) N10 0.0373(10) 0.0329(10) 0.0251(9) 0.0075(8) -0.0118(8) -0.0163(9) N11 0.0377(11) 0.0402(12) 0.0327(11) 0.0094(9) -0.0068(9) -0.0142(10) N12 0.0338(10) 0.0312(10) 0.0343(10) 0.0086(8) -0.0101(8) -0.0135(8) C1 0.0516(17) 0.0651(19) 0.0491(16) 0.0181(14) -0.0275(14) -0.0353(15) C2 0.0317(12) 0.0395(13) 0.0341(12) 0.0040(10) -0.0095(10) -0.0166(10) C3 0.0342(12) 0.0392(13) 0.0401(13) 0.0074(10) -0.0076(10) -0.0200(11) C4 0.0319(11) 0.0297(11) 0.0306(11) 0.0043(9) -0.0037(9) -0.0138(9) C5 0.0523(16) 0.0449(15) 0.0394(14) 0.0168(11) -0.0143(12) -0.0274(13) C6 0.077(2) 0.0298(14) 0.0510(17) 0.0030(12) -0.0168(16) -0.0171(14) C7 0.0402(13) 0.0305(12) 0.0364(13) -0.0014(10) -0.0048(10) -0.0137(10) C8 0.0441(14) 0.0351(13) 0.0369(13) -0.0062(10) -0.0061(11) -0.0185(11) C9 0.0323(12) 0.0397(13) 0.0274(11) -0.0035(9) -0.0049(9) -0.0186(10) C10 0.0515(16) 0.0492(15) 0.0323(13) 0.0019(11) -0.0166(11) -0.0227(13) C11 0.0423(15) 0.0642(19) 0.0332(13) 0.0060(13) 0.0052(11) -0.0156(14) C12 0.0327(12) 0.0411(13) 0.0298(11) 0.0001(10) -0.0032(9) -0.0154(11) C13 0.0308(12) 0.0407(14) 0.0389(13) -0.0007(11) -0.0052(10) -0.0109(11) C14 0.0302(11) 0.0323(12) 0.0372(12) 0.0028(9) -0.0108(10) -0.0117(10) C15 0.0394(15) 0.0454(16) 0.0530(17) 0.0186(13) -0.0163(13) -0.0093(12) C16 0.0299(11) 0.0280(11) 0.0245(10) 0.0037(8) -0.0076(8) -0.0133(9) C17 0.0416(14) 0.0414(14) 0.0479(15) 0.0035(11) -0.0146(12) -0.0227(12) C18 0.0453(15) 0.0434(15) 0.0544(17) 0.0060(12) -0.0060(13) -0.0267(13) C19 0.0454(14) 0.0350(13) 0.0411(14) 0.0093(10) -0.0048(11) -0.0218(12) C20 0.074(3) 0.085(3) 0.088(3) 0.017(2) -0.014(2) -0.061(2) C21 0.0428(14) 0.0308(12) 0.0354(12) 0.0037(10) -0.0115(10) -0.0142(11) C22 0.0437(14) 0.0395(14) 0.0370(13) -0.0005(10) -0.0123(11) -0.0195(11) C23 0.0404(13) 0.0441(14) 0.0295(12) 0.0030(10) -0.0131(10) -0.0188(11) C24 0.079(2) 0.0467(17) 0.0573(19) -0.0058(14) -0.0279(17) -0.0248(17) C25 0.0398(14) 0.0435(15) 0.0417(14) 0.0004(11) -0.0006(11) -0.0130(12) C26 0.0375(14) 0.0341(13) 0.0575(17) -0.0017(12) -0.0083(12) -0.0113(11) C27 0.0401(14) 0.0273(12) 0.0513(15) 0.0084(10) -0.0184(12) -0.0118(10) C28 0.0435(18) 0.061(2) 0.088(3) -0.001(2) -0.0066(18) -0.0027(16) C29 0.0372(12) 0.0302(11) 0.0304(11) 0.0094(9) -0.0121(9) -0.0166(10) N13 0.074(3) 0.074(3) 0.163(5) 0.031(3) -0.033(3) -0.033(2) C30 0.059(2) 0.0453(18) 0.091(3) 0.0064(18) -0.022(2) -0.0157(17) C31 0.099(4) 0.054(2) 0.120(4) 0.006(2) -0.003(3) -0.031(2) N14 0.118(8) 0.079(6) 0.119(8) 0.016(5) -0.005(6) -0.040(6) C32 0.164(11) 0.086(6) 0.147(10) 0.035(6) -0.003(8) -0.057(7) C33 0.165(11) 0.087(6) 0.147(10) 0.034(6) -0.003(8) -0.058(7) B1 0.061(2) 0.0470(19) 0.0477(19) 0.0108(15) -0.0228(16) -0.0145(17) F2 0.146(3) 0.142(3) 0.119(2) 0.065(2) -0.058(2) -0.098(3) F1A 0.0594(14) 0.109(3) 0.0603(15) 0.0271(16) -0.0233(12) -0.0343(16) F3A 0.156(4) 0.161(4) 0.066(2) -0.048(2) -0.018(2) -0.038(3) F4A 0.085(2) 0.0481(15) 0.151(4) 0.0143(18) -0.034(2) -0.0106(14) F1B 0.0594(14) 0.109(3) 0.0603(15) 0.0271(16) -0.0233(12) -0.0343(16) F3B 0.156(4) 0.161(4) 0.066(2) -0.048(2) -0.018(2) -0.038(3) F4B 0.085(2) 0.0481(15) 0.151(4) 0.0143(18) -0.034(2) -0.0106(14) B2A 0.055(5) 0.121(9) 0.036(5) 0.004(4) -0.012(3) -0.023(5) F5A 0.131(4) 0.141(4) 0.092(3) 0.015(3) -0.017(3) -0.040(3) F8A 0.103(8) 0.090(8) 0.105(7) 0.020(5) -0.059(6) -0.027(5) B2B 0.055(5) 0.121(9) 0.036(5) 0.004(4) -0.012(3) -0.023(5) F5B 0.131(4) 0.141(4) 0.092(3) 0.015(3) -0.017(3) -0.040(3) F8B 0.103(8) 0.090(8) 0.105(7) 0.020(5) -0.059(6) -0.027(5) F6 0.100(2) 0.186(4) 0.098(2) 0.007(2) -0.0183(18) -0.077(2) F7 0.0870(18) 0.115(2) 0.103(2) 0.0244(17) -0.0576(16) -0.0417(16) _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 N5 2.156(2) . ? Fe1 N9 2.160(2) . ? Fe1 N3 2.160(2) . ? Fe1 N7 2.180(2) . ? Fe1 N1 2.180(2) . ? Fe1 N11 2.201(2) . ? N1 C2 1.338(3) . ? N1 N2 1.373(3) . ? N2 C4 1.361(3) . ? N2 C16 1.456(3) . ? N3 C7 1.330(3) . ? N3 N4 1.372(3) . ? N4 C9 1.362(3) . ? N4 C16 1.452(3) . ? N5 C12 1.335(3) . ? N5 N6 1.371(3) . ? N6 C14 1.362(3) . ? N6 C16 1.439(3) . ? N7 C17 1.330(3) . ? N7 N8 1.361(3) . ? N8 C19 1.357(3) . ? N8 C29 1.448(3) . ? N9 C21 1.332(3) . ? N9 N10 1.355(3) . ? N10 C23 1.355(3) . ? N10 C29 1.452(3) . ? N11 C25 1.331(4) . ? N11 N12 1.360(3) . ? N12 C27 1.351(3) . ? N12 C29 1.441(3) . ? C1 C2 1.495(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.401(4) . ? C3 C4 1.370(4) . ? C3 H3 0.9500 . ? C4 C5 1.491(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.491(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.410(4) . ? C8 C9 1.368(4) . ? C8 H8 0.9500 . ? C9 C10 1.495(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.493(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.399(4) . ? C13 C14 1.370(4) . ? C13 H13 0.9500 . ? C14 C15 1.487(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16 1.0000 . ? C17 C18 1.405(4) . ? C17 H17 0.9500 . ? C18 C19 1.374(4) . ? C18 C20 1.509(4) . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.404(4) . ? C21 H21 0.9500 . ? C22 C23 1.376(4) . ? C22 C24 1.508(4) . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.396(4) . ? C25 H25 0.9500 . ? C26 C27 1.362(4) . ? C26 C28 1.506(4) . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29 1.0000 . ? N13 C30 1.121(5) . ? C30 C31 1.447(6) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? N14 C32 1.096(18) . ? C32 C33 1.49(2) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? B1 F3B 1.16(2) . ? B1 F1B 1.281(14) . ? B1 F4A 1.339(5) . ? B1 F3A 1.373(5) . ? B1 F2 1.391(5) . ? B1 F1A 1.392(5) . ? B1 F4B 1.447(18) . ? B2A F5A 1.289(14) . ? B2A F7 1.358(10) . ? B2A F8A 1.40(2) . ? B2A F6 1.426(12) . ? B2B F7 1.352(8) . ? B2B F6 1.353(9) . ? B2B F5B 1.372(13) . ? B2B F8B 1.45(2) . ? 