Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global #==================================================================== # 1. SUBMISSION DETAILS _journal_coden_Cambridge 222 _publ_contact_author_name 'Malcolm A. Halcrow' _publ_contact_author_address ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; _publ_contact_author_phone '+44 (0)113 3436506' _publ_contact_author_fax '+44 (0)113 3436565' _publ_contact_author_email m.a.halcrow@leeds.ac.uk _publ_requested_journal 'Dalton Transactions' #======================================================================= _publ_section_title ; Structural diversity in iron(II) complexes of 2,6-di(pyrazol-1-yl)pyridine and 2,6-di(3-methylpyrazol-1-yl)pyridine. ; loop_ _publ_author_name _publ_author_address 'Jerome Elhaik' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Colin A. Kilner' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Malcolm A. Halcrow' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; #================================================================= data_c:\datasets\leeds\mh139\mh139 _database_code_depnum_ccdc_archive 'CCDC 278897' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) hemiiodide sesqui(triiodide) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[C22 H18 Fe N10], I0.5, [I3]1.5' _chemical_formula_sum 'C22 H18 Fe I5 N10' _chemical_formula_weight 1112.81 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 15.9084(3) _cell_length_b 13.6094(3) _cell_length_c 15.1155(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.3473(8) _cell_angle_gamma 90.00 _cell_volume 3170.50(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 41942 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour Orange-brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2044 _exptl_absorpt_coefficient_mu 5.375 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.159 _exptl_absorpt_correction_T_max 0.833 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_ambient_temperature 150(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 area detector diffractometer' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41942 _diffrn_reflns_av_R_equivalents 0.1542 _diffrn_reflns_av_sigmaI/netI 0.0768 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7248 _reflns_number_gt 5473 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 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 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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. The asymmetric unit contains one complex dication lying on a general position; one half-occupied iodide anion (I34) lying on the C2 axis (1, y, 0.75); two half-occupied triiodide anions lying on C2 axes {I35 and I36 on (0.5, y, 0.75) and I37 and I38 on (0.5, y, 0.25)}; and a disordered half-occupied triiodide ion I39-I41 lying across the C2 axis (0, y, 0.25). The disordered half-anion was modelled over two sites: I39A and I40A, with I40A lying on the C2 axis (occupancy 0.25). I39B-I41B, lying on a general position across the C2 axis (occupancy 0.25). The I---I bonds within this disordered anion were restrained to 2.92(2)\%A. All non-H atoms were refined anisotropically, and all non-H atoms were placed in calculated positions and refined using a riding model. Two residual Fourier peaks of 1.0-1.7 e.\%A^-3^, and the deepest Fourier hole of -2.3 e.\%A^-3^, are all <1 \%A from an I atom. There is a third residual Fourier peak of 1.1 e.\%A^-3^, which lies 2.5\%A from both I37 and I38. ; _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^)+(0.0609P)^2^+1.8604P] 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 7248 _refine_ls_number_parameters 372 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1327 _refine_ls_wR_factor_gt 0.1186 _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 0.75780(5) 0.85402(5) 0.61215(5) 0.03113(18) Uani 1 1 d . . . N2 N 0.8128(3) 0.9785(3) 0.5606(3) 0.0299(9) Uani 1 1 d . . . C3 C 0.8055(3) 1.0680(3) 0.5934(3) 0.0314(11) Uani 1 1 d . . . C4 C 0.8375(4) 1.1515(4) 0.5616(4) 0.0385(12) Uani 1 1 d . . . H4 H 0.8312 1.2147 0.5859 0.046 Uiso 1 1 calc R . . C5 C 0.8793(4) 1.1383(4) 0.4921(4) 0.0425(14) Uani 1 1 d . . . H5 H 0.9003 1.1941 0.4665 0.051 Uiso 1 1 calc R . . C6 C 0.8911(3) 1.0461(4) 0.4591(4) 0.0382(12) Uani 1 1 d . . . H6 H 0.9209 1.0371 0.4125 0.046 Uiso 1 1 calc R . . C7 C 0.8574(3) 0.9671(4) 0.4974(3) 0.0313(11) Uani 1 1 d . . . N8 N 0.7604(3) 1.0691(3) 0.6632(3) 0.0326(9) Uani 1 1 d . . . N9 N 0.7383(3) 0.9801(3) 0.6938(3) 0.0352(10) Uani 1 1 d . . . C10 C 0.7023(4) 1.0023(4) 0.7618(4) 0.0414(13) Uani 1 1 d . . . H10 H 0.6802 0.9553 0.7968 0.050 Uiso 1 1 calc R . . C11 C 0.7011(4) 1.1047(4) 0.7753(4) 0.0454(14) Uani 1 1 d . . . H11 H 0.6790 1.1389 0.8194 0.054 Uiso 1 1 calc R . . C12 C 0.7383(4) 1.1440(4) 0.7119(4) 0.0420(13) Uani 1 1 d . . . H12 H 0.7473 1.2120 0.7031 0.050 Uiso 1 1 calc R . . N13 N 0.8683(3) 0.8684(3) 0.4766(3) 0.0345(10) Uani 1 1 d . . . N14 N 0.8416(3) 0.7989(3) 0.5286(3) 0.0364(10) Uani 1 1 d . . . C15 C 0.8694(4) 0.7133(4) 0.5033(4) 0.0429(13) Uani 1 1 d . . . H15 H 0.8609 0.6512 0.5285 0.051 Uiso 1 1 calc R . . C16 C 0.9125(4) 0.7283(5) 0.4348(5) 0.0480(15) Uani 1 1 d . . . H16 H 0.9374 0.6792 0.4045 0.058 Uiso 1 1 calc R . . C17 C 0.9122(4) 0.8270(4) 0.4195(4) 0.0416(13) Uani 1 1 d . . . H17 H 0.9376 0.8602 0.3773 0.050 Uiso 1 1 calc R . . N18 N 0.6679(3) 0.7341(3) 0.6074(3) 0.0302(9) Uani 1 1 d . . . C19 C 0.6897(4) 0.6576(4) 0.6635(4) 0.0340(11) Uani 1 1 d . . . C20 C 0.6376(4) 0.5756(4) 0.6622(4) 0.0403(13) Uani 1 1 d . . . H20 H 0.6546 0.5227 0.7038 0.048 Uiso 1 1 calc R . . C21 C 0.5595(4) 0.5754(4) 0.5967(4) 0.0419(13) Uani 1 1 d . . . H21 H 0.5220 0.5203 0.5925 0.050 Uiso 1 1 calc R . . C22 C 0.5345(4) 0.6534(4) 0.5371(4) 0.0372(12) Uani 1 1 d . . . H22 H 0.4811 0.6529 0.4919 0.045 Uiso 1 1 calc R . . C23 C 0.5902(3) 0.7311(3) 0.5464(3) 0.0308(11) Uani 1 1 d . . . N24 N 0.7722(3) 0.6692(3) 0.7255(3) 0.0333(9) Uani 1 1 d . . . N25 N 0.8178(3) 0.7537(3) 0.7213(3) 0.0343(10) Uani 1 1 d . . . C26 C 0.8908(4) 0.7428(4) 0.7860(4) 0.0394(12) Uani 1 1 d . . . H26 H 0.9363 0.7898 0.7993 0.047 Uiso 1 1 calc R . . C27 C 0.8922(4) 0.6534(4) 0.8322(4) 0.0424(13) Uani 1 1 d . . . H27 H 0.9371 0.6291 0.8810 0.051 Uiso 1 1 calc R . . C28 C 0.8153(4) 0.6083(4) 0.7923(4) 0.0388(12) Uani 1 1 d . . . H28 H 0.7960 0.5463 0.8083 0.047 Uiso 1 1 calc R . . N29 N 0.5733(3) 0.8171(3) 0.4930(3) 0.0332(9) Uani 1 1 d . . . N30 N 0.6358(3) 0.8888(3) 0.5073(3) 0.0321(9) Uani 1 1 d . . . C31 C 0.6017(4) 0.9611(4) 0.4512(4) 0.0407(13) Uani 1 1 d . . . H31 H 0.6297 1.0219 0.4469 0.049 Uiso 1 1 calc R . . C32 C 0.5180(4) 0.9359(4) 0.3985(4) 0.0425(13) Uani 1 1 d . . . H32 H 0.4807 0.9743 0.3526 0.051 Uiso 1 1 calc R . . C33 C 0.5026(4) 0.8451(4) 0.4277(4) 0.0383(12) Uani 1 1 d . . . H33 H 0.4511 0.8077 0.4061 0.046 Uiso 1 1 calc R . . I34 I 1.0000 0.99346(4) 0.7500 0.03579(14) Uani 1 2 d S . . I35 I 0.34381(3) 0.76351(3) 0.60061(3) 0.04655(13) Uani 1 1 d . . . I36 I 0.5000 0.77632(4) 0.7500 0.03889(15) Uani 1 2 d S . . I37 I 0.32221(3) 0.62643(3) 0.13843(3) 0.05517(15) Uani 1 1 d . . . I38 I 0.5000 0.63117(4) 0.2500 0.04252(15) Uani 1 2 d S . . I39A I 0.1576(8) 0.5628(6) 0.3987(6) 0.073(3) Uani 0.50 1 d PD A 1 I40A I 0.0000 0.5700(8) 0.2500 0.058(4) Uani 0.50 2 d SPD . 1 I39B I 0.1698(17) 0.5648(15) 0.4174(12) 0.069(3) Uani 0.25 1 d PD . 2 I40B I 0.0195(16) 0.5704(6) 0.2592(12) 0.0452(17) Uani 0.25 1 d PD . 2 I41B I -0.1359(9) 0.5717(13) 0.1059(15) 0.066(2) Uani 0.25 1 d PD . 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 0.0328(4) 0.0287(4) 0.0343(4) 0.0006(3) 0.0129(3) -0.0031(3) N2 0.029(2) 0.032(2) 0.028(2) 0.0048(17) 0.0060(17) -0.0031(17) C3 0.027(3) 0.031(3) 0.032(3) 0.003(2) 0.000(2) -0.002(2) C4 0.036(3) 0.034(3) 0.042(3) 0.003(2) 0.001(2) -0.002(2) C5 0.037(3) 0.041(3) 0.045(3) 0.014(2) 0.004(3) -0.011(2) C6 0.030(3) 0.051(3) 0.035(3) 0.009(2) 0.010(2) -0.004(2) C7 0.028(3) 0.038(3) 0.029(3) 0.003(2) 0.008(2) -0.002(2) N8 0.032(2) 0.031(2) 0.033(2) -0.0006(17) 0.0056(19) 0.0010(18) N9 0.038(3) 0.035(2) 0.034(2) 0.0003(18) 0.011(2) -0.0014(19) C10 0.040(3) 0.050(3) 0.037(3) -0.004(2) 0.014(3) 0.000(3) C11 0.045(3) 0.052(3) 0.040(3) -0.007(3) 0.012(3) 0.005(3) C12 0.042(3) 0.037(3) 0.044(3) -0.005(2) 0.006(3) 0.004(2) N13 0.028(2) 0.041(2) 0.033(2) -0.0009(19) 0.0060(18) -0.0032(19) N14 0.040(3) 0.027(2) 0.045(3) -0.0004(19) 0.017(2) -0.0025(19) C15 0.042(3) 0.042(3) 0.047(3) -0.007(3) 0.016(3) -0.001(2) C16 0.040(3) 0.054(4) 0.053(4) -0.017(3) 0.017(3) -0.002(3) C17 0.035(3) 0.054(3) 0.038(3) -0.007(3) 0.012(2) -0.001(3) N18 0.033(2) 0.029(2) 0.031(2) -0.0028(17) 0.0111(19) -0.0031(17) C19 0.037(3) 0.029(2) 0.036(3) -0.004(2) 0.009(2) 0.002(2) C20 0.050(4) 0.029(3) 0.040(3) 0.001(2) 0.006(3) -0.004(2) C21 0.045(3) 0.031(3) 0.049(3) -0.006(2) 0.009(3) -0.010(2) C22 0.035(3) 0.039(3) 0.036(3) -0.004(2) 0.006(2) -0.006(2) C23 0.035(3) 0.030(2) 0.028(3) -0.002(2) 0.009(2) -0.004(2) N24 0.036(2) 0.028(2) 0.036(2) 0.0001(18) 0.0089(19) -0.0015(18) N25 0.036(2) 0.034(2) 0.033(2) -0.0022(18) 0.010(2) -0.0077(19) C26 0.035(3) 0.047(3) 0.035(3) -0.003(2) 0.006(2) 0.000(2) C27 0.040(3) 0.047(3) 0.038(3) -0.001(2) 0.005(3) 0.008(3) C28 0.042(3) 0.031(3) 0.042(3) 0.003(2) 0.007(3) 0.006(2) N29 0.033(2) 0.032(2) 0.035(2) -0.0009(18) 0.0075(19) 0.0012(18) N30 0.037(2) 0.029(2) 0.032(2) 0.0006(17) 0.0112(19) -0.0008(18) C31 0.047(3) 0.036(3) 0.041(3) 0.008(2) 0.015(3) 0.003(2) C32 0.038(3) 0.052(3) 0.036(3) 0.005(2) 0.007(3) 0.002(3) C33 0.036(3) 0.042(3) 0.035(3) 0.002(2) 0.006(2) 0.001(2) I34 0.0288(3) 0.0475(3) 0.0311(3) 0.000 0.0075(2) 0.000 I35 0.0377(2) 0.0525(2) 0.0462(3) 0.00783(17) 0.00421(18) 0.00282(17) I36 0.0377(3) 0.0392(3) 0.0402(3) 0.000 0.0105(2) 0.000 I37 0.0511(3) 0.0565(3) 0.0566(3) 0.01566(19) 0.0108(2) -0.00066(19) I38 0.0538(3) 0.0331(3) 0.0446(3) 0.000 0.0194(3) 0.000 I39A 0.102(7) 0.039(2) 0.078(5) -0.006(3) 0.023(5) 0.016(3) I40A 0.070(10) 0.036(3) 0.085(6) 0.000 0.051(5) 0.000 I39B 0.114(7) 0.035(3) 0.053(3) -0.001(2) 0.011(3) 0.000(3) I40B 0.067(6) 0.024(3) 0.059(4) 0.0020(10) 0.045(3) 0.0051(17) I41B 0.067(3) 0.032(3) 0.098(5) 0.012(3) 0.017(3) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.141(4) . ? Fe1 N18 2.159(4) . ? Fe1 N25 2.171(5) . ? Fe1 N9 2.181(4) . ? Fe1 N14 2.185(5) . ? Fe1 N30 2.231(5) . ? N2 C3 1.331(6) . ? N2 C7 1.333(6) . ? C3 C4 1.380(7) . ? C3 N8 1.414(7) . ? C4 C5 1.388(8) . ? C5 C6 1.379(8) . ? C6 C7 1.391(7) . ? C7 N13 1.400(6) . ? N8 C12 1.354(7) . ? N8 N9 1.373(6) . ? N9 C10 1.330(7) . ? C10 C11 1.409(8) . ? C11 C12 1.355(9) . ? N13 C17 1.360(7) . ? N13 N14 1.362(6) . ? N14 C15 1.334(7) . ? C15 C16 1.392(9) . ? C16 C17 1.363(9) . ? N18 C19 1.334(7) . ? N18 C23 1.348(7) . ? C19 C20 1.386(8) . ? C19 N24 1.420(7) . ? C20 C21 1.384(9) . ? C21 C22 1.386(8) . ? C22 C23 1.363(7) . ? C23 N29 1.409(6) . ? N24 C28 1.354(7) . ? N24 N25 1.369(6) . ? N25 C26 1.329(7) . ? C26 C27 1.402(8) . ? C27 C28 1.368(8) . ? N29 C33 1.355(7) . ? N29 N30 1.372(6) . ? N30 C31 1.325(7) . ? C31 C32 1.413(8) . ? C32 C33 1.355(8) . ? I35 I36 2.9194(4) . ? I37 I38 2.9127(5) . ? I39A I40A 2.925(10) . ? I39B I40B 2.933(17) . ? I40B I41B 2.940(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N18 155.97(16) . . ? N2 Fe1 N25 129.20(16) . . ? N18 Fe1 N25 73.31(16) . . ? N2 Fe1 N9 73.22(16) . . ? N18 Fe1 N9 115.31(16) . . ? N25 Fe1 N9 99.32(16) . . ? N2 Fe1 N14 72.45(16) . . ? N18 Fe1 N14 102.44(16) . . ? N25 Fe1 N14 90.41(17) . . ? N9 Fe1 N14 142.24(17) . . ? N2 Fe1 N30 86.29(16) . . ? N18 Fe1 N30 71.62(16) . . ? N25 Fe1 N30 144.51(16) . . ? N9 Fe1 N30 90.82(16) . . ? N14 Fe1 N30 102.14(17) . . ? C3 N2 C7 119.1(4) . . ? C3 N2 Fe1 120.5(3) . . ? C7 N2 Fe1 120.4(3) . . ? N2 C3 C4 123.4(5) . . ? N2 C3 N8 113.3(4) . . ? C4 C3 N8 123.4(5) . . ? C3 C4 C5 116.4(5) . . ? C6 C5 C4 121.7(5) . . ? C5 C6 C7 116.8(5) . . ? N2 C7 C6 122.4(5) . . ? N2 C7 N13 113.0(4) . . ? C6 C7 N13 124.6(5) . . ? C12 N8 N9 111.0(4) . . ? C12 N8 C3 131.4(4) . . ? N9 N8 C3 117.5(4) . . ? C10 N9 N8 104.9(4) . . ? C10 N9 Fe1 139.9(4) . . ? N8 N9 Fe1 114.8(3) . . ? N9 C10 C11 111.0(5) . . ? C12 C11 C10 105.4(5) . . ? N8 C12 C11 107.8(5) . . ? C17 N13 N14 111.1(4) . . ? C17 N13 C7 130.6(5) . . ? N14 N13 C7 117.6(4) . . ? C15 N14 N13 105.6(5) . . ? C15 N14 Fe1 139.3(4) . . ? N13 N14 Fe1 114.6(3) . . ? N14 C15 C16 110.1(5) . . ? C17 C16 C15 106.8(5) . . ? N13 C17 C16 106.4(5) . . ? C19 N18 C23 117.4(4) . . ? C19 N18 Fe1 120.3(3) . . ? C23 N18 Fe1 122.3(3) . . ? N18 C19 C20 124.0(5) . . ? N18 C19 N24 112.6(4) . . ? C20 C19 N24 123.4(5) . . ? C21 C20 C19 116.1(5) . . ? C20 C21 C22 121.6(5) . . ? C23 C22 C21 117.0(5) . . ? N18 C23 C22 123.8(5) . . ? N18 C23 N29 112.2(4) . . ? C22 C23 N29 123.9(5) . . ? C28 N24 N25 111.9(5) . . ? C28 N24 C19 129.7(5) . . ? N25 N24 C19 118.4(4) . . ? C26 N25 N24 104.4(4) . . ? C26 N25 Fe1 140.3(4) . . ? N24 N25 Fe1 115.2(3) . . ? N25 C26 C27 111.6(5) . . ? C28 C27 C26 105.5(5) . . ? N24 C28 C27 106.7(5) . . ? C33 N29 N30 110.7(4) . . ? C33 N29 C23 131.0(5) . . ? N30 N29 C23 118.2(4) . . ? C31 N30 N29 105.1(4) . . ? C31 N30 Fe1 139.4(4) . . ? N29 N30 Fe1 115.4(3) . . ? N30 C31 C32 111.1(5) . . ? C33 C32 C31 105.1(5) . . ? C32 C33 N29 108.0(5) . . ? I35 I36 I35 173.15(2) . 2_656 ? I37 I38 I37 177.46(2) 2_655 . ? I39A I40A I39A 176.2(5) . 2 ? I39B I40B I41B 177.4(12) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C4 H4 I39A 0.95 3.04 3.932(10) 157.1 3_676 C4 H4 I39B 0.95 3.00 3.88(2) 154.0 3_676 C4 H4 I41B 0.95 2.96 3.830(19) 153.7 4_675 C6 H6 I34 0.95 3.05 3.999(5) 174.6 3_776 C10 H10 I35 0.95 3.11 4.022(6) 161.9 2_656 C11 H11 I37 0.95 3.26 3.933(6) 129.7 3_676 C15 H15 I39A 0.95 3.15 4.100(11) 175.1 3_666 C15 H15 I39B 0.95 3.12 4.06(2) 171.7 3_666 C15 H15 I41B 0.95 3.25 4.19(2) 169.9 4_665 C16 H16 I40A 0.95 3.13 4.038(8) 160.2 1_655 C16 H16 I40B 0.95 3.18 4.10(2) 161.9 1_655 C17 H17 I34 0.95 3.10 4.033(6) 168.0 3_776 C20 H20 I37 0.95 3.08 4.013(5) 166.1 3_666 C21 H21 I38 0.95 3.23 3.905(6) 129.4 3_666 C26 H26 I34 0.95 3.10 3.926(6) 145.9 . C28 H28 I37 0.95 3.23 4.150(6) 162.6 3_666 C31 H31 I35 0.95 3.06 3.968(6) 160.3 3_676 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.654 _refine_diff_density_min -2.338 _refine_diff_density_rms 0.302 #=END data_c:\datasets\leeds\mh143v~1\mh1433~1\mh143300 _database_code_depnum_ccdc_archive 'CCDC 278898' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) bis[di(dicarbollido)cobalt(III)] nitromethane solvate (1/0.75) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H18 Fe N10, 2[C4 H22 B18 Co], 0.75[C H3 N O2]' _chemical_formula_sum 'C30.75 H64.25 B36 Co2 Fe N10.75 O1.50' _chemical_formula_weight 1171.55 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 37.297(2) _cell_length_b 10.5955(6) _cell_length_c 29.6321(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11710.1(12) _cell_formula_units_Z 8 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 146512 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 23.95 _exptl_crystal_description Needle _exptl_crystal_colour Orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4768 _exptl_absorpt_coefficient_mu 0.847 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.756 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 4 kW. ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 146512 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 23.95 _reflns_number_total 18205 _reflns_number_gt 16344 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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. The crystal was refined as a racemic twin. The asymmetric unit contains two complex dications, four cobalticarborane anions and two nitromethane molecules. Both the solvent molecules are disordered, over two orientations: C126-O129 (occupancy 0.5) and C130-O133(occupancy 0.40) and C134-O137 (occupancy 0.3) and C138-O141(occupancy 0.3) This gives a total solvent content of 1.5 molecules per asymmetric unit, or 0.75 per formula unit. The following restraints were applied to these partial solvent molecules: C---N = 1.45(2), N---O = 1.15(2), C...O = 2.30(2) and O...O = 1.88(2)\%A. All non-H atoms except the disordered solvent were refined anisotropically. All H atoms were placed in calculated positions and refined using a riding model. The (partially occupied) methyl torsions in the solvent were refined in a fixed, staggered conformation. There is one notable residual Fourier peak of 1.3 e.\%A^-3^, lying 1.0 \%A from Fe1A. ; _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^)+(0.0682P)^2^+6.0839P] 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 0.496(11) _refine_ls_number_reflns 18205 _refine_ls_number_parameters 1488 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1169 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.002 _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 Fe1A Fe 0.941126(18) 0.29525(7) 0.21411(2) 0.05885(18) Uani 1 1 d . . . N2A N 0.98610(11) 0.2671(4) 0.24825(18) 0.0702(12) Uani 1 1 d . . . C3A C 1.01544(18) 0.2333(6) 0.2254(3) 0.101(3) Uani 1 1 d . . . C4A C 1.0465(2) 0.2138(7) 0.2461(5) 0.125(3) Uani 1 1 d . . . H4A H 1.0669 0.1928 0.2296 0.150 Uiso 1 1 calc R . . C5A C 1.0481(2) 0.2250(8) 0.2912(5) 0.143(5) Uani 1 1 d . . . H5A H 1.0695 0.2065 0.3059 0.171 Uiso 1 1 calc R . . C6A C 1.01729(19) 0.2652(6) 0.3178(3) 0.104(3) Uani 1 1 d . . . H6A H 1.0185 0.2781 0.3488 0.125 Uiso 1 1 calc R . . C7A C 0.98612(15) 0.2829(4) 0.2934(2) 0.0677(15) Uani 1 1 d . . . N8A N 1.00800(17) 0.2311(6) 0.1774(3) 0.104(2) Uani 1 1 d . . . N9A N 0.97340(18) 0.2584(6) 0.1635(2) 0.0968(17) Uani 1 1 d . . . C10A C 0.9749(3) 0.2583(10) 0.1183(3) 0.131(3) Uani 1 1 d . . . H10A H 0.9557 0.2749 0.0991 0.158 Uiso 1 1 calc R . . C11A C 1.0097(4) 0.2295(14) 0.1044(6) 0.202(8) Uani 1 1 d . . . H11A H 1.0173 0.2179 0.0748 0.242 Uiso 1 1 calc R . . C12A C 1.0306(3) 0.2216(12) 0.1419(6) 0.174(6) Uani 1 1 d . . . H12A H 1.0553 0.2116 0.1430 0.208 Uiso 1 1 calc R . . N13A N 0.95272(12) 0.3183(4) 0.30951(15) 0.0629(11) Uani 1 1 d . . . N14A N 0.92586(11) 0.3348(4) 0.27832(14) 0.0630(11) Uani 1 1 d . . . C15A C 0.89784(17) 0.3724(5) 0.3017(2) 0.0766(15) Uani 1 1 d . . . H15A H 0.8757 0.3919 0.2891 0.092 Uiso 1 1 calc R . . C16A C 0.9054(2) 0.3793(6) 0.3466(2) 0.0840(17) Uani 1 1 d . . . H16A H 0.8897 0.4023 0.3696 0.101 Uiso 1 1 calc R . . C17A C 0.9396(2) 0.3464(6) 0.35109(19) 0.0867(19) Uani 1 1 d . . . H17A H 0.9523 0.3433 0.3780 0.104 Uiso 1 1 calc R . . N18A N 0.89439(11) 0.3161(5) 0.18364(13) 0.0610(11) Uani 1 1 d . . . C19A C 0.87130(13) 0.2198(6) 0.18163(16) 0.0669(15) Uani 1 1 d . . . C20A C 0.83745(16) 0.2349(10) 0.1620(2) 0.101(3) Uani 1 1 d . . . H20A H 0.8213 0.1683 0.1606 0.121 Uiso 1 1 calc R . . C21A C 0.8291(2) 0.3511(13) 0.1451(3) 0.134(4) Uani 1 1 d . . . H21A H 0.8066 0.3638 0.1323 0.160 Uiso 1 1 calc R . . C22A C 0.8529(2) 0.4494(10) 0.1467(2) 0.116(3) Uani 1 1 d . . . H22A H 0.8474 0.5279 0.1344 0.140 Uiso 1 1 calc R . . C23A C 0.8849(2) 0.4262(7) 0.16699(19) 0.0821(17) Uani 1 1 d . . . N24A N 0.88518(12) 0.1124(5) 0.20017(15) 0.0674(11) Uani 1 1 d . . . N25A N 0.91938(11) 0.1199(5) 0.21808(15) 0.0664(11) Uani 1 1 d . . . C26A C 0.9268(2) 0.0069(7) 0.2347(2) 0.0896(19) Uani 1 1 d . . . H26A H 0.9481 -0.0148 0.2490 0.108 Uiso 1 1 calc R . . C27A C 0.8983(3) -0.0742(8) 0.2278(3) 0.108(2) Uani 1 1 d . . . H27A H 0.8969 -0.1583 0.2366 0.129 Uiso 1 1 calc R . . C28A C 0.8723(2) -0.0073(8) 0.2055(2) 0.103(3) Uani 1 1 d . . . H28A H 0.8502 -0.0376 0.1958 0.123 Uiso 1 1 calc R . . N29A N 0.91199(19) 0.5161(5) 0.17315(16) 0.0928(18) Uani 1 1 d . . . N30A N 0.94273(17) 0.4811(5) 0.19687(18) 0.0941(16) Uani 1 1 d . . . C31A C 0.9635(3) 0.5794(8) 0.1997(3) 0.121(3) Uani 1 1 d . . . H31A H 0.9860 0.5811 0.2133 0.145 Uiso 1 1 calc R . . C32A C 0.9463(4) 0.6845(10) 0.1786(4) 0.153(5) Uani 1 1 d . . . H32A H 0.9553 0.7661 0.1762 0.184 Uiso 1 1 calc R . . C33A C 0.9141(4) 0.6421(9) 0.1626(3) 0.143(4) Uani 1 1 d . . . H33A H 0.8969 0.6895 0.1474 0.172 Uiso 1 1 calc R . . Fe1B Fe 0.793894(17) 0.21441(8) 0.44908(2) 0.05825(19) Uani 1 1 d . . . N2B N 0.84407(14) 0.1812(7) 0.48104(15) 0.0898(18) Uani 1 1 d . . . C3B C 0.8515(3) 0.0718(14) 0.4961(2) 0.131(4) Uani 1 1 d . . . C4B C 0.8857(3) 0.0389(18) 0.5134(3) 0.219(11) Uani 1 1 d . . . H4B H 0.8895 -0.0411 0.5254 0.263 Uiso 1 1 calc R . . C5B C 0.9100(4) 0.115(3) 0.5125(5) 0.253(13) Uani 1 1 d . . . H5B H 0.9325 0.0927 0.5236 0.304 Uiso 1 1 calc R . . C6B C 0.9044(2) 0.2414(16) 0.4945(3) 0.181(7) Uani 1 1 d . . . H6B H 0.9230 0.3000 0.4929 0.217 Uiso 1 1 calc R . . C7B C 0.86980(16) 0.2701(12) 0.4797(3) 0.112(4) Uani 1 1 d . . . N8B N 0.8231(2) -0.0162(7) 0.49445(18) 0.111(2) Uani 1 1 d . . . N9B N 0.79055(16) 0.0247(6) 0.47608(16) 0.0848(14) Uani 1 1 d . . . C10B C 0.7686(3) -0.0682(9) 0.4771(3) 0.128(3) Uani 1 1 d . . . H10B H 0.7448 -0.0657 0.4678 0.154 Uiso 1 1 calc R . . C11B C 0.7862(7) -0.1738(17) 0.4945(6) 0.221(13) Uani 1 1 d . . . H11B H 0.7765 -0.2542 0.4976 0.265 Uiso 1 1 calc R . . C12B C 0.8156(6) -0.1429(14) 0.5046(5) 0.211(12) Uani 1 1 d . . . H12B H 0.8322 -0.1971 0.5180 0.253 Uiso 1 1 calc R . . N13B N 0.85768(17) 0.3808(9) 0.4634(2) 0.114(3) Uani 1 1 d . . . N14B N 0.82306(14) 0.3902(6) 0.44883(17) 0.0876(16) Uani 1 1 d . . . C15B C 0.8210(3) 0.5074(8) 0.4359(2) 0.113(3) Uani 1 1 d . . . H15B H 0.8004 0.5430 0.4236 0.136 Uiso 1 1 calc R . . C16B C 0.8525(5) 0.5733(15) 0.4421(5) 0.198(10) Uani 1 1 d . . . H16B H 0.8564 0.6585 0.4363 0.238 Uiso 1 1 calc R . . C17B C 0.8751(3) 0.4944(16) 0.4572(5) 0.174(9) Uani 1 1 d . . . H17B H 0.8992 0.5103 0.4630 0.209 Uiso 1 1 calc R . . N18B N 0.75275(9) 0.2365(3) 0.39979(12) 0.0442(8) Uani 1 1 d . . . C19B C 0.72108(11) 0.2781(4) 0.41151(15) 0.0460(10) Uani 1 1 d . . . C20B C 0.69228(12) 0.2827(5) 0.38248(17) 0.0557(12) Uani 1 1 d . . . H20B H 0.6698 0.3094 0.3921 0.067 Uiso 1 1 calc R . . C21B C 0.69826(12) 0.2458(5) 0.33805(16) 0.0571(12) Uani 1 1 d . . . H21B H 0.6797 0.2492 0.3172 0.068 Uiso 1 1 calc R . . C22B C 0.73134(13) 0.2046(5) 0.32509(16) 0.0551(12) Uani 1 1 d . . . H22B H 0.7358 0.1798 0.2955 0.066 Uiso 1 1 calc R . . C23B C 0.75779(11) 0.2009(4) 0.35716(14) 0.0434(9) Uani 1 1 d . . . N24B N 0.71923(9) 0.3210(4) 0.45638(13) 0.0516(9) Uani 1 1 d . . . N25B N 0.74851(11) 0.2990(4) 0.48368(14) 0.0660(11) Uani 1 1 d . . . C26B C 0.73993(17) 0.3557(7) 0.5218(2) 0.091(2) Uani 1 1 d . . . H26B H 0.7546 0.3577 0.5472 0.109 Uiso 1 1 calc R . . C27B C 0.70610(18) 0.4123(7) 0.5196(2) 0.095(2) Uani 1 1 d . . . H27B H 0.6944 0.4575 0.5421 0.114 Uiso 1 1 calc R . . C28B C 0.69417(14) 0.3876(6) 0.47813(19) 0.0730(15) Uani 1 1 d . . . H28B H 0.6722 0.4124 0.4663 0.088 Uiso 1 1 calc R . . N29B N 0.79353(9) 0.1628(4) 0.34833(12) 0.0486(8) Uani 1 1 d . . . N30B N 0.81659(11) 0.1505(4) 0.38408(13) 0.0598(10) Uani 1 1 d . . . C31B C 0.84654(14) 0.1121(6) 0.36570(18) 0.0729(16) Uani 1 1 d . . . H31B H 0.8672 0.0945 0.3820 0.087 Uiso 1 1 calc R . . C32B C 0.84404(16) 0.1005(6) 0.3195(2) 0.0798(16) Uani 1 1 d . . . H32B H 0.8620 0.0763 0.2996 0.096 Uiso 1 1 calc R . . C33B C 0.80971(13) 0.1318(5) 0.30948(17) 0.0582(12) Uani 1 1 d . . . H33B H 0.7993 0.1319 0.2809 0.070 Uiso 1 1 calc R . . Co34 Co 0.735733(14) -0.30195(5) 0.31329(2) 0.04376(14) Uani 1 1 d . . . C35 C 0.75476(13) -0.4311(5) 0.26773(16) 0.0557(11) Uani 1 1 d . . . H35 H 0.7320 -0.4903 0.2572 0.067 Uiso 1 1 calc R . . C36 C 0.75902(13) -0.2863(5) 0.25075(17) 0.0574(12) Uani 1 1 d . . . H36 H 0.7391 -0.2431 0.2282 0.069 Uiso 1 1 calc R . . B37 B 0.77941(15) -0.1958(6) 0.2904(2) 0.0614(15) Uani 1 1 d . . . H37 H 0.7751 -0.0941 0.2954 0.074 Uiso 1 1 calc R . . B38 B 0.78889(14) -0.2989(6) 0.3370(2) 0.0598(15) Uani 1 1 d . . . H38 H 0.7912 -0.2679 0.3723 0.072 Uiso 1 1 calc R . . B39 B 0.77156(13) -0.4520(5) 0.32095(18) 0.0534(12) Uani 1 1 d . . . H39 H 0.7621 -0.5215 0.3458 0.064 Uiso 1 1 calc R . . B40 B 0.78600(16) -0.3975(7) 0.2267(2) 0.0711(17) Uani 1 1 d . . . H40 H 0.7846 -0.4290 0.1914 0.085 Uiso 1 1 calc R . . B41 B 0.80155(17) -0.2478(8) 0.2416(3) 0.080(2) Uani 1 1 d . . . H41 H 0.8104 -0.1809 0.2155 0.096 Uiso 1 1 calc R . . B42 B 0.82240(15) -0.2583(7) 0.2955(2) 0.0716(17) Uani 1 1 d . . . H42 H 0.8454 -0.1988 0.3047 0.086 Uiso 1 1 calc R . . B43 B 0.81815(16) -0.4175(7) 0.3138(2) 0.0696(16) Uani 1 1 d . . . H43 H 0.8385 -0.4630 0.3351 0.083 Uiso 1 1 calc R . . B44 B 0.79549(15) -0.5009(7) 0.2709(2) 0.0672(16) Uani 1 1 d . . . H44 H 0.8005 -0.6015 0.2641 0.081 Uiso 1 1 calc R . . B45 B 0.82693(17) -0.3854(8) 0.2562(2) 0.081(2) Uani 1 1 d . . . H45 H 0.8528 -0.4088 0.2406 0.098 Uiso 1 1 calc R . . C46 C 0.68341(11) -0.2845(4) 0.29317(16) 0.0505(11) Uani 1 1 d . . . H46 H 0.6825 -0.3053 0.2568 0.061 Uiso 1 1 calc R . . C47 C 0.70060(12) -0.1554(4) 0.31193(19) 0.0575(12) Uani 1 1 d . . . H47 H 0.7119 -0.0840 0.2890 0.069 Uiso 1 1 calc R . . B48 B 0.72027(15) -0.1756(6) 0.3634(2) 0.0582(14) Uani 1 1 d . . . H48 H 0.7432 -0.1218 0.3768 0.070 Uiso 1 1 calc R . . B49 B 0.71259(15) -0.3393(5) 0.37668(18) 0.0534(13) Uani 1 1 d . . . H49 H 0.7302 -0.3944 0.3990 0.064 Uiso 1 1 calc R . . B50 B 0.68972(14) -0.4042(5) 0.32903(19) 0.0532(13) Uani 1 1 d . . . H50 H 0.6928 -0.5039 0.3194 0.064 Uiso 1 1 calc R . . B51 B 0.65501(15) -0.1700(6) 0.3111(2) 0.0682(16) Uani 1 1 d . . . H51 H 0.6369 -0.1150 0.2894 0.082 Uiso 1 1 calc R . . B52 B 0.67732(15) -0.1036(6) 0.3569(3) 0.0673(16) Uani 1 1 d . . . H52 H 0.6734 -0.0035 0.3655 0.081 Uiso 1 1 calc R . . B53 B 0.68345(16) -0.2204(6) 0.3987(2) 0.0668(16) Uani 1 1 d . . . H53 H 0.6834 -0.1985 0.4350 0.080 Uiso 1 1 calc R . . B54 B 0.66441(16) -0.3613(6) 0.3773(2) 0.0649(16) Uani 1 1 d . . . H54 H 0.6518 -0.4321 0.3994 0.078 Uiso 1 1 calc R . . B55 B 0.64754(14) -0.3289(6) 0.3230(2) 0.0617(15) Uani 1 1 d . . . H55 H 0.6242 -0.3787 0.3090 0.074 Uiso 1 1 calc R . . B56 B 0.64345(16) -0.2154(6) 0.3665(2) 0.0661(16) Uani 1 1 d . . . H56 H 0.6175 -0.1904 0.3818 0.079 Uiso 1 1 calc R . . Co57 Co 0.667489(15) 0.35235(6) 0.147816(19) 0.04688(14) Uani 1 1 d . . . C58 C 0.63920(15) 0.4886(5) 0.18170(18) 0.0681(14) Uani 1 1 d . . . H58 H 0.6375 0.4582 0.2171 0.082 Uiso 1 1 calc R . . C59 C 0.61652(14) 0.4217(5) 0.1434(2) 0.0760(16) Uani 1 1 d . . . H59 H 0.5985 0.3428 0.1518 0.091 Uiso 1 1 calc R . . B60 B 0.6387(2) 0.4226(6) 0.0931(2) 0.079(2) Uani 1 1 d . . . H60 H 0.6364 0.3509 0.0664 0.095 Uiso 1 1 calc R . . B61 B 0.6795(2) 0.5036(6) 0.1042(2) 0.0719(18) Uani 1 1 d . . . H61 H 0.7043 0.4892 0.0849 0.086 Uiso 1 1 calc R . . B62 B 0.67901(17) 0.5393(6) 0.1630(2) 0.0671(16) Uani 1 1 d . . . H62 H 0.7037 0.5464 0.1830 0.081 Uiso 1 1 calc R . . B63 B 0.60184(18) 0.5669(7) 0.1604(3) 0.081(2) Uani 1 1 d . . . H63 H 0.5765 0.5862 0.1782 0.097 Uiso 1 1 calc R . . B64 B 0.6026(2) 0.5270(8) 0.1038(3) 0.093(2) Uani 1 1 d . . . H64 H 0.5773 0.5201 0.0848 0.112 Uiso 1 1 calc R . . B65 B 0.6420(2) 0.5827(7) 0.0796(2) 0.080(2) Uani 1 1 d . . . H65 H 0.6426 0.6139 0.0442 0.096 Uiso 1 1 calc R . . B66 B 0.6670(2) 0.6571(7) 0.1232(3) 0.0803(19) Uani 1 1 d . . . H66 H 0.6845 0.7389 0.1172 0.096 Uiso 1 1 calc R . . B67 B 0.6417(2) 0.6428(6) 0.1730(2) 0.0773(19) Uani 1 1 d . . . H67 H 0.6422 0.7131 0.2003 0.093 Uiso 1 1 calc R . . B68 B 0.6211(2) 0.6737(6) 0.1212(2) 0.0749(18) Uani 1 1 d . . . H68 H 0.6091 0.7658 0.1131 0.090 Uiso 1 1 calc R . . C69 C 0.65837(13) 0.1989(4) 0.18840(15) 0.0513(11) Uani 1 1 d . . . H69 H 0.6333 0.2170 0.2068 0.062 Uiso 1 1 calc R . . C70 C 0.65868(15) 0.1646(5) 0.13560(16) 0.0604(13) Uani 1 1 d . . . H70 H 0.6334 0.1577 0.1166 0.073 Uiso 1 1 calc R . . B71 B 0.69503(19) 0.2229(6) 0.1085(2) 0.0676(16) Uani 1 1 d . . . H71 H 0.6963 0.2533 0.0730 0.081 Uiso 1 1 calc R . . B72 B 0.72120(17) 0.2963(6) 0.1528(2) 0.0657(15) Uani 1 1 d . . . H72 H 0.7403 0.3734 0.1467 0.079 Uiso 1 1 calc R . . B73 B 0.69475(16) 0.2811(6) 0.20343(18) 0.0582(14) Uani 1 1 d . . . H73 H 0.6960 0.3508 0.2309 0.070 Uiso 1 1 calc R . . B74 B 0.66577(19) 0.0438(6) 0.1722(2) 0.0673(16) Uani 1 1 d . . . H74 H 0.6476 -0.0364 0.1779 0.081 Uiso 1 1 calc R . . B75 B 0.6904(2) 0.0586(6) 0.1225(2) 0.0745(18) Uani 1 1 d . . . H75 H 0.6885 -0.0129 0.0957 0.089 Uiso 1 1 calc R . . B76 B 0.7307(2) 0.1373(7) 0.1354(2) 0.0808(19) Uani 1 1 d . . . H76 H 0.7557 0.1154 0.1171 0.097 Uiso 1 1 calc R . . B77 B 0.73061(18) 0.1748(6) 0.1936(2) 0.0688(16) Uani 1 1 d . . . H77 H 0.7554 0.1782 0.2138 0.083 Uiso 1 1 calc R . . B78 B 0.68958(17) 0.1181(6) 0.21598(19) 0.0620(14) Uani 1 1 d . . . H78 H 0.6868 0.0852 0.2510 0.074 Uiso 1 1 calc R . . B79 B 0.7126(2) 0.0281(7) 0.1751(2) 0.0800(19) Uani 1 1 d . . . H79 H 0.7256 -0.0624 0.1831 0.096 Uiso 1 1 calc R . . Co80 Co 0.580211(16) -0.14454(6) 0.507011(19) 0.04834(15) Uani 1 1 d . . . C81 C 0.61360(14) -0.0192(5) 0.47581(17) 0.0640(13) Uani 1 1 d . . . H81 H 0.6195 -0.0579 0.4422 0.077 Uiso 1 1 calc R . . C82 C 0.63121(15) -0.0826(6) 0.5204(2) 0.0720(15) Uani 1 1 d . . . H82 H 0.6491 -0.1649 0.5184 0.086 Uiso 1 1 calc R . . B83 B 0.6036(2) -0.0697(6) 0.5656(2) 0.0744(19) Uani 1 1 d . . . H83 H 0.6025 -0.1358 0.5942 0.089 Uiso 1 1 calc R . . B84 B 0.56469(18) 0.0126(6) 0.5452(2) 0.0634(15) Uani 1 1 d . . . H84 H 0.5380 0.0016 0.5605 0.076 Uiso 1 1 calc R . . B85 B 0.57281(16) 0.0406(6) 0.48597(19) 0.0591(14) Uani 1 1 d . . . H85 H 0.5511 0.0469 0.4610 0.071 Uiso 1 1 calc R . . B86 B 0.6483(2) 0.0621(8) 0.5010(3) 0.089(2) Uani 1 1 d . . . H86 H 0.6751 0.0776 0.4866 0.107 Uiso 1 1 calc R . . B87 B 0.6415(2) 0.0296(8) 0.5581(3) 0.089(2) Uani 1 1 d . . . H87 H 0.6646 0.0234 0.5811 0.106 Uiso 1 1 calc R . . B88 B 0.5994(3) 0.0963(7) 0.5736(2) 0.097(3) Uani 1 1 d . . . H88 H 0.5948 0.1370 0.6073 0.117 Uiso 1 1 calc R . . B89 B 0.5797(2) 0.1619(6) 0.5247(3) 0.078(2) Uani 1 1 d . . . H89 H 0.5618 0.2443 0.5258 0.093 Uiso 1 1 calc R . . B90 B 0.6105(2) 0.1400(6) 0.4804(2) 0.0779(19) Uani 1 1 d . . . H90 H 0.6130 0.2070 0.4522 0.093 Uiso 1 1 calc R . . B91 B 0.6265(2) 0.1747(7) 0.5347(3) 0.085(2) Uani 1 1 d . . . H91 H 0.6391 0.2655 0.5431 0.102 Uiso 1 1 calc R . . C92 C 0.59155(16) -0.3008(5) 0.4694(2) 0.0684(14) Uani 1 1 d . . . H92 H 0.6180 -0.2854 0.4539 0.082 Uiso 1 1 calc R . . C93 C 0.58801(18) -0.3298(5) 0.5229(2) 0.0792(17) Uani 1 1 d . . . H93 H 0.6118 -0.3372 0.5447 0.095 Uiso 1 1 calc R . . B94 B 0.54908(17) -0.2677(6) 0.5447(2) 0.0634(15) Uani 1 1 d . . . H94 H 0.5454 -0.2335 0.5795 0.076 Uiso 1 1 calc R . . B95 B 0.52668(16) -0.2011(6) 0.49637(19) 0.0594(14) Uani 1 1 d . . . H95 H 0.5074 -0.1229 0.4988 0.071 Uiso 1 1 calc R . . B96 B 0.55617(16) -0.2213(6) 0.45097(19) 0.0607(14) Uani 1 1 d . . . H96 H 0.5570 -0.1527 0.4231 0.073 Uiso 1 1 calc R . . B97 B 0.5813(2) -0.4535(7) 0.4844(3) 0.094(2) Uani 1 1 d . . . H97 H 0.5990 -0.5355 0.4800 0.113 Uiso 1 1 calc R . . B98 B 0.5534(2) -0.4312(6) 0.5329(3) 0.083(2) Uani 1 1 d . . . H98 H 0.5531 -0.4996 0.5608 0.099 Uiso 1 1 calc R . . B99 B 0.5144(2) -0.3533(7) 0.5156(3) 0.081(2) Uani 1 1 d . . . H99 H 0.4881 -0.3706 0.5313 0.097 Uiso 1 1 calc R . . B100 B 0.5196(2) -0.3244(8) 0.4569(3) 0.082(2) Uani 1 1 d . . . H100 H 0.4966 -0.3232 0.4338 0.098 Uiso 1 1 calc R . . B101 B 0.5610(2) -0.3838(7) 0.4388(3) 0.091(2) Uani 1 1 d . . . H101 H 0.5655 -0.4192 0.4043 0.110 Uiso 1 1 calc R . . B102 B 0.5357(2) -0.4667(7) 0.4799(3) 0.091(2) Uani 1 1 d . . . H102 H 0.5230 -0.5584 0.4729 0.109 Uiso 1 1 calc R . . Co10 Co 0.508814(14) 0.21008(5) 0.34965(2) 0.04404(14) Uani 1 1 d . . . C104 C 0.54584(11) 0.3516(4) 0.35017(19) 0.0537(11) Uani 1 1 d . . . H104 H 0.5370 0.4217 0.3752 0.064 Uiso 1 1 calc R . . C105 C 0.56215(11) 0.2168(4) 0.36529(16) 0.0515(11) Uani 1 1 d . . . H105 H 0.5646 0.1917 0.4012 0.062 Uiso 1 1 calc R . . B106 B 0.55239(14) 0.1013(5) 0.3280(2) 0.0589(14) Uani 1 1 d . . . H106 H 0.5486 0.0009 0.3362 0.071 Uiso 1 1 calc R . . B107 B 0.52767(16) 0.1764(6) 0.2838(2) 0.0630(15) Uani 1 1 d . . . H107 H 0.5082 0.1269 0.2623 0.076 Uiso 1 1 calc R . . B108 B 0.52276(15) 0.3411(6) 0.3007(2) 0.0613(15) Uani 1 1 d . . . H108 H 0.4998 0.3998 0.2904 0.074 Uiso 1 1 calc R . . B109 B 0.59183(13) 0.3298(5) 0.3463(2) 0.0602(14) Uani 1 1 d . . . H109 H 0.6123 0.3785 0.3666 0.072 Uiso 1 1 calc R . . B110 B 0.59598(14) 0.1689(6) 0.3312(2) 0.0606(15) Uani 1 1 d . . . H110 H 0.6193 0.1129 0.3419 0.073 Uiso 1 1 calc R . . B111 B 0.57507(16) 0.1470(7) 0.2787(2) 0.0698(17) Uani 1 1 d . . . H111 H 0.5853 0.0771 0.2544 0.084 Uiso 1 1 calc R . . B112 B 0.55686(17) 0.2951(8) 0.2612(2) 0.0746(19) Uani 1 1 d . . . H112 H 0.5552 0.3221 0.2254 0.089 Uiso 1 1 calc R . . B113 B 0.56676(15) 0.4062(6) 0.3047(3) 0.0727(18) Uani 1 1 d . . . H113 H 0.5711 0.5071 0.2979 0.087 Uiso 1 1 calc R . . B114 B 0.59883(17) 0.2899(6) 0.2902(2) 0.0692(16) Uani 1 1 d . . . H114 H 0.6241 0.3135 0.2731 0.083 Uiso 1 1 calc R . . C115 C 0.48838(12) 0.2270(5) 0.41299(17) 0.0588(12) Uani 1 1 d . . . H115 H 0.5099 0.2673 0.4338 0.071 Uiso 1 1 calc R . . C116 C 0.49041(13) 0.0839(5) 0.39592(17) 0.0579(12) Uani 1 1 d . . . H116 H 0.5131 0.0223 0.4047 0.070 Uiso 1 1 calc R . . B117 B 0.47101(13) 0.0647(5) 0.3447(2) 0.0560(13) Uani 1 1 d . . . H117 H 0.4786 -0.0060 0.3193 0.067 Uiso 1 1 calc R . . B118 B 0.45424(14) 0.2215(5) 0.3303(2) 0.0551(13) Uani 1 1 d . . . H118 H 0.4504 0.2545 0.2955 0.066 Uiso 1 1 calc R . . B119 B 0.46752(14) 0.3221(6) 0.3761(2) 0.0622(15) Uani 1 1 d . . . H119 H 0.4730 0.4233 0.3716 0.075 Uiso 1 1 calc R . . B120 B 0.46145(16) 0.1205(7) 0.4393(2) 0.0757(18) Uani 1 1 d . . . H120 H 0.4642 0.0891 0.4745 0.091 Uiso 1 1 calc R . . B121 B 0.44922(16) 0.0166(7) 0.3955(2) 0.0735(18) Uani 1 1 d . . . H121 H 0.4438 -0.0835 0.4026 0.088 Uiso 1 1 calc R . . B122 B 0.42538(14) 0.1063(6) 0.3543(2) 0.0678(16) Uani 1 1 d . . . H122 H 0.4038 0.0642 0.3340 0.081 Uiso 1 1 calc R . . B123 B 0.42387(15) 0.2635(6) 0.3735(2) 0.0668(16) Uani 1 1 d . . . H123 H 0.4012 0.3265 0.3658 0.080 Uiso 1 1 calc R . . B124 B 0.44591(17) 0.2689(8) 0.4258(3) 0.0789(19) Uani 1 1 d . . . H124 H 0.4382 0.3346 0.4529 0.095 Uiso 1 1 calc R . . B125 B 0.41928(16) 0.1390(8) 0.4122(2) 0.0755(18) Uani 1 1 d . . . H125 H 0.3937 0.1193 0.4292 0.091 Uiso 1 1 calc R . . C126 C 0.7703(4) -0.1829(14) 0.1051(4) 0.090(4) Uiso 0.50 1 d PD A 1 H12C H 0.7504 -0.1548 0.0872 0.134 Uiso 0.50 1 calc PR A 1 H12D H 0.7844 -0.1115 0.1142 0.134 Uiso 0.50 1 calc PR A 1 H12E H 0.7615 -0.2261 0.1314 0.134 Uiso 0.50 1 calc PR A 1 N127 N 0.7929(4) -0.2702(13) 0.0781(5) 0.108(4) Uiso 0.50 1 d PD A 1 O128 O 0.7937(4) -0.2574(14) 0.0394(4) 0.147(5) Uiso 0.50 1 d PD A 1 O129 O 0.8188(4) -0.3092(17) 0.0924(5) 0.139(5) Uiso 0.50 1 d PD A 1 C130 C 0.7626(4) -0.239(2) 0.1078(7) 0.103(6) Uiso 0.40 1 d PD B 2 H13A H 0.7514 -0.2633 0.0800 0.155 Uiso 0.40 1 calc PR B 2 H13B H 0.7568 -0.1533 0.1147 0.155 Uiso 0.40 1 calc PR B 2 H13C H 0.7541 -0.2931 0.1317 0.155 Uiso 0.40 1 calc PR B 2 N131 N 0.8012(4) -0.2527(15) 0.1037(5) 0.097(4) Uiso 0.40 1 d PD B 2 O132 O 0.8247(4) -0.2320(15) 0.1253(5) 0.129(5) Uiso 0.40 1 d PD B 2 O133 O 0.8096(6) -0.338(2) 0.0789(9) 0.197(12) Uiso 0.40 1 d PD B 2 C134 C 0.5184(5) 0.0636(19) 0.1702(7) 0.083(5) Uiso 0.30 1 d PD C 1 H13D H 0.5305 -0.0070 0.1836 0.125 Uiso 0.30 1 calc PR C 1 H13E H 0.4970 0.0349 0.1555 0.125 Uiso 0.30 1 calc PR C 1 H13F H 0.5123 0.1236 0.1932 0.125 Uiso 0.30 1 calc PR C 1 N135 N 0.5408(6) 0.120(2) 0.1387(8) 0.105(8) Uiso 0.30 1 d PD C 1 O136 O 0.5655(6) 0.076(3) 0.1215(10) 0.169(10) Uiso 0.30 1 d PD C 1 O137 O 0.5310(7) 0.210(2) 0.1184(8) 0.168(9) Uiso 0.30 1 d PD C 1 C138 C 0.5147(5) 0.113(2) 0.1453(9) 0.102(7) Uiso 0.30 1 d PD D 2 H13G H 0.5017 0.1702 0.1261 0.153 Uiso 0.30 1 calc PR D 2 H13H H 0.5134 0.1421 0.1759 0.153 Uiso 0.30 1 calc PR D 2 H13I H 0.5043 0.0305 0.1431 0.153 Uiso 0.30 1 calc PR D 2 N139 N 0.5516(6) 0.108(3) 0.1313(13) 0.137(11) Uiso 0.30 1 d PD D 2 O140 O 0.5720(5) 0.057(2) 0.1521(8) 0.159(9) Uiso 0.30 1 d PD D 2 O141 O 0.5664(7) 0.187(2) 0.1126(9) 0.186(11) Uiso 0.30 1 d PD D 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 Fe1A 0.0528(4) 0.0711(5) 0.0526(4) -0.0042(3) -0.0085(3) -0.0095(3) N2A 0.055(3) 0.053(3) 0.102(4) -0.012(2) -0.002(2) -0.010(2) C3A 0.058(4) 0.069(4) 0.176(8) -0.006(5) 0.017(4) -0.023(3) C4A 0.085(6) 0.069(5) 0.219(12) 0.026(6) 0.006(7) -0.001(4) C5A 0.052(4) 0.083(5) 0.293(15) 0.100(8) -0.066(7) -0.027(4) C6A 0.079(4) 0.085(4) 0.148(6) 0.053(5) -0.064(5) -0.034(4) C7A 0.066(3) 0.037(3) 0.100(4) 0.016(3) -0.027(3) -0.013(2) N8A 0.085(4) 0.098(4) 0.129(5) -0.036(4) 0.033(4) -0.017(3) N9A 0.108(5) 0.090(4) 0.092(4) -0.016(3) 0.006(3) -0.017(3) C10A 0.153(8) 0.165(8) 0.076(5) -0.027(5) 0.027(5) -0.065(7) C11A 0.201(15) 0.190(13) 0.215(16) -0.106(13) 0.120(13) -0.090(11) C12A 0.127(9) 0.165(10) 0.229(15) -0.083(11) 0.093(10) -0.060(8) N13A 0.075(3) 0.051(2) 0.063(3) 0.003(2) -0.017(2) -0.005(2) N14A 0.064(3) 0.064(3) 0.061(2) -0.007(2) -0.008(2) 0.008(2) C15A 0.087(4) 0.065(3) 0.078(4) -0.005(3) -0.001(3) 0.017(3) C16A 0.109(5) 0.085(4) 0.058(3) -0.013(3) 0.008(3) 0.014(4) C17A 0.140(6) 0.073(4) 0.047(3) -0.005(3) -0.023(3) -0.005(4) N18A 0.059(2) 0.077(3) 0.047(2) -0.003(2) -0.0057(18) 0.011(2) C19A 0.051(3) 0.105(5) 0.045(3) -0.023(3) 0.000(2) 0.004(3) C20A 0.049(3) 0.181(8) 0.073(4) -0.048(5) -0.009(3) 0.016(4) C21A 0.093(6) 0.224(12) 0.084(5) -0.049(7) -0.024(5) 0.084(7) C22A 0.121(6) 0.166(9) 0.062(4) -0.004(5) -0.007(4) 0.086(6) C23A 0.110(5) 0.086(5) 0.051(3) -0.010(3) -0.003(3) 0.024(4) N24A 0.060(3) 0.081(3) 0.062(3) -0.004(2) 0.008(2) -0.012(2) N25A 0.064(3) 0.081(3) 0.054(2) 0.002(2) 0.004(2) 0.008(2) C26A 0.113(5) 0.077(5) 0.079(4) -0.002(3) 0.012(3) -0.010(4) C27A 0.151(7) 0.077(5) 0.095(5) 0.006(4) 0.017(5) -0.011(5) C28A 0.107(5) 0.122(6) 0.079(4) -0.025(4) 0.036(4) -0.053(5) N29A 0.158(5) 0.072(4) 0.049(3) 0.010(2) 0.016(3) 0.030(4) N30A 0.135(5) 0.075(4) 0.073(3) 0.003(3) 0.008(3) -0.020(3) C31A 0.174(8) 0.085(5) 0.104(5) -0.019(4) 0.030(5) -0.054(5) C32A 0.239(14) 0.088(7) 0.133(9) 0.020(6) 0.072(9) -0.030(8) C33A 0.249(13) 0.092(7) 0.089(6) 0.024(5) 0.068(7) 0.019(7) Fe1B 0.0442(3) 0.0844(5) 0.0461(3) 0.0006(3) -0.0093(3) 0.0088(3) N2B 0.070(3) 0.159(6) 0.041(2) -0.021(3) -0.009(2) 0.043(4) C3B 0.127(7) 0.221(12) 0.045(4) -0.051(5) -0.018(4) 0.106(8) C4B 0.162(10) 0.40(3) 0.096(6) -0.124(11) -0.088(8) 0.210(15) C5B 0.130(10) 0.50(3) 0.135(9) -0.166(14) -0.089(9) 0.207(16) C6B 0.060(5) 0.348(18) 0.134(8) -0.155(11) -0.028(5) 0.038(8) C7B 0.036(3) 0.218(11) 0.081(5) -0.083(6) 0.001(3) -0.010(5) N8B 0.176(7) 0.112(5) 0.046(3) 0.014(3) 0.017(4) 0.089(5) N9B 0.116(4) 0.073(3) 0.066(3) 0.017(3) 0.013(3) 0.018(3) C10B 0.206(10) 0.089(6) 0.090(5) 0.016(4) 0.052(6) 0.020(7) C11B 0.44(4) 0.092(8) 0.128(15) -0.008(8) 0.110(18) -0.005(16) C12B 0.44(3) 0.125(13) 0.067(5) 0.024(8) 0.035(13) 0.160(17) N13B 0.067(4) 0.201(8) 0.072(4) -0.057(5) 0.024(3) -0.043(5) N14B 0.079(3) 0.123(5) 0.061(3) -0.014(3) 0.015(2) -0.029(3) C15B 0.179(8) 0.105(6) 0.056(3) -0.009(4) 0.022(4) -0.042(6) C16B 0.283(19) 0.192(15) 0.121(10) -0.090(10) 0.139(13) -0.166(15) C17B 0.129(9) 0.25(2) 0.147(11) -0.118(13) 0.076(8) -0.111(11) N18B 0.0397(18) 0.047(2) 0.046(2) 0.0012(16) -0.0025(15) -0.0018(16) C19B 0.042(2) 0.042(2) 0.054(2) 0.0023(19) -0.0004(19) -0.0016(19) C20B 0.042(2) 0.061(3) 0.064(3) 0.004(2) -0.010(2) 0.001(2) C21B 0.050(3) 0.059(3) 0.063(3) 0.006(2) -0.017(2) -0.008(2) C22B 0.059(3) 0.059(3) 0.048(3) -0.001(2) -0.011(2) -0.005(2) C23B 0.048(2) 0.036(2) 0.046(2) -0.0006(18) -0.0046(19) -0.0027(18) N24B 0.0447(19) 0.056(2) 0.054(2) 0.0009(17) -0.0044(17) 0.0023(17) N25B 0.049(2) 0.093(3) 0.055(2) -0.008(2) -0.0074(19) 0.009(2) C26B 0.079(4) 0.137(6) 0.057(3) -0.027(4) -0.002(3) 0.006(4) C27B 0.097(5) 0.112(5) 0.076(4) -0.021(4) 0.014(3) 0.025(4) C28B 0.056(3) 0.091(4) 0.071(3) -0.005(3) 0.010(3) 0.016(3) N29B 0.0486(19) 0.053(2) 0.0445(19) -0.0006(17) -0.0040(16) 0.0021(16) N30B 0.052(2) 0.076(3) 0.052(2) -0.004(2) -0.0058(18) 0.012(2) C31B 0.053(3) 0.105(5) 0.060(3) -0.010(3) -0.005(2) 0.026(3) C32B 0.082(4) 0.087(4) 0.070(3) -0.010(3) 0.009(3) 0.028(3) C33B 0.060(3) 0.062(3) 0.053(3) -0.011(2) -0.003(2) 0.009(2) Co34 0.0399(3) 0.0391(3) 0.0523(3) 0.0009(3) 0.0002(2) -0.0041(2) C35 0.050(3) 0.060(3) 0.057(3) -0.009(2) 0.002(2) 0.000(2) C36 0.049(3) 0.067(3) 0.056(3) 0.008(2) 0.002(2) -0.004(2) B37 0.051(3) 0.053(3) 0.081(4) 0.005(3) 0.006(3) -0.017(3) B38 0.044(3) 0.077(4) 0.058(3) -0.004(3) -0.006(2) -0.001(3) B39 0.049(3) 0.054(3) 0.057(3) -0.003(2) 0.002(2) 0.008(2) B40 0.058(3) 0.097(5) 0.059(3) -0.001(3) 0.011(3) 0.001(3) B41 0.051(3) 0.108(6) 0.082(4) 0.015(4) 0.021(3) -0.014(4) B42 0.040(3) 0.089(5) 0.086(4) -0.013(4) 0.000(3) -0.013(3) B43 0.052(3) 0.091(5) 0.065(3) -0.004(3) -0.002(3) 0.006(3) B44 0.057(3) 0.075(4) 0.070(4) -0.011(3) 0.008(3) 0.008(3) B45 0.053(3) 0.109(6) 0.082(4) -0.001(4) 0.014(3) 0.011(3) C46 0.037(2) 0.053(3) 0.061(3) 0.003(2) -0.0028(19) -0.0025(19) C47 0.054(3) 0.040(2) 0.078(3) 0.016(2) 0.005(2) 0.003(2) B48 0.049(3) 0.054(3) 0.072(4) -0.020(3) -0.002(3) -0.003(2) B49 0.054(3) 0.055(3) 0.051(3) -0.001(2) 0.007(2) 0.008(2) B50 0.051(3) 0.044(3) 0.065(3) 0.000(2) 0.009(2) -0.007(2) B51 0.050(3) 0.071(4) 0.084(4) 0.011(3) 0.000(3) 0.013(3) B52 0.053(3) 0.043(3) 0.105(5) -0.010(3) 0.003(3) 0.003(2) B53 0.058(3) 0.068(4) 0.074(4) -0.016(3) 0.005(3) 0.006(3) B54 0.057(3) 0.057(4) 0.080(4) 0.013(3) 0.018(3) -0.004(3) B55 0.042(3) 0.064(4) 0.079(4) -0.005(3) 0.003(3) -0.012(3) B56 0.046(3) 0.074(4) 0.079(4) -0.003(3) 0.013(3) -0.001(3) Co57 0.0535(3) 0.0477(3) 0.0395(3) -0.0032(3) -0.0031(3) -0.0058(3) C58 0.080(3) 0.072(4) 0.053(3) 0.001(2) 0.010(3) 0.018(3) C59 0.060(3) 0.063(3) 0.105(4) 0.014(3) -0.018(3) -0.009(3) B60 0.120(6) 0.057(4) 0.062(4) -0.006(3) -0.031(4) -0.002(4) B61 0.089(4) 0.055(4) 0.072(4) 0.006(3) 0.028(3) 0.002(3) B62 0.074(4) 0.045(3) 0.082(4) -0.008(3) -0.029(3) -0.001(3) B63 0.066(4) 0.078(5) 0.100(5) 0.022(4) 0.015(3) 0.018(3) B64 0.084(5) 0.081(5) 0.116(6) 0.011(5) -0.038(4) 0.014(4) B65 0.122(6) 0.071(4) 0.048(3) 0.010(3) -0.008(3) 0.001(4) B66 0.086(5) 0.059(4) 0.096(5) 0.007(4) 0.005(4) -0.008(3) B67 0.102(5) 0.055(4) 0.074(4) -0.011(3) -0.017(4) 0.019(4) B68 0.091(5) 0.056(4) 0.078(4) 0.015(3) 0.003(4) 0.008(3) C69 0.060(3) 0.050(3) 0.045(2) -0.001(2) -0.003(2) -0.010(2) C70 0.081(3) 0.052(3) 0.048(3) -0.005(2) -0.010(2) -0.012(2) B71 0.097(5) 0.057(4) 0.049(3) -0.009(3) 0.012(3) 0.010(3) B72 0.064(3) 0.062(4) 0.072(4) -0.003(3) 0.011(3) 0.001(3) B73 0.062(3) 0.064(4) 0.049(3) -0.005(3) -0.009(2) 0.004(3) B74 0.094(5) 0.043(3) 0.065(4) -0.001(3) -0.008(3) -0.005(3) B75 0.116(5) 0.053(4) 0.055(3) -0.015(3) -0.005(3) 0.007(4) B76 0.086(4) 0.080(5) 0.076(4) -0.011(4) 0.013(3) 0.022(4) B77 0.067(4) 0.068(4) 0.071(4) 0.001(3) -0.013(3) 0.008(3) B78 0.081(4) 0.060(3) 0.045(3) -0.002(3) -0.003(3) 0.005(3) B79 0.094(5) 0.078(4) 0.068(4) -0.003(4) -0.011(3) 0.031(4) Co80 0.0585(3) 0.0424(3) 0.0441(3) -0.0047(3) -0.0071(3) -0.0021(3) C81 0.077(3) 0.061(3) 0.055(3) -0.008(2) -0.005(2) -0.019(3) C82 0.068(3) 0.060(3) 0.088(4) -0.004(3) -0.010(3) -0.005(3) B83 0.112(5) 0.062(4) 0.049(3) 0.002(3) -0.024(3) -0.020(4) B84 0.079(4) 0.046(3) 0.065(3) -0.011(3) 0.002(3) -0.001(3) B85 0.073(4) 0.048(3) 0.056(3) 0.001(3) -0.013(3) -0.006(3) B86 0.075(4) 0.082(5) 0.111(6) -0.009(4) -0.015(4) -0.029(4) B87 0.107(5) 0.081(5) 0.078(4) -0.006(4) -0.041(4) -0.022(4) B88 0.171(9) 0.068(5) 0.053(4) -0.015(3) -0.015(4) -0.035(5) B89 0.105(5) 0.036(3) 0.093(5) -0.003(3) -0.005(4) 0.002(3) B90 0.108(5) 0.058(4) 0.067(4) 0.007(3) -0.003(4) -0.017(4) B91 0.118(6) 0.064(4) 0.073(4) -0.011(3) -0.016(4) -0.027(4) C92 0.078(3) 0.047(3) 0.081(3) -0.019(3) 0.007(3) -0.002(3) C93 0.091(4) 0.050(3) 0.097(4) 0.005(3) -0.008(3) -0.007(3) B94 0.074(4) 0.060(4) 0.056(3) 0.003(3) -0.005(3) -0.006(3) B95 0.053(3) 0.065(4) 0.061(3) 0.001(3) -0.007(2) -0.009(3) B96 0.077(4) 0.058(4) 0.047(3) -0.016(3) -0.004(3) -0.012(3) B97 0.111(6) 0.051(4) 0.121(6) -0.012(4) 0.013(5) -0.003(4) B98 0.108(6) 0.052(4) 0.088(5) 0.016(3) -0.015(4) -0.025(4) B99 0.081(4) 0.072(4) 0.089(5) -0.006(4) -0.001(4) -0.030(4) B100 0.077(4) 0.089(5) 0.079(4) -0.008(4) -0.021(4) -0.026(4) B101 0.102(5) 0.074(5) 0.099(5) -0.042(4) 0.007(4) -0.023(4) B102 0.103(5) 0.058(4) 0.112(6) -0.021(4) 0.000(5) -0.023(4) Co10 0.0342(3) 0.0390(3) 0.0589(3) -0.0041(3) -0.0029(2) -0.0013(2) C104 0.034(2) 0.043(2) 0.085(3) -0.007(2) -0.005(2) -0.0046(18) C105 0.039(2) 0.050(3) 0.066(3) 0.000(2) 0.002(2) 0.0053(19) B106 0.051(3) 0.040(3) 0.086(4) -0.014(3) 0.006(3) 0.001(2) B107 0.052(3) 0.072(4) 0.065(3) -0.015(3) 0.000(3) -0.010(3) B108 0.046(3) 0.063(4) 0.075(4) 0.015(3) -0.007(3) -0.018(3) B109 0.033(2) 0.055(3) 0.093(4) -0.010(3) -0.006(3) -0.004(2) B110 0.040(3) 0.058(3) 0.084(4) -0.001(3) 0.011(3) 0.005(2) B111 0.057(3) 0.080(5) 0.072(4) -0.024(3) 0.013(3) -0.004(3) B112 0.058(3) 0.114(6) 0.052(3) 0.009(3) 0.003(3) -0.017(4) B113 0.053(3) 0.051(3) 0.114(5) 0.021(3) -0.005(3) -0.014(3) B114 0.054(3) 0.072(4) 0.081(4) 0.000(3) 0.011(3) -0.013(3) C115 0.043(2) 0.074(3) 0.060(3) -0.013(2) -0.003(2) 0.007(2) C116 0.054(3) 0.053(3) 0.067(3) 0.009(2) -0.002(2) 0.001(2) B117 0.046(3) 0.045(3) 0.077(4) -0.006(3) 0.000(3) -0.011(2) B118 0.039(3) 0.053(3) 0.074(3) 0.011(3) -0.007(2) -0.004(2) B119 0.043(3) 0.058(3) 0.087(4) -0.003(3) 0.000(3) 0.004(2) B120 0.053(3) 0.103(5) 0.071(4) 0.007(4) 0.002(3) -0.003(3) B121 0.057(3) 0.073(4) 0.090(4) 0.018(4) 0.002(3) -0.009(3) B122 0.042(3) 0.081(4) 0.081(4) 0.009(3) -0.002(3) -0.016(3) B123 0.042(3) 0.070(4) 0.088(4) -0.004(3) -0.001(3) 0.002(3) B124 0.053(3) 0.097(5) 0.087(5) -0.010(4) 0.014(3) 0.003(3) B125 0.043(3) 0.111(6) 0.073(4) 0.013(4) 0.002(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1A N9A 1.962(6) . ? Fe1A N18A 1.975(4) . ? Fe1A N2A 1.981(5) . ? Fe1A N14A 2.030(4) . ? Fe1A N25A 2.031(5) . ? Fe1A N30A 2.035(6) . ? N2A C3A 1.336(8) . ? N2A C7A 1.348(8) . ? C3A C4A 1.328(12) . ? C3A N8A 1.449(11) . ? C4A C5A 1.345(15) . ? C5A C6A 1.456(15) . ? C6A C7A 1.382(8) . ? C7A N13A 1.386(7) . ? N8A C12A 1.350(12) . ? N8A N9A 1.385(9) . ? N9A C10A 1.341(9) . ? C10A C11A 1.398(16) . ? C11A C12A 1.36(2) . ? N13A C17A 1.359(8) . ? N13A N14A 1.374(6) . ? N14A C15A 1.315(7) . ? C15A C16A 1.363(8) . ? C16A C17A 1.329(9) . ? N18A C23A 1.316(8) . ? N18A C19A 1.336(7) . ? C19A N24A 1.365(7) . ? C19A C20A 1.399(8) . ? C20A C21A 1.365(14) . ? C21A C22A 1.370(13) . ? C22A C23A 1.359(10) . ? C23A N29A 1.401(9) . ? N24A C28A 1.365(9) . ? N24A N25A 1.384(6) . ? N25A C26A 1.324(8) . ? C26A C27A 1.384(10) . ? C27A C28A 1.370(11) . ? N29A C33A 1.373(10) . ? N29A N30A 1.395(8) . ? N30A C31A 1.301(9) . ? C31A C32A 1.429(14) . ? C32A C33A 1.368(15) . ? Fe1B N2B 2.127(5) . ? Fe1B N18B 2.131(3) . ? Fe1B N14B 2.158(6) . ? Fe1B N9B 2.167(6) . ? Fe1B N25B 2.173(4) . ? Fe1B N30B 2.210(4) . ? N2B C3B 1.273(13) . ? N2B C7B 1.345(11) . ? C3B N8B 1.411(13) . ? C3B C4B 1.419(12) . ? C4B C5B 1.22(3) . ? C5B C6B 1.45(3) . ? C6B C7B 1.397(12) . ? C7B N13B 1.346(12) . ? N8B N9B 1.399(9) . ? N8B C12B 1.403(18) . ? N9B C10B 1.280(11) . ? C10B C11B 1.40(2) . ? C11B C12B 1.19(3) . ? N13B N14B 1.365(9) . ? N13B C17B 1.381(16) . ? N14B C15B 1.301(10) . ? C15B C16B 1.379(15) . ? C16B C17B 1.27(2) . ? N18B C19B 1.308(6) . ? N18B C23B 1.331(6) . ? C19B C20B 1.377(6) . ? C19B N24B 1.407(6) . ? C20B C21B 1.391(7) . ? C21B C22B 1.364(7) . ? C22B C23B 1.370(6) . ? C23B N29B 1.417(5) . ? N24B C28B 1.337(6) . ? N24B N25B 1.379(5) . ? N25B C26B 1.319(7) . ? C26B C27B 1.399(9) . ? C27B C28B 1.332(8) . ? N29B C33B 1.340(6) . ? N29B N30B 1.371(5) . ? N30B C31B 1.308(6) . ? C31B C32B 1.377(8) . ? C32B C33B 1.356(7) . ? Co34 C47 2.032(4) . ? Co34 C46 2.049(4) . ? Co34 C35 2.049(5) . ? Co34 C36 2.053(5) . ? Co34 B48 2.081(5) . ? Co34 B50 2.082(5) . ? Co34 B39 2.089(5) . ? Co34 B37 2.093(5) . ? Co34 B38 2.103(5) . ? Co34 B49 2.105(5) . ? C35 C36 1.622(7) . ? C35 B44 1.693(7) . ? C35 B39 1.711(7) . ? C35 B40 1.721(7) . ? C36 B41 1.660(7) . ? C36 B37 1.695(8) . ? C36 B40 1.706(8) . ? B37 B42 1.741(9) . ? B37 B41 1.752(9) . ? B37 B38 1.796(9) . ? B38 B43 1.801(9) . ? B38 B42 1.805(8) . ? B38 B39 1.809(8) . ? B39 B43 1.788(8) . ? B39 B44 1.806(8) . ? B40 B44 1.745(10) . ? B40 B41 1.746(11) . ? B40 B45 1.764(9) . ? B41 B42 1.778(10) . ? B41 B45 1.791(11) . ? B42 B43 1.779(10) . ? B42 B45 1.788(10) . ? B43 B44 1.762(9) . ? B43 B45 1.769(10) . ? B44 B45 1.750(10) . ? C46 C47 1.609(7) . ? C46 B50 1.671(7) . ? C46 B55 1.672(7) . ? C46 B51 1.696(8) . ? C47 B52 1.684(8) . ? C47 B48 1.707(8) . ? C47 B51 1.707(7) . ? B48 B52 1.785(8) . ? B48 B53 1.790(9) . ? B48 B49 1.801(8) . ? B49 B53 1.787(8) . ? B49 B50 1.787(8) . ? B49 B54 1.812(8) . ? B50 B55 1.773(8) . ? B50 B54 1.774(8) . ? B51 B52 1.740(10) . ? B51 B55 1.743(9) . ? B51 B56 1.762(9) . ? B52 B56 1.754(8) . ? B52 B53 1.765(10) . ? B53 B54 1.770(9) . ? B53 B56 1.772(9) . ? B54 B55 1.761(9) . ? B54 B56 1.762(9) . ? B55 B56 1.768(9) . ? Co57 C59 2.042(5) . ? Co57 C70 2.049(5) . ? Co57 C69 2.050(5) . ? Co57 C58 2.051(5) . ? Co57 B71 2.073(6) . ? Co57 B62 2.076(6) . ? Co57 B73 2.078(5) . ? Co57 B60 2.081(6) . ? Co57 B72 2.094(6) . ? Co57 B61 2.107(6) . ? C58 C59 1.583(8) . ? C58 B67 1.656(9) . ? C58 B62 1.673(9) . ? C58 B63 1.740(8) . ? C59 B64 1.702(9) . ? C59 B60 1.705(10) . ? C59 B63 1.709(9) . ? B60 B65 1.747(10) . ? B60 B64 1.774(11) . ? B60 B61 1.777(10) . ? B61 B62 1.782(9) . ? B61 B66 1.784(10) . ? B61 B65 1.786(11) . ? B62 B66 1.774(10) . ? B62 B67 1.797(9) . ? B63 B67 1.731(10) . ? B63 B64 1.731(12) . ? B63 B68 1.774(9) . ? B64 B65 1.739(12) . ? B64 B68 1.778(11) . ? B65 B68 1.748(10) . ? B65 B66 1.779(11) . ? B66 B68 1.722(10) . ? B66 B67 1.758(11) . ? B67 B68 1.749(10) . ? C69 C70 1.606(6) . ? C69 B78 1.661(8) . ? C69 B73 1.672(7) . ? C69 B74 1.734(8) . ? C70 B75 1.678(9) . ? C70 B71 1.693(9) . ? C70 B74 1.699(8) . ? B71 B76 1.797(10) . ? B71 B75 1.798(9) . ? B71 B72 1.812(9) . ? B72 B76 1.798(9) . ? B72 B77 1.801(9) . ? B72 B73 1.803(8) . ? B73 B77 1.773(9) . ? B73 B78 1.777(9) . ? B74 B75 1.746(9) . ? B74 B79 1.755(10) . ? B74 B78 1.757(8) . ? B75 B76 1.761(11) . ? B75 B79 1.793(9) . ? B76 B77 1.771(9) . ? B76 B79 1.784(11) . ? B77 B78 1.773(9) . ? B77 B79 1.781(10) . ? B78 B79 1.765(9) . ? Co80 C93 2.040(6) . ? Co80 C92 2.040(5) . ? Co80 C81 2.042(5) . ? Co80 C82 2.051(5) . ? Co80 B96 2.055(5) . ? Co80 B94 2.074(6) . ? Co80 B85 2.076(6) . ? Co80 B84 2.094(6) . ? Co80 B83 2.098(6) . ? Co80 B95 2.108(6) . ? C81 C82 1.622(8) . ? C81 B85 1.675(8) . ? C81 B90 1.696(9) . ? C81 B86 1.725(8) . ? C82 B87 1.675(9) . ? C82 B83 1.696(10) . ? C82 B86 1.757(10) . ? B83 B87 1.777(11) . ? B83 B88 1.782(11) . ? B83 B84 1.797(10) . ? B84 B88 1.782(10) . ? B84 B89 1.786(9) . ? B84 B85 1.806(9) . ? B85 B89 1.742(9) . ? B85 B90 1.764(9) . ? B86 B87 1.744(12) . ? B86 B90 1.747(11) . ? B86 B91 1.755(12) . ? B87 B91 1.777(11) . ? B87 B88 1.782(13) . ? B88 B91 1.744(11) . ? B88 B89 1.769(11) . ? B89 B90 1.758(11) . ? B89 B91 1.775(11) . ? B90 B91 1.755(10) . ? C92 C93 1.622(9) . ? C92 B96 1.658(8) . ? C92 B101 1.700(9) . ? C92 B97 1.721(9) . ? C93 B98 1.704(9) . ? C93 B94 1.720(9) . ? C93 B97 1.755(10) . ? B94 B98 1.774(9) . ? B94 B99 1.799(9) . ? B94 B95 1.803(8) . ? B95 B96 1.751(8) . ? B95 B99 1.771(9) . ? B95 B100 1.773(9) . ? B96 B100 1.755(9) . ? B96 B101 1.769(9) . ? B97 B102 1.712(11) . ? B97 B101 1.716(13) . ? B97 B98 1.788(12) . ? B98 B102 1.746(11) . ? B98 B99 1.750(11) . ? B99 B100 1.777(11) . ? B99 B102 1.787(11) . ? B100 B101 1.752(11) . ? B100 B102 1.759(12) . ? B101 B102 1.775(12) . ? Co10 C115 2.034(5) . ? Co10 C116 2.035(5) . ? Co10 C104 2.039(4) . ? Co10 C105 2.044(4) . ? Co10 B108 2.075(6) . ? Co10 B117 2.093(5) . ? Co10 B106 2.094(5) . ? Co10 B119 2.097(6) . ? Co10 B107 2.103(6) . ? Co10 B118 2.118(5) . ? C104 C105 1.616(6) . ? C104 B113 1.660(8) . ? C104 B108 1.705(8) . ? C104 B109 1.735(6) . ? C105 B106 1.689(7) . ? C105 B110 1.695(7) . ? C105 B109 1.725(7) . ? B106 B111 1.757(9) . ? B106 B110 1.779(8) . ? B106 B107 1.788(9) . ? B107 B112 1.793(9) . ? B107 B111 1.802(8) . ? B107 B108 1.823(9) . ? B108 B113 1.784(7) . ? B108 B112 1.795(9) . ? B109 B114 1.733(9) . ? B109 B113 1.745(9) . ? B109 B110 1.769(8) . ? B110 B111 1.756(9) . ? B110 B114 1.767(9) . ? B111 B112 1.787(11) . ? B111 B114 1.787(9) . ? B112 B113 1.785(10) . ? B112 B114 1.787(9) . ? B113 B114 1.770(10) . ? C115 C116 1.600(7) . ? C115 B119 1.677(8) . ? C115 B124 1.688(7) . ? C115 B120 1.700(9) . ? C116 B121 1.693(8) . ? C116 B117 1.694(8) . ? C116 B120 1.723(8) . ? B117 B122 1.781(7) . ? B117 B121 1.786(9) . ? B117 B118 1.825(8) . ? B118 B123 1.766(9) . ? B118 B122 1.775(8) . ? B118 B119 1.796(9) . ? B119 B123 1.744(8) . ? B119 B124 1.769(10) . ? B120 B124 1.723(11) . ? B120 B121 1.760(10) . ? B120 B125 1.777(8) . ? B121 B125 1.781(10) . ? B121 B122 1.785(9) . ? B122 B123 1.762(9) . ? B122 B125 1.764(10) . ? B123 B124 1.754(10) . ? B123 B125 1.755(10) . ? B124 B125 1.744(11) . ? C126 N127 1.485(14) . ? N127 O129 1.136(14) . ? N127 O128 1.154(13) . ? C130 N131 1.452(14) . ? N131 O132 1.108(14) . ? N131 O133 1.210(16) . ? C134 N135 1.391(16) . ? N135 O136 1.153(17) . ? N135 O137 1.179(16) . ? C138 N139 1.441(18) . ? N139 O140 1.118(18) . ? N139 O141 1.146(18) . ? 