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 N5 Fe1 N9 92.27(8) . . ? N5 Fe1 N3 85.08(8) . . ? N9 Fe1 N3 175.69(7) . . ? N5 Fe1 N7 95.92(8) . . ? N9 Fe1 N7 83.52(8) . . ? N3 Fe1 N7 100.11(8) . . ? N5 Fe1 N1 85.27(8) . . ? N9 Fe1 N1 92.57(8) . . ? N3 Fe1 N1 83.84(8) . . ? N7 Fe1 N1 175.95(7) . . ? N5 Fe1 N11 176.15(8) . . ? N9 Fe1 N11 83.96(8) . . ? N3 Fe1 N11 98.73(8) . . ? N7 Fe1 N11 82.90(9) . . ? N1 Fe1 N11 95.66(9) . . ? C2 N1 N2 104.96(19) . . ? C2 N1 Fe1 139.03(16) . . ? N2 N1 Fe1 116.01(14) . . ? C4 N2 N1 111.72(19) . . ? C4 N2 C16 128.30(19) . . ? N1 N2 C16 119.73(18) . . ? C7 N3 N4 105.2(2) . . ? C7 N3 Fe1 138.62(17) . . ? N4 N3 Fe1 115.43(14) . . ? C9 N4 N3 111.91(19) . . ? C9 N4 C16 127.3(2) . . ? N3 N4 C16 120.79(18) . . ? C12 N5 N6 104.66(19) . . ? C12 N5 Fe1 138.29(17) . . ? N6 N5 Fe1 116.57(14) . . ? C14 N6 N5 111.96(19) . . ? C14 N6 C16 128.3(2) . . ? N5 N6 C16 119.78(18) . . ? C17 N7 N8 104.9(2) . . ? C17 N7 Fe1 138.15(18) . . ? N8 N7 Fe1 116.23(15) . . ? C19 N8 N7 111.5(2) . . ? C19 N8 C29 127.4(2) . . ? N7 N8 C29 121.08(19) . . ? C21 N9 N10 105.2(2) . . ? C21 N9 Fe1 134.92(17) . . ? N10 N9 Fe1 117.99(15) . . ? C23 N10 N9 111.3(2) . . ? C23 N10 C29 128.9(2) . . ? N9 N10 C29 119.60(19) . . ? C25 N11 N12 103.9(2) . . ? C25 N11 Fe1 139.36(19) . . ? N12 N11 Fe1 116.24(16) . . ? C27 N12 N11 111.6(2) . . ? C27 N12 C29 127.5(2) . . ? N11 N12 C29 120.9(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 110.5(2) . . ? N1 C2 C1 122.0(2) . . ? C3 C2 C1 127.5(2) . . ? C4 C3 C2 106.7(2) . . ? C4 C3 H3 126.7 . . ? C2 C3 H3 126.7 . . ? N2 C4 C3 106.2(2) . . ? N2 C4 C5 123.9(2) . . ? C3 C4 C5 129.9(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 110.4(2) . . ? N3 C7 C6 121.5(2) . . ? C8 C7 C6 128.1(2) . . ? C9 C8 C7 106.6(2) . . ? C9 C8 H8 126.7 . . ? C7 C8 H8 126.7 . . ? N4 C9 C8 105.9(2) . . ? N4 C9 C10 123.1(2) . . ? C8 C9 C10 131.0(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 110.9(2) . . ? N5 C12 C11 121.5(2) . . ? C13 C12 C11 127.6(2) . . ? C14 C13 C12 106.5(2) . . ? C14 C13 H13 126.7 . . ? C12 C13 H13 126.7 . . ? N6 C14 C13 106.0(2) . . ? N6 C14 C15 123.2(2) . . ? C13 C14 C15 130.8(2) . . ? 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 . . ? N6 C16 N4 111.40(18) . . ? N6 C16 N2 111.61(18) . . ? N4 C16 N2 111.12(18) . . ? N6 C16 H16 107.5 . . ? N4 C16 H16 107.5 . . ? N2 C16 H16 107.5 . . ? N7 C17 C18 111.7(2) . . ? N7 C17 H17 124.2 . . ? C18 C17 H17 124.2 . . ? C19 C18 C17 104.6(2) . . ? C19 C18 C20 127.4(3) . . ? C17 C18 C20 127.9(3) . . ? N8 C19 C18 107.3(2) . . ? N8 C19 H19 126.3 . . ? C18 C19 H19 126.3 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N9 C21 C22 111.5(2) . . ? N9 C21 H21 124.2 . . ? C22 C21 H21 124.2 . . ? C23 C22 C21 104.5(2) . . ? C23 C22 C24 129.0(3) . . ? C21 C22 C24 126.5(3) . . ? N10 C23 C22 107.5(2) . . ? N10 C23 H23 126.3 . . ? C22 C23 H23 126.3 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N11 C25 C26 112.4(3) . . ? N11 C25 H25 123.8 . . ? C26 C25 H25 123.8 . . ? C27 C26 C25 104.3(2) . . ? C27 C26 C28 127.5(3) . . ? C25 C26 C28 128.1(3) . . ? N12 C27 C26 107.7(2) . . ? N12 C27 H27 126.1 . . ? C26 C27 H27 126.1 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N12 C29 N8 111.1(2) . . ? N12 C29 N10 110.71(19) . . ? N8 C29 N10 110.9(2) . . ? N12 C29 H29 108.0 . . ? N8 C29 H29 108.0 . . ? N10 C29 H29 108.0 . . ? N13 C30 C31 179.6(5) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N14 C32 C33 173.3(17) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? F3B B1 F1B 127.0(13) . . ? F1B B1 F4A 157.8(9) . . ? F4A B1 F3A 105.8(4) . . ? F3B B1 F2 127.1(13) . . ? F1B B1 F2 86.1(7) . . ? F4A B1 F2 108.8(4) . . ? F3A B1 F2 109.0(4) . . ? F4A B1 F1A 110.3(4) . . ? F3A B1 F1A 111.2(4) . . ? F2 B1 F1A 111.5(3) . . ? F3B B1 F4B 112.8(13) . . ? F1B B1 F4B 107.1(9) . . ? F2 B1 F4B 88.8(7) . . ? F5A B2A F7 116.9(9) . . ? F5A B2A F8A 111.2(11) . . ? F7 B2A F8A 107.8(10) . . ? F5A B2A F6 102.5(8) . . ? F7 B2A F6 104.9(9) . . ? F8A B2A F6 113.5(13) . . ? F7 B2B F6 109.5(6) . . ? F7 B2B F5B 110.3(8) . . ? F6 B2B F5B 103.9(9) . . ? F7 B2B F8B 113.5(11) . . ? F6 B2B F8B 112.7(10) . . ? F5B B2B F8B 106.4(8) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 28.07 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.882 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.069 #=END data_3 _database_code_depnum_ccdc_archive 'CCDC 650150' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H39 B2 F8 Fe N14 O' _chemical_formula_weight 853.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' B B 0.0013 0.0007 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.668(2) _cell_length_b 17.794(4) _cell_length_c 19.935(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3784.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular block' _exptl_crystal_colour pink _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1756 _exptl_absorpt_coefficient_mu 0.487 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6969 _exptl_absorpt_correction_T_max 0.7930 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Nonius KappaCCD' _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 47499 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 28.29 _reflns_number_total 9324 _reflns_number_gt 7892 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0662P)^2^+1.7899P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(13) _refine_ls_number_reflns 9324 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1164 _refine_ls_wR_factor_gt 0.1087 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 0.72529(3) 0.653748(19) 0.218321(17) 0.01716(9) Uani 1 1 d . . . N9 N 0.7163(2) 0.74086(11) 0.27795(11) 0.0249(4) Uani 1 1 d . . . N7 N 0.61567(19) 0.60138(11) 0.28094(11) 0.0192(4) Uani 1 1 d . . . N3 N 0.7278(2) 0.56490(11) 0.15851(10) 0.0184(4) Uani 1 1 d . . . N8 N 0.5154(2) 0.63789(12) 0.30722(11) 0.0221(5) Uani 1 1 d . . . N12 N 0.4794(2) 0.71791(12) 0.21351(12) 0.0254(5) Uani 1 1 d . . . N5 N 0.8799(2) 0.61545(12) 0.26197(10) 0.0205(4) Uani 1 1 d . . . N4 N 0.8408(2) 0.54501(12) 0.13105(10) 0.0178(4) Uani 1 1 d . . . O9 O 0.2748(2) 0.70107(14) 0.30542(12) 0.0460(6) Uani 1 1 d . . . N1 N 0.8358(2) 0.70719(12) 0.15354(11) 0.0201(4) Uani 1 1 d . . . N6 N 0.97123(19) 0.58869(11) 0.22023(11) 0.0195(4) Uani 1 1 d . . . C21 C 0.7388(4) 0.84022(17) 0.34633(16) 0.0443(8) Uani 1 1 d . . . H21 H 0.7768 0.8802 0.3705 0.053 Uiso 1 1 calc R . . C17 C 0.6139(3) 0.53274(15) 0.30730(13) 0.0229(5) Uani 1 1 d . . . H17 H 0.6731 0.4943 0.2977 0.027 Uiso 1 1 calc R . . C7 C 0.6441(2) 0.51760(15) 0.13202(13) 0.0220(5) Uani 1 1 d . . . N2 N 0.9314(2) 0.66603(12) 0.12582(10) 0.0198(4) Uani 1 1 d . . . N10 N 0.6035(2) 0.75988(12) 0.30494(12) 0.0278(5) Uani 1 1 d . . . C4 C 0.9945(3) 0.70569(15) 0.07809(13) 0.0225(5) Uani 1 1 d . . . N11 N 0.5754(2) 0.69201(12) 0.17509(11) 0.0210(4) Uani 1 1 d . . . C19 C 0.4512(3) 0.59301(16) 0.35083(13) 0.0260(6) Uani 1 1 d . . . H19 H 0.3787 0.6062 0.3759 0.031 Uiso 1 1 calc R . . C2 C 0.8416(3) 0.77441(14) 0.12320(13) 