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 N9A Fe1A N18A 102.4(2) . . ? N9A Fe1A N2A 80.9(3) . . ? N18A Fe1A N2A 175.7(2) . . ? N9A Fe1A N14A 158.4(2) . . ? N18A Fe1A N14A 99.08(17) . . ? N2A Fe1A N14A 77.87(19) . . ? N9A Fe1A N25A 96.2(2) . . ? N18A Fe1A N25A 77.08(19) . . ? N2A Fe1A N25A 99.83(18) . . ? N14A Fe1A N25A 91.30(18) . . ? N9A Fe1A N30A 89.0(2) . . ? N18A Fe1A N30A 78.6(2) . . ? N2A Fe1A N30A 104.4(2) . . ? N14A Fe1A N30A 92.5(2) . . ? N25A Fe1A N30A 155.7(2) . . ? C3A N2A C7A 122.4(6) . . ? C3A N2A Fe1A 118.3(5) . . ? C7A N2A Fe1A 119.2(4) . . ? C4A C3A N2A 121.5(10) . . ? C4A C3A N8A 128.1(9) . . ? N2A C3A N8A 110.2(7) . . ? C3A C4A C5A 118.9(10) . . ? C4A C5A C6A 122.0(7) . . ? C7A C6A C5A 114.8(8) . . ? N2A C7A C6A 120.2(7) . . ? N2A C7A N13A 112.0(4) . . ? C6A C7A N13A 127.8(7) . . ? C12A N8A N9A 111.4(10) . . ? C12A N8A C3A 130.2(10) . . ? N9A N8A C3A 117.8(6) . . ? C10A N9A N8A 105.0(7) . . ? C10A N9A Fe1A 142.1(7) . . ? N8A N9A Fe1A 112.7(5) . . ? N9A C10A C11A 109.3(12) . . ? C12A C11A C10A 107.8(11) . . ? N8A C12A C11A 106.0(11) . . ? C17A N13A N14A 108.6(5) . . ? C17A N13A C7A 134.1(5) . . ? N14A N13A C7A 117.2(5) . . ? C15A N14A N13A 105.3(5) . . ? C15A N14A Fe1A 141.1(4) . . ? N13A N14A Fe1A 113.6(3) . . ? N14A C15A C16A 111.5(6) . . ? C17A C16A C15A 106.4(6) . . ? C16A C17A N13A 108.2(5) . . ? C23A N18A C19A 119.1(5) . . ? C23A N18A Fe1A 120.6(5) . . ? C19A N18A Fe1A 120.2(4) . . ? N18A C19A N24A 112.0(4) . . ? N18A C19A C20A 120.8(7) . . ? N24A C19A C20A 127.2(7) . . ? C21A C20A C19A 117.5(8) . . ? C20A C21A C22A 121.7(8) . . ? C23A C22A C21A 116.5(9) . . ? N18A C23A C22A 124.3(8) . . ? N18A C23A N29A 111.0(6) . . ? C22A C23A N29A 124.7(8) . . ? C28A N24A C19A 133.4(6) . . ? C28A N24A N25A 109.4(6) . . ? C19A N24A N25A 117.1(4) . . ? C26A N25A N24A 106.5(5) . . ? C26A N25A Fe1A 139.9(5) . . ? N24A N25A Fe1A 113.5(3) . . ? N25A C26A C27A 110.2(7) . . ? C28A C27A C26A 107.1(7) . . ? N24A C28A C27A 106.8(6) . . ? C33A N29A N30A 109.1(8) . . ? C33A N29A C23A 132.2(9) . . ? N30A N29A C23A 118.6(5) . . ? C31A N30A N29A 108.0(7) . . ? C31A N30A Fe1A 140.9(7) . . ? N29A N30A Fe1A 111.1(4) . . ? N30A C31A C32A 109.2(9) . . ? C33A C32A C31A 106.9(9) . . ? C32A C33A N29A 106.8(11) . . ? N2B Fe1B N18B 163.11(15) . . ? N2B Fe1B N14B 72.6(3) . . ? N18B Fe1B N14B 105.41(19) . . ? N2B Fe1B N9B 74.5(3) . . ? N18B Fe1B N9B 108.27(19) . . ? N14B Fe1B N9B 146.2(2) . . ? N2B Fe1B N25B 122.94(16) . . ? N18B Fe1B N25B 73.57(15) . . ? N14B Fe1B N25B 92.2(2) . . ? N9B Fe1B N25B 99.42(19) . . ? N2B Fe1B N30B 90.03(16) . . ? N18B Fe1B N30B 73.27(14) . . ? N14B Fe1B N30B 93.92(17) . . ? N9B Fe1B N30B 93.42(18) . . ? N25B Fe1B N30B 146.72(15) . . ? C3B N2B C7B 119.6(8) . . ? C3B N2B Fe1B 119.9(7) . . ? C7B N2B Fe1B 119.9(6) . . ? N2B C3B N8B 115.3(7) . . ? N2B C3B C4B 123.0(15) . . ? N8B C3B C4B 121.7(14) . . ? C5B C4B C3B 120(2) . . ? C4B C5B C6B 120.8(10) . . ? C7B C6B C5B 116.6(14) . . ? N2B C7B N13B 112.4(6) . . ? N2B C7B C6B 119.8(12) . . ? N13B C7B C6B 127.8(11) . . ? N9B N8B C12B 102.0(11) . . ? N9B N8B C3B 117.4(6) . . ? C12B N8B C3B 140.6(12) . . ? C10B N9B N8B 107.9(7) . . ? C10B N9B Fe1B 139.4(6) . . ? N8B N9B Fe1B 112.4(5) . . ? N9B C10B C11B 109.0(13) . . ? C12B C11B C10B 107.8(18) . . ? C11B C12B N8B 113.2(17) . . ? C7B N13B N14B 119.7(7) . . ? C7B N13B C17B 130.5(10) . . ? N14B N13B C17B 109.8(11) . . ? C15B N14B N13B 102.6(7) . . ? C15B N14B Fe1B 142.7(6) . . ? N13B N14B Fe1B 114.4(6) . . ? N14B C15B C16B 113.2(12) . . ? C17B C16B C15B 106.2(14) . . ? C16B C17B N13B 108.1(13) . . ? C19B N18B C23B 118.3(4) . . ? C19B N18B Fe1B 120.3(3) . . ? C23B N18B Fe1B 121.2(3) . . ? N18B C19B C20B 123.4(4) . . ? N18B C19B N24B 113.8(4) . . ? C20B C19B N24B 122.7(4) . . ? C19B C20B C21B 117.1(4) . . ? C22B C21B C20B 120.1(4) . . ? C21B C22B C23B 117.7(4) . . ? N18B C23B C22B 123.3(4) . . ? N18B C23B N29B 112.9(3) . . ? C22B C23B N29B 123.8(4) . . ? C28B N24B N25B 111.1(4) . . ? C28B N24B C19B 131.3(4) . . ? N25B N24B C19B 117.5(4) . . ? C26B N25B N24B 103.5(4) . . ? C26B N25B Fe1B 141.4(4) . . ? N24B N25B Fe1B 114.2(3) . . ? N25B C26B C27B 111.9(5) . . ? C28B C27B C26B 105.1(5) . . ? C27B C28B N24B 108.3(5) . . ? C33B N29B N30B 111.0(4) . . ? C33B N29B C23B 130.7(4) . . ? N30B N29B C23B 118.3(4) . . ? C31B N30B N29B 104.1(4) . . ? C31B N30B Fe1B 141.8(3) . . ? N29B N30B Fe1B 113.8(3) . . ? N30B C31B C32B 112.6(5) . . ? C33B C32B C31B 105.1(5) . . ? N29B C33B C32B 107.2(4) . . ? C47 Co34 C46 46.44(19) . . ? C47 Co34 C35 136.1(2) . . ? C46 Co34 C35 101.45(19) . . ? C47 Co34 C36 101.1(2) . . ? C46 Co34 C36 97.64(19) . . ? C35 Co34 C36 46.6(2) . . ? C47 Co34 B48 49.0(2) . . ? C46 Co34 B48 83.4(2) . . ? C35 Co34 B48 174.7(2) . . ? C36 Co34 B48 135.2(2) . . ? C47 Co34 B50 82.6(2) . . ? C46 Co34 B50 47.7(2) . . ? C35 Co34 B50 94.9(2) . . ? C36 Co34 B50 126.4(2) . . ? B48 Co34 B50 86.9(2) . . ? C47 Co34 B39 174.9(2) . . ? C46 Co34 B39 135.2(2) . . ? C35 Co34 B39 48.8(2) . . ? C36 Co34 B39 83.6(2) . . ? B48 Co34 B39 126.1(2) . . ? B50 Co34 B39 96.1(2) . . ? C47 Co34 B37 94.9(2) . . ? C46 Co34 B37 126.7(2) . . ? C35 Co34 B37 82.8(2) . . ? C36 Co34 B37 48.3(2) . . ? B48 Co34 B37 95.8(2) . . ? B50 Co34 B37 173.6(2) . . ? B39 Co34 B37 86.9(2) . . ? C47 Co34 B38 127.1(2) . . ? C46 Co34 B38 173.4(2) . . ? C35 Co34 B38 84.5(2) . . ? C36 Co34 B38 84.3(2) . . ? B48 Co34 B38 90.8(2) . . ? B50 Co34 B38 135.2(2) . . ? B39 Co34 B38 51.1(2) . . ? B37 Co34 B38 50.7(2) . . ? C47 Co34 B49 84.1(2) . . ? C46 Co34 B49 83.5(2) . . ? C35 Co34 B49 127.2(2) . . ? C36 Co34 B49 173.8(2) . . ? B48 Co34 B49 51.0(2) . . ? B50 Co34 B49 50.5(2) . . ? B39 Co34 B49 91.3(2) . . ? B37 Co34 B49 135.2(2) . . ? B38 Co34 B49 95.3(2) . . ? C36 C35 B44 110.1(4) . . ? C36 C35 B39 111.9(4) . . ? B44 C35 B39 64.1(3) . . ? C36 C35 B40 61.3(3) . . ? B44 C35 B40 61.5(4) . . ? B39 C35 B40 115.4(4) . . ? C36 C35 Co34 66.8(2) . . ? B44 C35 Co34 124.5(3) . . ? B39 C35 Co34 66.8(2) . . ? B40 C35 Co34 124.2(4) . . ? C35 C36 B41 112.1(4) . . ? C35 C36 B37 111.3(4) . . ? B41 C36 B37 62.9(4) . . ? C35 C36 B40 62.2(3) . . ? B41 C36 B40 62.5(4) . . ? B37 C36 B40 114.5(4) . . ? C35 C36 Co34 66.6(2) . . ? B41 C36 Co34 124.8(4) . . ? B37 C36 Co34 67.1(3) . . ? B40 C36 Co34 124.8(4) . . ? C36 B37 B42 105.0(4) . . ? C36 B37 B41 57.5(3) . . ? B42 B37 B41 61.2(4) . . ? C36 B37 B38 106.1(4) . . ? B42 B37 B38 61.4(4) . . ? B41 B37 B38 110.5(5) . . ? C36 B37 Co34 64.6(2) . . ? B42 B37 Co34 119.0(4) . . ? B41 B37 Co34 117.7(4) . . ? B38 B37 Co34 65.0(2) . . ? B37 B38 B43 104.5(4) . . ? B37 B38 B42 57.8(3) . . ? B43 B38 B42 59.1(4) . . ? B37 B38 B39 105.9(4) . . ? B43 B38 B39 59.4(3) . . ? B42 B38 B39 106.4(4) . . ? B37 B38 Co34 64.4(2) . . ? B43 B38 Co34 115.7(4) . . ? B42 B38 Co34 115.4(4) . . ? B39 B38 Co34 64.0(2) . . ? C35 B39 B43 102.7(4) . . ? C35 B39 B44 57.5(3) . . ? B43 B39 B44 58.7(3) . . ? C35 B39 B38 104.9(4) . . ? B43 B39 B38 60.1(3) . . ? B44 B39 B38 107.2(4) . . ? C35 B39 Co34 64.3(2) . . ? B43 B39 Co34 116.9(4) . . ? B44 B39 Co34 116.5(4) . . ? B38 B39 Co34 64.8(2) . . ? C36 B40 C35 56.5(3) . . ? C36 B40 B44 103.9(4) . . ? C35 B40 B44 58.5(3) . . ? C36 B40 B41 57.5(3) . . ? C35 B40 B41 103.5(4) . . ? B44 B40 B41 108.2(5) . . ? C36 B40 B45 104.6(5) . . ? C35 B40 B45 104.5(4) . . ? B44 B40 B45 59.8(4) . . ? B41 B40 B45 61.4(4) . . ? C36 B41 B40 60.1(4) . . ? C36 B41 B37 59.5(3) . . ? B40 B41 B37 109.8(4) . . ? C36 B41 B42 104.9(4) . . ? B40 B41 B42 108.4(5) . . ? B37 B41 B42 59.1(4) . . ? C36 B41 B45 105.4(5) . . ? B40 B41 B45 59.8(4) . . ? B37 B41 B45 107.8(5) . . ? B42 B41 B45 60.1(4) . . ? B37 B42 B41 59.7(4) . . ? B37 B42 B43 107.8(4) . . ? B41 B42 B43 107.0(5) . . ? B37 B42 B45 108.5(4) . . ? B41 B42 B45 60.3(4) . . ? B43 B42 B45 59.5(4) . . ? B37 B42 B38 60.8(3) . . ? B41 B42 B38 108.8(4) . . ? B43 B42 B38 60.3(4) . . ? B45 B42 B38 109.2(5) . . ? B44 B43 B45 59.4(4) . . ? B44 B43 B42 107.4(5) . . ? B45 B43 B42 60.5(4) . . ? B44 B43 B39 61.1(3) . . ? B45 B43 B39 109.5(4) . . ? B42 B43 B39 108.5(4) . . ? B44 B43 B38 109.5(4) . . ? B45 B43 B38 110.2(5) . . ? B42 B43 B38 60.6(4) . . ? B39 B43 B38 60.5(3) . . ? C35 B44 B40 60.1(3) . . ? C35 B44 B45 106.3(5) . . ? B40 B44 B45 60.6(4) . . ? C35 B44 B43 104.6(4) . . ? B40 B44 B43 108.8(5) . . ? B45 B44 B43 60.5(4) . . ? C35 B44 B39 58.5(3) . . ? B40 B44 B39 109.6(4) . . ? B45 B44 B39 109.5(5) . . ? B43 B44 B39 60.1(3) . . ? B44 B45 B40 59.5(4) . . ? B44 B45 B43 60.1(4) . . ? B40 B45 B43 107.7(4) . . ? B44 B45 B42 107.6(5) . . ? B40 B45 B42 107.2(5) . . ? B43 B45 B42 60.0(4) . . ? B44 B45 B41 106.0(4) . . ? B40 B45 B41 58.8(4) . . ? B43 B45 B41 106.9(5) . . ? B42 B45 B41 59.6(4) . . ? C47 C46 B50 111.7(4) . . ? C47 C46 B55 112.0(4) . . ? B50 C46 B55 64.0(3) . . ? C47 C46 B51 62.1(3) . . ? B50 C46 B51 115.5(4) . . ? B55 C46 B51 62.3(3) . . ? C47 C46 Co34 66.2(2) . . ? B50 C46 Co34 67.2(2) . . ? B55 C46 Co34 125.6(3) . . ? B51 C46 Co34 124.6(4) . . ? C46 C47 B52 110.2(4) . . ? C46 C47 B48 112.0(4) . . ? B52 C47 B48 63.5(3) . . ? C46 C47 B51 61.4(3) . . ? B52 C47 B51 61.7(4) . . ? B48 C47 B51 115.4(4) . . ? C46 C47 Co34 67.3(2) . . ? B52 C47 Co34 124.5(4) . . ? B48 C47 Co34 67.0(2) . . ? B51 C47 Co34 125.0(3) . . ? C47 B48 B52 57.6(3) . . ? C47 B48 B53 103.0(4) . . ? B52 B48 B53 59.2(4) . . ? C47 B48 B49 104.3(4) . . ? B52 B48 B49 107.0(4) . . ? B53 B48 B49 59.7(3) . . ? C47 B48 Co34 64.0(2) . . ? B52 B48 Co34 116.5(4) . . ? B53 B48 Co34 117.3(3) . . ? B49 B48 Co34 65.2(2) . . ? B53 B49 B50 105.6(4) . . ? B53 B49 B48 59.8(3) . . ? B50 B49 B48 105.9(4) . . ? B53 B49 B54 58.9(3) . . ? B50 B49 B54 59.0(3) . . ? B48 B49 B54 106.5(4) . . ? B53 B49 Co34 116.3(4) . . ? B50 B49 Co34 64.1(2) . . ? B48 B49 Co34 63.8(3) . . ? B54 B49 Co34 116.1(3) . . ? C46 B50 B55 58.0(3) . . ? C46 B50 B54 104.1(4) . . ? B55 B50 B54 59.6(3) . . ? C46 B50 B49 106.1(4) . . ? B55 B50 B49 109.2(4) . . ? B54 B50 B49 61.2(3) . . ? C46 B50 Co34 65.1(2) . . ? B55 B50 Co34 118.3(4) . . ? B54 B50 Co34 119.1(4) . . ? B49 B50 Co34 65.4(2) . . ? C46 B51 C47 56.4(3) . . ? C46 B51 B52 103.6(4) . . ? C47 B51 B52 58.5(3) . . ? C46 B51 B55 58.1(3) . . ? C47 B51 B55 104.1(4) . . ? B52 B51 B55 108.0(5) . . ? C46 B51 B56 104.5(4) . . ? C47 B51 B56 104.8(5) . . ? B52 B51 B56 60.1(4) . . ? B55 B51 B56 60.6(4) . . ? C47 B52 B51 59.8(3) . . ? C47 B52 B56 106.2(4) . . ? B51 B52 B56 60.6(4) . . ? C47 B52 B53 105.0(4) . . ? B51 B52 B53 109.0(4) . . ? B56 B52 B53 60.5(4) . . ? C47 B52 B48 58.9(3) . . ? B51 B52 B48 109.9(4) . . ? B56 B52 B48 109.9(4) . . ? B53 B52 B48 60.6(3) . . ? B52 B53 B54 106.8(5) . . ? B52 B53 B56 59.5(4) . . ? B54 B53 B56 59.7(4) . . ? B52 B53 B49 108.5(4) . . ? B54 B53 B49 61.3(3) . . ? B56 B53 B49 109.7(4) . . ? B52 B53 B48 60.3(4) . . ? B54 B53 B48 108.9(4) . . ? B56 B53 B48 108.9(5) . . ? B49 B53 B48 60.5(3) . . ? B55 B54 B56 60.2(4) . . ? B55 B54 B53 107.8(4) . . ? B56 B54 B53 60.2(4) . . ? B55 B54 B50 60.2(3) . . ? B56 B54 B50 108.3(4) . . ? B53 B54 B50 106.9(4) . . ? B55 B54 B49 108.6(4) . . ? B56 B54 B49 109.0(4) . . ? B53 B54 B49 59.8(3) . . ? B50 B54 B49 59.8(3) . . ? C46 B55 B51 59.5(3) . . ? C46 B55 B54 104.6(4) . . ? B51 B55 B54 108.4(5) . . ? C46 B55 B56 105.2(4) . . ? B51 B55 B56 60.2(4) . . ? B54 B55 B56 59.9(4) . . ? C46 B55 B50 58.0(3) . . ? B51 B55 B50 108.3(4) . . ? B54 B55 B50 60.3(3) . . ? B56 B55 B50 108.1(4) . . ? B52 B56 B51 59.3(4) . . ? B52 B56 B54 107.6(4) . . ? B51 B56 B54 107.5(4) . . ? B52 B56 B55 106.3(4) . . ? B51 B56 B55 59.2(4) . . ? B54 B56 B55 59.9(4) . . ? B52 B56 B53 60.1(4) . . ? B51 B56 B53 107.7(4) . . ? B54 B56 B53 60.1(4) . . ? B55 B56 B53 107.4(4) . . ? C59 Co57 C70 100.9(2) . . ? C59 Co57 C69 99.7(2) . . ? C70 Co57 C69 46.15(18) . . ? C59 Co57 C58 45.5(2) . . ? C70 Co57 C58 133.5(2) . . ? C69 Co57 C58 100.7(2) . . ? C59 Co57 B71 131.6(3) . . ? C70 Co57 B71 48.5(2) . . ? C69 Co57 B71 83.6(2) . . ? C58 Co57 B71 175.0(2) . . ? C59 Co57 B62 82.1(2) . . ? C70 Co57 B62 176.4(2) . . ? C69 Co57 B62 131.6(2) . . ? C58 Co57 B62 47.8(2) . . ? B71 Co57 B62 130.6(3) . . ? C59 Co57 B73 129.5(3) . . ? C70 Co57 B73 82.3(2) . . ? C69 Co57 B73 47.8(2) . . ? C58 Co57 B73 96.8(2) . . ? B71 Co57 B73 87.9(3) . . ? B62 Co57 B73 94.2(2) . . ? C59 Co57 B60 48.8(3) . . ? C70 Co57 B60 97.3(2) . . ? C69 Co57 B60 130.9(2) . . ? C58 Co57 B60 82.2(3) . . ? B71 Co57 B60 93.1(3) . . ? B62 Co57 B60 86.2(2) . . ? B73 Co57 B60 178.3(3) . . ? C59 Co57 B72 175.4(2) . . ? C70 Co57 B72 83.7(2) . . ? C69 Co57 B72 83.8(2) . . ? C58 Co57 B72 131.1(2) . . ? B71 Co57 B72 51.6(3) . . ? B62 Co57 B72 93.3(3) . . ? B73 Co57 B72 51.2(2) . . ? B60 Co57 B72 130.5(3) . . ? C59 Co57 B61 83.4(3) . . ? C70 Co57 B61 131.6(2) . . ? C69 Co57 B61 176.4(2) . . ? C58 Co57 B61 82.8(2) . . ? B71 Co57 B61 93.0(3) . . ? B62 Co57 B61 50.4(3) . . ? B73 Co57 B61 131.2(3) . . ? B60 Co57 B61 50.2(3) . . ? B72 Co57 B61 93.2(3) . . ? C59 C58 B67 111.1(4) . . ? C59 C58 B62 112.4(4) . . ? B67 C58 B62 65.3(4) . . ? C59 C58 B63 61.7(4) . . ? B67 C58 B63 61.2(4) . . ? B62 C58 B63 115.9(4) . . ? C59 C58 Co57 67.0(3) . . ? B67 C58 Co57 126.1(4) . . ? B62 C58 Co57 66.9(3) . . ? B63 C58 Co57 124.8(4) . . ? C58 C59 B64 111.4(5) . . ? C58 C59 B60 111.4(4) . . ? B64 C59 B60 62.7(5) . . ? C58 C59 B63 63.7(4) . . ? B64 C59 B63 61.0(4) . . ? B60 C59 B63 114.1(5) . . ? C58 C59 Co57 67.5(3) . . ? B64 C59 Co57 124.4(5) . . ? B60 C59 Co57 66.8(3) . . ? B63 C59 Co57 127.1(4) . . ? C59 B60 B65 103.8(5) . . ? C59 B60 B64 58.6(4) . . ? B65 B60 B64 59.2(5) . . ? C59 B60 B61 104.9(4) . . ? B65 B60 B61 60.9(4) . . ? B64 B60 B61 108.5(5) . . ? C59 B60 Co57 64.4(3) . . ? B65 B60 Co57 119.3(4) . . ? B64 B60 Co57 118.5(5) . . ? B61 B60 Co57 65.7(3) . . ? B60 B61 B62 105.9(5) . . ? B60 B61 B66 106.0(5) . . ? B62 B61 B66 59.6(4) . . ? B60 B61 B65 58.7(4) . . ? B62 B61 B65 106.9(5) . . ? B66 B61 B65 59.8(4) . . ? B60 B61 Co57 64.1(3) . . ? B62 B61 Co57 63.9(3) . . ? B66 B61 Co57 116.4(4) . . ? B65 B61 Co57 116.1(4) . . ? C58 B62 B66 102.8(4) . . ? C58 B62 B61 105.4(4) . . ? B66 B62 B61 60.2(4) . . ? C58 B62 B67 56.9(4) . . ? B66 B62 B67 59.0(4) . . ? B61 B62 B67 107.4(5) . . ? C58 B62 Co57 65.3(3) . . ? B66 B62 Co57 118.4(4) . . ? B61 B62 Co57 65.7(3) . . ? B67 B62 Co57 117.3(4) . . ? C59 B63 B67 101.9(4) . . ? C59 B63 B64 59.3(4) . . ? B67 B63 B64 108.0(5) . . ? C59 B63 C58 54.6(3) . . ? B67 B63 C58 57.0(4) . . ? B64 B63 C58 102.9(5) . . ? C59 B63 B68 104.6(5) . . ? B67 B63 B68 59.8(4) . . ? B64 B63 B68 60.9(4) . . ? C58 B63 B68 102.6(5) . . ? C59 B64 B63 59.7(4) . . ? C59 B64 B65 104.3(5) . . ? B63 B64 B65 109.2(5) . . ? C59 B64 B60 58.7(4) . . ? B63 B64 B60 109.7(5) . . ? B65 B64 B60 59.6(4) . . ? C59 B64 B68 104.7(5) . . ? B63 B64 B68 60.7(4) . . ? B65 B64 B68 59.6(4) . . ? B60 B64 B68 107.5(5) . . ? B64 B65 B60 61.2(5) . . ? B64 B65 B68 61.3(5) . . ? B60 B65 B68 110.1(5) . . ? B64 B65 B66 107.1(5) . . ? B60 B65 B66 107.5(5) . . ? B68 B65 B66 58.4(4) . . ? B64 B65 B61 109.6(5) . . ? B60 B65 B61 60.4(4) . . ? B68 B65 B61 108.7(5) . . ? B66 B65 B61 60.0(4) . . ? B68 B66 B67 60.3(4) . . ? B68 B66 B62 110.3(5) . . ? B67 B66 B62 61.2(4) . . ? B68 B66 B65 59.9(4) . . ? B67 B66 B65 106.9(5) . . ? B62 B66 B65 107.6(5) . . ? B68 B66 B61 110.0(5) . . ? B67 B66 B61 109.1(5) . . ? B62 B66 B61 60.1(4) . . ? B65 B66 B61 60.2(4) . . ? C58 B67 B63 61.8(4) . . ? C58 B67 B68 107.2(5) . . ? B63 B67 B68 61.3(4) . . ? C58 B67 B66 104.2(5) . . ? B63 B67 B66 108.7(5) . . ? B68 B67 B66 58.8(4) . . ? C58 B67 B62 57.8(3) . . ? B63 B67 B62 110.2(5) . . ? B68 B67 B62 108.0(5) . . ? B66 B67 B62 59.8(4) . . ? B66 B68 B65 61.7(4) . . ? B66 B68 B67 60.9(4) . . ? B65 B68 B67 108.7(5) . . ? B66 B68 B63 108.3(5) . . ? B65 B68 B63 106.9(5) . . ? B67 B68 B63 58.8(4) . . ? B66 B68 B64 107.9(5) . . ? B65 B68 B64 59.1(5) . . ? B67 B68 B64 105.2(5) . . ? B63 B68 B64 58.3(4) . . ? C70 C69 B78 110.9(4) . . ? C70 C69 B73 111.8(4) . . ? B78 C69 B73 64.4(3) . . ? C70 C69 B74 61.0(3) . . ? B78 C69 B74 62.3(3) . . ? B73 C69 B74 116.0(4) . . ? C70 C69 Co57 66.9(2) . . ? B78 C69 Co57 125.6(3) . . ? B73 C69 Co57 67.0(2) . . ? B74 C69 Co57 124.3(3) . . ? C69 C70 B75 112.5(4) . . ? C69 C70 B71 112.7(4) . . ? B75 C70 B71 64.5(4) . . ? C69 C70 B74 63.2(3) . . ? B75 C70 B74 62.2(4) . . ? B71 C70 B74 117.0(5) . . ? C69 C70 Co57 67.0(2) . . ? B75 C70 Co57 125.3(4) . . ? B71 C70 Co57 66.5(3) . . ? B74 C70 Co57 126.4(3) . . ? C70 B71 B76 101.4(5) . . ? C70 B71 B75 57.4(4) . . ? B76 B71 B75 58.6(4) . . ? C70 B71 B72 104.1(4) . . ? B76 B71 B72 59.7(4) . . ? B75 B71 B72 107.4(5) . . ? C70 B71 Co57 65.0(3) . . ? B76 B71 Co57 116.8(4) . . ? B75 B71 Co57 117.6(4) . . ? B72 B71 Co57 64.8(3) . . ? B76 B72 B77 59.0(4) . . ? B76 B72 B73 105.3(5) . . ? B77 B72 B73 58.9(3) . . ? B76 B72 B71 59.7(4) . . ? B77 B72 B71 106.6(5) . . ? B73 B72 B71 105.7(4) . . ? B76 B72 Co57 115.7(4) . . ? B77 B72 Co57 115.9(4) . . ? B73 B72 Co57 63.9(3) . . ? B71 B72 Co57 63.6(3) . . ? C69 B73 B77 103.7(4) . . ? C69 B73 B78 57.5(3) . . ? B77 B73 B78 59.9(4) . . ? C69 B73 B72 105.6(4) . . ? B77 B73 B72 60.5(3) . . ? B78 B73 B72 108.7(4) . . ? C69 B73 Co57 65.2(2) . . ? B77 B73 Co57 118.0(4) . . ? B78 B73 Co57 117.8(3) . . ? B72 B73 Co57 64.9(3) . . ? C70 B74 C69 55.8(3) . . ? C70 B74 B75 58.3(4) . . ? C69 B74 B75 103.4(4) . . ? C70 B74 B79 104.9(5) . . ? C69 B74 B79 103.6(5) . . ? B75 B74 B79 61.6(4) . . ? C70 B74 B78 102.3(4) . . ? C69 B74 B78 56.8(3) . . ? B75 B74 B78 108.5(5) . . ? B79 B74 B78 60.3(4) . . ? C70 B75 B74 59.5(4) . . ? C70 B75 B76 103.6(4) . . ? B74 B75 B76 108.0(5) . . ? C70 B75 B79 104.1(4) . . ? B74 B75 B79 59.5(4) . . ? B76 B75 B79 60.3(4) . . ? C70 B75 B71 58.2(3) . . ? B74 B75 B71 109.4(4) . . ? B76 B75 B71 60.6(4) . . ? B79 B75 B71 109.3(5) . . ? B75 B76 B77 108.4(5) . . ? B75 B76 B79 60.8(4) . . ? B77 B76 B79 60.1(4) . . ? B75 B76 B71 60.7(4) . . ? B77 B76 B71 108.5(4) . . ? B79 B76 B71 109.8(5) . . ? B75 B76 B72 109.7(5) . . ? B77 B76 B72 60.6(4) . . ? B79 B76 B72 110.1(5) . . ? B71 B76 B72 60.5(4) . . ? B76 B77 B73 107.7(4) . . ? B76 B77 B78 106.9(5) . . ? B73 B77 B78 60.2(4) . . ? B76 B77 B79 60.3(4) . . ? B73 B77 B79 108.7(5) . . ? B78 B77 B79 59.6(4) . . ? B76 B77 B72 60.4(4) . . ? B73 B77 B72 60.6(3) . . ? B78 B77 B72 109.0(4) . . ? B79 B77 B72 110.1(5) . . ? C69 B78 B74 60.9(3) . . ? C69 B78 B79 106.3(4) . . ? B74 B78 B79 59.8(4) . . ? C69 B78 B77 104.2(4) . . ? B74 B78 B77 108.2(4) . . ? B79 B78 B77 60.5(4) . . ? C69 B78 B73 58.1(3) . . ? B74 B78 B73 109.6(4) . . ? B79 B78 B73 109.2(5) . . ? B77 B78 B73 59.9(3) . . ? B74 B79 B78 59.9(4) . . ? B74 B79 B77 107.9(5) . . ? B78 B79 B77 60.0(4) . . ? B74 B79 B76 106.5(5) . . ? B78 B79 B76 106.7(5) . . ? B77 B79 B76 59.6(4) . . ? B74 B79 B75 58.9(4) . . ? B78 B79 B75 106.0(4) . . ? B77 B79 B75 106.5(5) . . ? B76 B79 B75 59.0(4) . . ? C93 Co80 C92 46.8(3) . . ? C93 Co80 C81 130.1(2) . . ? C92 Co80 C81 98.9(2) . . ? C93 Co80 C82 97.5(2) . . ? C92 Co80 C82 100.0(2) . . ? C81 Co80 C82 46.7(2) . . ? C93 Co80 B96 82.4(3) . . ? C92 Co80 B96 47.8(2) . . ? C81 Co80 B96 99.1(2) . . ? C82 Co80 B96 133.4(2) . . ? C93 Co80 B94 49.4(3) . . ? C92 Co80 B94 84.3(3) . . ? C81 Co80 B94 174.2(2) . . ? C82 Co80 B94 128.1(2) . . ? B96 Co80 B94 86.7(3) . . ? C93 Co80 B85 175.9(3) . . ? C92 Co80 B85 129.0(2) . . ? C81 Co80 B85 48.0(2) . . ? C82 Co80 B85 83.1(2) . . ? B96 Co80 B85 94.2(2) . . ? B94 Co80 B85 133.0(3) . . ? C93 Co80 B84 132.8(3) . . ? C92 Co80 B84 175.9(2) . . ? C81 Co80 B84 84.0(2) . . ? C82 Co80 B84 84.1(3) . . ? B96 Co80 B84 129.1(3) . . ? B94 Co80 B84 93.1(3) . . ? B85 Co80 B84 51.3(2) . . ? C93 Co80 B83 96.5(3) . . ? C92 Co80 B83 132.3(3) . . ? C81 Co80 B83 82.9(2) . . ? C82 Co80 B83 48.2(3) . . ? B96 Co80 B83 178.1(3) . . ? B94 Co80 B83 91.4(3) . . ? B85 Co80 B83 87.0(2) . . ? B84 Co80 B83 50.8(3) . . ? C93 Co80 B95 84.0(3) . . ? C92 Co80 B95 83.3(2) . . ? C81 Co80 B95 134.0(2) . . ? C82 Co80 B95 176.6(2) . . ? B96 Co80 B95 49.7(2) . . ? B94 Co80 B95 51.1(2) . . ? B85 Co80 B95 95.6(2) . . ? B84 Co80 B95 92.6(3) . . ? B83 Co80 B95 128.6(3) . . ? C82 C81 B85 112.2(4) . . ? C82 C81 B90 112.1(4) . . ? B85 C81 B90 63.1(4) . . ? C82 C81 B86 63.3(4) . . ? B85 C81 B86 114.6(5) . . ? B90 C81 B86 61.4(4) . . ? C82 C81 Co80 66.9(3) . . ? B85 C81 Co80 67.1(3) . . ? B90 C81 Co80 124.7(4) . . ? B86 C81 Co80 125.9(4) . . ? C81 C82 B87 110.0(5) . . ? C81 C82 B83 111.3(4) . . ? B87 C82 B83 63.6(4) . . ? C81 C82 B86 61.3(4) . . ? B87 C82 B86 61.0(4) . . ? B83 C82 B86 114.1(5) . . ? C81 C82 Co80 66.4(3) . . ? B87 C82 Co80 124.6(5) . . ? B83 C82 Co80 67.3(3) . . ? B86 C82 Co80 123.6(4) . . ? C82 B83 B87 57.6(4) . . ? C82 B83 B88 103.7(5) . . ? B87 B83 B88 60.1(5) . . ? C82 B83 B84 105.3(4) . . ? B87 B83 B84 108.2(5) . . ? B88 B83 B84 59.7(4) . . ? C82 B83 Co80 64.4(3) . . ? B87 B83 Co80 116.7(4) . . ? B88 B83 Co80 116.6(4) . . ? B84 B83 Co80 64.5(3) . . ? B88 B84 B89 59.4(4) . . ? B88 B84 B83 59.7(4) . . ? B89 B84 B83 106.9(5) . . ? B88 B84 B85 104.8(5) . . ? B89 B84 B85 58.0(4) . . ? B83 B84 B85 105.7(5) . . ? B88 B84 Co80 116.8(5) . . ? B89 B84 Co80 115.7(4) . . ? B83 B84 Co80 64.7(3) . . ? B85 B84 Co80 63.8(3) . . ? C81 B85 B89 105.2(4) . . ? C81 B85 B90 59.0(4) . . ? B89 B85 B90 60.2(4) . . ? C81 B85 B84 105.4(4) . . ? B89 B85 B84 60.4(3) . . ? B90 B85 B84 108.9(4) . . ? C81 B85 Co80 64.9(3) . . ? B89 B85 Co80 118.7(4) . . ? B90 B85 Co80 119.1(4) . . ? B84 B85 Co80 64.9(3) . . ? C81 B86 B87 102.2(5) . . ? C81 B86 B90 58.5(4) . . ? B87 B86 B90 108.4(6) . . ? C81 B86 B91 103.7(5) . . ? B87 B86 B91 61.0(5) . . ? B90 B86 B91 60.2(4) . . ? C81 B86 C82 55.5(3) . . ? B87 B86 C82 57.2(4) . . ? B90 B86 C82 103.5(5) . . ? B91 B86 C82 103.8(5) . . ? C82 B87 B86 61.8(4) . . ? C82 B87 B91 106.4(5) . . ? B86 B87 B91 59.8(5) . . ? C82 B87 B83 58.8(4) . . ? B86 B87 B83 110.8(5) . . ? B91 B87 B83 108.1(6) . . ? C82 B87 B88 104.6(5) . . ? B86 B87 B88 107.5(6) . . ? B91 B87 B88 58.7(5) . . ? B83 B87 B88 60.1(4) . . ? B91 B88 B89 60.7(4) . . ? B91 B88 B87 60.5(5) . . ? B89 B88 B87 108.0(6) . . ? B91 B88 B84 110.2(5) . . ? B89 B88 B84 60.4(4) . . ? B87 B88 B84 108.7(5) . . ? B91 B88 B83 109.4(6) . . ? B89 B88 B83 108.3(4) . . ? B87 B88 B83 59.8(5) . . ? B84 B88 B83 60.5(4) . . ? B85 B89 B90 60.5(4) . . ? B85 B89 B88 108.1(5) . . ? B90 B89 B88 106.8(6) . . ? B85 B89 B91 108.1(5) . . ? B90 B89 B91 59.6(4) . . ? B88 B89 B91 59.0(5) . . ? B85 B89 B84 61.5(3) . . ? B90 B89 B84 110.0(5) . . ? B88 B89 B84 60.2(4) . . ? B91 B89 B84 108.6(5) . . ? C81 B90 B86 60.1(4) . . ? C81 B90 B91 104.9(5) . . ? B86 B90 B91 60.1(5) . . ? C81 B90 B89 103.6(5) . . ? B86 B90 B89 109.1(5) . . ? B91 B90 B89 60.7(4) . . ? C81 B90 B85 57.9(3) . . ? B86 B90 B85 109.2(5) . . ? B91 B90 B85 108.0(5) . . ? B89 B90 B85 59.3(4) . . ? B88 B91 B86 108.7(6) . . ? B88 B91 B90 108.1(5) . . ? B86 B91 B90 59.7(4) . . ? B88 B91 B89 60.3(5) . . ? B86 B91 B89 108.0(5) . . ? B90 B91 B89 59.8(4) . . ? B88 B91 B87 60.8(5) . . ? B86 B91 B87 59.2(5) . . ? B90 B91 B87 106.5(5) . . ? B89 B91 B87 108.0(5) . . ? C93 C92 B96 110.7(5) . . ? C93 C92 B101 111.7(5) . . ? B96 C92 B101 63.6(4) . . ? C93 C92 B97 63.3(4) . . ? B96 C92 B97 112.7(5) . . ? B101 C92 B97 60.2(5) . . ? C93 C92 Co80 66.6(3) . . ? B96 C92 Co80 66.6(3) . . ? B101 C92 Co80 124.9(4) . . ? B97 C92 Co80 125.1(4) . . ? C92 C93 B98 110.6(5) . . ? C92 C93 B94 111.3(5) . . ? B98 C93 B94 62.4(4) . . ? C92 C93 B97 61.1(4) . . ? B98 C93 B97 62.2(4) . . ? B94 C93 B97 114.1(5) . . ? C92 C93 Co80 66.6(3) . . ? B98 C93 Co80 122.6(5) . . ? B94 C93 Co80 66.3(3) . . ? B97 C93 Co80 123.2(5) . . ? C93 B94 B98 58.3(4) . . ? C93 B94 B99 103.5(5) . . ? B98 B94 B99 58.7(4) . . ? C93 B94 B95 104.1(4) . . ? B98 B94 B95 105.6(4) . . ? B99 B94 B95 58.9(4) . . ? C93 B94 Co80 64.3(3) . . ? B98 B94 Co80 117.2(4) . . ? B99 B94 Co80 117.5(4) . . ? B95 B94 Co80 65.5(3) . . ? B96 B95 B99 107.4(5) . . ? B96 B95 B100 59.7(4) . . ? B99 B95 B100 60.2(4) . . ? B96 B95 B94 105.7(4) . . ? B99 B95 B94 60.5(4) . . ? B100 B95 B94 107.7(5) . . ? B96 B95 Co80 63.6(3) . . ? B99 B95 Co80 117.1(4) . . ? B100 B95 Co80 116.6(4) . . ? B94 B95 Co80 63.5(3) . . ? C92 B96 B95 108.0(4) . . ? C92 B96 B100 105.6(5) . . ? B95 B96 B100 60.8(4) . . ? C92 B96 B101 59.4(4) . . ? B95 B96 B101 109.9(5) . . ? B100 B96 B101 59.6(4) . . ? C92 B96 Co80 65.7(3) . . ? B95 B96 Co80 66.7(3) . . ? B100 B96 Co80 120.3(4) . . ? B101 B96 Co80 120.4(4) . . ? B102 B97 B101 62.4(5) . . ? B102 B97 C92 106.1(6) . . ? B101 B97 C92 59.3(4) . . ? B102 B97 C93 104.7(6) . . ? B101 B97 C93 104.7(5) . . ? C92 B97 C93 55.6(4) . . ? B102 B97 B98 59.8(5) . . ? B101 B97 B98 108.7(6) . . ? C92 B97 B98 102.3(5) . . ? C93 B97 B98 57.5(4) . . ? C93 B98 B102 105.5(5) . . ? C93 B98 B99 106.3(5) . . ? B102 B98 B99 61.4(4) . . ? C93 B98 B94 59.2(4) . . ? B102 B98 B94 110.7(5) . . ? B99 B98 B94 61.4(4) . . ? C93 B98 B97 60.3(4) . . ? B102 B98 B97 57.9(5) . . ? B99 B98 B97 108.0(5) . . ? B94 B98 B97 109.9(5) . . ? B98 B99 B95 108.0(5) . . ? B98 B99 B100 106.1(6) . . ? B95 B99 B100 60.0(4) . . ? B98 B99 B102 59.2(5) . . ? B95 B99 B102 107.9(5) . . ? B100 B99 B102 59.1(5) . . ? B98 B99 B94 60.0(4) . . ? B95 B99 B94 60.7(3) . . ? B100 B99 B94 107.7(5) . . ? B102 B99 B94 107.7(5) . . ? B101 B100 B96 60.6(4) . . ? B101 B100 B102 60.8(5) . . ? B96 B100 B102 108.0(5) . . ? B101 B100 B95 109.7(5) . . ? B96 B100 B95 59.5(3) . . ? B102 B100 B95 109.0(5) . . ? B101 B100 B99 109.6(6) . . ? B96 B100 B99 106.9(4) . . ? B102 B100 B99 60.7(4) . . ? B95 B100 B99 59.8(4) . . ? C92 B101 B97 60.5(4) . . ? C92 B101 B100 103.9(5) . . ? B97 B101 B100 107.5(6) . . ? C92 B101 B96 57.1(3) . . ? B97 B101 B96 107.7(5) . . ? B100 B101 B96 59.8(4) . . ? C92 B101 B102 104.3(6) . . ? B97 B101 B102 58.7(5) . . ? B100 B101 B102 59.8(5) . . ? B96 B101 B102 106.6(5) . . ? B97 B102 B98 62.3(5) . . ? B97 B102 B100 107.3(5) . . ? B98 B102 B100 107.0(5) . . ? B97 B102 B101 58.9(5) . . ? B98 B102 B101 108.0(5) . . ? B100 B102 B101 59.4(5) . . ? B97 B102 B99 109.8(5) . . ? B98 B102 B99 59.4(4) . . ? B100 B102 B99 60.2(4) . . ? B101 B102 B99 108.1(5) . . ? C115 Co10 C116 46.3(2) . . ? C115 Co10 C104 100.5(2) . . ? C116 Co10 C104 135.0(2) . . ? C115 Co10 C105 98.77(19) . . ? C116 Co10 C105 101.45(19) . . ? C104 Co10 C105 46.64(18) . . ? C115 Co10 B108 132.9(2) . . ? C116 Co10 B108 174.8(2) . . ? C104 Co10 B108 49.0(2) . . ? C105 Co10 B108 83.8(2) . . ? C115 Co10 B117 83.0(2) . . ? C116 Co10 B117 48.4(2) . . ? C104 Co10 B117 176.4(2) . . ? C105 Co10 B117 134.2(2) . . ? B108 Co10 B117 127.7(2) . . ? C115 Co10 B106 128.5(2) . . ? C116 Co10 B106 96.1(2) . . ? C104 Co10 B106 83.2(2) . . ? C105 Co10 B106 48.2(2) . . ? B108 Co10 B106 87.7(3) . . ? B117 Co10 B106 95.5(2) . . ? C115 Co10 B119 47.9(2) . . ? C116 Co10 B119 82.6(2) . . ? C104 Co10 B119 94.5(2) . . ? C105 Co10 B119 127.6(2) . . ? B108 Co10 B119 93.9(3) . . ? B117 Co10 B119 87.0(2) . . ? B106 Co10 B119 175.3(2) . . ? C115 Co10 B107 174.8(2) . . ? C116 Co10 B107 128.8(2) . . ? C104 Co10 B107 84.6(2) . . ? C105 Co10 B107 83.7(2) . . ? B108 Co10 B107 51.7(3) . . ? B117 Co10 B107 92.0(2) . . ? B106 Co10 B107 50.4(2) . . ? B119 Co10 B107 133.5(3) . . ? C115 Co10 B118 83.4(2) . . ? C116 Co10 B118 84.0(2) . . ? C104 Co10 B118 127.7(2) . . ? C105 Co10 B118 174.1(2) . . ? B108 Co10 B118 90.8(2) . . ? B117 Co10 B118 51.4(2) . . ? B106 Co10 B118 134.0(2) . . ? B119 Co10 B118 50.4(2) . . ? B107 Co10 B118 94.6(2) . . ? C105 C104 B113 110.8(4) . . ? C105 C104 B108 111.8(4) . . ? B113 C104 B108 64.0(3) . . ? C105 C104 B109 61.9(3) . . ? B113 C104 B109 61.8(3) . . ? B108 C104 B109 115.7(4) . . ? C105 C104 Co10 66.9(2) . . ? B113 C104 Co10 124.7(4) . . ? B108 C104 Co10 66.6(2) . . ? B109 C104 Co10 124.9(3) . . ? C104 C105 B106 112.2(4) . . ? C104 C105 B110 112.3(4) . . ? B106 C105 B110 63.5(3) . . ? C104 C105 B109 62.5(3) . . ? B106 C105 B109 115.3(4) . . ? B110 C105 B109 62.3(3) . . ? C104 C105 Co10 66.5(2) . . ? B106 C105 Co10 67.5(2) . . ? B110 C105 Co10 125.4(3) . . ? B109 C105 Co10 125.1(3) . . ? C105 B106 B111 103.9(4) . . ? C105 B106 B110 58.4(3) . . ? B111 B106 B110 59.5(3) . . ? C105 B106 B107 105.5(4) . . ? B111 B106 B107 61.1(4) . . ? B110 B106 B107 109.3(4) . . ? C105 B106 Co10 64.4(2) . . ? B111 B106 Co10 118.5(4) . . ? B110 B106 Co10 118.1(3) . . ? B107 B106 Co10 65.1(3) . . ? B106 B107 B112 105.9(4) . . ? B106 B107 B111 58.6(4) . . ? B112 B107 B111 59.6(4) . . ? B106 B107 B108 106.1(4) . . ? B112 B107 B108 59.5(4) . . ? B111 B107 B108 106.7(4) . . ? B106 B107 Co10 64.5(3) . . ? B112 B107 Co10 115.5(4) . . ? B111 B107 Co10 115.9(4) . . ? B108 B107 Co10 63.3(3) . . ? C104 B108 B113 56.8(3) . . ? C104 B108 B112 102.7(4) . . ? B113 B108 B112 59.8(4) . . ? C104 B108 B107 104.3(4) . . ? B113 B108 B107 107.2(4) . . ? B112 B108 B107 59.4(4) . . ? C104 B108 Co10 64.4(2) . . ? B113 B108 Co10 116.2(4) . . ? B112 B108 Co10 116.9(4) . . ? B107 B108 Co10 64.9(3) . . ? C105 B109 B114 103.9(4) . . ? C105 B109 C104 55.7(3) . . ? B114 B109 C104 104.2(4) . . ? C105 B109 B113 102.0(4) . . ? B114 B109 B113 61.2(4) . . ? C104 B109 B113 57.0(3) . . ? C105 B109 B110 58.0(3) . . ? B114 B109 B110 60.6(4) . . ? C104 B109 B110 103.4(4) . . ? B113 B109 B110 108.4(5) . . ? C105 B110 B111 103.7(4) . . ? C105 B110 B114 103.7(4) . . ? B111 B110 B114 61.0(4) . . ? C105 B110 B109 59.7(3) . . ? B111 B110 B109 108.2(5) . . ? B114 B110 B109 58.7(4) . . ? C105 B110 B106 58.1(3) . . ? B111 B110 B106 59.6(3) . . ? B114 B110 B106 108.1(4) . . ? B109 B110 B106 108.8(4) . . ? B110 B111 B106 60.9(3) . . ? B110 B111 B112 108.0(5) . . ? B106 B111 B112 107.5(4) . . ? B110 B111 B114 59.8(4) . . ? B106 B111 B114 108.2(4) . . ? B112 B111 B114 60.0(4) . . ? B110 B111 B107 109.7(4) . . ? B106 B111 B107 60.3(3) . . ? B112 B111 B107 60.0(4) . . ? B114 B111 B107 108.9(5) . . ? B113 B112 B111 106.9(5) . . ? B113 B112 B114 59.4(4) . . ? B111 B112 B114 60.0(4) . . ? B113 B112 B107 108.5(4) . . ? B111 B112 B107 60.4(4) . . ? B114 B112 B107 109.2(5) . . ? B113 B112 B108 59.8(3) . . ? B111 B112 B108 108.6(4) . . ? B114 B112 B108 108.4(4) . . ? B107 B112 B108 61.1(3) . . ? C104 B113 B109 61.2(3) . . ? C104 B113 B114 105.8(4) . . ? B109 B113 B114 59.1(4) . . ? C104 B113 B108 59.2(3) . . ? B109 B113 B108 111.2(4) . . ? B114 B113 B108 109.6(5) . . ? C104 B113 B112 105.0(4) . . ? B109 B113 B112 108.4(5) . . ? B114 B113 B112 60.4(4) . . ? B108 B113 B112 60.4(4) . . ? B109 B114 B110 60.7(4) . . ? B109 B114 B113 59.7(4) . . ? B110 B114 B113 107.3(4) . . ? B109 B114 B111 108.4(4) . . ? B110 B114 B111 59.2(4) . . ? B113 B114 B111 107.5(4) . . ? B109 B114 B112 108.8(4) . . ? B110 B114 B112 107.5(4) . . ? B113 B114 B112 60.2(4) . . ? B111 B114 B112 60.0(4) . . ? C116 C115 B119 112.7(4) . . ? C116 C115 B124 111.4(4) . . ? B119 C115 B124 63.4(4) . . ? C116 C115 B120 62.9(4) . . ? B119 C115 B120 115.0(4) . . ? B124 C115 B120 61.1(4) . . ? C116 C115 Co10 66.9(2) . . ? B119 C115 Co10 68.0(3) . . ? B124 C115 Co10 125.6(4) . . ? B120 C115 Co10 125.9(4) . . ? C115 C116 B121 111.0(4) . . ? C115 C116 B117 112.1(4) . . ? B121 C116 B117 63.7(3) . . ? C115 C116 B120 61.4(4) . . ? B121 C116 B120 62.0(4) . . ? B117 C116 B120 115.3(4) . . ? C115 C116 Co10 66.8(3) . . ? B121 C116 Co10 125.3(4) . . ? B117 C116 Co10 67.6(2) . . ? B120 C116 Co10 124.5(4) . . ? C116 B117 B122 103.6(4) . . ? C116 B117 B121 58.2(3) . . ? B122 B117 B121 60.1(3) . . ? C116 B117 B118 104.2(4) . . ? B122 B117 B118 59.0(3) . . ? B121 B117 B118 107.5(4) . . ? C116 B117 Co10 64.0(2) . . ? B122 B117 Co10 116.8(3) . . ? B121 B117 Co10 117.2(4) . . ? B118 B117 Co10 65.0(2) . . ? B123 B118 B122 59.7(4) . . ? B123 B118 B119 58.6(3) . . ? B122 B118 B119 105.9(4) . . ? B123 B118 B117 106.3(4) . . ? B122 B118 B117 59.3(3) . . ? B119 B118 B117 105.6(4) . . ? B123 B118 Co10 115.8(4) . . ? B122 B118 Co10 115.8(3) . . ? B119 B118 Co10 64.2(2) . . ? B117 B118 Co10 63.6(2) . . ? C115 B119 B123 104.4(4) . . ? C115 B119 B124 58.6(4) . . ? B123 B119 B124 59.9(4) . . ? C115 B119 B118 105.3(4) . . ? B123 B119 B118 59.8(3) . . ? B124 B119 B118 108.3(4) . . ? C115 B119 Co10 64.1(2) . . ? B123 B119 Co10 117.9(4) . . ? B124 B119 Co10 117.7(4) . . ? B118 B119 Co10 65.4(3) . . ? C115 B120 C116 55.8(3) . . ? C115 B120 B124 59.1(4) . . ? C116 B120 B124 104.1(5) . . ? C115 B120 B121 103.4(4) . . ? C116 B120 B121 58.2(3) . . ? B124 B120 B121 108.2(5) . . ? C115 B120 B125 104.0(5) . . ? C116 B120 B125 104.1(5) . . ? B124 B120 B125 59.8(4) . . ? B121 B120 B125 60.5(4) . . ? C116 B121 B120 59.8(3) . . ? C116 B121 B125 105.1(5) . . ? B120 B121 B125 60.2(4) . . ? C116 B121 B122 103.4(4) . . ? B120 B121 B122 107.5(5) . . ? B125 B121 B122 59.3(4) . . ? C116 B121 B117 58.2(3) . . ? B120 B121 B117 109.0(4) . . ? B125 B121 B117 108.1(5) . . ? B122 B121 B117 59.8(3) . . ? B123 B122 B125 59.7(4) . . ? B123 B122 B118 59.9(3) . . ? B125 B122 B118 109.4(5) . . ? B123 B122 B117 108.4(4) . . ? B125 B122 B117 109.1(4) . . ? B118 B122 B117 61.8(3) . . ? B123 B122 B121 107.3(5) . . ? B125 B122 B121 60.2(4) . . ? B118 B122 B121 109.7(4) . . ? B117 B122 B121 60.1(3) . . ? B119 B123 B124 60.8(4) . . ? B119 B123 B125 109.2(5) . . ? B124 B123 B125 59.6(4) . . ? B119 B123 B122 108.7(4) . . ? B124 B123 B122 107.5(5) . . ? B125 B123 B122 60.2(4) . . ? B119 B123 B118 61.5(3) . . ? B124 B123 B118 110.3(4) . . ? B125 B123 B118 110.2(5) . . ? B122 B123 B118 60.4(3) . . ? C115 B124 B120 59.8(4) . . ? C115 B124 B125 106.0(5) . . ? B120 B124 B125 61.7(4) . . ? C115 B124 B123 103.5(5) . . ? B120 B124 B123 109.4(5) . . ? B125 B124 B123 60.2(4) . . ? C115 B124 B119 58.0(3) . . ? B120 B124 B119 109.3(5) . . ? B125 B124 B119 108.6(5) . . ? B123 B124 B119 59.3(4) . . ? B124 B125 B123 60.2(4) . . ? B124 B125 B122 107.8(5) . . ? B123 B125 B122 60.1(4) . . ? B124 B125 B120 58.6(4) . . ? B123 B125 B120 107.0(4) . . ? B122 B125 B120 107.7(4) . . ? B124 B125 B121 106.3(4) . . ? B123 B125 B121 107.8(5) . . ? B122 B125 B121 60.5(4) . . ? B120 B125 B121 59.3(4) . . ? O129 N127 O128 113.0(14) . . ? O129 N127 C126 120.6(14) . . ? O128 N127 C126 118.5(13) . . ? O132 N131 O133 107.2(16) . . ? O132 N131 C130 135.7(16) . . ? O133 N131 C130 112.4(15) . . ? O136 N135 O137 110.7(18) . . ? O136 N135 C134 126.8(18) . . ? O137 N135 C134 120.1(18) . . ? O140 N139 O141 107(2) . . ? O140 N139 C138 120(2) . . ? O141 N139 C138 125(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.95 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.271 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.054 #=END data_c:\datasets\leeds\mh143v~1\mh1431~1\mh143 _database_code_depnum_ccdc_archive 'CCDC 278899' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) bis[di(dicarbollido)cobalt(III)] nitromethane solvate (1/0.75) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H18 Fe N10, 2[C4 H22 B18 Co], 0.75[C H3 N O2]' _chemical_formula_sum 'C30.75 H64.25 B36 Co2 Fe N10.75 O1.50' _chemical_formula_weight 1171.55 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 37.3516(19) _cell_length_b 10.5840(6) _cell_length_c 29.5118(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11666.9(11) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 105918 _cell_measurement_theta_min 1.09 _cell_measurement_theta_max 26.83 _exptl_crystal_description Needle _exptl_crystal_colour Brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4768 _exptl_absorpt_coefficient_mu 0.850 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.735 _exptl_absorpt_correction_T_max 1.008 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 4 kW. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 105918 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 26.83 _reflns_number_total 22460 _reflns_number_gt 18112 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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. The crystal was refined as a racemic twin. The asymmetric unit contains two complex dications, four cobalticarborane anions and two nitromethane molecules. Somewhat high thermal parameters on these residues led us to refine them with partial occupances of 0.9 (C126- O129) and 0.6 (C130-O133) This gives a total solvent content of 1.5 molecules per asymmetric unit, or 0.75 per formula unit. Although discrepancies in the C---N and N---O bond lengths in both solvent sites imply that there may be some site disorder between the C and O atoms in these molecules, attempts to refine this were unsuccessful. So, these molecules were refined as order in the final analysis. No other disorder was detected during refinement and no restraints were applied. All non-H atoms except the 60% occupied solvent site were refined anisotropically. One carbaborane C atom, C70, became non-positive definite during the refinement process, and was restrained so that its individual thermal parameters approximate to isotropic behaviour during the final least squares cycles with a SHELXL ISOR instruction. All H atoms were placed in calculated positions and refined using a riding model, with (partially occupied) methyl groups refined in a fixed, staggered conformation. There are three residual Fourier peaks of between 1.7-2.2 e.\%A^-3^, which are all <=1.1 \%A from one of the metal atoms in the model. ; _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^)+(0.0746P)^2^+87.5581P] 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 0.49(2) _refine_ls_number_reflns 22460 _refine_ls_number_parameters 1477 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.2141 _refine_ls_wR_factor_gt 0.2015 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 Fe1A Fe 0.94097(3) 0.29839(12) 0.21543(4) 0.0251(3) Uani 1 1 d . . . N2A N 0.98492(19) 0.2706(7) 0.2475(3) 0.0326(18) Uani 1 1 d . . . C3A C 1.0139(3) 0.2359(10) 0.2257(4) 0.043(3) Uani 1 1 d . . . C4A C 1.0468(3) 0.2145(11) 0.2489(5) 0.055(3) Uani 1 1 d . . . H4A H 1.0678 0.1894 0.2331 0.067 Uiso 1 1 calc R . . C5A C 1.0469(3) 0.2306(12) 0.2920(6) 0.065(4) Uani 1 1 d . . . H5A H 1.0688 0.2172 0.3076 0.078 Uiso 1 1 calc R . . C6A C 1.0160(3) 0.2677(10) 0.3186(4) 0.044(3) Uani 1 1 d . . . H6A H 1.0165 0.2760 0.3507 0.053 Uiso 1 1 calc R . . C7A C 0.9851(2) 0.2904(9) 0.2926(4) 0.036(2) Uani 1 1 d . . . N8A N 1.0070(2) 0.2296(8) 0.1774(4) 0.048(3) Uani 1 1 d . . . N9A N 0.9733(2) 0.2533(7) 0.1641(3) 0.0321(17) Uani 1 1 d . . . C10A C 0.9739(3) 0.2493(12) 0.1203(4) 0.054(3) Uani 1 1 d . . . H10A H 0.9540 0.2663 0.1013 0.065 Uiso 1 1 calc R . . C11A C 1.0092(3) 0.2155(16) 0.1042(5) 0.076(5) Uani 1 1 d . . . H11A H 1.0168 0.2020 0.0739 0.091 Uiso 1 1 calc R . . C12A C 1.0285(3) 0.2077(13) 0.1413(6) 0.079(5) Uani 1 1 d . . . H12A H 1.0534 0.1898 0.1425 0.094 Uiso 1 1 calc R . . N13A N 0.9515(2) 0.3262(7) 0.3097(3) 0.0319(17) Uani 1 1 d . . . N14A N 0.92498(19) 0.3387(7) 0.2779(2) 0.0272(16) Uani 1 1 d . . . C15A C 0.8962(3) 0.3799(9) 0.3009(3) 0.033(2) Uani 1 1 d . . . H15A H 0.8737 0.4010 0.2879 0.040 Uiso 1 1 calc R . . C16A C 0.9044(3) 0.3866(10) 0.3465(3) 0.040(2) Uani 1 1 d . . . H16A H 0.8886 0.4106 0.3702 0.048 Uiso 1 1 calc R . . C17A C 0.9392(3) 0.3525(10) 0.3511(3) 0.046(3) Uani 1 1 d . . . H17A H 0.9524 0.3481 0.3786 0.055 Uiso 1 1 calc R . . N18A N 0.89629(19) 0.3232(8) 0.1848(2) 0.0298(17) Uani 1 1 d . . . C19A C 0.8724(2) 0.2289(10) 0.1832(3) 0.035(2) Uani 1 1 d . . . C20A C 0.8385(2) 0.2442(12) 0.1624(3) 0.044(3) Uani 1 1 d . . . H20A H 0.8218 0.1765 0.1609 0.052 Uiso 1 1 calc R . . C21A C 0.8307(3) 0.3593(16) 0.1445(4) 0.066(4) Uani 1 1 d . . . H21A H 0.8083 0.3720 0.1298 0.080 Uiso 1 1 calc R . . C22A C 0.8551(4) 0.4597(17) 0.1473(4) 0.076(5) Uani 1 1 d . . . H22A H 0.8497 0.5409 0.1354 0.091 Uiso 1 1 calc R . . C23A C 0.8871(3) 0.4345(10) 0.1681(3) 0.038(2) Uani 1 1 d . . . N24A N 0.8867(2) 0.1178(8) 0.2020(2) 0.0351(19) Uani 1 1 d . . . N25A N 0.92102(19) 0.1279(7) 0.2205(2) 0.0301(17) Uani 1 1 d . . . C26A C 0.9284(3) 0.0093(9) 0.2349(3) 0.037(2) Uani 1 1 d . . . H26A H 0.9509 -0.0157 0.2467 0.045 Uiso 1 1 calc R . . C27A C 0.8990(3) -0.0731(10) 0.2305(4) 0.054(3) Uani 1 1 d . . . H27A H 0.8971 -0.1582 0.2404 0.065 Uiso 1 1 calc R . . C28A C 0.8727(3) 0.0013(11) 0.2075(4) 0.045(3) Uani 1 1 d . . . H28A H 0.8497 -0.0261 0.1979 0.054 Uiso 1 1 calc R . . N29A N 0.9155(2) 0.5224(8) 0.1759(2) 0.039(2) Uani 1 1 d . . . N30A N 0.9451(2) 0.4793(7) 0.1992(2) 0.0325(17) Uani 1 1 d . . . C31A C 0.9663(3) 0.5778(10) 0.2034(4) 0.052(3) Uani 1 1 d . . . H31A H 0.9888 0.5756 0.2185 0.063 Uiso 1 1 calc R . . C32A C 0.9515(4) 0.6908(11) 0.1825(4) 0.061(4) Uani 1 1 d . . . H32A H 0.9617 0.7729 0.1812 0.073 Uiso 1 1 calc R . . C33A C 0.9198(5) 0.6521(12) 0.1653(4) 0.071(5) Uani 1 1 d . . . H33A H 0.9033 0.7030 0.1490 0.086 Uiso 1 1 calc R . . Fe1B Fe 0.79398(3) 0.22987(12) 0.45117(4) 0.0264(3) Uani 1 1 d . . . N2B N 0.8469(2) 0.2145(9) 0.4806(2) 0.0349(19) Uani 1 1 d . . . C3B C 0.8581(3) 0.0997(12) 0.4957(3) 0.046(3) Uani 1 1 d . . . C4B C 0.8931(3) 0.0753(13) 0.5100(3) 0.051(3) Uani 1 1 d . . . H4B H 0.9001 -0.0027 0.5231 0.062 Uiso 1 1 calc R . . C5B C 0.9163(3) 0.1741(13) 0.5034(4) 0.061(3) Uani 1 1 d . . . H5B H 0.9406 0.1614 0.5116 0.074 Uiso 1 1 calc R . . C6B C 0.9070(3) 0.2918(14) 0.4854(4) 0.055(3) Uani 1 1 d . . . H6B H 0.9236 0.3584 0.4806 0.066 Uiso 1 1 calc R . . C7B C 0.8706(2) 0.3004(13) 0.4754(3) 0.045(3) Uani 1 1 d . . . N8B N 0.8303(2) 0.0103(9) 0.4975(2) 0.042(2) Uani 1 1 d . . . N9B N 0.7962(2) 0.0399(9) 0.4815(3) 0.045(2) Uani 1 1 d . . . C10B C 0.7751(4) -0.0649(13) 0.4844(4) 0.071(4) Uani 1 1 d . . . H10B H 0.7507 -0.0725 0.4759 0.085 Uiso 1 1 calc R . . C11B C 0.7981(4) -0.1630(11) 0.5031(4) 0.058(3) Uani 1 1 d . . . H11B H 0.7913 -0.2477 0.5091 0.069 Uiso 1 1 calc R . . C12B C 0.8304(4) -0.1140(12) 0.5105(4) 0.064(4) Uani 1 1 d . . . H12B H 0.8503 -0.1580 0.5228 0.077 Uiso 1 1 calc R . . N13B N 0.8559(2) 0.4123(9) 0.4593(3) 0.040(2) Uani 1 1 d . . . N14B N 0.8195(2) 0.4139(8) 0.4476(3) 0.0342(17) Uani 1 1 d . . . C15B C 0.8122(3) 0.5285(12) 0.4339(4) 0.053(3) Uani 1 1 d . . . H15B H 0.7891 0.5556 0.4246 0.064 Uiso 1 1 calc R . . C16B C 0.8438(3) 0.6101(12) 0.4346(3) 0.048(3) Uani 1 1 d . . . H16B H 0.8457 0.6960 0.4256 0.057 Uiso 1 1 calc R . . C17B C 0.8688(3) 0.5362(12) 0.4507(4) 0.049(3) Uani 1 1 d . . . H17B H 0.8928 0.5623 0.4560 0.059 Uiso 1 1 calc R . . N18B N 0.75320(18) 0.2454(6) 0.4011(2) 0.0193(13) Uani 1 1 d . . . C19B C 0.7206(2) 0.2893(8) 0.4117(3) 0.0254(18) Uani 1 1 d . . . C20B C 0.6922(2) 0.2886(9) 0.3832(3) 0.0301(19) Uani 1 1 d . . . H20B H 0.6691 0.3127 0.3935 0.036 Uiso 1 1 calc R . . C21B C 0.6978(2) 0.2517(8) 0.3386(3) 0.0277(19) Uani 1 1 d . . . H21B H 0.6785 0.2528 0.3177 0.033 Uiso 1 1 calc R . . C22B C 0.7316(2) 0.2133(9) 0.3246(3) 0.0270(18) Uani 1 1 d . . . H22B H 0.7363 0.1900 0.2941 0.032 Uiso 1 1 calc R . . C23B C 0.7579(2) 0.2111(9) 0.3577(3) 0.0259(18) Uani 1 1 d . . . N24B N 0.71856(18) 0.3299(7) 0.4581(2) 0.0248(15) Uani 1 1 d . . . N25B N 0.74734(19) 0.3071(8) 0.4859(3) 0.0326(17) Uani 1 1 d . . . C26B C 0.7382(3) 0.3650(10) 0.5249(3) 0.040(2) Uani 1 1 d . . . H26B H 0.7527 0.3646 0.5513 0.048 Uiso 1 1 calc R . . C27B C 0.7054(3) 0.4252(10) 0.5221(3) 0.043(2) Uani 1 1 d . . . H27B H 0.6937 0.4720 0.5452 0.051 Uiso 1 1 calc R . . C28B C 0.6932(2) 0.4026(10) 0.4785(3) 0.040(2) Uani 1 1 d . . . H28B H 0.6715 0.4320 0.4654 0.048 Uiso 1 1 calc R . . N29B N 0.79418(17) 0.1726(7) 0.3495(2) 0.0245(15) Uani 1 1 d . . . N30B N 0.8172(2) 0.1620(8) 0.3859(3) 0.0342(18) Uani 1 1 d . . . C31B C 0.8480(2) 0.1228(10) 0.3679(3) 0.033(2) Uani 1 1 d . . . H31B H 0.8689 0.1051 0.3852 0.040 Uiso 1 1 calc R . . C32B C 0.8463(3) 0.1104(9) 0.3207(3) 0.035(2) Uani 1 1 d . . . H32B H 0.8649 0.0870 0.3006 0.042 Uiso 1 1 calc R . . C33B C 0.8106(2) 0.1406(9) 0.3099(3) 0.0303(19) Uani 1 1 d . . . H33B H 0.8000 0.1391 0.2807 0.036 Uiso 1 1 calc R . . Co34 Co 0.73590(3) -0.29495(11) 0.31029(3) 0.0217(2) Uani 1 1 d . . . C35 C 0.7556(2) -0.4255(9) 0.2651(3) 0.0262(18) Uani 1 1 d . . . H35 H 0.7328 -0.4877 0.2546 0.031 Uiso 1 1 calc R . . C36 C 0.7590(2) -0.2768(9) 0.2478(3) 0.0268(19) Uani 1 1 d . . . H36 H 0.7383 -0.2327 0.2253 0.032 Uiso 1 1 calc R . . B37 B 0.7790(3) -0.1826(10) 0.2872(3) 0.028(2) Uani 1 1 d . . . H37 H 0.7741 -0.0792 0.2921 0.033 Uiso 1 1 calc R . . B38 B 0.7895(2) -0.2887(11) 0.3346(3) 0.028(2) Uani 1 1 d . . . H38 H 0.7919 -0.2575 0.3708 0.033 Uiso 1 1 calc R . . B39 B 0.7728(2) -0.4437(10) 0.3185(3) 0.029(2) Uani 1 1 d . . . H39 H 0.7636 -0.5142 0.3443 0.035 Uiso 1 1 calc R . . B40 B 0.7870(3) -0.3906(12) 0.2227(3) 0.037(3) Uani 1 1 d . . . H40 H 0.7856 -0.4236 0.1866 0.044 Uiso 1 1 calc R . . B41 B 0.8018(3) -0.2376(12) 0.2369(4) 0.036(3) Uani 1 1 d . . . H41 H 0.8103 -0.1712 0.2094 0.043 Uiso 1 1 calc R . . B42 B 0.8232(3) -0.2429(12) 0.2930(3) 0.031(2) Uani 1 1 d . . . H42 H 0.8461 -0.1800 0.3027 0.038 Uiso 1 1 calc R . . B43 B 0.8187(3) -0.4069(11) 0.3109(4) 0.034(2) Uani 1 1 d . . . H43 H 0.8394 -0.4527 0.3329 0.041 Uiso 1 1 calc R . . B44 B 0.7971(2) -0.4955(10) 0.2683(3) 0.025(2) Uani 1 1 d . . . H44 H 0.8026 -0.5979 0.2617 0.030 Uiso 1 1 calc R . . B45 B 0.8285(3) -0.3754(12) 0.2528(3) 0.033(2) Uani 1 1 d . . . H45 H 0.8551 -0.3979 0.2372 0.040 Uiso 1 1 calc R . . C46 C 0.6834(2) -0.2766(9) 0.2893(3) 0.0253(18) Uani 1 1 d . . . H46 H 0.6831 -0.2943 0.2519 0.030 Uiso 1 1 calc R . . C47 C 0.6999(2) -0.1482(8) 0.3096(3) 0.0280(18) Uani 1 1 d . . . H47 H 0.7109 -0.0733 0.2868 0.034 Uiso 1 1 calc R . . B48 B 0.7199(3) -0.1691(10) 0.3618(4) 0.031(2) Uani 1 1 d . . . H48 H 0.7429 -0.1136 0.3759 0.037 Uiso 1 1 calc R . . B49 B 0.7128(3) -0.3366(10) 0.3742(3) 0.027(2) Uani 1 1 d . . . H49 H 0.7310 -0.3922 0.3969 0.033 Uiso 1 1 calc R . . B50 B 0.6895(2) -0.4017(10) 0.3249(3) 0.026(2) Uani 1 1 d . . . H50 H 0.6925 -0.5028 0.3143 0.031 Uiso 1 1 calc R . . B51 B 0.6541(3) -0.1666(10) 0.3081(4) 0.033(2) Uani 1 1 d . . . H51 H 0.6353 -0.1120 0.2861 0.040 Uiso 1 1 calc R . . B52 B 0.6769(3) -0.0980(10) 0.3553(4) 0.032(2) Uani 1 1 d . . . H52 H 0.6732 0.0038 0.3646 0.039 Uiso 1 1 calc R . . B53 B 0.6823(3) -0.2202(10) 0.3968(3) 0.031(2) Uani 1 1 d . . . H53 H 0.6814 -0.2009 0.4341 0.037 Uiso 1 1 calc R . . B54 B 0.6646(3) -0.3618(11) 0.3739(4) 0.038(3) Uani 1 1 d . . . H54 H 0.6522 -0.4366 0.3958 0.046 Uiso 1 1 calc R . . B55 B 0.6476(2) -0.3245(10) 0.3194(4) 0.029(2) Uani 1 1 d . . . H55 H 0.6239 -0.3749 0.3047 0.035 Uiso 1 1 calc R . . B56 B 0.6427(2) -0.2138(11) 0.3639(3) 0.031(2) Uani 1 1 d . . . H56 H 0.6163 -0.1896 0.3795 0.037 Uiso 1 1 calc R . . Co57 Co 0.66697(3) 0.35916(11) 0.14765(4) 0.0222(2) Uani 1 1 d . . . C58 C 0.6375(2) 0.4966(9) 0.1809(3) 0.029(2) Uani 1 1 d . . . H58 H 0.6355 0.4671 0.2172 0.034 Uiso 1 1 calc R . . C59 C 0.6156(2) 0.4235(9) 0.1425(3) 0.037(2) Uani 1 1 d . . . H59 H 0.5978 0.3417 0.1511 0.044 Uiso 1 1 calc R . . B60 B 0.6389(3) 0.4273(12) 0.0911(4) 0.038(3) Uani 1 1 d . . . H60 H 0.6375 0.3547 0.0636 0.045 Uiso 1 1 calc R . . B61 B 0.6793(3) 0.5088(11) 0.1029(3) 0.033(2) Uani 1 1 d . . . H61 H 0.7050 0.4938 0.0840 0.040 Uiso 1 1 calc R . . B62 B 0.6774(3) 0.5493(11) 0.1632(4) 0.034(2) Uani 1 1 d . . . H62 H 0.7020 0.5594 0.1846 0.041 Uiso 1 1 calc R . . B63 B 0.6004(3) 0.5700(11) 0.1592(4) 0.034(2) Uani 1 1 d . . . H63 