0.0230(5) Uani 1 1 d . . . C22 C 0.6170(4) 0.82033(16) 0.34714(16) 0.0397(8) Uani 1 1 d . . . H22 H 0.5523 0.8438 0.3723 0.048 Uiso 1 1 calc R . . C14 C 1.0763(2) 0.56805(16) 0.25451(14) 0.0239(5) Uani 1 1 d . . . C13 C 1.0505(3) 0.58138(16) 0.32060(14) 0.0262(6) Uani 1 1 d . . . H13 H 1.1048 0.5723 0.3575 0.031 Uiso 1 1 calc R . . C26 C 0.4933(3) 0.71570(14) 0.28646(14) 0.0258(5) Uani 1 1 d . . . C18 C 0.5121(3) 0.52523(15) 0.35143(13) 0.0265(6) Uani 1 1 d . . . H18 H 0.4899 0.4819 0.3766 0.032 Uiso 1 1 calc R . . C9 C 0.8292(3) 0.48712(15) 0.08666(13) 0.0244(6) Uani 1 1 d . . . C10 C 0.9366(3) 0.45621(18) 0.04871(16) 0.0357(7) Uani 1 1 d . . . H10A H 0.9758 0.4963 0.0223 0.054 Uiso 1 1 calc R . . H10B H 0.9071 0.4165 0.0186 0.054 Uiso 1 1 calc R . . H10C H 0.9982 0.4353 0.0801 0.054 Uiso 1 1 calc R . . C3 C 0.9386(3) 0.77467(15) 0.07573(13) 0.0253(6) Uani 1 1 d . . . H3 H 0.9612 0.8153 0.0472 0.030 Uiso 1 1 calc R . . C15 C 1.1903(3) 0.53813(18) 0.22137(17) 0.0337(6) Uani 1 1 d . . . H15A H 1.1684 0.4934 0.1952 0.051 Uiso 1 1 calc R . . H15B H 1.2525 0.5248 0.2555 0.051 Uiso 1 1 calc R . . H15C H 1.2253 0.5765 0.1915 0.051 Uiso 1 1 calc R . . C24 C 0.4236(3) 0.7362(2) 0.10948(17) 0.0378(7) Uani 1 1 d . . . H24 H 0.3784 0.7499 0.0703 0.045 Uiso 1 1 calc R . . C12 C 0.9286(3) 0.61117(15) 0.32364(13) 0.0256(6) Uani 1 1 d . . . C23 C 0.5397(3) 0.70234(16) 0.11202(14) 0.0271(6) Uani 1 1 d . . . H23 H 0.5876 0.6883 0.0738 0.032 Uiso 1 1 calc R . . C20 C 0.7984(3) 0.78968(16) 0.30245(14) 0.0336(7) Uani 1 1 d . . . H20 H 0.8852 0.7904 0.2918 0.040 Uiso 1 1 calc R . . C8 C 0.7046(3) 0.46893(15) 0.08717(13) 0.0257(6) Uani 1 1 d . . . H8 H 0.6660 0.4302 0.0617 0.031 Uiso 1 1 calc R . . C16 C 0.9485(2) 0.58981(14) 0.14803(13) 0.0193(5) Uani 1 1 d . . . H16 H 1.0236 0.5684 0.1248 0.023 Uiso 1 1 calc R . . C25 C 0.3863(3) 0.74618(18) 0.17463(16) 0.0356(7) Uani 1 1 d . . . H25 H 0.3103 0.7685 0.1896 0.043 Uiso 1 1 calc R . . C5 C 1.0995(3) 0.67261(18) 0.03858(15) 0.0324(7) Uani 1 1 d . . . H5A H 1.1592 0.6485 0.0691 0.049 Uiso 1 1 calc R . . H5B H 1.1421 0.7124 0.0134 0.049 Uiso 1 1 calc R . . H5C H 1.0663 0.6352 0.0072 0.049 Uiso 1 1 calc R . . C6 C 0.5082(3) 0.51709(18) 0.14975(15) 0.0318(6) Uani 1 1 d . . . H6A H 0.4936 0.4810 0.1861 0.048 Uiso 1 1 calc R . . H6B H 0.4589 0.5025 0.1104 0.048 Uiso 1 1 calc R . . H6C H 0.4828 0.5674 0.1644 0.048 Uiso 1 1 calc R . . C11 C 0.8604(3) 0.63588(19) 0.38582(15) 0.0369(7) Uani 1 1 d . . . H11A H 0.8780 0.6891 0.3943 0.055 Uiso 1 1 calc R . . H11B H 0.8888 0.6058 0.4241 0.055 Uiso 1 1 calc R . . H11C H 0.7701 0.6288 0.3796 0.055 Uiso 1 1 calc R . . C27 C 0.3768(3) 0.74719(17) 0.32105(17) 0.0350(7) Uani 1 1 d . . . H27A H 0.3897 0.7484 0.3702 0.042 Uiso 1 1 calc R . . H27B H 0.3607 0.7991 0.3054 0.042 Uiso 1 1 calc R . . F2 F 0.23464(18) 0.49338(11) 0.06009(8) 0.0385(4) Uani 1 1 d . . . F1 F 0.36362(19) 0.56475(11) -0.00253(10) 0.0474(5) Uani 1 1 d . . . F3 F 0.2308(2) 0.48370(15) -0.05366(10) 0.0643(7) Uani 1 1 d . . . B1 B 0.3064(3) 0.4954(2) 0.00206(17) 0.0312(7) Uani 1 1 d . . . F4 F 0.3972(2) 0.43968(13) 0.00608(13) 0.0604(6) Uani 1 1 d . . . F5 F 0.7773(2) 0.39370(13) 0.24319(11) 0.0572(6) Uani 1 1 d . . . F6 F 0.8821(2) 0.32441(14) 0.16538(12) 0.0612(6) Uani 1 1 d . . . F7 F 0.9045(2) 0.29984(15) 0.27205(14) 0.0713(7) Uani 1 1 d . . . F8 F 0.9817(2) 0.41090(15) 0.2283(2) 0.0998(12) Uani 1 1 d . . . B2 B 0.8888(4) 0.3603(2) 0.2291(2) 0.0424(9) Uani 1 1 d . . . C30 C 0.2021(3) 0.89476(18) 0.04679(16) 0.0348(7) Uani 1 1 d . . . C31 C 0.1255(4) 0.9374(2) 0.0940(2) 0.0566(11) Uani 1 1 d . . . H31A H 0.0526 0.9582 0.0706 0.085 Uiso 1 1 calc R . . H31B H 0.1754 0.9785 0.1130 0.085 Uiso 1 1 calc R . . H31C H 0.0972 0.9042 0.1302 0.085 Uiso 1 1 calc R . . N14 N 0.2587(3) 0.86043(18) 0.01011(16) 0.0531(8) Uani 1 1 d . . . C28 C 0.4336(5) 0.2486(3) -0.0024(2) 0.0571(11) Uani 1 1 d . . . N13 N 0.5247(5) 0.2290(3) 0.0220(2) 0.0940(16) Uani 1 1 d . . . C29 C 0.3198(6) 0.2718(3) -0.0316(3) 0.0895(18) Uani 1 1 d . . . H29A H 0.2629 0.2287 -0.0349 0.134 Uiso 1 1 calc R . . H29B H 0.3360 0.2919 -0.0765 0.134 Uiso 1 1 calc R . . H29C H 0.2814 0.3108 -0.0037 0.134 Uiso 1 1 calc R . . C1 C 0.7579(3) 0.83929(15) 0.14115(14) 0.0301(6) Uani 1 1 d . . . H1A H 0.6775 0.8201 0.1577 0.045 Uiso 1 1 calc R . . H1B H 0.7436 0.8704 0.1013 0.045 Uiso 1 1 calc R . . H1C H 0.7979 0.8696 0.1761 0.045 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 0.01822(15) 0.01784(15) 0.01543(16) 0.00088(13) 0.00214(13) 0.00004(14) N9 0.0317(12) 0.0209(10) 0.0220(11) -0.0004(9) 0.0071(11) -0.0025(9) N7 0.0206(10) 0.0191(9) 0.0180(10) 0.0002(9) 0.0018(9) 0.0018(8) N3 0.0164(9) 0.0199(9) 0.0189(10) 0.0011(8) 0.0013(9) 0.0005(9) N8 0.0228(11) 0.0237(11) 0.0197(10) 0.0033(8) 0.0085(9) 0.0024(9) N12 0.0246(11) 0.0261(11) 0.0255(11) 0.0045(10) 0.0071(10) 0.0102(9) N5 0.0194(10) 0.0245(11) 0.0174(11) 0.0025(8) 0.0014(8) -0.0017(9) N4 0.0165(10) 0.0195(10) 0.0174(10) 0.0000(8) 0.0039(8) 0.0004(8) O9 0.0364(12) 0.0484(13) 0.0534(14) 0.0007(11) 0.0068(11) 0.0047(12) N1 0.0200(10) 0.0201(10) 0.0203(10) 0.0011(8) 0.0015(8) 0.0006(8) N6 0.0174(10) 0.0232(10) 0.0180(10) 0.0005(9) -0.0009(9) 0.0002(8) C21 0.072(3) 0.0245(14) 0.0362(16) -0.0085(12) 0.0085(16) -0.0144(17) C17 0.0274(14) 0.0213(12) 0.0200(12) 0.0017(10) 0.0000(10) 0.0002(11) C7 0.0189(12) 0.0251(13) 0.0219(13) 0.0039(10) -0.0017(10) -0.0049(10) N2 0.0190(10) 0.0213(11) 0.0192(10) 0.0020(8) 0.0044(8) -0.0008(8) N10 0.0386(14) 0.0185(11) 0.0264(12) -0.0013(9) 0.0123(10) 0.0008(10) C4 0.0221(13) 0.0264(13) 0.0189(12) 0.0038(10) 0.0006(10) -0.0064(11) N11 0.0204(11) 0.0209(11) 0.0216(11) 0.0040(8) 0.0048(8) 0.0051(8) C19 0.0274(14) 0.0300(14) 0.0206(13) 0.0025(11) 0.0078(11) -0.0051(11) C2 0.0273(14) 0.0204(12) 0.0213(13) 0.0032(10) 0.0003(11) -0.0013(11) C22 0.065(2) 0.0193(13) 0.0352(17) -0.0027(12) 0.0202(16) -0.0032(14) C14 0.0189(12) 0.0260(13) 0.0269(14) 0.0074(11) -0.0050(11) -0.0040(10) C13 0.0231(14) 0.0335(15) 0.0219(14) 0.0026(11) -0.0066(11) -0.0031(11) C26 0.0293(14) 0.0211(12) 0.0269(14) 0.0026(11) 0.0085(12) 0.0055(10) C18 0.0329(15) 0.0253(13) 0.0212(13) 0.0077(10) 0.0052(11) -0.0033(11) C9 0.0298(14) 0.0213(12) 0.0220(13) -0.0014(10) 0.0036(11) -0.0010(11) C10 0.0381(17) 0.0335(16) 0.0354(16) -0.0108(13) 0.0155(14) -0.0036(13) C3 0.0281(14) 0.0258(13) 0.0221(13) 0.0048(11) 0.0018(11) -0.0054(11) C15 0.0223(13) 0.0425(16) 0.0363(15) 0.0041(14) -0.0040(12) 0.0049(11) C24 0.0332(17) 0.0467(19) 0.0334(16) 0.0136(14) -0.0029(13) 0.0098(14) C12 0.0289(14) 0.0252(13) 0.0227(14) 0.0012(11) -0.0029(11) -0.0043(11) C23 0.0254(14) 0.0324(14) 0.0234(13) 0.0040(11) 0.0017(11) 0.0046(12) C20 0.047(2) 0.0273(14) 0.0262(14) -0.0026(11) 0.0030(12) -0.0130(13) C8 0.0297(16) 0.0246(13) 0.0229(13) -0.0032(10) 0.0008(11) -0.0064(11) C16 0.0168(12) 0.0212(12) 0.0200(12) 0.0021(10) 0.0003(10) -0.0013(9) C25 0.0292(15) 0.0426(17) 0.0350(17) 0.0140(13) 0.0052(13) 0.0171(13) C5 0.0275(15) 0.0366(16) 0.0331(16) 0.0075(12) 0.0108(12) -0.0018(12) C6 0.0199(13) 0.0396(16) 0.0358(16) -0.0048(13) 0.0012(12) -0.0065(12) C11 0.0424(18) 0.0447(18) 0.0237(14) -0.0011(12) -0.0003(13) 0.0012(14) C27 0.0396(18) 0.0261(14) 0.0395(18) 0.0033(12) 0.0195(14) 0.0110(13) F2 0.0339(9) 0.0503(10) 0.0313(9) 0.0088(8) 0.0067(8) -0.0018(9) F1 0.0460(12) 0.0521(12) 0.0440(11) 0.0171(9) -0.0063(9) -0.0189(9) F3 0.0593(14) 0.0986(18) 0.0352(11) -0.0010(11) -0.0201(10) -0.0250(14) B1 0.0306(17) 0.0398(18) 0.0233(16) 0.0028(13) -0.0040(12) -0.0085(14) F4 0.0507(13) 0.0550(13) 0.0756(16) -0.0240(11) -0.0012(11) 0.0161(11) F5 0.0513(12) 0.0573(13) 0.0631(13) -0.0115(10) -0.0023(11) 0.0232(11) F6 0.0553(14) 0.0750(16) 0.0532(13) -0.0089(11) 0.0152(11) -0.0021(12) F7 0.0620(15) 0.0711(15) 0.0808(17) 0.0404(14) 0.0182(13) 0.0238(13) F8 0.0472(14) 0.0536(15) 0.199(4) -0.030(2) 0.004(2) -0.0131(12) B2 0.0378(19) 0.037(2) 0.052(2) 0.0021(16) 0.0084(17) -0.0003(15) C30 0.0347(18) 0.0320(15) 0.0377(17) 0.0065(13) -0.0094(13) 0.0038(13) C31 0.048(2) 0.056(2) 0.066(3) -0.0292(19) -0.0122(19) 0.0035(19) N14 0.0504(19) 0.0564(19) 0.0526(18) 0.0145(15) 0.0049(15) 0.0168(16) C28 0.076(3) 0.054(2) 0.042(2) 0.0003(17) -0.014(2) -0.008(2) N13 0.106(4) 0.104(4) 0.072(3) -0.017(3) -0.034(3) 0.027(3) C29 0.099(4) 0.080(4) 0.089(4) 0.006(3) -0.046(3) -0.002(3) C1 0.0392(17) 0.0186(12) 0.0325(14) 0.0030(10) 0.0063(12) 0.0017(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 N11 1.939(2) . ? Fe1 N7 1.948(2) . ? Fe1 N9 1.956(2) . ? Fe1 N3 1.980(2) . ? Fe1 N5 1.986(2) . ? Fe1 N1 1.990(2) . ? N9 C20 1.327(4) . ? N9 N10 1.362(3) . ? N7 C17 1.330(3) . ? N7 N8 1.357(3) . ? N3 C7 1.335(3) . ? N3 N4 1.371(3) . ? N8 C19 1.364(3) . ? N8 C26 1.464(3) . ? N12 C25 1.357(4) . ? N12 N11 1.360(3) . ? N12 C26 1.462(4) . ? N5 C12 1.337(3) . ? N5 N6 1.367(3) . ? N4 C9 1.364(3) . ? N4 C16 1.439(3) . ? O9 C27 1.399(4) . ? N1 C2 1.342(3) . ? N1 N2 1.372(3) . ? N6 C14 1.363(3) . ? N6 C16 1.460(3) . ? C21 C22 1.347(5) . ? C21 C20 1.407(4) . ? C17 C18 1.404(4) . ? C7 C8 1.402(4) . ? C7 C6 1.493(4) . ? N2 C4 1.363(3) . ? N2 C16 1.438(3) . ? N10 C22 1.373(4) . ? N10 C26 1.461(4) . ? C4 C3 1.366(4) . ? C4 C5 1.491(4) . ? N11 C23 1.326(4) . ? C19 C18 1.370(4) . ? C2 C3 1.402(4) . ? C2 C1 1.503(4) . ? C14 C13 1.367(4) . ? C14 C15 1.483(4) . ? C13 C12 1.406(4) . ? C26 C27 1.528(4) . ? C9 C8 1.368(4) . ? C9 C10 1.479(4) . ? C24 C25 1.370(5) . ? C24 C23 1.378(4) . ? C12 C11 1.503(4) . ? F2 B1 1.388(4) . ? F1 B1 1.379(4) . ? F3 B1 1.388(4) . ? B1 F4 1.389(4) . ? F5 B2 1.359(4) . ? F6 B2 1.423(5) . ? F7 B2 1.385(5) . ? F8 B2 1.339(5) . ? C30 N14 1.128(4) . ? C30 C31 1.460(5) . ? C28 N13 1.141(6) . ? C28 C29 1.408(7) . ? 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 N11 Fe1 N7 87.59(9) . . ? N11 Fe1 N9 87.23(10) . . ? N7 Fe1 N9 87.73(9) . . ? N11 Fe1 N3 91.36(9) . . ? N7 Fe1 N3 90.68(9) . . ? N9 Fe1 N3 177.92(10) . . ? N11 Fe1 N5 179.31(10) . . ? N7 Fe1 N5 93.08(9) . . ? N9 Fe1 N5 92.65(10) . . ? N3 Fe1 N5 88.78(9) . . ? N11 Fe1 N1 91.83(9) . . ? N7 Fe1 N1 179.35(10) . . ? N9 Fe1 N1 92.55(9) . . ? N3 Fe1 N1 89.02(9) . . ? N5 Fe1 N1 87.50(9) . . ? C20 N9 N10 106.0(2) . . ? C20 N9 Fe1 135.3(2) . . ? N10 N9 Fe1 118.71(17) . . ? C17 N7 N8 106.0(2) . . ? C17 N7 Fe1 134.51(18) . . ? N8 N7 Fe1 119.45(15) . . ? C7 N3 N4 105.5(2) . . ? C7 N3 Fe1 137.08(19) . . ? N4 N3 Fe1 117.27(15) . . ? N7 N8 C19 111.2(2) . . ? N7 N8 C26 118.0(2) . . ? C19 N8 C26 130.8(2) . . ? C25 N12 N11 110.8(2) . . ? C25 N12 C26 130.7(2) . . ? N11 N12 C26 118.3(2) . . ? C12 N5 N6 105.3(2) . . ? C12 N5 Fe1 138.16(19) . . ? N6 N5 Fe1 116.42(15) . . ? C9 N4 N3 112.0(2) . . ? C9 N4 C16 130.1(2) . . ? N3 N4 C16 117.75(19) . . ? C2 N1 N2 105.1(2) . . ? C2 N1 Fe1 138.25(19) . . ? N2 N1 Fe1 116.52(15) . . ? C14 N6 N5 112.0(2) . . ? C14 N6 C16 129.4(2) . . ? N5 N6 C16 118.52(19) . . ? C22 C21 C20 106.0(3) . . ? N7 C17 C18 110.2(2) . . ? N3 C7 C8 109.5(2) . . ? N3 C7 C6 124.0(2) . . ? C8 C7 C6 126.5(2) . . ? C4 N2 N1 111.8(2) . . ? C4 N2 C16 129.8(2) . . ? N1 N2 C16 118.30(19) . . ? N9 N10 C22 110.1(3) . . ? N9 N10 C26 118.5(2) . . ? C22 N10 C26 131.4(3) . . ? N2 C4 C3 105.9(2) . . ? N2 C4 C5 122.4(2) . . ? C3 C4 C5 131.7(2) . . ? C23 N11 N12 105.7(2) . . ? C23 N11 Fe1 134.95(19) . . ? N12 N11 Fe1 119.32(17) . . ? N8 C19 C18 106.5(2) . . ? N1 C2 C3 110.0(2) . . ? N1 C2 C1 123.3(2) . . ? C3 C2 C1 126.6(2) . . ? C21 C22 N10 107.5(3) . . ? N6 C14 C13 105.8(2) . . ? N6 C14 C15 123.2(3) . . ? C13 C14 C15 131.0(3) . . ? C14 C13 C12 107.0(2) . . ? N10 C26 N12 108.6(2) . . ? N10 C26 N8 108.0(2) . . ? N12 C26 N8 108.8(2) . . ? N10 C26 C27 110.1(2) . . ? N12 C26 C27 110.9(2) . . ? N8 C26 C27 110.5(2) . . ? C19 C18 C17 106.1(2) . . ? N4 C9 C8 105.2(2) . . ? N4 C9 C10 122.9(3) . . ? C8 C9 C10 131.9(3) . . ? C4 C3 C2 107.2(2) . . ? C25 C24 C23 106.5(3) . . ? N5 C12 C13 109.9(2) . . ? N5 C12 C11 123.7(3) . . ? C13 C12 C11 126.4(3) . . ? N11 C23 C24 110.7(3) . . ? N9 C20 C21 110.4(3) . . ? C9 C8 C7 107.8(2) . . ? N2 C16 N4 110.4(2) . . ? N2 C16 N6 109.7(2) . . ? N4 C16 N6 110.90(19) . . ? N12 C25 C24 106.3(3) . . ? O9 C27 C26 108.5(2) . . ? F1 B1 F3 109.8(3) . . ? F1 B1 F2 108.8(3) . . ? F3 B1 F2 110.1(3) . . ? F1 B1 F4 109.5(3) . . ? F3 B1 F4 110.1(3) . . ? F2 B1 F4 108.5(3) . . ? F8 B2 F5 110.8(3) . . ? F8 B2 F7 116.1(4) . . ? F5 B2 F7 108.5(3) . . ? F8 B2 F6 109.1(3) . . ? F5 B2 F6 109.7(3) . . ? F7 B2 F6 102.1(3) . . ? N14 C30 C31 178.1(4) . . ? N13 C28 C29 178.9(6) . . ? 