H 0.5747 0.5873 0.1776 0.041 Uiso 1 1 calc R . . B64 B 0.6012(3) 0.5290(13) 0.1013(4) 0.045(3) Uani 1 1 d . . . H64 H 0.5757 0.5196 0.0816 0.054 Uiso 1 1 calc R . . B65 B 0.6413(4) 0.5869(12) 0.0770(4) 0.042(3) Uani 1 1 d . . . H65 H 0.6425 0.6179 0.0407 0.051 Uiso 1 1 calc R . . B66 B 0.6648(3) 0.6658(10) 0.1212(4) 0.033(2) Uani 1 1 d . . . H66 H 0.6819 0.7505 0.1145 0.040 Uiso 1 1 calc R . . B67 B 0.6390(3) 0.6528(11) 0.1719(4) 0.035(2) Uani 1 1 d . . . H67 H 0.6388 0.7264 0.1992 0.042 Uiso 1 1 calc R . . B68 B 0.6182(3) 0.6787(10) 0.1189(3) 0.029(2) Uani 1 1 d . . . H68 H 0.6048 0.7703 0.1102 0.035 Uiso 1 1 calc R . . C69 C 0.6588(2) 0.2021(9) 0.1891(3) 0.0275(18) Uani 1 1 d . . . H69 H 0.6332 0.2192 0.2077 0.033 Uiso 1 1 calc R . . C70 C 0.6605(2) 0.1623(8) 0.1370(2) 0.0221(17) Uani 1 1 d U . . H70 H 0.6349 0.1472 0.1180 0.027 Uiso 1 1 calc R . . B71 B 0.6961(3) 0.2325(9) 0.1075(3) 0.028(2) Uani 1 1 d . . . H71 H 0.6972 0.2650 0.0714 0.033 Uiso 1 1 calc R . . B72 B 0.7206(3) 0.3085(11) 0.1535(3) 0.032(2) Uani 1 1 d . . . H72 H 0.7392 0.3900 0.1479 0.038 Uiso 1 1 calc R . . B73 B 0.6946(3) 0.2912(10) 0.2042(3) 0.027(2) Uani 1 1 d . . . H73 H 0.6954 0.3632 0.2320 0.033 Uiso 1 1 calc R . . B74 B 0.6668(3) 0.0460(11) 0.1728(4) 0.040(3) Uani 1 1 d . . . H74 H 0.6486 -0.0368 0.1784 0.048 Uiso 1 1 calc R . . B75 B 0.6922(3) 0.0647(11) 0.1225(4) 0.040(3) Uani 1 1 d . . . H75 H 0.6908 -0.0080 0.0950 0.048 Uiso 1 1 calc R . . B76 B 0.7324(3) 0.1481(12) 0.1345(4) 0.039(3) Uani 1 1 d . . . H76 H 0.7578 0.1288 0.1155 0.046 Uiso 1 1 calc R . . B77 B 0.7313(3) 0.1836(11) 0.1946(3) 0.035(2) Uani 1 1 d . . . H77 H 0.7564 0.1873 0.2153 0.041 Uiso 1 1 calc R . . B78 B 0.6905(3) 0.1249(10) 0.2174(4) 0.032(2) Uani 1 1 d . . . H78 H 0.6878 0.0920 0.2533 0.039 Uiso 1 1 calc R . . B79 B 0.7148(3) 0.0367(12) 0.1760(4) 0.040(3) Uani 1 1 d . . . H79 H 0.7289 -0.0535 0.1845 0.048 Uiso 1 1 calc R . . Co80 Co 0.58287(3) -0.14669(11) 0.50590(4) 0.0226(2) Uani 1 1 d . . . C81 C 0.6162(3) -0.0182(10) 0.4734(3) 0.035(2) Uani 1 1 d . . . H81 H 0.6213 -0.0545 0.4383 0.042 Uiso 1 1 calc R . . C82 C 0.6346(2) -0.0830(9) 0.5179(3) 0.032(2) Uani 1 1 d . . . H82 H 0.6529 -0.1664 0.5147 0.038 Uiso 1 1 calc R . . B83 B 0.6074(3) -0.0762(10) 0.5656(3) 0.027(2) Uani 1 1 d . . . H83 H 0.6067 -0.1456 0.5942 0.032 Uiso 1 1 calc R . . B84 B 0.5682(3) 0.0082(10) 0.5459(3) 0.028(2) Uani 1 1 d . . . H84 H 0.5413 -0.0041 0.5619 0.034 Uiso 1 1 calc R . . B85 B 0.5741(3) 0.0406(10) 0.4859(3) 0.030(2) Uani 1 1 d . . . H85 H 0.5511 0.0492 0.4617 0.036 Uiso 1 1 calc R . . B86 B 0.6522(4) 0.0579(12) 0.4980(5) 0.048(3) Uani 1 1 d . . . H86 H 0.6792 0.0713 0.4821 0.058 Uiso 1 1 calc R . . B87 B 0.6462(3) 0.0261(11) 0.5574(4) 0.035(2) Uani 1 1 d . . . H87 H 0.6700 0.0203 0.5803 0.042 Uiso 1 1 calc R . . B88 B 0.6033(3) 0.0887(11) 0.5752(3) 0.035(3) Uani 1 1 d . . . H88 H 0.5989 0.1258 0.6103 0.042 Uiso 1 1 calc R . . B89 B 0.5831(3) 0.1615(10) 0.5267(4) 0.035(3) Uani 1 1 d . . . H89 H 0.5654 0.2467 0.5297 0.042 Uiso 1 1 calc R . . B90 B 0.6134(3) 0.1391(11) 0.4795(3) 0.033(2) Uani 1 1 d . . . H90 H 0.6156 0.2083 0.4509 0.040 Uiso 1 1 calc R . . B91 B 0.6309(4) 0.1728(13) 0.5345(4) 0.046(3) Uani 1 1 d . . . H91 H 0.6441 0.2648 0.5430 0.056 Uiso 1 1 calc R . . C92 C 0.5930(2) -0.3035(8) 0.4663(3) 0.0300(19) Uani 1 1 d . . . H92 H 0.6195 -0.2872 0.4495 0.036 Uiso 1 1 calc R . . C93 C 0.5891(2) -0.3385(8) 0.5186(3) 0.032(2) Uani 1 1 d . . . H93 H 0.6137 -0.3521 0.5398 0.038 Uiso 1 1 calc R . . B94 B 0.5525(2) -0.2699(10) 0.5427(4) 0.029(2) Uani 1 1 d . . . H94 H 0.5503 -0.2327 0.5781 0.034 Uiso 1 1 calc R . . B95 B 0.5280(3) -0.2034(11) 0.4965(4) 0.034(2) Uani 1 1 d . . . H95 H 0.5078 -0.1257 0.5004 0.041 Uiso 1 1 calc R . . B96 B 0.5564(3) -0.2166(11) 0.4488(3) 0.032(2) Uani 1 1 d . . . H96 H 0.5565 -0.1442 0.4211 0.039 Uiso 1 1 calc R . . B97 B 0.5841(3) -0.4579(12) 0.4814(3) 0.036(2) Uani 1 1 d . . . H97 H 0.6025 -0.5401 0.4761 0.043 Uiso 1 1 calc R . . B98 B 0.5564(3) -0.4351(11) 0.5319(4) 0.039(3) Uani 1 1 d . . . H98 H 0.5568 -0.5043 0.5606 0.046 Uiso 1 1 calc R . . B99 B 0.5164(3) -0.3553(12) 0.5162(4) 0.039(3) Uani 1 1 d . . . H99 H 0.4904 -0.3740 0.5338 0.047 Uiso 1 1 calc R . . B100 B 0.5205(3) -0.3212(12) 0.4560(4) 0.040(3) Uani 1 1 d . . . H100 H 0.4968 -0.3166 0.4329 0.048 Uiso 1 1 calc R . . B101 B 0.5609(3) -0.3847(11) 0.4363(4) 0.038(3) Uani 1 1 d . . . H101 H 0.5642 -0.4211 0.4010 0.045 Uiso 1 1 calc R . . B102 B 0.5361(3) -0.4687(14) 0.4776(4) 0.046(3) Uani 1 1 d . . . H102 H 0.5224 -0.5605 0.4700 0.056 Uiso 1 1 calc R . . Co10 Co 0.50924(3) 0.20530(11) 0.35148(4) 0.0220(2) Uani 1 1 d . . . C104 C 0.5461(2) 0.3471(8) 0.3520(3) 0.0254(17) Uani 1 1 d . . . H104 H 0.5372 0.4166 0.3783 0.031 Uiso 1 1 calc R . . C105 C 0.5624(2) 0.2123(9) 0.3660(3) 0.0270(18) Uani 1 1 d . . . H105 H 0.5649 0.1849 0.4025 0.032 Uiso 1 1 calc R . . B106 B 0.5527(3) 0.0973(9) 0.3278(3) 0.028(2) Uani 1 1 d . . . H106 H 0.5494 -0.0058 0.3351 0.033 Uiso 1 1 calc R . . B107 B 0.5271(3) 0.1754(11) 0.2849(4) 0.032(2) Uani 1 1 d . . . H107 H 0.5069 0.1255 0.2633 0.039 Uiso 1 1 calc R . . B108 B 0.5226(2) 0.3402(10) 0.3025(3) 0.025(2) Uani 1 1 d . . . H108 H 0.4992 0.4004 0.2927 0.030 Uiso 1 1 calc R . . B109 B 0.5923(2) 0.3277(9) 0.3474(3) 0.0216(19) Uani 1 1 d . . . H109 H 0.6132 0.3764 0.3682 0.026 Uiso 1 1 calc R . . B110 B 0.5961(2) 0.1674(9) 0.3316(4) 0.029(2) Uani 1 1 d . . . H110 H 0.6199 0.1104 0.3423 0.035 Uiso 1 1 calc R . . B111 B 0.5744(3) 0.1474(11) 0.2779(3) 0.031(2) Uani 1 1 d . . . H111 H 0.5843 0.0782 0.2520 0.037 Uiso 1 1 calc R . . B112 B 0.5562(3) 0.2989(11) 0.2620(4) 0.033(2) Uani 1 1 d . . . H112 H 0.5540 0.3296 0.2258 0.040 Uiso 1 1 calc R . . B113 B 0.5669(3) 0.4071(11) 0.3064(4) 0.035(2) Uani 1 1 d . . . H113 H 0.5714 0.5103 0.3002 0.042 Uiso 1 1 calc R . . B114 B 0.5990(3) 0.2912(10) 0.2903(4) 0.031(2) Uani 1 1 d . . . H114 H 0.6246 0.3157 0.2726 0.037 Uiso 1 1 calc R . . C115 C 0.4893(2) 0.2182(8) 0.4157(3) 0.0251(18) Uani 1 1 d . . . H115 H 0.5116 0.2579 0.4368 0.030 Uiso 1 1 calc R . . C116 C 0.4914(2) 0.0746(9) 0.3976(3) 0.0290(19) Uani 1 1 d . . . H116 H 0.5145 0.0114 0.4060 0.035 Uiso 1 1 calc R . . B117 B 0.4715(2) 0.0585(8) 0.3456(3) 0.0237(19) Uani 1 1 d . . . H117 H 0.4793 -0.0116 0.3189 0.028 Uiso 1 1 calc R . . B118 B 0.4547(2) 0.2200(10) 0.3329(3) 0.026(2) Uani 1 1 d . . . H118 H 0.4506 0.2576 0.2978 0.031 Uiso 1 1 calc R . . B119 B 0.4682(3) 0.3193(10) 0.3801(4) 0.028(2) Uani 1 1 d . . . H119 H 0.4735 0.4229 0.3766 0.034 Uiso 1 1 calc R . . B120 B 0.4621(3) 0.1080(11) 0.4424(4) 0.034(2) Uani 1 1 d . . . H120 H 0.4650 0.0735 0.4781 0.040 Uiso 1 1 calc R . . B121 B 0.4490(3) 0.0080(12) 0.3965(4) 0.035(2) Uani 1 1 d . . . H121 H 0.4429 -0.0943 0.4025 0.042 Uiso 1 1 calc R . . B122 B 0.4258(3) 0.0960(11) 0.3565(4) 0.035(2) Uani 1 1 d . . . H122 H 0.4041 0.0524 0.3355 0.043 Uiso 1 1 calc R . . B123 B 0.4242(2) 0.2585(11) 0.3777(3) 0.028(2) Uani 1 1 d . . . H123 H 0.4010 0.3230 0.3711 0.034 Uiso 1 1 calc R . . B124 B 0.4476(3) 0.2585(10) 0.4300(3) 0.027(2) Uani 1 1 d . . . H124 H 0.4406 0.3234 0.4586 0.032 Uiso 1 1 calc R . . B125 B 0.4200(3) 0.1261(11) 0.4157(4) 0.032(2) Uani 1 1 d . . . H125 H 0.3942 0.1040 0.4333 0.039 Uiso 1 1 calc R . . C126 C 0.7657(4) -0.2094(15) 0.1062(4) 0.059(4) Uani 0.90 1 d P . . H12C H 0.7502 -0.2796 0.1155 0.089 Uiso 0.90 1 calc PR . . H12D H 0.7513 -0.1456 0.0904 0.089 Uiso 0.90 1 calc PR . . H12E H 0.7768 -0.1715 0.1330 0.089 Uiso 0.90 1 calc PR . . N127 N 0.7930(3) -0.2554(9) 0.0765(4) 0.048(2) Uani 0.90 1 d P . . O128 O 0.7889(3) -0.2429(10) 0.0327(3) 0.060(3) Uani 0.90 1 d P . . O129 O 0.8183(3) -0.3058(10) 0.0893(4) 0.069(3) Uani 0.90 1 d P . . C130 C 0.5286(7) 0.199(3) 0.1142(9) 0.085(8) Uiso 0.60 1 d P . . H13A H 0.5033 0.2119 0.1218 0.128 Uiso 0.60 1 calc PR . . H13B H 0.5306 0.1726 0.0825 0.128 Uiso 0.60 1 calc PR . . H13C H 0.5416 0.2789 0.1184 0.128 Uiso 0.60 1 calc PR . . N131 N 0.5420(4) 0.1139(16) 0.1400(6) 0.055(4) Uiso 0.60 1 d P . . O132 O 0.5712(5) 0.0837(17) 0.1372(6) 0.081(5) Uiso 0.60 1 d P . . O133 O 0.5191(4) 0.0754(16) 0.1669(6) 0.077(4) Uiso 0.60 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1A 0.0275(6) 0.0250(6) 0.0226(5) -0.0016(5) -0.0020(5) -0.0019(5) N2A 0.023(4) 0.022(4) 0.053(5) -0.003(4) -0.010(3) -0.004(3) C3A 0.035(5) 0.032(5) 0.061(7) 0.001(5) -0.011(5) -0.011(4) C4A 0.027(5) 0.036(6) 0.103(11) 0.014(7) -0.009(6) -0.002(5) C5A 0.038(6) 0.044(7) 0.113(12) 0.026(8) -0.042(7) -0.018(5) C6A 0.039(5) 0.039(6) 0.054(6) 0.020(5) -0.028(5) -0.017(4) C7A 0.029(5) 0.020(4) 0.060(6) 0.016(5) -0.017(4) -0.004(4) N8A 0.018(4) 0.037(5) 0.088(7) -0.032(5) 0.015(4) -0.014(3) N9A 0.032(4) 0.025(4) 0.039(4) -0.005(3) 0.009(3) -0.012(3) C10A 0.054(7) 0.073(9) 0.037(6) -0.013(6) 0.018(5) -0.025(6) C11A 0.045(7) 0.098(12) 0.084(10) -0.043(9) 0.029(7) -0.010(7) C12A 0.038(6) 0.071(9) 0.127(13) -0.050(10) 0.041(8) -0.025(6) N13A 0.045(4) 0.026(4) 0.024(3) 0.005(3) -0.008(3) -0.005(3) N14A 0.036(4) 0.023(4) 0.023(3) -0.005(3) -0.014(3) 0.001(3) C15A 0.049(6) 0.030(5) 0.020(4) 0.004(4) -0.002(4) 0.005(4) C16A 0.056(6) 0.045(6) 0.020(4) -0.006(4) -0.006(4) 0.001(5) C17A 0.093(9) 0.031(5) 0.014(4) -0.001(4) -0.014(5) -0.004(5) N18A 0.028(4) 0.038(5) 0.023(3) -0.002(3) -0.002(3) 0.005(3) C19A 0.023(4) 0.054(7) 0.029(5) -0.007(5) -0.006(3) 0.003(4) C20A 0.018(4) 0.085(9) 0.029(4) -0.031(5) -0.001(3) 0.002(5) C21A 0.044(6) 0.108(12) 0.047(6) -0.028(8) -0.024(5) 0.041(8) C22A 0.074(9) 0.121(13) 0.033(5) -0.008(8) -0.006(6) 0.072(9) C23A 0.044(5) 0.048(6) 0.023(4) -0.001(4) -0.005(4) 0.014(5) N24A 0.030(4) 0.049(5) 0.026(4) -0.002(4) 0.004(3) -0.008(4) N25A 0.030(4) 0.035(4) 0.026(4) -0.010(3) 0.006(3) 0.020(3) C26A 0.054(6) 0.024(5) 0.033(5) -0.004(4) 0.006(4) 0.006(4) C27A 0.081(8) 0.027(5) 0.054(6) -0.013(5) 0.034(6) -0.027(6) C28A 0.044(6) 0.047(6) 0.046(6) -0.022(5) 0.019(5) -0.026(5) N29A 0.066(6) 0.031(5) 0.021(4) -0.001(3) 0.004(4) 0.018(4) N30A 0.056(5) 0.021(4) 0.021(3) -0.004(3) 0.006(3) -0.007(4) C31A 0.078(8) 0.035(6) 0.043(6) -0.003(5) 0.014(5) -0.025(6) C32A 0.114(11) 0.036(7) 0.032(5) -0.004(5) 0.002(6) -0.027(7) C33A 0.143(14) 0.037(7) 0.034(6) 0.021(6) 0.025(7) 0.035(8) Fe1B 0.0212(5) 0.0365(7) 0.0214(5) 0.0012(6) -0.0046(5) 0.0023(5) N2B 0.036(4) 0.052(5) 0.017(3) -0.006(4) -0.003(3) 0.011(4) C3B 0.057(6) 0.055(7) 0.027(5) -0.006(5) -0.004(4) 0.025(6) C4B 0.045(6) 0.078(9) 0.031(5) -0.024(6) -0.006(4) 0.028(6) C5B 0.057(7) 0.066(9) 0.061(7) -0.031(7) -0.023(6) 0.013(7) C6B 0.037(6) 0.080(9) 0.048(6) 0.003(7) 0.003(5) -0.006(6) C7B 0.022(4) 0.094(10) 0.018(4) -0.020(5) 0.006(3) -0.009(5) N8B 0.064(6) 0.044(5) 0.017(3) 0.009(4) 0.005(3) 0.025(4) N9B 0.046(5) 0.046(5) 0.043(5) 0.018(4) 0.014(4) 0.012(4) C10B 0.086(9) 0.063(9) 0.064(8) 0.020(7) 0.035(7) 0.013(8) C11B 0.087(9) 0.037(6) 0.049(6) -0.012(6) 0.018(7) -0.009(6) C12B 0.101(11) 0.048(7) 0.044(6) -0.003(6) 0.008(7) 0.011(7) N13B 0.040(4) 0.055(6) 0.026(4) -0.002(4) 0.002(3) -0.016(4) N14B 0.039(4) 0.035(4) 0.029(4) -0.003(4) 0.002(3) -0.010(4) C15B 0.071(8) 0.048(7) 0.041(6) 0.003(6) -0.003(5) -0.013(6) C16B 0.064(7) 0.047(7) 0.033(5) -0.007(5) 0.008(5) -0.011(6) C17B 0.041(6) 0.064(8) 0.042(6) -0.018(6) 0.018(5) -0.032(6) N18B 0.025(3) 0.015(3) 0.018(3) 0.000(3) 0.003(3) 0.001(3) C19B 0.019(4) 0.025(4) 0.033(4) 0.017(4) -0.001(3) 0.003(3) C20B 0.025(4) 0.033(5) 0.033(4) -0.003(4) -0.002(3) -0.001(4) C21B 0.022(4) 0.028(5) 0.033(4) 0.008(4) -0.016(3) -0.004(3) C22B 0.031(4) 0.030(5) 0.020(4) -0.005(4) -0.008(3) 0.000(4) C23B 0.025(4) 0.033(5) 0.019(4) -0.006(4) -0.005(3) 0.005(4) N24B 0.026(3) 0.021(4) 0.028(4) -0.001(3) 0.001(3) -0.002(3) N25B 0.024(4) 0.040(5) 0.034(4) -0.008(4) -0.009(3) 0.007(3) C26B 0.039(5) 0.051(6) 0.030(5) -0.002(5) 0.005(4) -0.004(5) C27B 0.040(5) 0.048(6) 0.039(5) -0.016(5) 0.004(4) 0.015(5) C28B 0.028(5) 0.048(6) 0.045(5) -0.003(5) 0.005(4) 0.007(4) N29B 0.025(3) 0.026(4) 0.024(3) -0.003(3) -0.003(3) 0.004(3) N30B 0.029(4) 0.044(5) 0.030(4) 0.005(4) -0.003(3) 0.004(4) C31B 0.026(4) 0.042(6) 0.032(5) -0.006(4) -0.004(3) 0.016(4) C32B 0.050(6) 0.029(5) 0.026(4) -0.002(4) 0.006(4) 0.006(4) C33B 0.037(5) 0.030(5) 0.024(4) 0.000(4) 0.003(4) 0.000(4) Co34 0.0210(5) 0.0223(6) 0.0220(5) -0.0004(5) 0.0011(4) -0.0021(4) C35 0.029(4) 0.030(5) 0.019(4) -0.001(4) 0.002(3) 0.005(4) C36 0.017(4) 0.034(5) 0.029(4) 0.005(4) 0.009(3) -0.005(3) B37 0.034(5) 0.018(5) 0.031(5) -0.005(4) 0.006(4) -0.005(4) B38 0.022(5) 0.037(6) 0.024(4) 0.001(4) -0.001(3) 0.004(4) B39 0.023(5) 0.033(6) 0.031(5) -0.005(5) 0.009(4) 0.010(4) B40 0.031(5) 0.053(7) 0.026(5) 0.002(5) 0.012(4) -0.008(5) B41 0.031(5) 0.049(7) 0.027(5) 0.005(5) 0.008(4) -0.011(5) B42 0.023(5) 0.050(7) 0.021(4) -0.007(5) -0.001(4) -0.007(5) B43 0.023(5) 0.048(7) 0.032(5) -0.009(5) -0.005(4) 0.008(4) B44 0.018(4) 0.026(5) 0.032(5) -0.002(4) -0.001(4) -0.002(4) B45 0.033(5) 0.045(7) 0.022(4) -0.007(5) 0.001(4) 0.004(5) C46 0.016(4) 0.038(5) 0.021(4) -0.006(4) -0.004(3) -0.001(4) C47 0.023(4) 0.023(4) 0.037(5) 0.009(4) 0.006(4) -0.003(3) B48 0.024(5) 0.026(5) 0.042(6) -0.007(5) -0.003(4) 0.005(4) B49 0.024(5) 0.024(5) 0.034(5) 0.004(4) 0.004(4) 0.004(4) B50 0.024(5) 0.020(5) 0.035(5) -0.001(4) 0.010(4) -0.002(4) B51 0.023(5) 0.032(6) 0.045(6) 0.000(5) -0.008(4) 0.007(4) B52 0.036(5) 0.019(5) 0.042(6) -0.002(5) 0.002(5) -0.001(4) B53 0.034(5) 0.029(6) 0.029(5) -0.004(4) 0.007(4) 0.000(4) B54 0.031(6) 0.032(6) 0.051(7) 0.014(6) 0.005(5) -0.008(5) B55 0.015(4) 0.023(5) 0.048(6) -0.003(5) 0.000(4) -0.001(4) B56 0.017(4) 0.043(6) 0.031(5) -0.004(5) 0.002(3) -0.014(4) Co57 0.0291(6) 0.0210(6) 0.0164(4) -0.0014(5) -0.0007(4) 0.0004(5) C58 0.036(5) 0.032(5) 0.019(4) -0.004(4) 0.001(3) 0.008(4) C59 0.034(5) 0.031(5) 0.044(5) 0.014(5) -0.012(4) 0.000(4) B60 0.047(6) 0.038(7) 0.029(5) -0.012(5) -0.009(4) 0.013(5) B61 0.047(6) 0.031(6) 0.022(5) 0.004(4) 0.012(4) -0.002(5) B62 0.032(5) 0.037(6) 0.034(5) 0.008(5) -0.015(4) 0.000(5) B63 0.030(5) 0.030(6) 0.042(6) 0.003(5) 0.008(4) 0.004(4) B64 0.035(6) 0.053(8) 0.047(7) 0.018(6) -0.006(5) 0.007(6) B65 0.066(8) 0.042(7) 0.019(5) 0.003(5) 0.003(5) 0.007(6) B66 0.041(6) 0.021(5) 0.038(6) -0.002(5) -0.001(5) 0.001(4) B67 0.043(6) 0.030(6) 0.032(5) -0.006(5) 0.006(4) 0.007(5) B68 0.035(5) 0.025(5) 0.026(5) 0.007(4) -0.001(4) 0.013(4) C69 0.037(5) 0.028(5) 0.017(4) 0.006(4) 0.001(3) -0.001(4) C70 0.031(3) 0.019(3) 0.017(3) -0.016(3) 0.009(3) -0.011(3) B71 0.049(6) 0.018(5) 0.016(4) -0.009(4) 0.000(4) 0.012(4) B72 0.038(6) 0.030(6) 0.027(5) -0.006(5) 0.003(4) 0.001(5) B73 0.031(5) 0.024(5) 0.026(5) 0.000(4) -0.009(4) -0.007(4) B74 0.057(7) 0.023(6) 0.040(6) 0.010(5) 0.008(5) 0.012(5) B75 0.070(8) 0.027(6) 0.022(5) 0.002(5) -0.005(5) 0.015(6) B76 0.034(5) 0.040(6) 0.042(6) -0.007(5) -0.003(4) 0.017(5) B77 0.035(6) 0.043(7) 0.025(5) 0.000(5) -0.006(4) 0.012(5) B78 0.040(6) 0.026(5) 0.030(5) -0.007(5) 0.000(4) 0.002(4) B79 0.050(7) 0.029(6) 0.041(6) -0.005(5) -0.005(5) 0.014(5) Co80 0.0266(5) 0.0206(6) 0.0205(5) -0.0024(5) -0.0011(4) -0.0012(5) C81 0.042(5) 0.036(6) 0.025(4) -0.004(4) 0.003(4) -0.012(4) C82 0.025(4) 0.036(5) 0.034(5) -0.011(4) -0.003(3) 0.000(4) B83 0.040(5) 0.029(6) 0.011(4) -0.013(4) -0.004(4) 0.002(5) B84 0.036(5) 0.021(5) 0.027(5) 0.001(4) -0.010(4) -0.006(4) B85 0.049(6) 0.022(5) 0.020(4) 0.003(4) -0.002(4) -0.016(5) B86 0.054(7) 0.038(7) 0.053(7) -0.007(6) -0.003(6) -0.011(6) B87 0.041(6) 0.030(6) 0.033(5) -0.006(5) -0.009(5) -0.012(5) B88 0.059(7) 0.023(5) 0.024(5) -0.009(4) -0.002(5) 0.004(5) B89 0.057(7) 0.013(5) 0.034(5) -0.007(5) 0.006(5) 0.003(5) B90 0.049(6) 0.028(6) 0.023(5) -0.005(4) -0.002(4) -0.011(5) B91 0.061(8) 0.042(7) 0.036(6) -0.016(6) -0.004(5) -0.012(6) C92 0.040(5) 0.020(5) 0.030(4) -0.012(4) -0.003(4) 0.003(4) C93 0.025(4) 0.018(4) 0.052(6) 0.022(4) 0.014(4) 0.012(3) B94 0.016(4) 0.023(5) 0.046(6) -0.016(5) 0.000(4) 0.004(4) B95 0.035(5) 0.029(6) 0.039(6) -0.004(5) -0.012(4) -0.009(5) B96 0.032(5) 0.041(6) 0.024(5) -0.005(5) -0.004(4) -0.009(5) B97 0.047(6) 0.033(6) 0.026(5) -0.004(5) 0.002(4) -0.005(5) B98 0.050(7) 0.022(5) 0.044(6) 0.010(5) -0.005(5) -0.012(5) B99 0.036(6) 0.045(7) 0.037(6) -0.003(5) 0.002(4) -0.022(5) B100 0.038(6) 0.050(7) 0.033(5) -0.005(6) -0.002(5) -0.001(5) B101 0.043(6) 0.036(6) 0.034(5) -0.004(5) -0.009(5) -0.015(5) B102 0.042(6) 0.046(8) 0.050(7) -0.019(6) -0.001(5) -0.012(6) Co10 0.0184(5) 0.0213(6) 0.0264(5) -0.0015(5) 0.0005(4) 0.0002(4) C104 0.022(4) 0.019(4) 0.035(4) -0.006(4) -0.001(3) -0.006(3) C105 0.024(4) 0.030(5) 0.027(4) 0.002(4) 0.004(3) 0.004(4) B106 0.033(5) 0.015(4) 0.036(5) -0.011(4) -0.005(4) -0.002(4) B107 0.024(5) 0.036(6) 0.037(5) -0.010(5) 0.002(4) -0.001(4) B108 0.024(5) 0.024(5) 0.027(5) 0.006(4) -0.003(4) -0.010(4) B109 0.013(4) 0.022(5) 0.030(5) -0.002(4) -0.006(3) 0.001(3) B110 0.017(4) 0.016(5) 0.055(6) 0.001(5) 0.002(4) 0.003(4) B111 0.032(5) 0.033(6) 0.027(5) -0.009(5) 0.006(4) -0.003(5) B112 0.031(5) 0.039(6) 0.030(5) 0.004(5) 0.003(4) -0.006(5) B113 0.024(5) 0.031(6) 0.049(6) 0.024(5) -0.002(4) 0.001(4) B114 0.030(5) 0.028(5) 0.035(5) -0.001(5) -0.003(4) -0.008(4) C115 0.024(4) 0.026(5) 0.025(4) -0.007(4) 0.003(3) 0.006(4) C116 0.032(4) 0.023(5) 0.032(4) 0.006(4) -0.008(4) 0.004(4) B117 0.021(4) 0.011(4) 0.039(5) 0.002(4) -0.003(4) -0.001(3) B118 0.017(4) 0.033(6) 0.028(5) 0.010(4) 0.001(3) 0.000(4) B119 0.027(5) 0.021(5) 0.037(5) 0.003(4) 0.001(4) 0.006(4) B120 0.031(5) 0.039(6) 0.031(5) 0.007(5) 0.009(4) -0.003(5) B121 0.031(5) 0.036(6) 0.037(6) 0.000(5) 0.008(4) -0.003(5) B122 0.029(5) 0.039(6) 0.038(6) -0.005(5) 0.002(4) -0.014(5) B123 0.016(4) 0.039(6) 0.030(5) 0.004(5) 0.001(4) 0.005(4) B124 0.027(5) 0.021(5) 0.031(5) 0.000(4) 0.000(4) 0.003(4) B125 0.018(4) 0.042(7) 0.037(5) 0.011(5) 0.008(4) 0.001(4) C126 0.059(8) 0.086(11) 0.033(6) 0.017(7) 0.003(5) 0.014(8) N127 0.047(6) 0.035(5) 0.061(7) 0.016(5) 0.000(5) 0.002(5) O128 0.069(6) 0.076(7) 0.035(4) 0.001(5) 0.007(4) -0.003(5) O129 0.059(6) 0.058(6) 0.089(7) 0.012(6) -0.011(5) 0.016(5) _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 Fe1A N18A 1.916(7) . ? Fe1A N2A 1.917(7) . ? Fe1A N25A 1.958(8) . ? Fe1A N30A 1.980(8) . ? Fe1A N14A 1.983(7) . ? Fe1A N9A 1.996(8) . ? N2A C3A 1.311(13) . ? N2A C7A 1.349(13) . ? C3A C4A 1.426(15) . ? C3A N8A 1.449(15) . ? C4A C5A 1.284(19) . ? C5A C6A 1.452(19) . ? C6A C7A 1.406(12) . ? C7A N13A 1.404(13) . ? N8A N9A 1.343(12) . ? N8A C12A 1.357(15) . ? N9A C10A 1.292(13) . ? C10A C11A 1.447(16) . ? C11A C12A 1.31(2) . ? N13A C17A 1.334(12) . ? N13A N14A 1.371(10) . ? N14A C15A 1.344(12) . ? C15A C16A 1.381(12) . ? C16A C17A 1.357(15) . ? N18A C23A 1.322(13) . ? N18A C19A 1.340(13) . ? C19A N24A 1.407(13) . ? C19A C20A 1.416(12) . ? C20A C21A 1.359(19) . ? C21A C22A 1.40(2) . ? C22A C23A 1.371(15) . ? C23A N29A 1.429(14) . ? N24A C28A 1.349(13) . ? N24A N25A 1.397(10) . ? N25A C26A 1.354(12) . ? C26A C27A 1.408(15) . ? C27A C28A 1.430(18) . ? N29A N30A 1.380(11) . ? N29A C33A 1.417(15) . ? N30A C31A 1.315(13) . ? C31A C32A 1.455(18) . ? C32A C33A 1.35(2) . ? Fe1B N18B 2.129(7) . ? Fe1B N2B 2.163(8) . ? Fe1B N14B 2.172(8) . ? Fe1B N25B 2.180(7) . ? Fe1B N9B 2.202(9) . ? Fe1B N30B 2.231(8) . ? N2B C7B 1.279(14) . ? N2B C3B 1.361(14) . ? C3B C4B 1.394(14) . ? C3B N8B 1.406(15) . ? C4B C5B 1.372(18) . ? C5B C6B 1.397(19) . ? C6B C7B 1.395(14) . ? C7B N13B 1.389(16) . ? N8B C12B 1.370(15) . ? N8B N9B 1.395(12) . ? N9B C10B 1.363(17) . ? C10B C11B 1.457(18) . ? C11B C12B 1.329(18) . ? N13B N14B 1.400(11) . ? N13B C17B 1.421(14) . ? N14B C15B 1.308(15) . ? C15B C16B 1.462(16) . ? C16B C17B 1.308(17) . ? N18B C19B 1.341(10) . ? N18B C23B 1.343(10) . ? C19B C20B 1.352(12) . ? C19B N24B 1.438(11) . ? C20B C21B 1.388(12) . ? C21B C22B 1.389(12) . ? C22B C23B 1.386(11) . ? C23B N29B 1.434(10) . ? N24B C28B 1.361(12) . ? N24B N25B 1.373(10) . ? N25B C26B 1.347(12) . ? C26B C27B 1.384(14) . ? C27B C28B 1.385(14) . ? N29B C33B 1.363(11) . ? N29B N30B 1.381(10) . ? N30B C31B 1.334(11) . ? C31B C32B 1.400(12) . ? C32B C33B 1.407(13) . ? Co34 C36 2.045(8) . ? Co34 C47 2.055(9) . ? Co34 C35 2.057(8) . ? Co34 C46 2.064(8) . ? Co34 B48 2.107(10) . ? Co34 B39 2.107(10) . ? Co34 B50 2.113(9) . ? Co34 B37 2.115(10) . ? Co34 B49 2.121(10) . ? Co34 B38 2.128(9) . ? C35 C36 1.659(12) . ? C35 B39 1.716(13) . ? C35 B44 1.720(12) . ? C35 B40 1.755(12) . ? C36 B41 1.683(12) . ? C36 B37 1.704(13) . ? C36 B40 1.760(14) . ? B37 B42 1.778(14) . ? B37 B41 1.807(14) . ? B37 B38 1.837(14) . ? B38 B43 1.801(14) . ? B38 B39 1.818(16) . ? B38 B42 1.823(14) . ? B39 B43 1.771(14) . ? B39 B44 1.822(13) . ? B40 B41 1.763(17) . ? B40 B44 1.785(15) . ? B40 B45 1.795(15) . ? B41 B45 1.828(17) . ? B41 B42 1.840(14) . ? B42 B43 1.822(17) . ? B42 B45 1.848(15) . ? B43 B44 1.765(14) . ? B43 B45 1.785(15) . ? B44 B45 1.790(15) . ? C46 C47 1.608(12) . ? C46 B55 1.685(12) . ? C46 B51 1.692(13) . ? C46 B50 1.705(13) . ? C47 B52 1.683(14) . ? C47 B51 1.720(12) . ? C47 B48 1.726(14) . ? B48 B52 1.784(14) . ? B48 B53 1.825(14) . ? B48 B49 1.830(15) . ? B49 B53 1.804(14) . ? B49 B54 1.822(14) . ? B49 B50 1.831(14) . ? B50 B54 1.773(15) . ? B50 B55 1.774(13) . ? B51 B55 1.722(15) . ? B51 B56 1.772(15) . ? B51 B52 1.786(15) . ? B52 B56 1.788(14) . ? B52 B53 1.793(15) . ? B53 B56 1.771(14) . ? B53 B54 1.772(16) . ? B54 B55 1.775(16) . ? B54 B56 1.791(17) . ? B55 B56 1.769(15) . ? Co57 C59 2.043(9) . ? Co57 C58 2.071(9) . ? Co57 B72 2.081(11) . ? Co57 C69 2.086(9) . ? Co57 B73 2.091(9) . ? Co57 B71 2.094(9) . ? Co57 B60 2.098(11) . ? Co57 B62 2.100(12) . ? Co57 B61 2.114(10) . ? Co57 C70 2.121(8) . ? C58 C59 1.595(13) . ? C58 B62 1.675(14) . ? C58 B67 1.675(15) . ? C58 B63 1.711(14) . ? C59 B63 1.722(15) . ? C59 B64 1.736(15) . ? C59 B60 1.751(15) . ? B60 B65 1.742(18) . ? B60 B61 1.772(17) . ? B60 B64 1.798(17) . ? B61 B65 1.811(17) . ? B61 B66 1.831(16) . ? B61 B62 1.834(15) . ? B62 B66 1.812(15) . ? B62 B67 1.823(15) . ? B63 B67 1.727(16) . ? B63 B64 1.763(17) . ? B63 B68 1.782(15) . ? B64 B65 1.771(18) . ? B64 B68 1.784(18) . ? B65 B66 1.779(16) . ? B65 B68 1.794(15) . ? B66 B68 1.746(15) . ? B66 B67 1.784(15) . ? B67 B68 1.768(14) . ? C69 C70 1.597(10) . ? C69 B78 1.662(14) . ? C69 B73 1.695(13) . ? C69 B74 1.747(15) . ? C70 B75 1.629(14) . ? C70 B74 1.640(14) . ? C70 B71 1.753(13) . ? B71 B76 1.811(14) . ? B71 B72 1.825(14) . ? B71 B75 1.837(16) . ? B72 B73 1.794(14) . ? B72 B77 1.838(15) . ? B72 B76 1.841(16) . ? B73 B77 1.804(15) . ? B73 B78 1.808(15) . ? B74 B75 1.772(16) . ? B74 B78 1.793(16) . ? B74 B79 1.798(17) . ? B75 B76 1.777(18) . ? B75 B79 1.812(16) . ? B76 B77 1.812(15) . ? B76 B79 1.822(18) . ? B77 B79 1.761(17) . ? B77 B78 1.778(16) . ? B78 B79 1.785(15) . ? Co80 B94 2.041(11) . ? Co80 C92 2.066(8) . ? Co80 C82 2.076(9) . ? Co80 C93 2.078(8) . ? Co80 C81 2.078(9) . ? Co80 B96 2.090(10) . ? Co80 B84 2.093(11) . ? Co80 B85 2.095(11) . ? Co80 B83 2.120(9) . ? Co80 B95 2.155(10) . ? C81 C82 1.634(13) . ? C81 B90 1.678(15) . ? C81 B86 1.729(15) . ? C81 B85 1.732(15) . ? C82 B87 1.697(13) . ? C82 B86 1.734(16) . ? C82 B83 1.736(13) . ? B83 B88 1.775(16) . ? B83 B84 1.809(14) . ? B83 B87 1.826(15) . ? B84 B88 1.786(15) . ? B84 B89 1.806(15) . ? B84 B85 1.819(14) . ? B85 B89 1.791(14) . ? B85 B90 1.811(14) . ? B86 B90 1.771(18) . ? B86 B87 1.799(17) . ? B86 B91 1.810(18) . ? B87 B91 1.786(18) . ? B87 B88 1.811(17) . ? B88 B89 1.791(16) . ? B88 B91 1.814(17) . ? B89 B91 1.805(17) . ? B89 B90 1.812(15) . ? B90 B91 1.786(15) . ? C92 C93 1.596(13) . ? C92 B101 1.719(13) . ? C92 B97 1.727(15) . ? C92 B96 1.728(14) . ? C93 B98 1.641(14) . ? C93 B97 1.686(15) . ? C93 B94 1.704(12) . ? B94 B98 1.783(15) . ? B94 B95 1.787(15) . ? B94 B99 1.801(14) . ? B95 B100 1.749(16) . ? B95 B99 1.763(16) . ? B95 B96 1.771(15) . ? B96 B100 1.753(16) . ? B96 B101 1.825(17) . ? B97 B101 1.764(16) . ? B97 B102 1.799(16) . ? B97 B98 1.831(16) . ? B98 B99 1.778(17) . ? B98 B102 1.808(17) . ? B99 B102 1.810(18) . ? B99 B100 1.818(16) . ? B100 B101 1.752(17) . ? B100 B102 1.78(2) . ? B101 B102 1.770(18) . ? Co10 C105 2.032(8) . ? Co10 C104 2.037(8) . ? Co10 C115 2.042(8) . ? Co10 C116 2.051(9) . ? Co10 B108 2.092(9) . ? Co10 B107 2.097(10) . ? Co10 B106 2.104(10) . ? Co10 B117 2.104(9) . ? Co10 B118 2.115(9) . ? Co10 B119 2.126(10) . ? C104 C105 1.604(12) . ? C104 B113 1.679(13) . ? C104 B108 1.705(12) . ? C104 B109 1.741(11) . ? C105 B110 1.687(12) . ? C105 B106 1.699(13) . ? C105 B109 1.744(13) . ? B106 B111 1.764(14) . ? B106 B110 1.786(13) . ? B106 B107 1.788(15) . ? B107 B111 1.806(14) . ? B107 B108 1.827(15) . ? B107 B112 1.831(15) . ? B108 B112 1.788(14) . ? B108 B113 1.804(13) . ? B109 B114 1.745(14) . ? B109 B113 1.751(13) . ? B109 B110 1.765(14) . ? B110 B111 1.792(15) . ? B110 B114 1.792(15) . ? B111 B112 1.803(17) . ? B111 B114 1.816(15) . ? B112 B113 1.785(17) . ? B112 B114 1.807(15) . ? B113 B114 1.779(15) . ? C115 C116 1.614(12) . ? C115 B124 1.670(12) . ? C115 B119 1.694(13) . ? C115 B120 1.735(13) . ? C116 B117 1.711(13) . ? C116 B121 1.734(14) . ? C116 B120 1.753(13) . ? B117 B122 