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 N11 Fe1 N9 C20 -136.8(3) . . . . ? N7 Fe1 N9 C20 135.5(3) . . . . ? N3 Fe1 N9 C20 176(37) . . . . ? N5 Fe1 N9 C20 42.5(3) . . . . ? N1 Fe1 N9 C20 -45.1(3) . . . . ? N11 Fe1 N9 N10 45.2(2) . . . . ? N7 Fe1 N9 N10 -42.49(19) . . . . ? N3 Fe1 N9 N10 -2(3) . . . . ? N5 Fe1 N9 N10 -135.47(19) . . . . ? N1 Fe1 N9 N10 136.9(2) . . . . ? N11 Fe1 N7 C17 136.4(3) . . . . ? N9 Fe1 N7 C17 -136.3(3) . . . . ? N3 Fe1 N7 C17 45.1(3) . . . . ? N5 Fe1 N7 C17 -43.7(3) . . . . ? N1 Fe1 N7 C17 108(8) . . . . ? N11 Fe1 N7 N8 -44.01(19) . . . . ? N9 Fe1 N7 N8 43.31(19) . . . . ? N3 Fe1 N7 N8 -135.34(19) . . . . ? N5 Fe1 N7 N8 135.85(19) . . . . ? N1 Fe1 N7 N8 -72(8) . . . . ? N11 Fe1 N3 C7 -39.9(3) . . . . ? N7 Fe1 N3 C7 47.7(3) . . . . ? N9 Fe1 N3 C7 7(3) . . . . ? N5 Fe1 N3 C7 140.8(3) . . . . ? N1 Fe1 N3 C7 -131.7(3) . . . . ? N11 Fe1 N3 N4 134.92(17) . . . . ? N7 Fe1 N3 N4 -137.48(17) . . . . ? N9 Fe1 N3 N4 -178(100) . . . . ? N5 Fe1 N3 N4 -44.41(17) . . . . ? N1 Fe1 N3 N4 43.11(17) . . . . ? C17 N7 N8 C19 0.9(3) . . . . ? Fe1 N7 N8 C19 -178.80(18) . . . . ? C17 N7 N8 C26 -179.7(2) . . . . ? Fe1 N7 N8 C26 0.6(3) . . . . ? N11 Fe1 N5 C12 117(9) . . . . ? N7 Fe1 N5 C12 -50.5(3) . . . . ? N9 Fe1 N5 C12 37.4(3) . . . . ? N3 Fe1 N5 C12 -141.1(3) . . . . ? N1 Fe1 N5 C12 129.8(3) . . . . ? N11 Fe1 N5 N6 -58(9) . . . . ? N7 Fe1 N5 N6 134.55(18) . . . . ? N9 Fe1 N5 N6 -137.58(17) . . . . ? N3 Fe1 N5 N6 43.93(17) . . . . ? N1 Fe1 N5 N6 -45.14(17) . . . . ? C7 N3 N4 C9 1.3(3) . . . . ? Fe1 N3 N4 C9 -174.97(16) . . . . ? C7 N3 N4 C16 176.6(2) . . . . ? Fe1 N3 N4 C16 0.3(3) . . . . ? N11 Fe1 N1 C2 41.5(3) . . . . ? N7 Fe1 N1 C2 70(8) . . . . ? N9 Fe1 N1 C2 -45.8(3) . . . . ? N3 Fe1 N1 C2 132.8(3) . . . . ? N5 Fe1 N1 C2 -138.4(3) . . . . ? N11 Fe1 N1 N2 -132.73(18) . . . . ? N7 Fe1 N1 N2 -104(8) . . . . ? N9 Fe1 N1 N2 139.97(18) . . . . ? N3 Fe1 N1 N2 -41.40(18) . . . . ? N5 Fe1 N1 N2 47.42(18) . . . . ? C12 N5 N6 C14 -0.3(3) . . . . ? Fe1 N5 N6 C14 176.25(17) . . . . ? C12 N5 N6 C16 -176.9(2) . . . . ? Fe1 N5 N6 C16 -0.3(3) . . . . ? N8 N7 C17 C18 -0.5(3) . . . . ? Fe1 N7 C17 C18 179.10(19) . . . . ? N4 N3 C7 C8 -1.0(3) . . . . ? Fe1 N3 C7 C8 174.24(19) . . . . ? N4 N3 C7 C6 177.8(2) . . . . ? Fe1 N3 C7 C6 -7.0(4) . . . . ? C2 N1 N2 C4 -1.3(3) . . . . ? Fe1 N1 N2 C4 174.73(17) . . . . ? C2 N1 N2 C16 -179.3(2) . . . . ? Fe1 N1 N2 C16 -3.3(3) . . . . ? C20 N9 N10 C22 -0.9(3) . . . . ? Fe1 N9 N10 C22 177.69(19) . . . . ? C20 N9 N10 C26 179.6(2) . . . . ? Fe1 N9 N10 C26 -1.9(3) . . . . ? N1 N2 C4 C3 0.7(3) . . . . ? C16 N2 C4 C3 178.5(2) . . . . ? N1 N2 C4 C5 -177.6(2) . . . . ? C16 N2 C4 C5 0.1(4) . . . . ? C25 N12 N11 C23 -1.8(3) . . . . ? C26 N12 N11 C23 -178.4(2) . . . . ? C25 N12 N11 Fe1 176.5(2) . . . . ? C26 N12 N11 Fe1 0.0(3) . . . . ? N7 Fe1 N11 C23 -138.7(3) . . . . ? N9 Fe1 N11 C23 133.5(3) . . . . ? N3 Fe1 N11 C23 -48.1(3) . . . . ? N5 Fe1 N11 C23 54(9) . . . . ? N1 Fe1 N11 C23 41.0(3) . . . . ? N7 Fe1 N11 N12 43.61(19) . . . . ? N9 Fe1 N11 N12 -44.23(19) . . . . ? N3 Fe1 N11 N12 134.24(19) . . . . ? N5 Fe1 N11 N12 -124(9) . . . . ? N1 Fe1 N11 N12 -136.70(19) . . . . ? N7 N8 C19 C18 -0.9(3) . . . . ? C26 N8 C19 C18 179.8(3) . . . . ? N2 N1 C2 C3 1.3(3) . . . . ? Fe1 N1 C2 C3 -173.3(2) . . . . ? N2 N1 C2 C1 -176.4(2) . . . . ? Fe1 N1 C2 C1 9.0(4) . . . . ? C20 C21 C22 N10 -0.2(4) . . . . ? N9 N10 C22 C21 0.7(3) . . . . ? C26 N10 C22 C21 -179.9(3) . . . . ? N5 N6 C14 C13 0.6(3) . . . . ? C16 N6 C14 C13 176.8(2) . . . . ? N5 N6 C14 C15 -179.1(2) . . . . ? C16 N6 C14 C15 -3.0(4) . . . . ? N6 C14 C13 C12 -0.7(3) . . . . ? C15 C14 C13 C12 179.0(3) . . . . ? N9 N10 C26 N12 -57.4(3) . . . . ? C22 N10 C26 N12 123.1(3) . . . . ? N9 N10 C26 N8 60.4(3) . . . . ? C22 N10 C26 N8 -119.0(3) . . . . ? N9 N10 C26 C27 -178.9(2) . . . . ? C22 N10 C26 C27 1.6(4) . . . . ? C25 N12 C26 N10 -117.0(3) . . . . ? N11 N12 C26 N10 58.8(3) . . . . ? C25 N12 C26 N8 125.7(3) . . . . ? N11 N12 C26 N8 -58.5(3) . . . . ? C25 N12 C26 C27 4.0(4) . . . . ? N11 N12 C26 C27 179.8(2) . . . . ? N7 N8 C26 N10 -59.7(3) . . . . ? C19 N8 C26 N10 119.6(3) . . . . ? N7 N8 C26 N12 58.0(3) . . . . ? C19 N8 C26 N12 -122.7(3) . . . . ? N7 N8 C26 C27 180.0(2) . . . . ? C19 N8 C26 C27 -0.8(4) . . . . ? N8 C19 C18 C17 0.6(3) . . . . ? N7 C17 C18 C19 0.0(3) . . . . ? N3 N4 C9 C8 -1.2(3) . . . . ? C16 N4 C9 C8 -175.7(2) . . . . ? N3 N4 C9 C10 178.4(3) . . . . ? C16 N4 C9 C10 3.8(4) . . . . ? N2 C4 C3 C2 0.1(3) . . . . ? C5 C4 C3 C2 178.3(3) . . . . ? N1 C2 C3 C4 -0.9(3) . . . . ? C1 C2 C3 C4 176.7(3) . . . . ? N6 N5 C12 C13 -0.2(3) . . . . ? Fe1 N5 C12 C13 -175.5(2) . . . . ? N6 N5 C12 C11 179.2(3) . . . . ? Fe1 N5 C12 C11 3.9(5) . . . . ? C14 C13 C12 N5 0.6(3) . . . . ? C14 C13 C12 C11 -178.8(3) . . . . ? N12 N11 C23 C24 1.5(3) . . . . ? Fe1 N11 C23 C24 -176.4(2) . . . . ? C25 C24 C23 N11 -0.7(4) . . . . ? N10 N9 C20 C21 0.7(3) . . . . ? Fe1 N9 C20 C21 -177.5(2) . . . . ? C22 C21 C20 N9 -0.3(4) . . . . ? N4 C9 C8 C7 0.5(3) . . . . ? C10 C9 C8 C7 -178.9(3) . . . . ? N3 C7 C8 C9 0.3(3) . . . . ? C6 C7 C8 C9 -178.5(3) . . . . ? C4 N2 C16 N4 -114.1(3) . . . . ? N1 N2 C16 N4 63.5(3) . . . . ? C4 N2 C16 N6 123.4(3) . . . . ? N1 N2 C16 N6 -59.0(3) . . . . ? C9 N4 C16 N2 112.7(3) . . . . ? N3 N4 C16 N2 -61.6(3) . . . . ? C9 N4 C16 N6 -125.5(3) . . . . ? N3 N4 C16 N6 60.2(3) . . . . ? C14 N6 C16 N2 -114.3(3) . . . . ? N5 N6 C16 N2 61.6(3) . . . . ? C14 N6 C16 N4 123.5(3) . . . . ? N5 N6 C16 N4 -60.6(3) . . . . ? N11 N12 C25 C24 1.4(4) . . . . ? C26 N12 C25 C24 177.4(3) . . . . ? C23 C24 C25 N12 -0.4(4) . . . . ? N10 C26 C27 O9 -176.6(2) . . . . ? N12 C26 C27 O9 63.3(3) . . . . ? N8 C26 C27 O9 -57.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.931 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.066 #=END data_4 _database_code_depnum_ccdc_archive 'CCDC 650151' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H35 B2 F8 Fe N9' _chemical_formula_weight 775.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.5079(17) _cell_length_b 10.459(2) _cell_length_c 19.534(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.72(3) _cell_angle_gamma 90.00 _cell_volume 1726.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular block' _exptl_crystal_colour red _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.70 _exptl_crystal_size_min 0.60 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 0.519 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _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 23175 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 28.21 _reflns_number_total 8373 _reflns_number_gt 7984 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Structure refined as a racemic twin. 