1.783(14) . ? B117 B121 1.803(14) . ? B117 B118 1.860(14) . ? B118 B123 1.795(13) . ? B118 B119 1.818(15) . ? B118 B122 1.838(14) . ? B119 B123 1.767(14) . ? B119 B124 1.780(14) . ? B120 B124 1.722(15) . ? B120 B125 1.771(14) . ? B120 B121 1.786(16) . ? B121 B122 1.737(16) . ? B121 B125 1.749(15) . ? B122 B125 1.789(15) . ? B122 B123 1.832(16) . ? B123 B124 1.773(14) . ? B123 B125 1.801(15) . ? B124 B125 1.791(15) . ? C126 N127 1.429(16) . ? N127 O129 1.152(13) . ? N127 O128 1.307(13) . ? C130 N131 1.29(3) . ? N131 O132 1.14(2) . ? N131 O133 1.23(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 N18A Fe1A N2A 178.3(3) . . ? N18A Fe1A N25A 80.2(3) . . ? N2A Fe1A N25A 98.5(3) . . ? N18A Fe1A N30A 79.7(3) . . ? N2A Fe1A N30A 101.6(3) . . ? N25A Fe1A N30A 160.0(3) . . ? N18A Fe1A N14A 98.5(3) . . ? N2A Fe1A N14A 80.4(3) . . ? N25A Fe1A N14A 90.8(3) . . ? N30A Fe1A N14A 92.3(3) . . ? N18A Fe1A N9A 101.6(3) . . ? N2A Fe1A N9A 79.6(4) . . ? N25A Fe1A N9A 93.9(3) . . ? N30A Fe1A N9A 90.0(3) . . ? N14A Fe1A N9A 159.9(3) . . ? C3A N2A C7A 121.6(8) . . ? C3A N2A Fe1A 120.6(7) . . ? C7A N2A Fe1A 117.8(6) . . ? N2A C3A C4A 121.5(11) . . ? N2A C3A N8A 110.3(8) . . ? C4A C3A N8A 128.1(11) . . ? C5A C4A C3A 117.1(12) . . ? C4A C5A C6A 124.8(10) . . ? C7A C6A C5A 113.9(10) . . ? N2A C7A N13A 113.1(7) . . ? N2A C7A C6A 121.0(10) . . ? N13A C7A C6A 125.8(10) . . ? N9A N8A C12A 110.8(11) . . ? N9A N8A C3A 116.6(8) . . ? C12A N8A C3A 132.5(11) . . ? C10A N9A N8A 105.7(9) . . ? C10A N9A Fe1A 141.1(8) . . ? N8A N9A Fe1A 112.8(6) . . ? N9A C10A C11A 110.6(12) . . ? C12A C11A C10A 104.1(11) . . ? C11A C12A N8A 108.7(12) . . ? C17A N13A N14A 111.0(8) . . ? C17A N13A C7A 133.8(9) . . ? N14A N13A C7A 115.2(7) . . ? C15A N14A N13A 105.2(7) . . ? C15A N14A Fe1A 141.3(6) . . ? N13A N14A Fe1A 113.5(6) . . ? N14A C15A C16A 109.5(9) . . ? C17A C16A C15A 107.1(9) . . ? N13A C17A C16A 107.1(8) . . ? C23A N18A C19A 118.5(8) . . ? C23A N18A Fe1A 121.6(7) . . ? C19A N18A Fe1A 119.7(6) . . ? N18A C19A N24A 110.8(7) . . ? N18A C19A C20A 121.7(10) . . ? N24A C19A C20A 127.4(10) . . ? C21A C20A C19A 117.6(11) . . ? C20A C21A C22A 121.1(10) . . ? C23A C22A C21A 116.5(13) . . ? N18A C23A C22A 124.5(12) . . ? N18A C23A N29A 109.1(8) . . ? C22A C23A N29A 126.4(12) . . ? C28A N24A N25A 112.3(9) . . ? C28A N24A C19A 131.6(9) . . ? N25A N24A C19A 116.0(8) . . ? C26A N25A N24A 103.7(8) . . ? C26A N25A Fe1A 143.3(7) . . ? N24A N25A Fe1A 113.0(6) . . ? N25A C26A C27A 112.7(10) . . ? C26A C27A C28A 103.9(9) . . ? N24A C28A C27A 107.0(9) . . ? N30A N29A C33A 109.8(10) . . ? N30A N29A C23A 117.4(8) . . ? C33A N29A C23A 132.8(10) . . ? C31A N30A N29A 105.5(9) . . ? C31A N30A Fe1A 142.3(8) . . ? N29A N30A Fe1A 112.2(6) . . ? N30A C31A C32A 112.5(11) . . ? C33A C32A C31A 104.1(10) . . ? C32A C33A N29A 108.2(11) . . ? N18B Fe1B N2B 159.6(3) . . ? N18B Fe1B N14B 102.2(3) . . ? N2B Fe1B N14B 71.7(3) . . ? N18B Fe1B N25B 74.1(3) . . ? N2B Fe1B N25B 124.7(3) . . ? N14B Fe1B N25B 92.2(3) . . ? N18B Fe1B N9B 112.3(3) . . ? N2B Fe1B N9B 74.6(3) . . ? N14B Fe1B N9B 145.3(3) . . ? N25B Fe1B N9B 100.4(3) . . ? N18B Fe1B N30B 72.8(3) . . ? N2B Fe1B N30B 88.1(3) . . ? N14B Fe1B N30B 94.3(3) . . ? N25B Fe1B N30B 146.9(3) . . ? N9B Fe1B N30B 92.4(3) . . ? C7B N2B C3B 117.3(10) . . ? C7B N2B Fe1B 122.1(7) . . ? C3B N2B Fe1B 118.8(7) . . ? N2B C3B C4B 123.6(12) . . ? N2B C3B N8B 112.6(9) . . ? C4B C3B N8B 123.7(11) . . ? C5B C4B C3B 114.1(12) . . ? C4B C5B C6B 125.2(11) . . ? C7B C6B C5B 112.3(12) . . ? N2B C7B N13B 111.8(8) . . ? N2B C7B C6B 127.2(13) . . ? N13B C7B C6B 120.9(11) . . ? C12B N8B N9B 108.2(10) . . ? C12B N8B C3B 130.9(10) . . ? N9B N8B C3B 120.7(8) . . ? C10B N9B N8B 108.9(10) . . ? C10B N9B Fe1B 138.3(8) . . ? N8B N9B Fe1B 112.1(7) . . ? N9B C10B C11B 105.2(12) . . ? C12B C11B C10B 108.6(12) . . ? C11B C12B N8B 109.1(12) . . ? C7B N13B N14B 118.6(8) . . ? C7B N13B C17B 135.5(9) . . ? N14B N13B C17B 105.8(9) . . ? C15B N14B N13B 107.0(9) . . ? C15B N14B Fe1B 139.0(7) . . ? N13B N14B Fe1B 113.7(6) . . ? N14B C15B C16B 111.9(11) . . ? C17B C16B C15B 103.2(11) . . ? C16B C17B N13B 112.0(9) . . ? C19B N18B C23B 115.9(7) . . ? C19B N18B Fe1B 120.9(5) . . ? C23B N18B Fe1B 123.2(5) . . ? N18B C19B C20B 124.4(8) . . ? N18B C19B N24B 112.0(7) . . ? C20B C19B N24B 123.5(8) . . ? C19B C20B C21B 118.2(8) . . ? C20B C21B C22B 120.1(7) . . ? C23B C22B C21B 116.1(7) . . ? N18B C23B C22B 124.9(7) . . ? N18B C23B N29B 111.1(7) . . ? C22B C23B N29B 123.9(7) . . ? C28B N24B N25B 112.4(7) . . ? C28B N24B C19B 128.8(7) . . ? N25B N24B C19B 118.4(6) . . ? C26B N25B N24B 103.4(7) . . ? C26B N25B Fe1B 140.8(6) . . ? N24B N25B Fe1B 114.3(5) . . ? N25B C26B C27B 112.5(9) . . ? C26B C27B C28B 105.5(8) . . ? N24B C28B C27B 106.2(8) . . ? C33B N29B N30B 111.6(7) . . ? C33B N29B C23B 129.6(7) . . ? N30B N29B C23B 118.8(7) . . ? C31B N30B N29B 104.7(7) . . ? C31B N30B Fe1B 141.3(6) . . ? N29B N30B Fe1B 113.7(5) . . ? N30B C31B C32B 112.6(8) . . ? C31B C32B C33B 104.4(8) . . ? N29B C33B C32B 106.7(8) . . ? C36 Co34 C47 101.3(4) . . ? C36 Co34 C35 47.7(3) . . ? C47 Co34 C35 137.4(4) . . ? C36 Co34 C46 96.9(3) . . ? C47 Co34 C46 46.0(3) . . ? C35 Co34 C46 102.0(3) . . ? C36 Co34 B48 135.3(4) . . ? C47 Co34 B48 49.0(4) . . ? C35 Co34 B48 173.6(4) . . ? C46 Co34 B48 83.6(4) . . ? C36 Co34 B39 84.2(4) . . ? C47 Co34 B39 173.9(4) . . ? C35 Co34 B39 48.6(3) . . ? C46 Co34 B39 136.6(4) . . ? B48 Co34 B39 125.0(4) . . ? C36 Co34 B50 125.5(4) . . ? C47 Co34 B50 82.5(4) . . ? C35 Co34 B50 93.8(4) . . ? C46 Co34 B50 48.2(4) . . ? B48 Co34 B50 87.7(4) . . ? B39 Co34 B50 96.5(4) . . ? C36 Co34 B37 48.3(4) . . ? C47 Co34 B37 94.0(4) . . ? C35 Co34 B37 84.0(4) . . ? C46 Co34 B37 125.0(4) . . ? B48 Co34 B37 95.3(4) . . ? B39 Co34 B37 87.6(4) . . ? B50 Co34 B37 172.3(4) . . ? C36 Co34 B49 173.4(4) . . ? C47 Co34 B49 84.2(4) . . ? C35 Co34 B49 125.7(4) . . ? C46 Co34 B49 84.3(4) . . ? B48 Co34 B49 51.3(4) . . ? B39 Co34 B49 90.5(4) . . ? B50 Co34 B49 51.2(4) . . ? B37 Co34 B49 135.5(4) . . ? C36 Co34 B38 84.5(4) . . ? C47 Co34 B38 126.6(4) . . ? C35 Co34 B38 84.5(4) . . ? C46 Co34 B38 172.5(4) . . ? B48 Co34 B38 90.2(4) . . ? B39 Co34 B38 50.8(4) . . ? B50 Co34 B38 136.0(4) . . ? B37 Co34 B38 51.3(4) . . ? B49 Co34 B38 95.1(4) . . ? C36 C35 B39 111.1(7) . . ? C36 C35 B44 110.9(7) . . ? B39 C35 B44 64.1(5) . . ? C36 C35 B40 62.0(6) . . ? B39 C35 B40 115.4(7) . . ? B44 C35 B40 61.8(6) . . ? C36 C35 Co34 65.8(4) . . ? B39 C35 Co34 67.2(4) . . ? B44 C35 Co34 125.1(6) . . ? B40 C35 Co34 124.1(6) . . ? C35 C36 B41 111.4(7) . . ? C35 C36 B37 112.3(7) . . ? B41 C36 B37 64.5(6) . . ? C35 C36 B40 61.7(5) . . ? B41 C36 B40 61.5(6) . . ? B37 C36 B40 115.3(7) . . ? C35 C36 Co34 66.5(4) . . ? B41 C36 Co34 126.6(6) . . ? B37 C36 Co34 68.0(4) . . ? B40 C36 Co34 124.5(6) . . ? C36 B37 B42 105.3(7) . . ? C36 B37 B41 57.2(5) . . ? B42 B37 B41 61.8(6) . . ? C36 B37 B38 104.8(7) . . ? B42 B37 B38 60.6(6) . . ? B41 B37 B38 109.2(7) . . ? C36 B37 Co34 63.7(4) . . ? B42 B37 Co34 118.3(6) . . ? B41 B37 Co34 116.3(6) . . ? B38 B37 Co34 64.7(4) . . ? B43 B38 B39 58.6(6) . . ? B43 B38 B42 60.4(6) . . ? B39 B38 B42 107.5(7) . . ? B43 B38 B37 105.0(7) . . ? B39 B38 B37 106.2(7) . . ? B42 B38 B37 58.1(5) . . ? B43 B38 Co34 114.7(6) . . ? B39 B38 Co34 64.0(4) . . ? B42 B38 Co34 115.5(6) . . ? B37 B38 Co34 64.0(4) . . ? C35 B39 B43 102.8(7) . . ? C35 B39 B38 105.5(7) . . ? B43 B39 B38 60.2(6) . . ? C35 B39 B44 58.1(5) . . ? B43 B39 B44 58.8(5) . . ? B38 B39 B44 108.3(7) . . ? C35 B39 Co34 64.1(4) . . ? B43 B39 Co34 117.0(7) . . ? B38 B39 Co34 65.2(4) . . ? B44 B39 Co34 117.1(6) . . ? C35 B40 C36 56.3(5) . . ? C35 B40 B41 103.4(7) . . ? C36 B40 B41 57.1(6) . . ? C35 B40 B44 58.2(5) . . ? C36 B40 B44 103.5(7) . . ? B41 B40 B44 109.0(8) . . ? C35 B40 B45 104.1(7) . . ? C36 B40 B45 104.1(7) . . ? B41 B40 B45 61.8(7) . . ? B44 B40 B45 60.0(6) . . ? C36 B41 B40 61.4(6) . . ? C36 B41 B37 58.3(5) . . ? B40 B41 B37 110.2(7) . . ? C36 B41 B45 105.9(8) . . ? B40 B41 B45 60.0(6) . . ? B37 B41 B45 107.7(7) . . ? C36 B41 B42 103.5(7) . . ? B40 B41 B42 108.9(8) . . ? B37 B41 B42 58.4(6) . . ? B45 B41 B42 60.5(6) . . ? B37 B42 B43 106.5(7) . . ? B37 B42 B38 61.3(5) . . ? B43 B42 B38 59.2(6) . . ? B37 B42 B41 59.9(6) . . ? B43 B42 B41 104.5(7) . . ? B38 B42 B41 108.3(6) . . ? B37 B42 B45 108.0(7) . . ? B43 B42 B45 58.2(6) . . ? B38 B42 B45 107.7(8) . . ? B41 B42 B45 59.4(6) . . ? B44 B43 B39 62.0(6) . . ? B44 B43 B45 60.5(6) . . ? B39 B43 B45 111.2(7) . . ? B44 B43 B38 111.6(7) . . ? B39 B43 B38 61.2(6) . . ? B45 B43 B38 111.6(8) . . ? B44 B43 B42 110.0(7) . . ? B39 B43 B42 109.6(7) . . ? B45 B43 B42 61.6(6) . . ? B38 B43 B42 60.4(6) . . ? C35 B44 B43 102.9(7) . . ? C35 B44 B40 60.1(5) . . ? B43 B44 B40 107.7(8) . . ? C35 B44 B45 105.7(7) . . ? B43 B44 B45 60.3(6) . . ? B40 B44 B45 60.3(6) . . ? C35 B44 B39 57.8(5) . . ? B43 B44 B39 59.1(6) . . ? B40 B44 B39 108.8(7) . . ? B45 B44 B39 108.7(7) . . ? B43 B45 B44 59.2(6) . . ? B43 B45 B40 106.4(7) . . ? B44 B45 B40 59.7(6) . . ? B43 B45 B41 106.5(7) . . ? B44 B45 B41 105.9(7) . . ? B40 B45 B41 58.2(6) . . ? B43 B45 B42 60.2(6) . . ? B44 B45 B42 107.7(7) . . ? B40 B45 B42 107.1(7) . . ? B41 B45 B42 60.1(6) . . ? C47 C46 B55 111.2(7) . . ? C47 C46 B51 62.8(6) . . ? B55 C46 B51 61.3(6) . . ? C47 C46 B50 112.1(7) . . ? B55 C46 B50 63.1(6) . . ? B51 C46 B50 114.8(7) . . ? C47 C46 Co34 66.7(4) . . ? B55 C46 Co34 124.6(6) . . ? B51 C46 Co34 125.5(6) . . ? B50 C46 Co34 67.4(4) . . ? C46 C47 B52 111.8(6) . . ? C46 C47 B51 61.0(5) . . ? B52 C47 B51 63.3(6) . . ? C46 C47 B48 112.9(7) . . ? B52 C47 B48 63.1(6) . . ? B51 C47 B48 116.1(7) . . ? C46 C47 Co34 67.3(4) . . ? B52 C47 Co34 124.4(6) . . ? B51 C47 Co34 124.4(6) . . ? B48 C47 Co34 67.1(4) . . ? C47 B48 B52 57.3(5) . . ? C47 B48 B53 102.0(7) . . ? B52 B48 B53 59.5(6) . . ? C47 B48 B49 103.9(7) . . ? B52 B48 B49 107.4(7) . . ? B53 B48 B49 59.2(6) . . ? C47 B48 Co34 64.0(5) . . ? B52 B48 Co34 116.3(6) . . ? B53 B48 Co34 116.0(6) . . ? B49 B48 Co34 64.8(4) . . ? B53 B49 B54 58.5(6) . . ? B53 B49 B48 60.3(6) . . ? B54 B49 B48 106.5(7) . . ? B53 B49 B50 104.5(7) . . ? B54 B49 B50 58.1(6) . . ? B48 B49 B50 105.9(7) . . ? B53 B49 Co34 116.3(6) . . ? B54 B49 Co34 115.4(6) . . ? B48 B49 Co34 64.0(4) . . ? B50 B49 Co34 64.1(4) . . ? C46 B50 B54 104.3(7) . . ? C46 B50 B55 57.9(5) . . ? B54 B50 B55 60.0(6) . . ? C46 B50 B49 105.1(7) . . ? B54 B50 B49 60.7(6) . . ? B55 B50 B49 108.6(7) . . ? C46 B50 Co34 64.4(4) . . ? B54 B50 Co34 118.0(6) . . ? B55 B50 Co34 117.3(6) . . ? B49 B50 Co34 64.6(4) . . ? C46 B51 C47 56.2(5) . . ? C46 B51 B55 59.2(6) . . ? C47 B51 B55 104.3(7) . . ? C46 B51 B56 105.4(7) . . ? C47 B51 B56 104.3(7) . . ? B55 B51 B56 60.8(6) . . ? C46 B51 B52 103.1(7) . . ? C47 B51 B52 57.3(6) . . ? B55 B51 B52 108.1(8) . . ? B56 B51 B52 60.3(6) . . ? C47 B52 B48 59.6(6) . . ? C47 B52 B51 59.4(6) . . ? B48 B52 B51 110.0(7) . . ? C47 B52 B56 105.1(7) . . ? B48 B52 B56 109.8(8) . . ? B51 B52 B56 59.5(6) . . ? C47 B52 B53 105.2(7) . . ? B48 B52 B53 61.4(6) . . ? B51 B52 B53 107.0(7) . . ? B56 B52 B53 59.3(6) . . ? B56 B53 B54 60.7(6) . . ? B56 B53 B52 60.2(6) . . ? B54 B53 B52 108.0(8) . . ? B56 B53 B49 110.6(7) . . ? B54 B53 B49 61.2(6) . . ? B52 B53 B49 108.2(7) . . ? B56 B53 B48 108.7(7) . . ? B54 B53 B48 108.9(7) . . ? B52 B53 B48 59.1(6) . . ? B49 B53 B48 60.5(5) . . ? B53 B54 B50 108.4(7) . . ? B53 B54 B55 106.9(8) . . ? B50 B54 B55 60.0(6) . . ? B53 B54 B56 59.6(6) . . ? B50 B54 B56 108.2(8) . . ? B55 B54 B56 59.5(6) . . ? B53 B54 B49 60.3(6) . . ? B50 B54 B49 61.2(6) . . ? B55 B54 B49 109.0(7) . . ? B56 B54 B49 108.9(7) . . ? C46 B55 B51 59.5(6) . . ? C46 B55 B56 105.9(7) . . ? B51 B55 B56 61.0(6) . . ? C46 B55 B50 59.0(5) . . ? B51 B55 B50 109.8(7) . . ? B56 B55 B50 109.1(7) . . ? C46 B55 B54 105.1(7) . . ? B51 B55 B54 109.9(8) . . ? B56 B55 B54 60.7(7) . . ? B50 B55 B54 59.9(6) . . ? B55 B56 B53 107.2(7) . . ? B55 B56 B51 58.2(6) . . ? B53 B56 B51 108.6(7) . . ? B55 B56 B52 106.0(7) . . ? B53 B56 B52 60.5(6) . . ? B51 B56 B52 60.2(6) . . ? B55 B56 B54 59.8(6) . . ? B53 B56 B54 59.7(6) . . ? B51 B56 B54 106.9(8) . . ? B52 B56 B54 107.3(7) . . ? C59 Co57 C58 45.6(4) . . ? C59 Co57 B72 175.4(4) . . ? C58 Co57 B72 130.9(4) . . ? C59 Co57 C69 99.9(4) . . ? C58 Co57 C69 101.8(4) . . ? B72 Co57 C69 83.5(4) . . ? C59 Co57 B73 129.7(4) . . ? C58 Co57 B73 97.3(4) . . ? B72 Co57 B73 50.9(4) . . ? C69 Co57 B73 47.9(4) . . ? C59 Co57 B71 131.2(4) . . ? C58 Co57 B71 173.5(4) . . ? B72 Co57 B71 51.8(4) . . ? C69 Co57 B71 84.1(4) . . ? B73 Co57 B71 88.6(4) . . ? C59 Co57 B60 50.0(4) . . ? C58 Co57 B60 82.5(4) . . ? B72 Co57 B60 129.4(4) . . ? C69 Co57 B60 131.9(4) . . ? B73 Co57 B60 179.7(4) . . ? B71 Co57 B60 91.6(4) . . ? C59 Co57 B62 82.6(4) . . ? C58 Co57 B62 47.3(4) . . ? B72 Co57 B62 92.9(4) . . ? C69 Co57 B62 131.4(4) . . ? B73 Co57 B62 93.6(4) . . ? B71 Co57 B62 129.9(4) . . ? B60 Co57 B62 86.4(4) . . ? C59 Co57 B61 84.8(4) . . ? C58 Co57 B61 83.5(4) . . ? B72 Co57 B61 92.0(4) . . ? C69 Co57 B61 174.5(4) . . ? B73 Co57 B61 130.5(4) . . ? B71 Co57 B61 90.7(4) . . ? B60 Co57 B61 49.8(5) . . ? B62 Co57 B61 51.6(4) . . ? C59 Co57 C70 102.1(4) . . ? C58 Co57 C70 134.4(3) . . ? B72 Co57 C70 82.4(4) . . ? C69 Co57 C70 44.6(3) . . ? B73 Co57 C70 80.6(4) . . ? B71 Co57 C70 49.1(4) . . ? B60 Co57 C70 99.4(4) . . ? B62 Co57 C70 174.1(4) . . ? B61 Co57 C70 131.9(4) . . ? C59 C58 B62 113.4(7) . . ? C59 C58 B67 112.6(7) . . ? B62 C58 B67 65.9(6) . . ? C59 C58 B63 62.7(6) . . ? B62 C58 B63 116.9(7) . . ? B67 C58 B63 61.3(6) . . ? C59 C58 Co57 66.2(5) . . ? B62 C58 Co57 67.2(5) . . ? B67 C58 Co57 126.9(6) . . ? B63 C58 Co57 124.9(6) . . ? C58 C59 B63 62.0(6) . . ? C58 C59 B64 110.1(8) . . ? B63 C59 B64 61.3(7) . . ? C58 C59 B60 110.4(7) . . ? B63 C59 B60 113.0(8) . . ? B64 C59 B60 62.1(7) . . ? C58 C59 Co57 68.1(4) . . ? B63 C59 Co57 126.0(6) . . ? B64 C59 Co57 123.8(7) . . ? B60 C59 Co57 66.6(5) . . ? B65 B60 C59 104.8(8) . . ? B65 B60 B61 62.0(7) . . ? C59 B60 B61 105.4(7) . . ? B65 B60 B64 60.0(7) . . ? C59 B60 B64 58.6(6) . . ? B61 B60 B64 110.1(9) . . ? B65 B60 Co57 119.9(7) . . ? C59 B60 Co57 63.3(5) . . ? B61 B60 Co57 65.6(5) . . ? B64 B60 Co57 117.6(7) . . ? B60 B61 B65 58.2(7) . . ? B60 B61 B66 104.3(8) . . ? B65 B61 B66 58.5(6) . . ? B60 B61 B62 105.7(7) . . ? B65 B61 B62 105.8(7) . . ? B66 B61 B62 59.3(6) . . ? B60 B61 Co57 64.7(5) . . ? B65 B61 Co57 115.8(7) . . ? B66 B61 Co57 115.5(6) . . ? B62 B61 Co57 63.8(5) . . ? C58 B62 B66 101.9(7) . . ? C58 B62 B67 57.0(6) . . ? B66 B62 B67 58.8(6) . . ? C58 B62 B61 105.0(7) . . ? B66 B62 B61 60.3(6) . . ? B67 B62 B61 107.9(7) . . ? C58 B62 Co57 65.4(5) . . ? B66 B62 Co57 117.0(6) . . ? B67 B62 Co57 117.4(7) . . ? B61 B62 Co57 64.6(5) . . ? C58 B63 C59 55.4(5) . . ? C58 B63 B67 58.3(6) . . ? C59 B63 B67 104.2(7) . . ? C58 B63 B64 103.7(7) . . ? C59 B63 B64 59.8(6) . . ? B67 B63 B64 108.8(8) . . ? C58 B63 B68 104.0(7) . . ? C59 B63 B68 105.6(7) . . ? B67 B63 B68 60.5(6) . . ? B64 B63 B68 60.4(7) . . ? C59 B64 B63 58.9(6) . . ? C59 B64 B65 104.2(8) . . ? B63 B64 B65 108.7(9) . . ? C59 B64 B68 104.9(8) . . ? B63 B64 B68 60.3(7) . . ? B65 B64 B68 60.6(7) . . ? C59 B64 B60 59.4(6) . . ? B63 B64 B60 108.8(8) . . ? B65 B64 B60 58.4(7) . . ? B68 B64 B60 107.6(8) . . ? B60 B65 B64 61.6(7) . . ? B60 B65 B66 107.7(8) . . ? B64 B65 B66 106.3(8) . . ? B60 B65 B68 109.6(8) . . ? B64 B65 B68 60.0(7) . . ? B66 B65 B68 58.5(6) . . ? B60 B65 B61 59.8(7) . . ? B64 B65 B61 109.5(8) . . ? B66 B65 B61 61.3(6) . . ? B68 B65 B61 109.5(7) . . ? B68 B66 B65 61.2(6) . . ? B68 B66 B67 60.1(6) . . ? B65 B66 B67 108.3(8) . . ? B68 B66 B62 109.9(8) . . ? B65 B66 B62 108.1(8) . . ? B67 B66 B62 60.9(6) . . ? B68 B66 B61 110.8(8) . . ? B65 B66 B61 60.2(6) . . ? B67 B66 B61 109.8(8) . . ? B62 B66 B61 60.5(6) . . ? C58 B67 B63 60.4(6) . . ? C58 B67 B68 106.1(8) . . ? B63 B67 B68 61.3(6) . . ? C58 B67 B66 103.1(7) . . ? B63 B67 B66 107.9(8) . . ? B68 B67 B66 58.9(6) . . ? C58 B67 B62 57.0(6) . . ? B63 B67 B62 108.7(8) . . ? B68 B67 B62 108.4(7) . . ? B66 B67 B62 60.3(6) . . ? B66 B68 B67 61.0(6) . . ? B66 B68 B63 107.1(7) . . ? B67 B68 B63 58.2(6) . . ? B66 B68 B64 107.2(7) . . ? B67 B68 B64 106.0(8) . . ? B63 B68 B64 59.2(6) . . ? B66 B68 B65 60.3(6) . . ? B67 B68 B65 108.3(7) . . ? B63 B68 B65 106.8(8) . . ? B64 B68 B65 59.3(7) . . ? C70 C69 B78 109.0(7) . . ? C70 C69 B73 111.7(6) . . ? B78 C69 B73 65.2(6) . . ? C70 C69 B74 58.5(6) . . ? B78 C69 B74 63.4(6) . . ? B73 C69 B74 117.7(8) . . ? C70 C69 Co57 68.9(4) . . ? B78 C69 Co57 125.6(6) . . ? B73 C69 Co57 66.2(4) . . ? B74 C69 Co57 124.6(6) . . ? C69 C70 B75 116.6(7) . . ? C69 C70 B74 65.3(6) . . ? B75 C70 B74 65.7(7) . . ? C69 C70 B71 113.4(6) . . ? B75 C70 B71 65.7(6) . . ? B74 C70 B71 122.0(7) . . ? C69 C70 Co57 66.5(4) . . ? B75 C70 Co57 125.4(6) . . ? B74 C70 Co57 128.7(6) . . ? B71 C70 Co57 64.6(4) . . ? C70 B71 B76 98.0(7) . . ? C70 B71 B72 101.4(6) . . ? B76 B71 B72 60.8(6) . . ? C70 B71 B75 53.9(6) . . ? B76 B71 B75 58.3(6) . . ? B72 B71 B75 106.6(7) . . ? C70 B71 Co57 66.2(4) . . ? B76 B71 Co57 117.1(6) . . ? B72 B71 Co57 63.7(4) . . ? B75 B71 Co57 116.2(6) . . ? B73 B72 B71 107.7(7) . . ? B73 B72 B77 59.6(6) . . ? B71 B72 B77 106.5(8) . . ? B73 B72 B76 106.8(8) . . ? B71 B72 B76 59.2(6) . . ? B77 B72 B76 59.0(6) . . ? B73 B72 Co57 64.8(5) . . ? B71 B72 Co57 64.4(5) . . ? B77 B72 Co57 116.7(6) . . ? B76 B72 Co57 116.3(7) . . ? C69 B73 B72 105.3(7) . . ? C69 B73 B77 101.9(7) . . ? B72 B73 B77 61.4(6) . . ? C69 B73 B78 56.5(5) . . ? B72 B73 B78 108.9(7) . . ? B77 B73 B78 59.0(6) . . ? C69 B73 Co57 65.9(4) . . ? B72 B73 Co57 64.2(5) . . ? B77 B73 Co57 117.8(6) . . ? B78 B73 Co57 117.7(6) . . ? C70 B74 C69 56.2(5) . . ? C70 B74 B75 56.9(6) . . ? C69 B74 B75 102.5(8) . . ? C70 B74 B78 101.2(8) . . ? C69 B74 B78 56.0(6) . . ? B75 B74 B78 107.2(8) . . ? C70 B74 B79 102.5(8) . . ? C69 B74 B79 101.9(8) . . ? B75 B74 B79 61.0(7) . . ? B78 B74 B79 59.6(6) . . ? C70 B75 B74 57.5(6) . . ? C70 B75 B76 104.3(8) . . ? B74 B75 B76 110.0(8) . . ? C70 B75 B79 102.4(7) . . ? B74 B75 B79 60.2(6) . . ? B76 B75 B79 61.0(7) . . ? C70 B75 B71 60.4(6) . . ? B74 B75 B71 110.6(8) . . ? B76 B75 B71 60.1(6) . . ? B79 B75 B71 109.4(8) . . ? B75 B76 B71 61.6(6) . . ? B75 B76 B77 106.2(8) . . ? B71 B76 B77 108.2(7) . . ? B75 B76 B79 60.4(6) . . ? B71 B76 B79 110.1(8) . . ? B77 B76 B79 58.0(6) . . ? B75 B76 B72 108.4(7) . . ? B71 B76 B72 59.9(6) . . ? B77 B76 B72 60.4(6) . . ? B79 B76 B72 107.8(7) . . ? B79 B77 B78 60.6(6) . . ? B79 B77 B73 109.9(8) . . ? B78 B77 B73 60.6(6) . . ? B79 B77 B76 61.3(7) . . ? B78 B77 B76 108.5(8) . . ? B73 B77 B76 107.6(7) . . ? B79 B77 B72 110.7(7) . . ? B78 B77 B72 108.3(7) . . ? B73 B77 B72 59.0(5) . . ? B76 B77 B72 60.6(6) . . ? C69 B78 B77 104.4(7) . . ? C69 B78 B79 106.0(7) . . ? B77 B78 B79 59.2(6) . . ? C69 B78 B74 60.6(6) . . ? B77 B78 B74 108.0(7) . . ? B79 B78 B74 60.3(6) . . ? C69 B78 B73 58.3(6) . . ? B77 B78 B73 60.4(6) . . ? B79 B78 B73 108.6(8) . . ? B74 B78 B73 109.8(7) . . ? B77 B79 B78 60.2(6) . . ? B77 B79 B74 108.5(8) . . ? B78 B79 B74 60.1(6) . . ? B77 B79 B75 106.9(8) . . ? B78 B79 B75 105.9(8) . . ? B74 B79 B75 58.8(6) . . ? B77 B79 B76 60.7(6) . . ? B78 B79 B76 107.7(8) . . ? B74 B79 B76 106.9(8) . . ? B75 B79 B76 58.6(7) . . ? B94 Co80 C92 83.7(4) . . ? B94 Co80 C82 129.3(4) . . ? C92 Co80 C82 100.7(4) . . ? B94 Co80 C93 48.9(3) . . ? C92 Co80 C93 45.3(4) . . ? C82 Co80 C93 100.4(4) . . ? B94 Co80 C81 175.2(4) . . ? C92 Co80 C81 98.9(4) . . ? C82 Co80 C81 46.3(4) . . ? C93 Co80 C81 130.9(4) . . ? B94 Co80 B96 86.6(4) . . ? C92 Co80 B96 49.1(4) . . ? C82 Co80 B96 133.8(4) . . ? C93 Co80 B96 81.6(4) . . ? C81 Co80 B96 98.1(4) . . ? B94 Co80 B84 93.2(4) . . ? C92 Co80 B84 175.4(4) . . ? C82 Co80 B84 83.8(4) . . ? C93 Co80 B84 133.8(4) . . ? C81 Co80 B84 84.5(4) . . ? B96 Co80 B84 127.5(4) . . ? B94 Co80 B85 131.9(4) . . ? C92 Co80 B85 129.0(4) . . ? C82 Co80 B85 83.5(4) . . ? C93 Co80 B85 173.4(4) . . ? C81 Co80 B85 49.0(4) . . ? B96 Co80 B85 91.9(4) . . ? B84 Co80 B85 51.5(4) . . ? B94 Co80 B83 91.3(4) . . ? C92 Co80 B83 132.3(4) . . ? C82 Co80 B83 48.9(4) . . ? C93 Co80 B83 98.3(4) . . ? C81 Co80 B83 84.0(4) . . ? B96 Co80 B83 177.3(4) . . ? B84 Co80 B83 50.9(4) . . ? B85 Co80 B83 88.2(4) . . ? B94 Co80 B95 50.3(4) . . ? C92 Co80 B95 83.0(4) . . ? C82 Co80 B95 176.2(4) . . ? C93 Co80 B95 81.9(4) . . ? C81 Co80 B95 133.8(4) . . ? B96 Co80 B95 49.3(4) . . ? B84 Co80 B95 92.4(4) . . ? B85 Co80 B95 94.5(4) . . ? B83 Co80 B95 128.0(4) . . ? C82 C81 B90 110.8(7) . . ? C82 C81 B86 62.0(6) . . ? B90 C81 B86 62.6(7) . . ? C82 C81 B85 111.2(7) . . ? B90 C81 B85 64.1(6) . . ? B86 C81 B85 116.8(8) . . ? C82 C81 Co80 66.8(5) . . ? B90 C81 Co80 124.2(7) . . ? B86 C81 Co80 125.3(7) . . ? B85 C81 Co80 66.0(4) . . ? C81 C82 B87 111.9(8) . . ? C81 C82 B86 61.7(6) . . ? B87 C82 B86 63.2(7) . . ? C81 C82 B83 112.8(7) . . ? B87 C82 B83 64.3(6) . . ? B86 C82 B83 117.5(8) . . ? C81 C82 Co80 66.9(4) . . ? B87 C82 Co80 125.2(6) . . ? B86 C82 Co80 125.1(7) . . ? B83 C82 Co80 66.9(4) . . ? C82 B83 B88 102.7(8) . . ? C82 B83 B84 103.5(7) . . ? B88 B83 B84 59.8(6) . . ? C82 B83 B87 56.8(6) . . ? B88 B83 B87 60.4(7) . . ? B84 B83 B87 107.8(8) . . ? C82 B83 Co80 64.2(4) . . ? B88 B83 Co80 116.2(6) . . ? B84 B83 Co80 63.8(4) . . ? B87 B83 Co80 116.2(6) . . ? B88 B84 B89 59.8(6) . . ? B88 B84 B83 59.2(6) . . ? B89 B84 B83 107.2(8) . . ? B88 B84 B85 107.0(7) . . ? B89 B84 B85 59.2(6) . . ? B83 B84 B85 108.0(7) . . ? B88 B84 Co80 117.1(7) . . ? B89 B84 Co80 116.5(6) . . ? B83 B84 Co80 65.3(4) . . ? B85 B84 Co80 64.3(5) . . ? C81 B85 B89 103.3(7) . . ? C81 B85 B90 56.5(6) . . ? B89 B85 B90 60.4(6) . . ? C81 B85 B84 104.4(7) . . ? B89 B85 B84 60.0(6) . . ? B90 B85 B84 107.9(7) . . ? C81 B85 Co80 65.0(5) . . ? B89 B85 Co80 117.2(6) . . ? B90 B85 Co80 116.5(7) . . ? B84 B85 Co80 64.2(5) . . ? C81 B86 C82 56.3(6) . . ? C81 B86 B90 57.3(6) . . ? C82 B86 B90 102.1(8) . . ? C81 B86 B87 103.0(8) . . ? C82 B86 B87 57.4(6) . . ? B90 B86 B87 106.7(9) . . ? C81 B86 B91 102.8(9) . . ? C82 B86 B91 102.0(9) . . ? B90 B86 B91 59.8(7) . . ? B87 B86 B91 59.3(7) . . ? C82 B87 B91 104.5(7) . . ? C82 B87 B86 59.4(6) . . ? B91 B87 B86 60.7(7) . . ? C82 B87 B88 102.8(7) . . ? B91 B87 B88 60.6(7) . . ? B86 B87 B88 109.0(8) . . ? C82 B87 B83 58.9(5) . . ? B91 B87 B83 108.2(8) . . ? B86 B87 B83 109.9(7) . . ? B88 B87 B83 58.4(6) . . ? B83 B88 B84 61.1(6) . . ? B83 B88 B89 109.4(7) . . ? B84 B88 B89 60.7(6) . . ? B83 B88 B87 61.2(6) . . ? B84 B88 B87 109.5(7) . . ? B89 B88 B87 107.4(7) . . ? B83 B88 B91 109.2(8) . . ? B84 B88 B91 109.3(7) . . ? B89 B88 B91 60.1(7) . . ? B87 B88 B91 59.0(7) . . ? B85 B89 B88 108.0(7) . . ? B85 B89 B91 108.6(8) . . ? B88 B89 B91 60.6(7) . . ? B85 B89 B84 60.8(6) . . ? B88 B89 B84 59.5(6) . . ? B91 B89 B84 108.9(8) . . ? B85 B89 B90 60.4(6) . . ? B88 B89 B90 107.1(8) . . ? B91 B89 B90 59.2(6) . . ? B84 B89 B90 108.4(7) . . ? C81 B90 B86 60.1(7) . . ? C81 B90 B91 105.9(8) . . ? B86 B90 B91 61.2(7) . . ? C81 B90 B85 59.4(6) . . ? B86 B90 B85 110.7(8) . . ? B91 B90 B85 108.5(7) . . ? C81 B90 B89 104.6(7) . . ? B86 B90 B89 109.8(8) . . ? B91 B90 B89 60.2(6) . . ? B85 B90 B89 59.2(6) . . ? B90 B91 B87 106.6(8) . . ? B90 B91 B89 60.6(6) . . ? B87 B91 B89 107.9(8) . . ? B90 B91 B86 59.0(7) . . ? B87 B91 B86 60.0(7) . . ? B89 B91 B86 108.4(8) . . ? B90 B91 B88 107.2(8) . . ? B87 B91 B88 60.4(7) . . ? B89 B91 B88 59.3(7) . . ? B86 B91 B88 108.3(9) . . ? C93 C92 B101 108.5(8) . . ? C93 C92 B97 60.8(6) . . ? B101 C92 B97 61.6(6) . . ? C93 C92 B96 109.9(7) . . ? B101 C92 B96 63.9(6) . . ? B97 C92 B96 115.3(8) . . ? C93 C92 Co80 67.8(4) . . ? B101 C92 Co80 124.3(7) . . ? B97 C92 Co80 125.4(6) . . ? B96 C92 Co80 66.1(5) . . ? C92 C93 B98 116.4(8) . . ? C92 C93 B97 63.4(6) . . ? B98 C93 B97 66.8(7) . . ? C92 C93 B94 112.2(7) . . ? B98 C93 B94 64.4(6) . . ? B97 C93 B94 120.1(8) . . ? C92 C93 Co80 67.0(4) . . ? B98 C93 Co80 124.6(6) . . ? B97 C93 Co80 127.0(6) . . ? B94 C93 Co80 64.4(5) . . ? C93 B94 B98 56.1(6) . . ? C93 B94 B95 105.2(8) . . ? B98 B94 B95 107.0(7) . . ? C93 B94 B99 101.9(7) . . ? B98 B94 B99 59.5(7) . . ? B95 B94 B99 58.8(6) . . ? C93 B94 Co80 66.7(4) . . ? B98 B94 Co80 119.1(6) . . ? B95 B94 Co80 68.2(5) . . ? B99 B94 Co80 120.4(7) . . ? B100 B95 B99 62.3(7) . . ? B100 B95 B96 59.7(6) . . ? B99 B95 B96 109.7(8) . . ? B100 B95 B94 108.7(8) . . ? B99 B95 B94 61.0(6) . . ? B96 B95 B94 105.5(8) . . ? B100 B95 Co80 116.0(7) . . ? B99 B95 Co80 116.3(7) . . ? B96 B95 Co80 63.4(5) . . ? B94 B95 Co80 61.5(4) . . ? C92 B96 B100 103.4(8) . . ? C92 B96 B95 106.2(7) . . ? B100 B96 B95 59.5(6) . . ? C92 B96 B101 57.8(6) . . ? B100 B96 B101 58.6(6) . . ? B95 B96 B101 107.0(8) . . ? C92 B96 Co80 64.7(4) . . ? B100 B96 Co80 119.1(7) . . ? B95 B96 Co80 67.3(5) . . ? B101 B96 Co80 117.6(7) . . ? C93 B97 C92 55.7(5) . . ? C93 B97 B101 102.5(8) . . ? C92 B97 B101 59.0(6) . . ? C93 B97 B102 101.5(8) . . ? C92 B97 B102 103.7(9) . . ? B101 B97 B102 59.6(7) . . ? C93 B97 B98 55.4(5) . . ? C92 B97 B98 101.2(7) . . ? B101 