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^)+(0.0357P)^2^+0.6660P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.682(8) _refine_ls_number_reflns 8373 _refine_ls_number_parameters 476 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0760 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.54101(2) 0.06052(2) 0.242299(11) 0.01619(6) Uani 1 1 d . . . N9 N 0.65812(15) 0.07065(17) 0.16106(7) 0.0197(3) Uani 1 1 d . . . N1 N 0.67389(19) 0.19814(15) 0.29174(8) 0.0199(3) Uani 1 1 d . . . N11 N 0.69018(18) -0.07248(15) 0.28058(8) 0.0186(3) Uani 1 1 d . . . N5 N 0.39049(19) 0.19774(15) 0.20588(8) 0.0193(3) Uani 1 1 d . . . N7 N 0.40542(19) -0.07214(15) 0.19448(8) 0.0195(3) Uani 1 1 d . . . N3 N 0.42145(15) 0.04758(15) 0.32414(7) 0.0181(3) Uani 1 1 d . . . C7 C 0.3609(2) -0.04421(19) 0.36059(10) 0.0214(4) Uani 1 1 d . . . N4 N 0.37963(18) 0.16060(14) 0.35323(8) 0.0173(3) Uani 1 1 d . . . C26 C 0.6999(2) -0.03900(19) 0.13201(10) 0.0199(3) Uani 1 1 d . . . C22 C 0.6996(2) 0.1823(2) 0.13310(11) 0.0248(4) Uani 1 1 d . . . H22 H 0.6699 0.2604 0.1529 0.030 Uiso 1 1 calc R . . C8 C 0.2806(2) 0.00920(19) 0.41239(10) 0.0218(4) Uani 1 1 d . . . H8 H 0.2268 -0.0361 0.4448 0.026 Uiso 1 1 calc R . . C9 C 0.2948(2) 0.13936(19) 0.40733(9) 0.0203(4) Uani 1 1 d . . . C25 C 0.7846(2) -0.0409(2) 0.07527(10) 0.0258(4) Uani 1 1 d . . . H25 H 0.8122 -0.1198 0.0558 0.031 Uiso 1 1 calc R . . C23 C 0.7840(3) 0.1866(2) 0.07656(12) 0.0322(5) Uani 1 1 d . . . H23 H 0.8114 0.2663 0.0579 0.039 Uiso 1 1 calc R . . N6 N 0.35516(17) 0.28907(15) 0.25242(7) 0.0187(3) Uani 1 1 d . . . C24 C 0.8277(2) 0.0734(2) 0.04779(10) 0.0325(4) Uani 1 1 d . . . H24 H 0.8869 0.0742 0.0095 0.039 Uiso 1 1 calc R . . C4 C 0.6952(2) 0.37419(18) 0.36049(10) 0.0243(4) Uani 1 1 d . . . C21 C 0.4737(2) -0.16758(17) 0.16202(9) 0.0201(3) Uani 1 1 d . . . N2 N 0.59543(17) 0.28724(14) 0.32642(7) 0.0188(3) Uani 1 1 d . . . C14 C 0.2554(2) 0.38023(18) 0.22183(10) 0.0228(4) Uani 1 1 d . . . C31 C 0.72741(19) -0.16812(17) 0.23911(9) 0.0189(3) Uani 1 1 d . . . C16 C 0.4256(2) 0.27860(17) 0.32334(9) 0.0194(3) Uani 1 1 d . . . H16 H 0.3871 0.3513 0.3501 0.023 Uiso 1 1 calc R . . C13 C 0.2245(2) 0.34506(19) 0.15396(10) 0.0267(4) Uani 1 1 d . . . H13 H 0.1575 0.3884 0.1191 0.032 Uiso 1 1 calc R . . C19 C 0.2237(2) -0.2644(2) 0.12668(11) 0.0308(4) Uani 1 1 d . . . H19 H 0.1612 -0.3305 0.1039 0.037 Uiso 1 1 calc R . . C20 C 0.3867(2) -0.2647(2) 0.12717(10) 0.0266(4) Uani 1 1 d . . . H20 H 0.4377 -0.3300 0.1042 0.032 Uiso 1 1 calc R . . C32 C 0.6514(2) -0.16140(17) 0.16510(9) 0.0190(3) Uani 1 1 d . . . H32 H 0.6888 -0.2357 0.1391 0.023 Uiso 1 1 calc R . . C17 C 0.2465(2) -0.07350(19) 0.19288(10) 0.0236(4) Uani 1 1 d . . . H17 H 0.1970 -0.0071 0.2157 0.028 Uiso 1 1 calc R . . F7 F 0.2224(2) -0.44301(17) 0.41594(7) 0.0574(4) Uani 1 1 d . . . F5 F 0.07782(17) -0.45527(17) 0.50586(9) 0.0574(4) Uani 1 1 d . . . F4 F 0.90648(16) 0.46387(12) 0.04141(7) 0.0384(3) Uani 1 1 d . . . F6 F 0.16302(18) -0.26403(13) 0.47120(7) 0.0440(3) Uani 1 1 d . . . F2 F 0.66482(15) 0.52392(16) 0.06931(8) 0.0491(4) Uani 1 1 d . . . F1 F 0.86203(19) 0.47909(16) 0.15331(7) 0.0499(4) Uani 1 1 d . . . C28 C 0.8650(2) -0.16367(19) 0.37267(9) 0.0238(4) Uani 1 1 d . . . H28 H 0.9131 -0.1590 0.4190 0.029 Uiso 1 1 calc R . . C27 C 0.7579(2) -0.07124(18) 0.34656(9) 0.0211(3) Uani 1 1 d . . . H27 H 0.7312 -0.0046 0.3762 0.025 Uiso 1 1 calc R . . C29 C 0.9010(2) -0.2630(2) 0.33031(10) 0.0269(4) Uani 1 1 d . . . H29 H 0.9725 -0.3285 0.3474 0.032 Uiso 1 1 calc R . . B1 B 0.8254(3) 0.5302(2) 0.08764(11) 0.0269(5) Uani 1 1 d . . . C6 C 0.3821(2) -0.18402(18) 0.34792(10) 0.0281(4) Uani 1 1 d . . . H6A H 0.4450 -0.1954 0.3094 0.042 Uiso 1 1 calc R . . H6B H 0.2783 -0.2242 0.3366 0.042 Uiso 1 1 calc R . . H6C H 0.4370 -0.2238 0.3894 0.042 Uiso 1 1 calc R . . B2 B 0.2008(3) -0.3918(2) 0.48024(12) 0.0302(5) Uani 1 1 d . . . F3 F 0.87306(16) 0.65752(13) 0.08755(8) 0.0434(3) Uani 1 1 d . . . F8 F 0.33672(17) -0.4047(2) 0.52437(8) 0.0656(6) Uani 1 1 d . . . C3 C 0.8438(2) 0.3391(2) 0.34682(11) 0.0295(4) Uani 1 1 d . . . H3 H 0.9403 0.3805 0.3632 0.035 Uiso 1 1 calc R . . C30 C 0.8310(2) -0.26568(18) 0.26238(10) 0.0236(4) Uani 1 1 d . . . H30 H 0.8536 -0.3330 0.2324 0.028 Uiso 1 1 calc R . . C15 C 0.1999(3) 0.49149(19) 0.25991(11) 0.0323(4) Uani 1 1 d . . . H15A H 0.1627 0.4619 0.3028 0.048 Uiso 1 1 calc R . . H15B H 0.1130 0.5341 0.2313 0.048 Uiso 1 1 calc R . . H15C H 0.2874 0.5518 0.2707 0.048 Uiso 1 1 calc R . . C10 C 0.2412(2) 0.24403(19) 0.45123(10) 0.0283(4) Uani 1 1 d . . . H10A H 0.3289 0.2695 0.4856 0.042 Uiso 1 1 calc R . . H10B H 0.1526 0.2136 0.4747 0.042 Uiso 1 1 calc R . . H10C H 0.2070 0.3176 0.4222 0.042 Uiso 1 1 calc R . . C2 C 0.8269(2) 0.23094(19) 0.30412(10) 0.0242(4) Uani 1 1 d . . . C12 C 0.3110(2) 0.23250(19) 0.14581(9) 0.0234(4) Uani 1 1 d . . . C18 C 0.1532(2) -0.1669(2) 0.15964(10) 0.0282(4) Uani 1 1 d . . . H18 H 0.0415 -0.1645 0.1593 0.034 Uiso 1 1 calc R . . C1 C 0.9552(2) 0.1586(2) 0.27495(12) 0.0337(5) Uani 1 1 d . . . H1A H 0.9092 0.0858 0.2481 0.051 Uiso 1 1 calc R . . H1B H 1.0319 0.1275 0.3126 0.051 Uiso 1 1 calc R . . H1C H 1.0088 0.2151 0.2450 0.051 Uiso 1 1 calc R . . C5 C 0.6388(3) 0.4805(2) 0.40194(12) 0.0349(5) Uani 1 1 d . . . H5A H 0.5675 0.5358 0.3721 0.052 Uiso 1 1 calc R . . H5B H 0.7297 0.5305 0.4225 0.052 Uiso 1 1 calc R . . H5C H 0.5822 0.4452 0.4385 0.052 Uiso 1 1 calc R . . C11 C 0.3140(3) 0.1596(2) 0.07996(10) 0.0333(5) Uani 1 1 d . . . H11A H 0.4124 0.1103 0.0820 0.050 Uiso 0.50 1 calc PR . . H11B H 0.3081 0.2195 0.0412 0.050 Uiso 0.50 1 calc PR . . H11C H 0.2233 0.1012 0.0737 0.050 Uiso 0.50 1 calc PR . . H11D H 0.2168 0.1770 0.0492 0.050 Uiso 0.50 1 calc PR . . H11E H 0.3211 0.0678 0.0900 0.050 Uiso 0.50 1 calc PR . . H11F H 0.4059 0.1862 0.0575 0.050 Uiso 0.50 1 calc PR . . 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 0.01515(9) 0.01596(10) 0.01769(10) -0.00151(10) 0.00284(7) 0.00134(9) N9 0.0185(6) 0.0207(7) 0.0204(6) 0.0000(7) 0.0037(5) 0.0018(7) N1 0.0177(7) 0.0187(7) 0.0235(7) -0.0019(6) 0.0036(6) -0.0002(6) N11 0.0171(7) 0.0185(7) 0.0204(7) -0.0003(6) 0.0040(6) -0.0001(5) N5 0.0208(7) 0.0173(7) 0.0199(7) -0.0034(6) 0.0030(6) 0.0039(6) N7 0.0182(7) 0.0197(7) 0.0207(7) -0.0011(6) 0.0023(6) 0.0013(6) N3 0.0191(6) 0.0149(7) 0.0206(6) -0.0038(6) 0.0038(5) 0.0007(6) C7 0.0221(9) 0.0190(9) 0.0231(9) -0.0006(7) 0.0024(7) 0.0000(7) N4 0.0188(7) 0.0147(7) 0.0191(7) -0.0017(6) 0.0053(6) 0.0021(5) C26 0.0185(8) 0.0216(9) 0.0198(8) 0.0016(7) 0.0025(7) 0.0019(7) C22 0.0258(10) 0.0211(9) 0.0282(10) 0.0020(8) 0.0062(8) 0.0001(7) C8 0.0232(9) 0.0234(9) 0.0197(8) 0.0011(7) 0.0060(7) -0.0019(7) C9 0.0190(8) 0.0239(9) 0.0182(8) -0.0018(7) 0.0033(7) 0.0017(7) C25 0.0261(9) 0.0301(10) 0.0224(9) 0.0011(8) 0.0077(7) 0.0074(8) C23 0.0390(12) 0.0267(10) 0.0331(11) 0.0068(8) 0.0135(9) 0.0008(9) N6 0.0196(7) 0.0176(7) 0.0190(6) -0.0013(6) 0.0031(5) 0.0043(5) C24 0.0360(9) 0.0364(11) 0.0275(8) 0.0048(9) 0.0144(7) 0.0014(10) C4 0.0275(9) 0.0223(9) 0.0228(9) -0.0011(7) 0.0010(7) -0.0066(7) C21 0.0197(8) 0.0206(8) 0.0201(8) -0.0007(7) 0.0029(6) 0.0012(6) N2 0.0186(7) 0.0180(7) 0.0199(6) -0.0041(5) 0.0029(5) -0.0020(5) C14 0.0226(8) 0.0190(8) 0.0275(9) 0.0031(7) 0.0052(7) 0.0048(7) C31 0.0164(7) 0.0200(8) 0.0206(8) 0.0003(7) 0.0040(6) 0.0001(6) C16 0.0200(8) 0.0178(8) 0.0206(8) -0.0012(7) 0.0039(6) -0.0012(6) C13 0.0279(9) 0.0259(10) 0.0258(9) 0.0043(8) 0.0015(7) 0.0080(8) C19 0.0274(9) 0.0319(10) 0.0325(10) -0.0092(9) 0.0006(8) -0.0059(8) C20 0.0285(9) 0.0252(9) 0.0262(9) -0.0084(8) 0.0041(7) -0.0010(8) C32 0.0187(7) 0.0195(8) 0.0193(7) -0.0015(7) 0.0044(6) 0.0030(6) C17 0.0195(8) 0.0258(9) 0.0254(9) -0.0034(7) 0.0029(7) 0.0004(7) F7 0.1018(12) 0.0332(7) 0.0399(7) -0.0022(7) 0.0196(7) 0.0030(9) F5 0.0457(7) 0.0527(10) 0.0765(10) 0.0234(9) 0.0188(7) -0.0060(7) F4 0.0538(8) 0.0250(6) 0.0411(7) -0.0004(5) 0.0254(6) 0.0032(6) F6 0.0576(8) 0.0288(6) 0.0469(8) 0.0047(6) 0.0110(6) 0.0063(6) F2 0.0252(6) 0.0671(10) 0.0546(8) 0.0025(7) 0.0034(6) -0.0088(6) F1 0.0618(9) 0.0570(9) 0.0309(7) 0.0027(6) 0.0047(6) 0.0186(7) C28 0.0232(8) 0.0260(9) 0.0219(8) 0.0021(7) 0.0018(7) 0.0023(7) C27 0.0195(8) 0.0217(9) 0.0222(8) 0.0005(7) 0.0027(6) 0.0010(7) C29 0.0260(9) 0.0255(9) 0.0289(9) 0.0062(8) 0.0023(7) 0.0056(7) B1 0.0241(9) 0.0277(12) 0.0291(10) -0.0032(8) 0.0031(8) 0.0024(8) C6 0.0366(10) 0.0167(9) 0.0328(10) -0.0014(7) 0.0117(8) -0.0014(7) B2 0.0308(11) 0.0307(11) 0.0289(11) 0.0093(9) 0.0026(9) 0.0044(9) F3 0.0377(7) 0.0254(6) 0.0688(9) -0.0109(6) 0.0138(6) -0.0039(5) F8 0.0347(7) 0.1094(16) 0.0510(8) 0.0349(9) -0.0020(6) 0.0100(8) C3 0.0246(9) 0.0296(10) 0.0337(10) -0.0042(9) 0.0008(7) -0.0081(8) C30 0.0235(8) 0.0216(8) 0.0263(9) -0.0009(7) 0.0058(7) 0.0053(7) C15 0.0395(11) 0.0259(11) 0.0322(10) -0.0007(8) 0.0070(8) 0.0118(8) C10 0.0364(10) 0.0232(9) 0.0276(9) -0.0042(7) 0.0140(8) 0.0003(8) C2 0.0187(8) 0.0251(9) 0.0289(9) -0.0007(7) 0.0027(7) -0.0023(7) C12 0.0241(8) 0.0247(9) 0.0211(8) -0.0013(7) 0.0010(6) 0.0053(7) C18 0.0202(8) 0.0346(11) 0.0291(9) -0.0040(8) 0.0005(7) -0.0039(8) C1 0.0163(8) 0.0385(12) 0.0467(12) -0.0101(10) 0.0052(8) -0.0021(8) C5 0.0372(11) 0.0297(11) 0.0380(11) -0.0132(9) 0.0047(9) -0.0059(8) C11 0.0395(11) 0.0386(11) 0.0201(9) -0.0069(8) -0.0034(8) 0.0122(9) _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 N7 1.9688(17) . ? Fe1 N11 1.9705(16) . ? Fe1 N9 1.9728(14) . ? Fe1 N3 1.9972(14) . ? Fe1 N5 1.9981(16) . ? Fe1 N1 2.0068(17) . ? N9 C26 1.346(3) . ? N9 C22 1.354(3) . ? N1 C2 1.341(2) . ? N1 N2 1.371(2) . ? N11 C31 1.348(2) . ? N11 C27 1.349(2) . ? N5 C12 1.334(2) . ? N5 N6 1.376(2) . ? N7 C17 1.349(2) . ? N7 C21 1.350(2) . ? N3 C7 1.334(3) . ? N3 N4 1.376(2) . ? C7 C8 1.401(3) . ? C7 C6 1.498(3) . ? N4 C9 1.366(2) . ? N4 C16 1.439(2) . ? C26 C25 1.391(3) . ? C26 C32 1.513(3) . ? C22 C23 1.387(3) . ? C8 C9 1.371(3) . ? C9 C10 1.494(3) . ? C25 C24 1.378(3) . ? C23 C24 1.381(3) . ? N6 C14 1.367(2) . ? N6 C16 1.448(2) . ? C4 N2 1.363(2) . ? C4 C3 1.372(3) . ? C4 C5 1.487(3) . ? C21 C20 1.388(3) . ? C21 C32 1.508(2) . ? N2 C16 1.442(2) . ? C14 C13 1.371(3) . ? C14 C15 1.487(3) . ? C31 C30 1.389(2) . ? C31 C32 1.515(2) . ? C13 C12 1.407(3) . ? C19 C18 1.380(3) . ? C19 C20 1.385(3) . ? C17 C18 1.373(3) . ? F7 B2 1.397(3) . ? F5 B2 1.381(3) . ? F4 B1 1.385(2) . ? F6 B2 1.381(3) . ? F2 B1 1.373(3) . ? F1 B1 1.391(3) . ? C28 C27 1.384(3) . ? C28 C29 1.385(3) . ? C29 C30 1.390(3) . ? B1 F3 1.392(3) . ? B2 F8 1.366(3) . ? C3 C2 1.403(3) . ? C2 C1 1.495(3) . ? C12 C11 1.498(3) . ? 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 N7 Fe1 N11 89.90(7) . . ? N7 Fe1 N9 88.81(7) . . ? N11 Fe1 N9 88.84(7) . . ? N7 Fe1 N3 90.40(6) . . ? N11 Fe1 N3 90.81(6) . . ? N9 Fe1 N3 179.14(7) . . ? N7 Fe1 N5 91.25(6) . . ? N11 Fe1 N5 178.49(7) . . ? N9 Fe1 N5 92.18(7) . . ? N3 Fe1 N5 88.19(6) . . ? N7 Fe1 N1 178.43(7) . . ? N11 Fe1 N1 91.27(6) . . ? N9 Fe1 N1 92.26(7) . . ? N3 Fe1 N1 88.53(6) . . ? N5 Fe1 N1 87.57(7) . . ? C26 N9 C22 118.12(14) . . ? C26 N9 Fe1 118.45(13) . . ? C22 N9 Fe1 123.43(13) . . ? C2 N1 N2 104.81(15) . . ? C2 N1 Fe1 138.66(14) . . ? N2 N1 Fe1 116.49(11) . . ? C31 N11 C27 118.49(16) . . ? C31 N11 Fe1 118.81(12) . . ? C27 N11 Fe1 122.69(13) . . ? C12 N5 N6 105.34(15) . . ? C12 N5 Fe1 138.28(13) . . ? N6 N5 Fe1 116.36(12) . . ? C17 N7 C21 117.82(16) . . ? C17 N7 Fe1 123.27(13) . . ? C21 N7 Fe1 118.91(12) . . ? C7 N3 N4 105.25(13) . . ? C7 N3 Fe1 137.78(13) . . ? N4 N3 Fe1 116.92(11) . . ? N3 C7 C8 110.47(17) . . ? N3 C7 C6 123.56(17) . . ? C8 C7 C6 125.95(18) . . ? C9 N4 N3 111.42(15) . . ? C9 N4 C16 130.30(16) . . ? N3 N4 C16 118.26(13) . . ? N9 C26 C25 122.35(18) . . ? N9 C26 C32 116.27(15) . . ? C25 C26 C32 121.38(18) . . ? N9 C22 C23 122.18(18) . . ? C9 C8 C7 106.83(18) . . ? N4 C9 C8 106.03(17) . . ? N4 C9 C10 123.30(17) . . ? C8 C9 C10 130.60(18) . . ? C24 C25 C26 119.00(19) . . ? C24 C23 C22 119.09(19) . . ? C14 N6 N5 111.60(14) . . ? C14 N6 C16 129.60(15) . . ? N5 N6 C16 118.80(14) . . ? C25 C24 C23 119.25(16) . . ? N2 C4 C3 105.18(17) . . ? N2 C4 C5 122.85(17) . . ? C3 C4 C5 131.97(18) . . ? N7 C21 C20 122.50(16) . . ? N7 C21 C32 115.74(16) . . ? C20 C21 C32 121.75(16) . . ? C4 N2 N1 112.55(14) . . ? C4 N2 C16 128.75(15) . . ? N1 N2 C16 118.70(14) . . ? N6 C14 C13 105.93(16) . . ? N6 C14 C15 122.98(17) . . ? C13 C14 C15 131.08(18) . . ? N11 C31 C30 122.21(16) . . ? N11 C31 C32 115.79(15) . . ? C30 C31 C32 121.99(16) . . ? N4 C16 N2 110.82(15) . . ? N4 C16 N6 110.57(14) . . ? N2 C16 N6 109.63(14) . . ? C14 C13 C12 106.86(17) . . ? C18 C19 C20 119.22(18) . . ? C19 C20 C21 118.54(18) . . ? C21 C32 C26 109.95(15) . . ? C21 C32 C31 110.50(14) . . ? C26 C32 C31 109.88(15) . . ? N7 C17 C18 122.74(18) . . ? C27 C28 C29 119.09(17) . . ? N11 C27 C28 122.31(17) . . ? C28 C29 C30 119.02(17) . . ? F2 B1 F4 111.24(17) . . ? F2 B1 F1 109.34(18) . . ? F4 B1 F1 109.51(17) . . ? F2 B1 F3 109.05(17) . . ? F4 B1 F3 108.10(17) . . ? F1 B1 F3 109.57(18) . . ? F8 B2 F6 110.1(2) . . ? F8 B2 F5 110.20(18) . . ? F6 B2 F5 109.68(18) . . ? F8 B2 F7 109.81(19) . . ? F6 B2 F7 108.01(18) . . ? F5 B2 F7 109.0(2) . . ? C4 C3 C2 107.39(17) . . ? C31 C30 C29 118.84(17) . . ? N1 C2 C3 110.07(17) . . ? N1 C2 C1 122.60(17) . . ? C3 C2 C1 127.33(17) . . ? N5 C12 C13 110.27(16) . . ? N5 C12 C11 123.97(17) . . ? C13 C12 C11 125.76(17) . . ? C17 C18 C19 119.17(18) . . ? 