B97 B98 106.2(8) . . ? B102 B97 B98 59.7(6) . . ? C93 B98 B99 105.5(8) . . ? C93 B98 B94 59.5(5) . . ? B99 B98 B94 60.8(6) . . ? C93 B98 B102 102.9(8) . . ? B99 B98 B102 60.6(7) . . ? B94 B98 B102 108.4(8) . . ? C93 B98 B97 57.8(6) . . ? B99 B98 B97 108.9(8) . . ? B94 B98 B97 108.7(8) . . ? B102 B98 B97 59.3(6) . . ? B95 B99 B98 108.3(7) . . ? B95 B99 B94 60.2(6) . . ? B98 B99 B94 59.8(6) . . ? B95 B99 B102 107.4(8) . . ? B98 B99 B102 60.5(7) . . ? B94 B99 B102 107.6(8) . . ? B95 B99 B100 58.4(6) . . ? B98 B99 B100 106.2(8) . . ? B94 B99 B100 105.2(8) . . ? B102 B99 B100 58.9(7) . . ? B95 B100 B101 111.3(8) . . ? B95 B100 B96 60.8(6) . . ? B101 B100 B96 62.8(6) . . ? B95 B100 B102 109.2(8) . . ? B101 B100 B102 60.1(7) . . ? B96 B100 B102 110.3(8) . . ? B95 B100 B99 59.2(6) . . ? B101 B100 B99 108.7(8) . . ? B96 B100 B99 108.0(8) . . ? B102 B100 B99 60.3(7) . . ? C92 B101 B100 103.8(8) . . ? C92 B101 B97 59.4(6) . . ? B100 B101 B97 109.9(8) . . ? C92 B101 B102 105.3(8) . . ? B100 B101 B102 60.8(7) . . ? B97 B101 B102 61.2(7) . . ? C92 B101 B96 58.3(6) . . ? B100 B101 B96 58.6(7) . . ? B97 B101 B96 108.8(7) . . ? B102 B101 B96 107.6(8) . . ? B101 B102 B100 59.1(7) . . ? B101 B102 B97 59.2(6) . . ? B100 B102 B97 107.0(9) . . ? B101 B102 B98 106.9(8) . . ? B100 B102 B98 106.3(9) . . ? B97 B102 B98 61.0(6) . . ? B101 B102 B99 108.2(9) . . ? B100 B102 B99 60.8(7) . . ? B97 B102 B99 108.9(8) . . ? B98 B102 B99 58.8(7) . . ? C105 Co10 C104 46.4(3) . . ? C105 Co10 C115 99.0(3) . . ? C104 Co10 C115 101.0(4) . . ? C105 Co10 C116 101.6(3) . . ? C104 Co10 C116 135.4(4) . . ? C115 Co10 C116 46.5(4) . . ? C105 Co10 B108 83.6(4) . . ? C104 Co10 B108 48.8(4) . . ? C115 Co10 B108 133.1(4) . . ? C116 Co10 B108 174.8(4) . . ? C105 Co10 B107 83.9(4) . . ? C104 Co10 B107 84.4(4) . . ? C115 Co10 B107 174.5(4) . . ? C116 Co10 B107 128.5(4) . . ? B108 Co10 B107 51.7(4) . . ? C105 Co10 B106 48.5(4) . . ? C104 Co10 B106 83.2(4) . . ? C115 Co10 B106 128.8(4) . . ? C116 Co10 B106 96.0(4) . . ? B108 Co10 B106 87.5(4) . . ? B107 Co10 B106 50.4(4) . . ? C105 Co10 B117 134.3(4) . . ? C104 Co10 B117 175.7(4) . . ? C115 Co10 B117 83.2(4) . . ? C116 Co10 B117 48.6(4) . . ? B108 Co10 B117 127.4(4) . . ? B107 Co10 B117 91.4(4) . . ? B106 Co10 B117 95.0(4) . . ? C105 Co10 B118 173.0(4) . . ? C104 Co10 B118 126.8(4) . . ? C115 Co10 B118 83.4(4) . . ? C116 Co10 B118 84.8(4) . . ? B108 Co10 B118 90.0(4) . . ? B107 Co10 B118 94.2(4) . . ? B106 Co10 B118 134.1(4) . . ? B117 Co10 B118 52.3(4) . . ? C105 Co10 B119 126.8(4) . . ? C104 Co10 B119 93.8(4) . . ? C115 Co10 B119 47.9(4) . . ? C116 Co10 B119 83.4(4) . . ? B108 Co10 B119 93.4(4) . . ? B107 Co10 B119 133.4(4) . . ? B106 Co10 B119 175.1(4) . . ? B117 Co10 B119 88.2(4) . . ? B118 Co10 B119 50.8(4) . . ? C105 C104 B113 111.6(7) . . ? C105 C104 B108 112.2(7) . . ? B113 C104 B108 64.4(6) . . ? C105 C104 B109 62.7(5) . . ? B113 C104 B109 61.6(5) . . ? B108 C104 B109 116.0(7) . . ? C105 C104 Co10 66.6(4) . . ? B113 C104 Co10 125.9(6) . . ? B108 C104 Co10 67.3(4) . . ? B109 C104 Co10 125.6(6) . . ? C104 C105 B110 112.1(7) . . ? C104 C105 B106 112.6(7) . . ? B110 C105 B106 63.7(6) . . ? C104 C105 B109 62.5(5) . . ? B110 C105 B109 61.9(5) . . ? B106 C105 B109 115.4(7) . . ? C104 C105 Co10 67.0(4) . . ? B110 C105 Co10 126.2(6) . . ? B106 C105 Co10 68.0(5) . . ? B109 C105 Co10 125.8(6) . . ? C105 B106 B111 104.0(7) . . ? C105 B106 B110 57.8(5) . . ? B111 B106 B110 60.6(6) . . ? C105 B106 B107 104.6(7) . . ? B111 B106 B107 61.1(6) . . ? B110 B106 B107 109.7(7) . . ? C105 B106 Co10 63.5(4) . . ? B111 B106 Co10 118.0(7) . . ? B110 B106 Co10 117.0(6) . . ? B107 B106 Co10 64.6(5) . . ? B106 B107 B111 58.8(6) . . ? B106 B107 B108 106.8(7) . . ? B111 B107 B108 106.2(7) . . ? B106 B107 B112 105.9(7) . . ? B111 B107 B112 59.4(6) . . ? B108 B107 B112 58.5(6) . . ? B106 B107 Co10 65.0(5) . . ? B111 B107 Co10 116.4(6) . . ? B108 B107 Co10 64.0(4) . . ? B112 B107 Co10 115.3(6) . . ? C104 B108 B112 102.8(7) . . ? C104 B108 B113 57.1(5) . . ? B112 B108 B113 59.6(6) . . ? C104 B108 B107 103.7(7) . . ? B112 B108 B107 60.8(6) . . ? B113 B108 B107 108.0(7) . . ? C104 B108 Co10 63.9(4) . . ? B112 B108 Co10 117.6(7) . . ? B113 B108 Co10 116.3(6) . . ? B107 B108 Co10 64.3(5) . . ? C104 B109 C105 54.8(5) . . ? C104 B109 B114 104.1(6) . . ? C105 B109 B114 104.0(7) . . ? C104 B109 B113 57.5(5) . . ? C105 B109 B113 102.0(6) . . ? B114 B109 B113 61.2(6) . . ? C104 B109 B110 102.3(6) . . ? C105 B109 B110 57.5(5) . . ? B114 B109 B110 61.4(6) . . ? B113 B109 B110 108.8(7) . . ? C105 B110 B109 60.6(5) . . ? C105 B110 B106 58.5(5) . . ? B109 B110 B106 110.0(7) . . ? C105 B110 B111 103.3(7) . . ? B109 B110 B111 108.1(7) . . ? B106 B110 B111 59.1(6) . . ? C105 B110 B114 104.4(7) . . ? B109 B110 B114 58.8(6) . . ? B106 B110 B114 108.5(7) . . ? B111 B110 B114 60.9(6) . . ? B106 B111 B110 60.3(5) . . ? B106 B111 B112 108.1(7) . . ? B110 B111 B112 107.2(7) . . ? B106 B111 B107 60.1(6) . . ? B110 B111 B107 108.7(7) . . ? B112 B111 B107 61.0(6) . . ? B106 B111 B114 108.4(7) . . ? B110 B111 B114 59.6(6) . . ? B112 B111 B114 59.9(6) . . ? B107 B111 B114 109.6(8) . . ? B113 B112 B108 60.6(6) . . ? B113 B112 B111 107.2(7) . . ? B108 B112 B111 108.0(7) . . ? B113 B112 B114 59.4(6) . . ? B108 B112 B114 108.8(7) . . ? B111 B112 B114 60.4(6) . . ? B113 B112 B107 108.6(7) . . ? B108 B112 B107 60.6(6) . . ? B111 B112 B107 59.6(6) . . ? B114 B112 B107 108.9(7) . . ? C104 B113 B109 60.9(5) . . ? C104 B113 B114 105.3(7) . . ? B109 B113 B114 59.3(6) . . ? C104 B113 B112 104.0(7) . . ? B109 B113 B112 108.7(8) . . ? B114 B113 B112 60.9(6) . . ? C104 B113 B108 58.5(5) . . ? B109 B113 B108 110.6(7) . . ? B114 B113 B108 109.4(8) . . ? B112 B113 B108 59.8(6) . . ? B109 B114 B113 59.6(6) . . ? B109 B114 B110 59.9(6) . . ? B113 B114 B110 106.4(7) . . ? B109 B114 B112 108.0(7) . . ? B113 B114 B112 59.7(6) . . ? B110 B114 B112 107.0(7) . . ? B109 B114 B111 107.9(7) . . ? B113 B114 B111 106.9(7) . . ? B110 B114 B111 59.6(6) . . ? B112 B114 B111 59.7(6) . . ? C116 C115 B124 111.7(7) . . ? C116 C115 B119 114.3(7) . . ? B124 C115 B119 63.9(6) . . ? C116 C115 B120 63.0(6) . . ? B124 C115 B120 60.7(6) . . ? B119 C115 B120 115.6(7) . . ? C116 C115 Co10 67.1(4) . . ? B124 C115 Co10 126.2(6) . . ? B119 C115 Co10 68.6(4) . . ? B120 C115 Co10 126.1(6) . . ? C115 C116 B117 111.7(6) . . ? C115 C116 B121 110.2(7) . . ? B117 C116 B121 63.1(6) . . ? C115 C116 B120 61.9(6) . . ? B117 C116 B120 115.1(7) . . ? B121 C116 B120 61.6(6) . . ? C115 C116 Co10 66.5(4) . . ? B117 C116 Co10 67.3(4) . . ? B121 C116 Co10 124.0(6) . . ? B120 C116 Co10 124.5(6) . . ? C116 B117 B122 103.4(7) . . ? C116 B117 B121 59.0(6) . . ? B122 B117 B121 57.9(6) . . ? C116 B117 B118 103.7(7) . . ? B122 B117 B118 60.6(5) . . ? B121 B117 B118 106.5(7) . . ? C116 B117 Co10 64.1(4) . . ? B122 B117 Co10 117.5(6) . . ? B121 B117 Co10 117.6(6) . . ? B118 B117 Co10 64.1(4) . . ? B123 B118 B119 58.6(5) . . ? B123 B118 B122 60.6(6) . . ? B119 B118 B122 106.5(7) . . ? B123 B118 B117 105.9(7) . . ? B119 B118 B117 106.4(6) . . ? B122 B118 B117 57.6(5) . . ? B123 B118 Co10 115.9(6) . . ? B119 B118 Co10 64.9(4) . . ? B122 B118 Co10 114.5(6) . . ? B117 B118 Co10 63.6(4) . . ? C115 B119 B123 103.2(7) . . ? C115 B119 B124 57.4(5) . . ? B123 B119 B124 60.0(6) . . ? C115 B119 B118 103.9(7) . . ? B123 B119 B118 60.1(6) . . ? B124 B119 B118 107.8(7) . . ? C115 B119 Co10 63.4(4) . . ? B123 B119 Co10 116.6(6) . . ? B124 B119 Co10 115.8(6) . . ? B118 B119 Co10 64.3(4) . . ? B124 B120 C115 57.8(5) . . ? B124 B120 C116 102.9(7) . . ? C115 B120 C116 55.1(5) . . ? B124 B120 B125 61.7(6) . . ? C115 B120 B125 104.3(7) . . ? C116 B120 B125 103.9(7) . . ? B124 B120 B121 107.5(8) . . ? C115 B120 B121 102.5(7) . . ? C116 B120 B121 58.7(5) . . ? B125 B120 B121 58.9(6) . . ? C116 B121 B122 104.5(7) . . ? C116 B121 B125 105.7(8) . . ? B122 B121 B125 61.7(6) . . ? C116 B121 B120 59.7(6) . . ? B122 B121 B120 109.5(8) . . ? B125 B121 B120 60.1(6) . . ? C116 B121 B117 57.8(5) . . ? B122 B121 B117 60.4(6) . . ? B125 B121 B117 110.3(8) . . ? B120 B121 B117 109.1(7) . . ? B121 B122 B117 61.6(6) . . ? B121 B122 B125 59.5(6) . . ? B117 B122 B125 109.4(7) . . ? B121 B122 B123 106.7(8) . . ? B117 B122 B123 107.6(7) . . ? B125 B122 B123 59.6(6) . . ? B121 B122 B118 110.3(7) . . ? B117 B122 B118 61.8(5) . . ? B125 B122 B118 108.3(7) . . ? B123 B122 B118 58.5(6) . . ? B119 B123 B124 60.4(6) . . ? B119 B123 B118 61.4(6) . . ? B124 B123 B118 109.1(7) . . ? B119 B123 B125 109.8(7) . . ? B124 B123 B125 60.1(6) . . ? B118 B123 B125 109.7(7) . . ? B119 B123 B122 109.0(7) . . ? B124 B123 B122 106.3(7) . . ? B118 B123 B122 60.9(6) . . ? B125 B123 B122 59.0(6) . . ? C115 B124 B120 61.5(6) . . ? C115 B124 B123 104.0(7) . . ? B120 B124 B123 109.9(8) . . ? C115 B124 B119 58.7(5) . . ? B120 B124 B119 111.9(7) . . ? B123 B124 B119 59.7(6) . . ? C115 B124 B125 106.2(7) . . ? B120 B124 B125 60.5(6) . . ? B123 B124 B125 60.7(6) . . ? B119 B124 B125 109.7(7) . . ? B121 B125 B120 61.0(6) . . ? B121 B125 B122 58.8(6) . . ? B120 B125 B122 107.9(7) . . ? B121 B125 B124 106.1(7) . . ? B120 B125 B124 57.8(6) . . ? B122 B125 B124 107.4(7) . . ? B121 B125 B123 107.5(7) . . ? B120 B125 B123 106.4(7) . . ? B122 B125 B123 61.4(6) . . ? B124 B125 B123 59.2(6) . . ? O129 N127 O128 117.9(12) . . ? O129 N127 C126 122.9(11) . . ? O128 N127 C126 119.2(10) . . ? O132 N131 O133 128(2) . . ? O132 N131 C130 122(2) . . ? O133 N131 C130 110(2) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.83 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.182 _refine_diff_density_min -0.826 _refine_diff_density_rms 0.132 #=END data_c:\datasets\leeds\mh132\mh132 _database_code_depnum_ccdc_archive 'CCDC 278900' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-bis(3-methylpyrazol-1-yl)pyridine]iron(II) dihexafluoroantimonate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Fe N10, 2[F6 Sb]' _chemical_formula_sum 'C26 H26 F12 Fe N10 Sb2' _chemical_formula_weight 1005.92 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.7007(4) _cell_length_b 11.1095(2) _cell_length_c 16.8557(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.9156(6) _cell_angle_gamma 90.00 _cell_volume 3446.02(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 51570 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 27.49 _exptl_crystal_description Yellow _exptl_crystal_colour Plate _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.939 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 2.073 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.547 _exptl_absorpt_correction_T_max 0.860 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_ambient_temperature 150(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 area detector diffractometer' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51570 _diffrn_reflns_av_R_equivalents 0.1005 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7885 _reflns_number_gt 5859 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 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 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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. No disorder was detected during refinement and no restraints were applied. All non-H atoms were refined anisotropically, while H atoms were placed in calculated positions and refined using a riding model. The deepest Fourier hole of -1.4 e.\%A^-3^ is 0.9\%A from Sb38. ; _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^)+(0.0572P)^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 7885 _refine_ls_number_parameters 464 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.26871(3) -0.27911(5) 0.12957(3) 0.02936(13) Uani 1 1 d . . . N2 N 0.22597(15) -0.4383(3) 0.05971(18) 0.0302(6) Uani 1 1 d . . . C3 C 0.23214(18) -0.5444(3) 0.0989(2) 0.0317(8) Uani 1 1 d . . . C4 C 0.2003(2) -0.6489(3) 0.0577(2) 0.0362(8) Uani 1 1 d . . . H4 H 0.2062 -0.7236 0.0868 0.043 Uiso 1 1 calc R . . C5 C 0.1594(2) -0.6394(3) -0.0281(3) 0.0403(9) Uani 1 1 d . . . H5 H 0.1364 -0.7091 -0.0585 0.048 Uiso 1 1 calc R . . C6 C 0.1515(2) -0.5316(3) -0.0699(2) 0.0363(8) Uani 1 1 d . . . H6 H 0.1234 -0.5252 -0.1287 0.044 Uiso 1 1 calc R . . C7 C 0.18608(18) -0.4324(3) -0.0232(2) 0.0315(8) Uani 1 1 d . . . N8 N 0.27372(15) -0.5373(2) 0.18592(18) 0.0307(6) Uani 1 1 d . . . N9 N 0.29510(15) -0.4260(3) 0.22157(18) 0.0326(7) Uani 1 1 d . . . C10 C 0.32948(19) -0.4465(4) 0.3042(2) 0.0364(8) Uani 1 1 d . . . C11 C 0.3294(2) -0.5706(4) 0.3210(2) 0.0399(9) Uani 1 1 d . . . H11 H 0.3501 -0.6089 0.3747 0.048 Uiso 1 1 calc R . . C12 C 0.2941(2) -0.6244(4) 0.2460(2) 0.0381(9) Uani 1 1 d . . . H12 H 0.2852 -0.7082 0.2368 0.046 Uiso 1 1 calc R . . C13 C 0.3593(2) -0.3455(4) 0.3649(3) 0.0503(11) Uani 1 1 d . . . H13A H 0.3895 -0.2938 0.3438 0.076 Uiso 1 1 calc R . . H13B H 0.3889 -0.3781 0.4205 0.076 Uiso 1 1 calc R . . H13C H 0.3192 -0.2982 0.3703 0.076 Uiso 1 1 calc R . . N14 N 0.18328(17) -0.3156(2) -0.05668(18) 0.0328(7) Uani 1 1 d . . . N15 N 0.21863(16) -0.2239(3) -0.0020(2) 0.0343(7) Uani 1 1 d . . . C16 C 0.2059(2) -0.1256(3) -0.0508(2) 0.0399(9) Uani 1 1 d . . . C17 C 0.1636(2) -0.1540(4) -0.1362(2) 0.0462(10) Uani 1 1 d . . . H17 H 0.1481 -0.1002 -0.1831 0.055 Uiso 1 1 calc R . . C18 C 0.1499(2) -0.2734(4) -0.1372(3) 0.0436(10) Uani 1 1 d . . . H18 H 0.1220 -0.3194 -0.1853 0.052 Uiso 1 1 calc R . . C19 C 0.2354(3) -0.0065(4) -0.0127(3) 0.0564(12) Uani 1 1 d . . . H19A H 0.2056 0.0255 0.0181 0.085 Uiso 1 1 calc R . . H19B H 0.2346 0.0497 -0.0579 0.085 Uiso 1 1 calc R . . H19C H 0.2856 -0.0166 0.0267 0.085 Uiso 1 1 calc R . . N20 N 0.30799(15) -0.1189(2) 0.20037(18) 0.0292(6) Uani 1 1 d . . . C21 C 0.37837(18) -0.0895(3) 0.2232(2) 0.0288(7) Uani 1 1 d . . . C22 C 0.4114(2) -0.0041(3) 0.2849(2) 0.0359(8) Uani 1 1 d . . . H22 H 0.4616 0.0145 0.3012 0.043 Uiso 1 1 calc R . . C23 C 0.3666(2) 0.0533(3) 0.3218(2) 0.0394(9) Uani 1 1 d . . . H23 H 0.3872 0.1111 0.3653 0.047 Uiso 1 1 calc R . . C24 C 0.2937(2) 0.0281(3) 0.2966(2) 0.0366(8) Uani 1 1 d . . . H24 H 0.2632 0.0692 0.3204 0.044 Uiso 1 1 calc R . . C25 C 0.26665(19) -0.0595(3) 0.2351(2) 0.0320(8) Uani 1 1 d . . . N26 N 0.41359(15) -0.1533(3) 0.17738(17) 0.0292(6) Uani 1 1 d . . . N27 N 0.37767(16) -0.2484(2) 0.12799(18) 0.0294(6) Uani 1 1 d . . . C28 C 0.41962(19) -0.2838(3) 0.0855(2) 0.0318(8) Uani 1 1 d . . . C29 C 0.4815(2) -0.2098(3) 0.1063(2) 0.0351(8) Uani 1 1 d . . . H29 H 0.5195 -0.2152 0.0842 0.042 Uiso 1 1 calc R . . C30 C 0.47614(19) -0.1290(3) 0.1645(2) 0.0334(8) Uani 1 1 d . . . H30 H 0.5099 -0.0671 0.1910 0.040 Uiso 1 1 calc R . . C31 C 0.3982(2) -0.3865(3) 0.0249(2) 0.0380(9) Uani 1 1 d . . . H31A H 0.3574 -0.4296 0.0321 0.057 Uiso 1 1 calc R . . H31B H 0.4395 -0.4415 0.0360 0.057 Uiso 1 1 calc R . . H31C H 0.3836 -0.3561 -0.0334 0.057 Uiso 1 1 calc R . . N32 N 0.19349(16) -0.0948(3) 0.20094(19) 0.0348(7) Uani 1 1 d . . . N33 N 0.17589(17) -0.2022(3) 0.1573(2) 0.0363(7) Uani 1 1 d . . . C34 C 0.1034(2) -0.2075(4) 0.1273(3) 0.0418(9) Uani 1 1 d . . . C35 C 0.0746(2) -0.1023(4) 0.1510(3) 0.0463(10) Uani 1 1 d . . . H35 H 0.0247 -0.0836 0.1377 0.056 Uiso 1 1 calc R . . C36 C 0.1323(2) -0.0335(4) 0.1966(3) 0.0441(10) Uani 1 1 d . . . H36 H 0.1304 0.0431 0.2208 0.053 Uiso 1 1 calc R . . C37 C 0.0634(2) -0.3127(4) 0.0776(3) 0.0529(11) Uani 1 1 d . . . H37A H 0.0403 -0.2899 0.0178 0.079 Uiso 1 1 calc R . . H37B H 0.0261 -0.3386 0.0998 0.079 Uiso 1 1 calc R . . H37C H 0.0975 -0.3790 0.0825 0.079 Uiso 1 1 calc R . . Sb38 Sb 0.410802(13) -0.75830(2) 0.089448(15) 0.03311(9) Uani 1 1 d . . . F39 F 0.48094(14) -0.6848(2) 0.05445(16) 0.0534(6) Uani 1 1 d . . . F40 F 0.48433(12) -0.8211(2) 0.18500(13) 0.0441(5) Uani 1 1 d . . . F41 F 0.33968(12) -0.8279(2) 0.12492(14) 0.0457(5) Uani 1 1 d . . . F42 F 0.33837(14) -0.6968(2) -0.00768(14) 0.0544(6) Uani 1 1 d . . . F43 F 0.40742(12) -0.61855(19) 0.14999(14) 0.0429(5) Uani 1 1 d . . . F44 F 0.41497(14) -0.8973(2) 0.02868(15) 0.0546(6) Uani 1 1 d . . . Sb45 Sb 0.079938(14) -0.68085(2) 0.228920(16) 0.03827(9) Uani 1 1 d . . . F46 F 0.13226(12) -0.5510(2) 0.20827(15) 0.0496(6) Uani 1 1 d . . . F47 F 0.16713(14) -0.7662(2) 0.27945(19) 0.0618(7) Uani 1 1 d . . . F48 F 0.03060(15) -0.8110(2) 0.25175(19) 0.0668(8) Uani 1 1 d . . . F49 F -0.00636(13) -0.5952(3) 0.1802(2) 0.0745(9) Uani 1 1 d . . . F50 F 0.09134(14) -0.6173(2) 0.33580(16) 0.0590(7) Uani 1 1 d . . . F51 F 0.07163(19) -0.7485(3) 0.12489(19) 0.0765(9) 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 0.0274(3) 0.0302(3) 0.0289(3) -0.0028(2) 0.0081(2) -0.0017(2) N2 0.0243(15) 0.0339(16) 0.0303(16) 0.0029(12) 0.0073(12) 0.0046(12) C3 0.0261(18) 0.037(2) 0.033(2) 0.0000(15) 0.0117(15) 0.0034(14) C4 0.039(2) 0.0290(19) 0.040(2) 0.0001(15) 0.0145(17) -0.0005(16) C5 0.044(2) 0.0249(19) 0.048(2) -0.0053(16) 0.0111(19) -0.0003(16) C6 0.036(2) 0.037(2) 0.031(2) -0.0032(15) 0.0051(16) -0.0012(16) C7 0.0288(18) 0.0309(19) 0.0320(19) 0.0019(14) 0.0077(15) 0.0030(14) N8 0.0296(15) 0.0309(16) 0.0297(16) 0.0016(12) 0.0083(13) 0.0004(12) N9 0.0283(15) 0.0368(17) 0.0318(16) -0.0002(13) 0.0096(13) -0.0005(13) C10 0.0290(19) 0.047(2) 0.033(2) -0.0010(16) 0.0118(16) -0.0014(16) C11 0.037(2) 0.048(2) 0.033(2) 0.0085(17) 0.0104(17) 0.0055(17) C12 0.040(2) 0.039(2) 0.036(2) 0.0080(16) 0.0150(18) 0.0070(17) C13 0.049(3) 0.058(3) 0.038(2) -0.0025(19) 0.0074(19) -0.009(2) N14 0.0344(16) 0.0283(16) 0.0295(16) -0.0019(12) 0.0036(13) -0.0032(12) N15 0.0316(17) 0.0322(16) 0.0348(17) -0.0009(13) 0.0068(14) -0.0056(13) C16 0.043(2) 0.035(2) 0.038(2) 0.0030(16) 0.0088(18) -0.0040(17) C17 0.056(3) 0.037(2) 0.036(2) 0.0083(17) 0.0035(19) -0.0067(19) C18 0.044(2) 0.041(2) 0.034(2) 0.0027(16) -0.0009(18) 0.0002(18) C19 0.069(3) 0.038(2) 0.050(3) 0.0007(19) 0.007(2) -0.012(2) N20 0.0289(15) 0.0292(15) 0.0288(15) 0.0000(12) 0.0096(12) -0.0001(12) C21 0.0304(18) 0.0274(18) 0.0277(18) 0.0033(13) 0.0094(14) 0.0022(14) C22 0.038(2) 0.037(2) 0.0286(19) -0.0025(15) 0.0059(16) -0.0058(16) C23 0.052(2) 0.0289(19) 0.036(2) -0.0067(15) 0.0134(18) -0.0058(17) C24 0.045(2) 0.0297(19) 0.039(2) -0.0031(15) 0.0186(18) 0.0045(16) C25 0.0308(19) 0.0290(18) 0.036(2) 0.0036(15) 0.0122(16) 0.0038(15) N26 0.0275(15) 0.0328(15) 0.0255(15) -0.0013(12) 0.0074(12) -0.0029(12) N27 0.0305(16) 0.0296(15) 0.0272(15) -0.0013(11) 0.0090(13) 0.0000(12) C28 0.033(2) 0.0323(19) 0.0293(19) 0.0043(14) 0.0102(16) 0.0052(15) C29 0.0287(19) 0.042(2) 0.036(2) 0.0037(16) 0.0139(16) 0.0030(16) C30 0.0271(18) 0.034(2) 0.036(2) 0.0000(15) 0.0082(15) -0.0048(15) C31 0.042(2) 0.037(2) 0.039(2) -0.0021(16) 0.0191(17) -0.0017(16) N32 0.0345(17) 0.0336(17) 0.0389(18) -0.0015(13) 0.0161(14) 0.0028(13) N33 0.0308(17) 0.0388(17) 0.0387(18) -0.0033(14) 0.0116(14) 0.0019(13) C34 0.032(2) 0.053(2) 0.042(2) 0.0047(19) 0.0146(18) 0.0034(18) C35 0.033(2) 0.059(3) 0.049(2) 0.005(2) 0.0171(19) 0.0098(19) C36 0.042(2) 0.042(2) 0.054(3) 0.0046(18) 0.025(2) 0.0130(18) C37 0.032(2) 0.066(3) 0.058(3) -0.007(2) 0.012(2) -0.0063(19) Sb38 0.03452(15) 0.03664(16) 0.02794(14) -0.00110(9) 0.01086(11) -0.00139(10) F39 0.0532(15) 0.0592(16) 0.0605(16) 0.0029(12) 0.0356(13) -0.0013(12) F40 0.0404(13) 0.0478(14) 0.0370(12) -0.0022(10) 0.0053(10) 0.0031(10) F41 0.0408(13) 0.0491(14) 0.0469(13) 0.0039(10) 0.0153(10) -0.0082(10) F42 0.0541(15) 0.0674(17) 0.0350(13) 0.0104(11) 0.0077(11) 0.0034(12) F43 0.0487(14) 0.0388(12) 0.0447(13) -0.0024(9) 0.0208(11) 0.0021(10) F44 0.0641(16) 0.0521(15) 0.0430(13) -0.0137(11) 0.0136(12) 0.0020(12) Sb45 0.03414(15) 0.03410(16) 0.04298(17) 0.00172(10) 0.00937(12) 0.00368(10) F46 0.0476(14) 0.0426(13) 0.0649(16) 0.0027(11) 0.0278(12) 0.0017(11) F47 0.0432(15) 0.0470(15) 0.089(2) 0.0034(13) 0.0159(14) 0.0140(11) F48 0.0573(17) 0.0498(16) 0.085(2) 0.0127(14) 0.0150(15) -0.0117(12) F49 0.0376(14) 0.0705(19) 0.106(2) 0.0343(16) 0.0137(14) 0.0144(13) F50 0.0732(18) 0.0571(16) 0.0524(15) -0.0060(12) 0.0295(14) 0.0010(13) F51 0.103(3) 0.0694(19) 0.0544(18) -0.0191(14) 0.0252(18) -0.0122(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 N2 2.125(3) . ? Fe1 N20 2.129(3) . ? Fe1 N15 2.169(3) . ? Fe1 N9 2.182(3) . ? Fe1 N27 2.183(3) . ? Fe1 N33 2.214(3) . ? N2 C3 1.335(5) . ? N2 C7 1.338(4) . ? C3 C4 1.383(5) . ? C3 N8 1.404(4) . ? C4 C5 1.385(5) . ? C5 C6 1.371(5) . ? C6 C7 1.384(5) . ? C7 N14 1.408(4) . ? N8 C12 1.353(4) . ? N8 N9 1.374(4) . ? N9 C10 1.333(5) . ? C10 C11 1.408(6) . ? C10 C13 1.490(5) . ? C11 C12 1.346(5) . ? N14 C18 1.362(5) . ? N14 N15 1.384(4) . ? N15 C16 1.337(5) . ? C16 C17 1.417(5) . ? C16 C19 1.495(5) . ? C17 C18 1.353(5) . ? N20 C25 1.335(4) . ? N20 C21 1.340(4) . ? C21 C22 1.385(5) . ? C21 N26 1.402(4) . ? C22 C23 1.401(5) . ? C23 C24 1.374(5) . ? C24 C25 1.382(5) . ? C25 N32 1.404(4) . ? N26 C30 1.353(4) . ? N26 N27 1.375(4) . ? N27 C28 1.331(5) . ? C28 C29 1.407(5) . ? C28 C31 1.489(5) . ? C29 C30 1.361(5) . ? N32 C36 1.364(5) . ? N32 N33 1.380(4) . ? N33 C34 1.336(5) . ? C34 C35 1.418(6) . ? C34 C37 1.489(6) . ? C35 C36 1.358(6) . ? Sb38 F44 1.871(2) . ? Sb38 F43 1.872(2) . ? Sb38 F39 1.872(2) . ? Sb38 F40 1.874(2) . ? Sb38 F42 1.875(2) . ? Sb38 F41 1.875(2) . ? Sb45 F48 1.858(2) . ? Sb45 F51 1.861(3) . ? Sb45 F49 1.863(2) . ? Sb45 F50 1.872(2) . ? Sb45 F46 1.877(2) . ? Sb45 F47 1.879(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 N2 Fe1 N20 177.95(11) . . ? N2 Fe1 N15 73.94(11) . . ? N20 Fe1 N15 106.15(11) . . ? N2 Fe1 N9 73.63(11) . . ? N20 Fe1 N9 106.28(11) . . ? N15 Fe1 N9 147.56(11) . . ? N2 Fe1 N27 108.67(11) . . ? N20 Fe1 N27 73.38(11) . . ? N15 Fe1 N27 91.94(11) . . ? N9 Fe1 N27 98.03(11) . . ? N2 Fe1 N33 104.14(11) . . ? N20 Fe1 N33 73.83(11) . . ? N15 Fe1 N33 89.87(12) . . ? N9 Fe1 N33 98.28(11) . . ? N27 Fe1 N33 146.32(11) . . ? C3 N2 C7 118.4(3) . . ? C3 N2 Fe1 120.8(2) . . ? C7 N2 Fe1 120.4(2) . . ? N2 C3 C4 123.2(3) . . ? N2 C3 N8 112.6(3) . . ? C4 C3 N8 124.2(3) . . ? C3 C4 C5 116.7(3) . . ? C6 C5 C4 121.4(3) . . ? C5 C6 C7 117.4(3) . . ? N2 C7 C6 122.8(3) . . ? N2 C7 N14 112.8(3) . . ? C6 C7 N14 124.4(3) . . ? C12 N8 N9 110.7(3) . . ? C12 N8 C3 130.4(3) . . ? N9 N8 C3 118.7(3) . . ? C10 N9 N8 105.4(3) . . ? C10 N9 Fe1 140.6(3) . . ? N8 N9 Fe1 113.8(2) . . ? N9 C10 C11 109.9(3) . . ? N9 C10 C13 121.2(4) . . ? C11 C10 C13 128.8(4) . . ? C12 C11 C10 106.4(3) . . ? C11 C12 N8 107.6(3) . . ? C18 N14 N15 111.1(3) . . ? C18 N14 C7 130.7(3) . . ? N15 N14 C7 118.2(3) . . ? C16 N15 N14 104.6(3) . . ? C16 N15 Fe1 141.1(3) . . ? N14 N15 Fe1 114.2(2) . . ? N15 C16 C17 110.9(3) . . ? N15 C16 C19 119.9(3) . . ? C17 C16 C19 129.1(4) . . ? C18 C17 C16 105.9(3) . . ? C17 C18 N14 107.6(3) . . ? C25 N20 C21 118.9(3) . . ? C25 N20 Fe1 120.2(2) . . ? C21 N20 Fe1 119.8(2) . . ? N20 C21 C22 122.9(3) . . ? N20 C21 N26 112.5(3) . . ? C22 C21 N26 124.6(3) . . ? C21 C22 C23 116.3(3) . . ? C24 C23 C22 121.6(3) . . ? C23 C24 C25 117.1(3) . . ? N20 C25 C24 123.0(3) . . ? N20 C25 N32 112.3(3) . . ? C24 C25 N32 124.7(3) . . ? C30 N26 N27 111.0(3) . . ? C30 N26 C21 130.3(3) . . ? N27 N26 C21 118.3(3) . . ? C28 N27 N26 105.6(3) . . ? C28 N27 Fe1 139.7(2) . . ? N26 N27 Fe1 114.1(2) . . ? N27 C28 C29 110.1(3) . . ? N27 C28 C31 121.1(3) . . ? C29 C28 C31 128.8(3) . . ? C30 C29 C28 106.3(3) . . ? N26 C30 C29 107.1(3) . . ? C36 N32 N33 110.8(3) . . ? C36 N32 C25 129.8(3) . . ? N33 N32 C25 119.1(3) . . ? C34 N33 N32 105.7(3) . . ? C34 N33 Fe1 139.1(3) . . ? N32 N33 Fe1 112.1(2) . . ? N33 C34 C35 109.8(4) . . ? N33 C34 C37 121.8(4) . . ? C35 C34 C37 128.4(4) . . ? C36 C35 C34 106.6(4) . . ? C35 C36 N32 107.1(4) . . ? F44 Sb38 F43 179.41(11) . . ? F44 Sb38 F39 90.33(11) . . ? F43 Sb38 F39 89.09(10) . . ? F44 Sb38 F40 89.53(10) . . ? F43 Sb38 F40 90.42(9) . . ? F39 Sb38 F40 90.12(11) . . ? F44 Sb38 F42 89.49(11) . . ? F43 Sb38 F42 90.56(10) . . ? F39 Sb38 F42 89.04(11) . . ? F40 Sb38 F42 178.70(11) . . ? F44 Sb38 F41 91.05(11) . . ? F43 Sb38 F41 89.54(10) . . ? F39 Sb38 F41 178.49(10) . . ? F40 Sb38 F41 90.51(10) . . ? F42 Sb38 F41 90.35(11) . . ? F48 Sb45 F51 90.24(14) . . ? F48 Sb45 F49 91.50(12) . . ? F51 Sb45 F49 91.82(15) . . ? F48 Sb45 F50 89.22(13) . . ? F51 Sb45 F50 177.65(13) . . ? F49 Sb45 F50 90.48(13) . . ? F48 Sb45 F46 178.34(12) . . ? F51 Sb45 F46 90.30(12) . . ? F49 Sb45 F46 90.05(11) . . ? F50 Sb45 F46 90.19(11) . . ? F48 Sb45 F47 88.54(12) . . ? F51 Sb45 F47 88.97(14) . . ? F49 Sb45 F47 179.21(14) . . ? F50 Sb45 F47 88.73(12) . . ? F46 Sb45 F47 89.90(11) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.645 _refine_diff_density_min -1.416 _refine_diff_density_rms 0.194 data_je34c _database_code_depnum_ccdc_archive 'CCDC 278901' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-(3-methylpyrazol-1-yl)pyridine]iron(II) diperchlorate acetone solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Fe N10, 2[Cl O4], C3 H6 O' _chemical_formula_sum 'C29 H32 Cl2 Fe N10 O9' _chemical_formula_weight 791.