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 N7 Fe1 N9 C26 -44.96(13) . . . . ? N11 Fe1 N9 C26 44.96(13) . . . . ? N3 Fe1 N9 C26 -21(4) . . . . ? N5 Fe1 N9 C26 -136.17(13) . . . . ? N1 Fe1 N9 C26 136.18(13) . . . . ? N7 Fe1 N9 C22 135.39(15) . . . . ? N11 Fe1 N9 C22 -134.69(15) . . . . ? N3 Fe1 N9 C22 159(4) . . . . ? N5 Fe1 N9 C22 44.19(15) . . . . ? N1 Fe1 N9 C22 -43.47(15) . . . . ? N7 Fe1 N1 C2 -178(100) . . . . ? N11 Fe1 N1 C2 44.2(2) . . . . ? N9 Fe1 N1 C2 -44.7(2) . . . . ? N3 Fe1 N1 C2 135.0(2) . . . . ? N5 Fe1 N1 C2 -136.7(2) . . . . ? N7 Fe1 N1 N2 5(3) . . . . ? N11 Fe1 N1 N2 -133.14(13) . . . . ? N9 Fe1 N1 N2 137.98(13) . . . . ? N3 Fe1 N1 N2 -42.36(13) . . . . ? N5 Fe1 N1 N2 45.89(13) . . . . ? N7 Fe1 N11 C31 42.94(13) . . . . ? N9 Fe1 N11 C31 -45.87(13) . . . . ? N3 Fe1 N11 C31 133.34(13) . . . . ? N5 Fe1 N11 C31 -178(49) . . . . ? N1 Fe1 N11 C31 -138.11(14) . . . . ? N7 Fe1 N11 C27 -137.67(15) . . . . ? N9 Fe1 N11 C27 133.52(15) . . . . ? N3 Fe1 N11 C27 -47.27(15) . . . . ? N5 Fe1 N11 C27 1(3) . . . . ? N1 Fe1 N11 C27 41.28(15) . . . . ? N7 Fe1 N5 C12 -47.5(2) . . . . ? N11 Fe1 N5 C12 174(3) . . . . ? N9 Fe1 N5 C12 41.4(2) . . . . ? N3 Fe1 N5 C12 -137.8(2) . . . . ? N1 Fe1 N5 C12 133.6(2) . . . . ? N7 Fe1 N5 N6 134.86(14) . . . . ? N11 Fe1 N5 N6 -4(3) . . . . ? N9 Fe1 N5 N6 -136.28(13) . . . . ? N3 Fe1 N5 N6 44.50(13) . . . . ? N1 Fe1 N5 N6 -44.11(13) . . . . ? N11 Fe1 N7 C17 136.02(16) . . . . ? N9 Fe1 N7 C17 -135.14(16) . . . . ? N3 Fe1 N7 C17 45.21(16) . . . . ? N5 Fe1 N7 C17 -42.98(15) . . . . ? N1 Fe1 N7 C17 -2(3) . . . . ? N11 Fe1 N7 C21 -43.37(14) . . . . ? N9 Fe1 N7 C21 45.47(14) . . . . ? N3 Fe1 N7 C21 -134.18(14) . . . . ? N5 Fe1 N7 C21 137.62(14) . . . . ? N1 Fe1 N7 C21 179(100) . . . . ? N7 Fe1 N3 C7 41.86(18) . . . . ? N11 Fe1 N3 C7 -48.04(18) . . . . ? N9 Fe1 N3 C7 18(4) . . . . ? N5 Fe1 N3 C7 133.09(18) . . . . ? N1 Fe1 N3 C7 -139.29(18) . . . . ? N7 Fe1 N3 N4 -135.20(12) . . . . ? N11 Fe1 N3 N4 134.90(12) . . . . ? N9 Fe1 N3 N4 -159(4) . . . . ? N5 Fe1 N3 N4 -43.96(12) . . . . ? N1 Fe1 N3 N4 43.66(12) . . . . ? N4 N3 C7 C8 0.18(18) . . . . ? Fe1 N3 C7 C8 -177.09(13) . . . . ? N4 N3 C7 C6 -178.12(19) . . . . ? Fe1 N3 C7 C6 4.6(3) . . . . ? C7 N3 N4 C9 0.31(17) . . . . ? Fe1 N3 N4 C9 178.25(12) . . . . ? C7 N3 N4 C16 -178.45(17) . . . . ? Fe1 N3 N4 C16 -0.51(19) . . . . ? C22 N9 C26 C25 0.6(2) . . . . ? Fe1 N9 C26 C25 -179.03(15) . . . . ? C22 N9 C26 C32 179.83(18) . . . . ? Fe1 N9 C26 C32 0.2(2) . . . . ? C26 N9 C22 C23 -0.6(3) . . . . ? Fe1 N9 C22 C23 179.02(16) . . . . ? N3 C7 C8 C9 -0.6(2) . . . . ? C6 C7 C8 C9 177.66(19) . . . . ? N3 N4 C9 C8 -0.7(2) . . . . ? C16 N4 C9 C8 177.90(18) . . . . ? N3 N4 C9 C10 176.48(16) . . . . ? C16 N4 C9 C10 -5.0(3) . . . . ? C7 C8 C9 N4 0.7(2) . . . . ? C7 C8 C9 C10 -176.12(19) . . . . ? N9 C26 C25 C24 0.1(3) . . . . ? C32 C26 C25 C24 -179.02(17) . . . . ? N9 C22 C23 C24 -0.1(3) . . . . ? C12 N5 N6 C14 -0.3(2) . . . . ? Fe1 N5 N6 C14 178.13(12) . . . . ? C12 N5 N6 C16 -179.46(15) . . . . ? Fe1 N5 N6 C16 -1.1(2) . . . . ? C26 C25 C24 C23 -0.9(3) . . . . ? C22 C23 C24 C25 0.9(3) . . . . ? C17 N7 C21 C20 0.6(3) . . . . ? Fe1 N7 C21 C20 179.98(14) . . . . ? C17 N7 C21 C32 179.79(16) . . . . ? Fe1 N7 C21 C32 -0.8(2) . . . . ? C3 C4 N2 N1 0.1(2) . . . . ? C5 C4 N2 N1 -179.97(18) . . . . ? C3 C4 N2 C16 179.71(18) . . . . ? C5 C4 N2 C16 -0.4(3) . . . . ? C2 N1 N2 C4 -0.4(2) . . . . ? Fe1 N1 N2 C4 177.78(12) . . . . ? C2 N1 N2 C16 179.93(15) . . . . ? Fe1 N1 N2 C16 -1.9(2) . . . . ? N5 N6 C14 C13 0.8(2) . . . . ? C16 N6 C14 C13 179.90(17) . . . . ? N5 N6 C14 C15 -179.01(17) . . . . ? C16 N6 C14 C15 0.1(3) . . . . ? C27 N11 C31 C30 0.9(3) . . . . ? Fe1 N11 C31 C30 -179.69(13) . . . . ? C27 N11 C31 C32 -178.05(15) . . . . ? Fe1 N11 C31 C32 1.4(2) . . . . ? C9 N4 C16 N2 120.9(2) . . . . ? N3 N4 C16 N2 -60.67(19) . . . . ? C9 N4 C16 N6 -117.4(2) . . . . ? N3 N4 C16 N6 61.1(2) . . . . ? C4 N2 C16 N4 -117.36(19) . . . . ? N1 N2 C16 N4 62.2(2) . . . . ? C4 N2 C16 N6 120.32(19) . . . . ? N1 N2 C16 N6 -60.1(2) . . . . ? C14 N6 C16 N4 120.62(19) . . . . ? N5 N6 C16 N4 -60.4(2) . . . . ? C14 N6 C16 N2 -116.91(19) . . . . ? N5 N6 C16 N2 62.1(2) . . . . ? N6 C14 C13 C12 -1.0(2) . . . . ? C15 C14 C13 C12 178.8(2) . . . . ? C18 C19 C20 C21 1.1(3) . . . . ? N7 C21 C20 C19 -1.0(3) . . . . ? C32 C21 C20 C19 179.83(18) . . . . ? N7 C21 C32 C26 -60.3(2) . . . . ? C20 C21 C32 C26 118.94(19) . . . . ? N7 C21 C32 C31 61.2(2) . . . . ? C20 C21 C32 C31 -119.61(19) . . . . ? N9 C26 C32 C21 60.9(2) . . . . ? C25 C26 C32 C21 -119.94(19) . . . . ? N9 C26 C32 C31 -61.0(2) . . . . ? C25 C26 C32 C31 118.24(19) . . . . ? N11 C31 C32 C21 -61.6(2) . . . . ? C30 C31 C32 C21 119.48(18) . . . . ? N11 C31 C32 C26 59.93(19) . . . . ? C30 C31 C32 C26 -119.03(18) . . . . ? C21 N7 C17 C18 -0.3(3) . . . . ? Fe1 N7 C17 C18 -179.66(15) . . . . ? C31 N11 C27 C28 0.7(3) . . . . ? Fe1 N11 C27 C28 -178.69(13) . . . . ? C29 C28 C27 N11 -1.8(3) . . . . ? C27 C28 C29 C30 1.3(3) . . . . ? N2 C4 C3 C2 0.2(2) . . . . ? C5 C4 C3 C2 -179.7(2) . . . . ? N11 C31 C30 C29 -1.3(3) . . . . ? C32 C31 C30 C29 177.55(17) . . . . ? C28 C29 C30 C31 0.2(3) . . . . ? N2 N1 C2 C3 0.6(2) . . . . ? Fe1 N1 C2 C3 -177.00(16) . . . . ? N2 N1 C2 C1 -179.37(18) . . . . ? Fe1 N1 C2 C1 3.1(3) . . . . ? C4 C3 C2 N1 -0.5(2) . . . . ? C4 C3 C2 C1 179.4(2) . . . . ? N6 N5 C12 C13 -0.4(2) . . . . ? Fe1 N5 C12 C13 -178.22(15) . . . . ? N6 N5 C12 C11 -179.70(19) . . . . ? Fe1 N5 C12 C11 2.5(3) . . . . ? C14 C13 C12 N5 0.9(2) . . . . ? C14 C13 C12 C11 -179.8(2) . . . . ? N7 C17 C18 C19 0.4(3) . . . . ? C20 C19 C18 C17 -0.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.718 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.049 #=END OF CIF