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.3113(3) _cell_length_b 11.2528(2) _cell_length_c 28.4066(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.3076(8) _cell_angle_gamma 90.00 _cell_volume 7114.13(19) _cell_formula_units_Z 8 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 35705 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 27.50 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 0.640 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.226 _exptl_absorpt_correction_T_max 1.016 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings The high value of Rint reflects the highly redundant dataset collected for this crystal. ; _diffrn_ambient_temperature 250(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 diffractometer' _diffrn_measurement_method 'Area detector scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35705 _diffrn_reflns_av_R_equivalents 0.1834 _diffrn_reflns_av_sigmaI/netI 0.1053 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8106 _reflns_number_gt 5534 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 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 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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. Both the ClO~4~^-^ anions are disordered: Cl38A-O42A (occupancy 0.50) and Cl38B-O42B (occupancy 0.50) and Cl43A-O47A (occupancy 0.35), Cl43B-O47B (occupancy 0.35) and Cl43C-O47C (occupancy 0.30). All disordered Cl-O distances were restrained to 1.43(2)\%A, and O...O distances within a given disorder orientation to 2.34(2)\%A. The acetone molecule is also disordered, over two different orientations: C48A-O51A (occupancy 0.50) and C48B-O51B (occupancy 0.50). Although the thermal ellipsoids on these two partial molecules are slightly high, we were unable to locate, or refine, a third disorder orientation at this temperature (c.f. the datasets at 100 K and 150 K, where a third partial molecule was clearly evident. The following restraints were applied to this molecule: C-C = 1.49(2)\%A, C=O = 1.24(2)\%A and 1,3-C...O = 2.36(2)\%A. All wholly occupied non-H atoms were refined anisotropically. All H atoms were placed in calculated positions and refined using a riding model, except for the solvent methyl groups whose torsions were not allowed to refine. The residual Fourier hole at -1.5 e.\%A^-3^ lies 0.9\%A from Fe1. ; _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^)+(0.1552P)^2^+7.5223P] 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 SHELXL _refine_ls_extinction_coef 0.0088(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8106 _refine_ls_number_parameters 475 _refine_ls_number_restraints 62 _refine_ls_R_factor_all 0.1266 _refine_ls_R_factor_gt 0.0851 _refine_ls_wR_factor_ref 0.2566 _refine_ls_wR_factor_gt 0.2223 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.057 _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 0.59339(2) 0.32703(5) 0.640323(18) 0.0446(2) Uani 1 1 d . . . N2 N 0.60430(13) 0.4833(3) 0.68323(10) 0.0459(7) Uani 1 1 d . . . C3 C 0.55633(17) 0.5398(4) 0.68953(13) 0.0492(9) Uani 1 1 d . . . C4 C 0.5622(2) 0.6411(4) 0.71780(15) 0.0565(10) Uani 1 1 d . . . H4 H 0.5282 0.6813 0.7210 0.068 Uiso 1 1 calc R . . C5 C 0.6196(2) 0.6820(4) 0.74128(16) 0.0620(11) Uani 1 1 d . . . H5 H 0.6247 0.7493 0.7617 0.074 Uiso 1 1 calc R . . C6 C 0.6696(2) 0.6252(4) 0.73517(15) 0.0589(10) Uani 1 1 d . . . H6 H 0.7087 0.6522 0.7511 0.071 Uiso 1 1 calc R . . C7 C 0.65923(17) 0.5271(4) 0.70466(13) 0.0485(8) Uani 1 1 d . . . N8 N 0.50229(14) 0.4861(3) 0.66470(11) 0.0501(7) Uani 1 1 d . . . N9 N 0.50344(14) 0.3835(3) 0.63919(12) 0.0515(8) Uani 1 1 d . . . C10 C 0.44629(19) 0.3486(4) 0.62073(16) 0.0578(10) Uani 1 1 d . . . C11 C 0.40871(19) 0.4325(5) 0.63470(18) 0.0647(12) Uani 1 1 d . . . H11 H 0.3666 0.4298 0.6267 0.078 Uiso 1 1 calc R . . C12 C 0.44470(19) 0.5154(5) 0.66137(16) 0.0616(11) Uani 1 1 d . . . H12 H 0.4324 0.5826 0.6755 0.074 Uiso 1 1 calc R . . C13 C 0.4308(2) 0.2386(5) 0.5906(2) 0.0820(15) Uani 1 1 d . . . H13A H 0.4341 0.2534 0.5579 0.123 Uiso 1 1 calc R . . H13B H 0.3900 0.2152 0.5882 0.123 Uiso 1 1 calc R . . H13C H 0.4582 0.1754 0.6062 0.123 Uiso 1 1 calc R . . N14 N 0.70419(14) 0.4653(3) 0.69123(11) 0.0518(8) Uani 1 1 d . . . N15 N 0.68902(14) 0.3648(3) 0.66308(12) 0.0507(8) Uani 1 1 d . . . C16 C 0.73957(19) 0.3292(4) 0.65428(15) 0.0560(10) Uani 1 1 d . . . C17 C 0.78647(19) 0.4086(5) 0.67659(16) 0.0638(11) Uani 1 1 d . . . H17 H 0.8264 0.4043 0.6756 0.077 Uiso 1 1 calc R . . C18 C 0.76296(18) 0.4925(4) 0.69967(15) 0.0592(10) Uani 1 1 d . . . H18 H 0.7835 0.5572 0.7180 0.071 Uiso 1 1 calc R . . C19 C 0.7415(2) 0.2239(5) 0.6243(2) 0.0748(13) Uani 1 1 d . . . H19A H 0.7406 0.1528 0.6434 0.112 Uiso 1 1 calc R . . H19B H 0.7780 0.2250 0.6147 0.112 Uiso 1 1 calc R . . H19C H 0.7069 0.2242 0.5951 0.112 Uiso 1 1 calc R . . N20 N 0.58435(15) 0.1770(3) 0.59371(11) 0.0473(7) Uani 1 1 d . . . C21 C 0.58301(19) 0.1905(4) 0.54625(14) 0.0537(10) Uani 1 1 d . . . C22 C 0.5816(2) 0.0965(5) 0.51551(16) 0.0693(12) Uani 1 1 d . . . H22 H 0.5801 0.1075 0.4824 0.083 Uiso 1 1 calc R . . C23 C 0.5824(3) -0.0167(5) 0.53574(19) 0.0795(15) Uani 1 1 d . . . H23 H 0.5819 -0.0834 0.5157 0.095 Uiso 1 1 calc R . . C24 C 0.5841(2) -0.0338(5) 0.58432(18) 0.0693(12) Uani 1 1 d . . . H24 H 0.5846 -0.1101 0.5979 0.083 Uiso 1 1 calc R . . C25 C 0.58485(18) 0.0671(4) 0.61149(14) 0.0514(9) Uani 1 1 d . . . N26 N 0.58469(15) 0.0674(3) 0.66096(11) 0.0503(8) Uani 1 1 d . . . N27 N 0.58829(14) 0.1740(3) 0.68489(11) 0.0482(7) Uani 1 1 d . . . C28 C 0.58315(18) 0.1455(4) 0.72970(14) 0.0544(10) Uani 1 1 d . . . C29 C 0.5763(2) 0.0238(5) 0.73327(16) 0.0650(12) Uani 1 1 d . . . H29 H 0.5717 -0.0177 0.7607 0.078 Uiso 1 1 calc R . . C30 C 0.5774(2) -0.0240(4) 0.68967(16) 0.0629(11) Uani 1 1 d . . . H30 H 0.5738 -0.1050 0.6811 0.075 Uiso 1 1 calc R . . C31 C 0.5848(2) 0.2397(5) 0.76684(16) 0.0710(13) Uani 1 1 d . . . H31A H 0.6247 0.2744 0.7777 0.107 Uiso 1 1 calc R . . H31B H 0.5752 0.2052 0.7949 0.107 Uiso 1 1 calc R . . H31C H 0.5556 0.3008 0.7522 0.107 Uiso 1 1 calc R . . N32 N 0.58320(17) 0.3099(3) 0.53239(12) 0.0563(9) Uani 1 1 d . . . N33 N 0.58313(15) 0.3972(3) 0.56585(11) 0.0521(8) Uani 1 1 d . . . C34 C 0.5825(2) 0.4998(4) 0.54298(16) 0.0609(11) Uani 1 1 d . . . C35 C 0.5824(3) 0.4778(5) 0.49436(17) 0.0798(15) Uani 1 1 d . . . H35 H 0.5820 0.5353 0.4703 0.096 Uiso 1 1 calc R . . C36 C 0.5830(3) 0.3600(5) 0.48866(16) 0.0764(15) Uani 1 1 d . . . H36 H 0.5833 0.3192 0.4598 0.092 Uiso 1 1 calc R . . C37 C 0.5832(3) 0.6158(5) 0.5679(2) 0.0790(14) Uani 1 1 d . . . H37A H 0.5507 0.6183 0.5827 0.118 Uiso 1 1 calc R . . H37B H 0.5780 0.6794 0.5439 0.118 Uiso 1 1 calc R . . H37C H 0.6213 0.6257 0.5933 0.118 Uiso 1 1 calc R . . Cl38A Cl 0.75961(16) 0.3438(3) 0.82588(12) 0.0628(11) Uiso 0.50 1 d PD A 1 O39A O 0.7275(4) 0.2973(11) 0.7809(3) 0.065(3) Uiso 0.50 1 d PD A 1 O40A O 0.7928(4) 0.4535(8) 0.8127(3) 0.086(3) Uiso 0.50 1 d PD A 1 O41A O 0.7255(5) 0.4088(10) 0.8536(4) 0.112(3) Uiso 0.50 1 d PD A 1 O42A O 0.8025(4) 0.2729(9) 0.8556(4) 0.101(3) Uiso 0.50 1 d PD A 1 Cl38B Cl 0.76486(15) 0.3705(3) 0.82824(12) 0.0614(10) Uiso 0.50 1 d PD B 2 O39B O 0.7272(8) 0.3116(15) 0.7834(5) 0.125(8) Uiso 0.50 1 d PD B 2 O40B O 0.7802(5) 0.4797(9) 0.8187(4) 0.111(4) Uiso 0.50 1 d PD B 2 O41B O 0.7293(5) 0.3504(11) 0.8615(4) 0.122(4) Uiso 0.50 1 d PD B 2 O42B O 0.8173(4) 0.2933(8) 0.8465(3) 0.085(3) Uiso 0.50 1 d PD B 2 Cl43A Cl 0.9229(3) 0.3469(7) 0.62727(19) 0.0536(16) Uiso 0.35 1 d PD C 1 O44A O 0.8739(6) 0.2916(14) 0.5960(5) 0.061(4) Uiso 0.35 1 d PD C 1 O45A O 0.9367(7) 0.3032(14) 0.6790(4) 0.061(4) Uiso 0.35 1 d PD C 1 O46A O 0.9775(5) 0.3238(9) 0.6132(4) 0.059(3) Uiso 0.35 1 d PD C 1 O47A O 0.9184(7) 0.4721(10) 0.6312(6) 0.107(5) Uiso 0.35 1 d PD C 1 Cl43B Cl 0.9323(4) 0.3311(5) 0.62933(19) 0.0506(16) Uiso 0.35 1 d PD D 2 O44B O 0.8786(7) 0.2717(14) 0.6052(6) 0.094(7) Uiso 0.35 1 d PD D 2 O45B O 0.9433(5) 0.3334(10) 0.6817(3) 0.052(3) Uiso 0.35 1 d PD D 2 O46B O 0.9857(5) 0.2753(11) 0.6211(4) 0.052(3) Uiso 0.35 1 d PD D 2 O47B O 0.9334(6) 0.4540(9) 0.6136(4) 0.080(3) Uiso 0.35 1 d PD D 2 Cl43C Cl 0.9352(3) 0.3562(7) 0.63122(18) 0.0474(16) Uiso 0.30 1 d PD E 3 O44C O 0.8762(5) 0.3357(11) 0.5921(4) 0.064(3) Uiso 0.30 1 d PD E 3 O45C O 0.9210(6) 0.3090(13) 0.6734(4) 0.057(4) Uiso 0.30 1 d PD E 3 O46C O 0.9730(7) 0.2785(14) 0.6141(5) 0.055(4) Uiso 0.30 1 d PD E 3 O47C O 0.9468(7) 0.4749(10) 0.6353(6) 0.092(5) Uiso 0.30 1 d PD E 3 C48A C 0.7634(8) 0.619(2) 0.5692(6) 0.132(7) Uiso 0.50 1 d PD F 1 H48A H 0.7359 0.6061 0.5885 0.198 Uiso 0.50 1 calc PR F 1 H48B H 0.7810 0.6974 0.5760 0.198 Uiso 0.50 1 calc PR F 1 H48C H 0.7950 0.5594 0.5779 0.198 Uiso 0.50 1 calc PR F 1 C49A C 0.7303(6) 0.6087(15) 0.5160(5) 0.094(4) Uiso 0.50 1 d PD F 1 C50A C 0.7583(11) 0.546(2) 0.4816(8) 0.184(10) Uiso 0.50 1 d PD F 1 H50A H 0.7829 0.6019 0.4701 0.277 Uiso 0.50 1 calc PR F 1 H50B H 0.7269 0.5153 0.4537 0.277 Uiso 0.50 1 calc PR F 1 H50C H 0.7831 0.4813 0.4989 0.277 Uiso 0.50 1 calc PR F 1 O51A O 0.6883(5) 0.6803(11) 0.5009(4) 0.122(4) Uiso 0.50 1 d PD F 1 C48B C 0.7563(8) 0.5654(19) 0.5614(5) 0.127(6) Uiso 0.50 1 d PD G 2 H48D H 0.7264 0.6022 0.5742 0.190 Uiso 0.50 1 calc PR G 2 H48E H 0.7927 0.6128 0.5705 0.190 Uiso 0.50 1 calc PR G 2 H48F H 0.7652 0.4862 0.5751 0.190 Uiso 0.50 1 calc PR G 2 C49B C 0.7325(10) 0.5576(18) 0.5062(7) 0.141(7) Uiso 0.50 1 d PD G 2 C50B C 0.7497(10) 0.4570(19) 0.4799(7) 0.173(9) Uiso 0.50 1 d PD G 2 H50D H 0.7393 0.4751 0.4450 0.260 Uiso 0.50 1 calc PR G 2 H50E H 0.7283 0.3862 0.4847 0.260 Uiso 0.50 1 calc PR G 2 H50F H 0.7926 0.4435 0.4929 0.260 Uiso 0.50 1 calc PR G 2 O51B O 0.6921(5) 0.6293(12) 0.4852(4) 0.126(4) Uiso 0.50 1 d PD G 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 0.0490(4) 0.0463(4) 0.0389(3) -0.0017(2) 0.0138(2) -0.0005(2) N2 0.0470(16) 0.0517(19) 0.0407(14) 0.0013(13) 0.0157(12) -0.0005(14) C3 0.051(2) 0.057(2) 0.0421(18) 0.0041(16) 0.0184(15) 0.0053(17) C4 0.064(2) 0.059(3) 0.052(2) -0.0013(18) 0.0253(19) 0.008(2) C5 0.081(3) 0.054(3) 0.055(2) -0.0107(18) 0.025(2) -0.003(2) C6 0.060(2) 0.062(3) 0.050(2) -0.0070(18) 0.0104(18) -0.011(2) C7 0.055(2) 0.051(2) 0.0407(17) 0.0021(15) 0.0157(15) 0.0005(17) N8 0.0510(17) 0.0500(19) 0.0524(17) 0.0017(14) 0.0200(14) 0.0031(14) N9 0.0470(17) 0.0504(19) 0.0558(18) 0.0065(15) 0.0131(14) -0.0019(14) C10 0.051(2) 0.058(3) 0.059(2) 0.0174(19) 0.0084(18) -0.0051(18) C11 0.046(2) 0.076(3) 0.074(3) 0.018(2) 0.0204(19) 0.004(2) C12 0.053(2) 0.074(3) 0.063(2) 0.007(2) 0.0249(19) 0.011(2) C13 0.067(3) 0.069(3) 0.093(4) 0.005(3) -0.003(3) -0.010(3) N14 0.0439(16) 0.064(2) 0.0458(16) 0.0020(14) 0.0104(13) -0.0004(15) N15 0.0463(16) 0.058(2) 0.0482(17) 0.0005(14) 0.0142(13) 0.0029(15) C16 0.054(2) 0.064(3) 0.052(2) 0.0062(18) 0.0175(17) 0.0110(19) C17 0.046(2) 0.083(3) 0.062(2) 0.008(2) 0.0147(18) 0.005(2) C18 0.048(2) 0.068(3) 0.059(2) 0.004(2) 0.0113(17) -0.0049(19) C19 0.066(3) 0.081(4) 0.083(3) -0.012(3) 0.031(2) 0.009(3) N20 0.0538(17) 0.0500(19) 0.0360(14) -0.0021(12) 0.0101(13) -0.0038(14) C21 0.059(2) 0.063(3) 0.0379(18) -0.0007(16) 0.0124(16) -0.0042(19) C22 0.090(3) 0.072(3) 0.047(2) -0.011(2) 0.022(2) -0.007(3) C23 0.114(4) 0.062(3) 0.065(3) -0.022(2) 0.031(3) -0.009(3) C24 0.084(3) 0.058(3) 0.066(3) -0.008(2) 0.021(2) -0.008(2) C25 0.052(2) 0.052(2) 0.0463(19) -0.0036(16) 0.0096(16) -0.0040(17) N26 0.0552(18) 0.0493(19) 0.0453(16) 0.0044(14) 0.0131(13) -0.0010(14) N27 0.0496(17) 0.052(2) 0.0436(16) 0.0020(13) 0.0150(13) -0.0020(14) C28 0.0455(19) 0.075(3) 0.0409(18) 0.0058(17) 0.0101(15) 0.0016(18) C29 0.065(2) 0.078(3) 0.052(2) 0.019(2) 0.0166(19) -0.002(2) C30 0.075(3) 0.049(2) 0.062(2) 0.0109(19) 0.016(2) -0.005(2) C31 0.074(3) 0.095(4) 0.048(2) -0.005(2) 0.024(2) -0.004(3) N32 0.069(2) 0.060(2) 0.0405(16) 0.0014(14) 0.0174(15) -0.0034(16) N33 0.0635(19) 0.053(2) 0.0410(16) 0.0008(14) 0.0180(14) 0.0006(16) C34 0.067(2) 0.061(3) 0.053(2) 0.0106(19) 0.0153(19) -0.002(2) C35 0.119(4) 0.071(3) 0.049(2) 0.016(2) 0.024(3) -0.013(3) C36 0.108(4) 0.084(4) 0.038(2) 0.004(2) 0.024(2) -0.005(3) C37 0.108(4) 0.053(3) 0.074(3) 0.005(2) 0.024(3) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.112(3) . ? Fe1 N20 2.117(3) . ? Fe1 N27 2.161(3) . ? Fe1 N15 2.170(3) . ? Fe1 N9 2.182(3) . ? Fe1 N33 2.204(3) . ? N2 C7 1.337(5) . ? N2 C3 1.344(5) . ? C3 C4 1.378(6) . ? C3 N8 1.386(5) . ? C4 C5 1.384(7) . ? C5 C6 1.384(7) . ? C6 C7 1.380(6) . ? C7 N14 1.402(5) . ? N8 C12 1.358(5) . ? N8 N9 1.367(5) . ? N9 C10 1.337(5) . ? C10 C11 1.422(7) . ? C10 C13 1.486(7) . ? C11 C12 1.330(7) . ? N14 C18 1.354(5) . ? N14 N15 1.369(5) . ? N15 C16 1.337(5) . ? C16 C17 1.409(7) . ? C16 C19 1.467(7) . ? C17 C18 1.354(7) . ? N20 C25 1.335(5) . ? N20 C21 1.348(5) . ? C21 C22 1.366(6) . ? C21 N32 1.400(6) . ? C22 C23 1.395(7) . ? C23 C24 1.383(7) . ? C24 C25 1.369(6) . ? C25 N26 1.406(5) . ? N26 C30 1.355(5) . ? N26 N27 1.369(5) . ? N27 C28 1.352(5) . ? C28 C29 1.386(7) . ? C28 C31 1.487(6) . ? C29 C30 1.358(7) . ? N32 C36 1.363(5) . ? N32 N33 1.368(5) . ? N33 C34 1.322(5) . ? C34 C35 1.403(6) . ? C34 C37 1.483(7) . ? C35 C36 1.336(8) . ? Cl38A O42A 1.358(9) . ? Cl38A O39A 1.377(8) . ? Cl38A O41A 1.470(9) . ? Cl38A O40A 1.561(8) . ? Cl38B O40B 1.329(9) . ? Cl38B O41B 1.449(10) . ? Cl38B O42B 1.464(8) . ? Cl38B O39B 1.472(11) . ? Cl43A O44A 1.370(11) . ? Cl43A O47A 1.420(12) . ? Cl43A O46A 1.466(10) . ? Cl43A O45A 1.492(10) . ? Cl43B O44B 1.404(12) . ? Cl43B O45B 1.432(9) . ? Cl43B O47B 1.456(10) . ? Cl43B O46B 1.474(10) . ? Cl43C O47C 1.361(11) . ? Cl43C O46C 1.424(12) . ? Cl43C O45C 1.438(10) . ? Cl43C O44C 1.507(11) . ? C48A C49A 1.484(16) . ? C49A O51A 1.241(15) . ? C49A C50A 1.500(18) . ? C48B C49B 1.502(17) . ? C49B O51B 1.249(17) . ? C49B C50B 1.474(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N20 176.10(12) . . ? N2 Fe1 N27 110.10(12) . . ? N20 Fe1 N27 73.65(13) . . ? N2 Fe1 N15 74.24(12) . . ? N20 Fe1 N15 104.16(13) . . ? N27 Fe1 N15 102.24(13) . . ? N2 Fe1 N9 73.51(12) . . ? N20 Fe1 N9 107.86(13) . . ? N27 Fe1 N9 91.18(12) . . ? N15 Fe1 N9 147.65(14) . . ? N2 Fe1 N33 102.45(12) . . ? N20 Fe1 N33 73.94(12) . . ? N27 Fe1 N33 147.02(13) . . ? N15 Fe1 N33 91.39(13) . . ? N9 Fe1 N33 92.99(13) . . ? C7 N2 C3 119.2(3) . . ? C7 N2 Fe1 120.3(3) . . ? C3 N2 Fe1 120.6(3) . . ? N2 C3 C4 121.8(4) . . ? N2 C3 N8 113.1(3) . . ? C4 C3 N8 125.1(4) . . ? C3 C4 C5 118.0(4) . . ? C4 C5 C6 121.0(4) . . ? C7 C6 C5 116.9(4) . . ? N2 C7 C6 123.0(4) . . ? N2 C7 N14 112.7(3) . . ? C6 C7 N14 124.3(4) . . ? C12 N8 N9 110.1(3) . . ? C12 N8 C3 131.2(4) . . ? N9 N8 C3 118.7(3) . . ? C10 N9 N8 106.3(3) . . ? C10 N9 Fe1 139.6(3) . . ? N8 N9 Fe1 114.1(2) . . ? N9 C10 C11 108.7(4) . . ? N9 C10 C13 120.9(4) . . ? C11 C10 C13 130.4(4) . . ? C12 C11 C10 106.7(4) . . ? C11 C12 N8 108.2(4) . . ? C18 N14 N15 111.2(3) . . ? C18 N14 C7 129.7(4) . . ? N15 N14 C7 119.0(3) . . ? C16 N15 N14 105.5(3) . . ? C16 N15 Fe1 140.4(3) . . ? N14 N15 Fe1 113.5(2) . . ? N15 C16 C17 109.6(4) . . ? N15 C16 C19 122.1(4) . . ? C17 C16 C19 128.4(4) . . ? C18 C17 C16 106.8(4) . . ? N14 C18 C17 106.9(4) . . ? C25 N20 C21 118.6(3) . . ? C25 N20 Fe1 121.0(2) . . ? C21 N20 Fe1 120.3(3) . . ? N20 C21 C22 122.7(4) . . ? N20 C21 N32 112.9(3) . . ? C22 C21 N32 124.4(4) . . ? C21 C22 C23 116.7(4) . . ? C24 C23 C22 122.1(4) . . ? C25 C24 C23 116.0(5) . . ? N20 C25 C24 123.9(4) . . ? N20 C25 N26 111.9(3) . . ? C24 C25 N26 124.2(4) . . ? C30 N26 N27 111.5(3) . . ? C30 N26 C25 129.6(4) . . ? N27 N26 C25 118.7(3) . . ? C28 N27 N26 104.5(3) . . ? C28 N27 Fe1 140.9(3) . . ? N26 N27 Fe1 114.4(2) . . ? N27 C28 C29 110.4(4) . . ? N27 C28 C31 120.5(4) . . ? C29 C28 C31 129.1(4) . . ? C30 C29 C28 106.9(4) . . ? N26 C30 C29 106.7(4) . . ? C36 N32 N33 109.6(4) . . ? C36 N32 C21 130.8(4) . . ? N33 N32 C21 119.6(3) . . ? C34 N33 N32 106.7(3) . . ? C34 N33 Fe1 140.1(3) . . ? N32 N33 Fe1 112.8(2) . . ? N33 C34 C35 109.1(4) . . ? N33 C34 C37 122.5(4) . . ? C35 C34 C37 128.4(4) . . ? C36 C35 C34 107.3(4) . . ? C35 C36 N32 107.3(4) . . ? O42A Cl38A O39A 116.7(7) . . ? O42A Cl38A O41A 112.0(6) . . ? O39A Cl38A O41A 117.0(6) . . ? O42A Cl38A O40A 106.7(6) . . ? O39A Cl38A O40A 104.4(6) . . ? O41A Cl38A O40A 97.0(6) . . ? O40B Cl38B O41B 121.2(7) . . ? O40B Cl38B O42B 111.9(7) . . ? O41B Cl38B O42B 104.8(7) . . ? O40B Cl38B O39B 111.6(8) . . ? O41B Cl38B O39B 100.6(8) . . ? O42B Cl38B O39B 105.1(8) . . ? O44A Cl43A O47A 115.8(10) . . ? O44A Cl43A O46A 111.5(9) . . ? O47A Cl43A O46A 106.7(8) . . ? O44A Cl43A O45A 112.5(10) . . ? O47A Cl43A O45A 104.4(8) . . ? O46A Cl43A O45A 105.0(7) . . ? O44B Cl43B O45B 111.9(9) . . ? O44B Cl43B O47B 113.4(9) . . ? O45B Cl43B O47B 106.7(7) . . ? O44B Cl43B O46B 113.1(10) . . ? O45B Cl43B O46B 105.9(7) . . ? O47B Cl43B O46B 105.2(8) . . ? O47C Cl43C O46C 120.4(10) . . ? O47C Cl43C O45C 112.3(9) . . ? O46C Cl43C O45C 112.1(9) . . ? O47C Cl43C O44C 109.1(9) . . ? O46C Cl43C O44C 100.1(9) . . ? O45C Cl43C O44C 99.8(8) . . ? O51A C49A C48A 114.8(13) . . ? O51A C49A C50A 122.1(13) . . ? C48A C49A C50A 120.2(13) . . ? O51B C49B C50B 122.3(15) . . ? O51B C49B C48B 116.8(15) . . ? C50B C49B C48B 120.1(15) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.866 _refine_diff_density_min -1.459 _refine_diff_density_rms 0.231 #=END data_je34b200 _database_code_depnum_ccdc_archive 'CCDC 278902' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-(3-methylpyrazol-1-yl)pyridine]iron(II) diperchlorate acetone solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Fe N10, 2[Cl O4], C3 H6 O' _chemical_formula_sum 'C29 H32 Cl2 Fe N10 O9' _chemical_formula_weight 791.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.1702(4) _cell_length_b 11.1910(2) _cell_length_c 28.3275(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.0868(9) _cell_angle_gamma 90.00 _cell_volume 7021.0(2) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 27294 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 27.49 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour Red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 0.648 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.565 _exptl_absorpt_correction_T_max 0.875 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings The high value of Rint reflects the highly redundant dataset collected for this crystal. ; _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 'Nonius KappaCCD diffractometer' _diffrn_measurement_method 'Area detector scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27294 _diffrn_reflns_av_R_equivalents 0.0801 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7625 _reflns_number_gt 5668 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 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 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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. Both the ClO~4~^-^ anions are disordered: Cl38A-O42A (occupancy 0.50) and Cl38B-O42B (occupancy 0.50) and Cl43A-O47A (occupancy 0.35), Cl43B-O47B (occupancy 0.35) and Cl43C-O47C (occupancy 0.30). All disordered Cl-O distances were restrained to 1.44(2)\%A, and O...O distances within a given disorder orientation to 2.35(2)\%A. The acetone molecule is also disordered, over two different orientations: C48A-O51A (occupancy 0.50) and C48B-O51B (occupancy 0.50). Although the thermal ellipsoids on these two partial molecules are slightly high, we were unable to locate, or refine, a third disorder orientation at this temperature (c.f. the datasets at 100 K and 150 K, where a third partial molecule was clearly evident. The following restraints were applied to this molecule: C-C = 1.48(2)\%A, C=O = 1.25(2)\%A and 1,3-C...O = 2.38(2)\%A. All wholly occupied non-H atoms were refined anisotropically. All H atoms were placed in calculated positions and refined using a riding model, except for the solvent methyl groups whose torsions were not allowed to refine. ; _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^)+(0.1220P)^2^+7.6011P] 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 SHELXL _refine_ls_extinction_coef 0.0029(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7625 _refine_ls_number_parameters 475 _refine_ls_number_restraints 62 _refine_ls_R_factor_all 0.0898 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.2046 _refine_ls_wR_factor_gt 0.1840 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.067 _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 0.59285(2) 0.32527(4) 0.639891(16) 0.03775(19) Uani 1 1 d . . . N2 N 0.60373(12) 0.4801(2) 0.68265(10) 0.0418(6) Uani 1 1 d . . . C3 C 0.55545(15) 0.5376(3) 0.68864(12) 0.0438(7) Uani 1 1 d . . . C4 C 0.56090(18) 0.6390(3) 0.71731(14) 0.0529(9) Uani 1 1 d . . . H4 H 0.5262 0.6797 0.7205 0.063 Uiso 1 1 calc R . . C5 C 0.6181(2) 0.6792(3) 0.74115(15) 0.0570(10) Uani 1 1 d . . . H5 H 0.6230 0.7474 0.7619 0.068 Uiso 1 1 calc R . . C6 C 0.66920(17) 0.6216(3) 0.73538(13) 0.0509(8) Uani 1 1 d . . . H6 H 0.7089 0.6484 0.7519 0.061 Uiso 1 1 calc R . . C7 C 0.65876(15) 0.5238(3) 0.70437(12) 0.0448(8) Uani 1 1 d . . . N8 N 0.50127(13) 0.4826(3) 0.66356(11) 0.0467(7) Uani 1 1 d . . . N9 N 0.50290(12) 0.3800(3) 0.63783(11) 0.0480(7) Uani 1 1 d . . . C10 C 0.44557(17) 0.3465(4) 0.61868(16) 0.0574(10) Uani 1 1 d . . . C11 C 0.40756(18) 0.4296(4) 0.63225(16) 0.0641(11) Uani 1 1 d . . . H11 H 0.3647 0.4265 0.6234 0.077 Uiso 1 1 calc R . . C12 C 0.44292(16) 0.5138(4) 0.65988(15) 0.0581(10) Uani 1 1 d . . . H12 H 0.4301 0.5818 0.6742 0.070 Uiso 1 1 calc R . . C13 C 0.4303(2) 0.2364(4) 0.5885(2) 0.0785(14) Uani 1 1 d . . . H13A H 0.4591 0.2258 0.5695 0.118 Uiso 1 1 calc R . . H13B H 0.3894 0.2432 0.5659 0.118 Uiso 1 1 calc R . . H13C H 0.4325 0.1674 0.6103 0.118 Uiso 1 1 calc R . . N14 N 0.70415(12) 0.4616(3) 0.69131(10) 0.0453(6) Uani 1 1 d . . . N15 N 0.68824(14) 0.3607(3) 0.66253(11) 0.0478(7) Uani 1 1 d . . . C16 C 0.73918(18) 0.3255(3) 0.65382(14) 0.0522(9) Uani 1 1 d . . . C17 C 0.78634(18) 0.4035(4) 0.67601(15) 0.0605(10) Uani 1 1 d . . . H17 H 0.8269 0.3982 0.6750 0.073 Uiso 1 1 calc R . . C18 C 0.76287(16) 0.4886(4) 0.69929(14) 0.0542(9) Uani 1 1 d . . . H18 H 0.7839 0.5545 0.7177 0.065 Uiso 1 1 calc R . . C19 C 0.7415(2) 0.2197(4) 0.62340(17) 0.0677(11) Uani 1 1 d . . . H19A H 0.7395 0.1470 0.6422 0.102 Uiso 1 1 calc R . . H19B H 0.7793 0.2203 0.6145 0.102 Uiso 1 1 calc R . . H19C H 0.7072 0.2214 0.5933 0.102 Uiso 1 1 calc R . . N20 N 0.58414(13) 0.1766(2) 0.59393(10) 0.0398(6) Uani 1 1 d . . . C21 C 0.58356(17) 0.1894(3) 0.54698(12) 0.0456(8) Uani 1 1 d . . . C22 C 0.5824(2) 0.0938(4) 0.51589(14) 0.0591(10) Uani 1 1 d . . . H22 H 0.5811 0.1048 0.4823 0.071 Uiso 1 1 calc R . . C23 C 0.5834(2) -0.0191(4) 0.53631(16) 0.0682(12) Uani 1 1 d . . . H23 H 0.5836 -0.0873 0.5164 0.082 Uiso 1 1 calc R . . C24 C 0.58416(19) -0.0352(3) 0.58514(15) 0.0579(9) Uani 1 1 d . . . H24 H 0.5842 -0.1125 0.5990 0.069 Uiso 1 1 calc R . . C25 C 0.58476(16) 0.0665(3) 0.61239(13) 0.0449(7) Uani 1 1 d . . . N26 N 0.58463(13) 0.0676(2) 0.66181(10) 0.0445(6) Uani 1 1 d . . . N27 N 0.58788(13) 0.1750(2) 0.68520(10) 0.0434(6) Uani 1 1 d . . . C28 C 0.58306(16) 0.1478(4) 0.73021(13) 0.0511(9) Uani 1 1 d . . . C29 C 0.57658(18) 0.0247(4) 0.73454(14) 0.0608(10) Uani 1 1 d . . . H29 H 0.5722 -0.0170 0.7625 0.073 Uiso 1 1 calc R . . C30 C 0.57785(19) -0.0237(4) 0.69101(15) 0.0593(10) Uani 1 1 d . . . H30 H 0.5746 -0.1061 0.6826 0.071 Uiso 1 1 calc R . . C31 C 0.58457(19) 0.2435(4) 0.76720(14) 0.0648(11) Uani 1 1 d . . . H31A H 0.6265 0.2599 0.7861 0.097 Uiso 1 1 calc R . . H31B H 0.5621 0.2171 0.7897 0.097 Uiso 1 1 calc R . . H31C H 0.5661 0.3163 0.7501 0.097 Uiso 1 1 calc R . . N32 N 0.58335(14) 0.3095(3) 0.53302(10) 0.0470(7) Uani 1 1 d . . . N33 N 0.58300(13) 0.3964(2) 0.56668(10) 0.0426(6) Uani 1 1 d . . . C34 C 0.58276(16) 0.4999(3) 0.54377(13) 0.0499(8) Uani 1 1 d . . . C35 C 0.5830(2) 0.4792(4) 0.49518(14) 0.0645(11) Uani 1 1 d . . . H35 H 0.5830 0.5382 0.4711 0.077 Uiso 1 1 calc R . . C36 C 0.5831(2) 0.3591(4) 0.48890(14) 0.0629(11) Uani 1 1 d . . . H36 H 0.5831 0.3176 0.4596 0.076 Uiso 1 1 calc R . . C37 C 0.5824(2) 0.6160(3) 0.56860(16) 0.0646(11) Uani 1 1 d . . . H37A H 0.5458 0.6224 0.5790 0.097 Uiso 1 1 calc R . . H37B H 0.5832 0.6811 0.5457 0.097 Uiso 1 1 calc R . . H37C H 0.6180 0.6216 0.5976 0.097 Uiso 1 1 calc R . . Cl38A Cl 0.76031(11) 0.3424(2) 0.82495(9) 0.0488(7) Uiso 0.50 1 d PD A 1 O39A O 0.7268(5) 0.2958(12) 0.7806(3) 0.060(4) Uiso 0.50 1 d PD A 1 O40A O 0.7922(4) 0.4563(7) 0.8129(3) 0.069(2) Uiso 0.50 1 d PD A 1 O41A O 0.7284(3) 0.4033(7) 0.8565(3) 0.079(2) Uiso 0.50 1 d PD A 1 O42A O 0.8058(3) 0.2694(7) 0.8531(3) 0.076(2) Uiso 0.50 1 d PD A 1 Cl38B Cl 0.76513(11) 0.3697(2) 0.82757(9) 0.0488(7) Uiso 0.50 1 d PD B 2 O39B O 0.7279(7) 0.3062(15) 0.7818(5) 0.095(7) Uiso 0.50 1 d PD B 2 O40B O 0.7796(4) 0.4773(7) 0.8159(4) 0.087(3) Uiso 0.50 1 d PD B 2 O41B O 0.7270(4) 0.3471(8) 0.8595(3) 0.095(3) Uiso 0.50 1 d PD B 2 O42B O 0.8187(3) 0.2922(7) 0.8463(3) 0.076(2) Uiso 0.50 1 d PD B 2 Cl43A Cl 0.9236(2) 0.3427(6) 0.62606(17) 0.0428(13) Uiso 0.35 1 d PD C 1 O44A O 0.8730(5) 0.2967(12) 0.5940(4) 0.050(3) Uiso 0.35 1 d PD C 1 O45A O 0.9355(7) 0.3015(13) 0.6785(4) 0.053(4) Uiso 0.35 1 d PD C 1 O46A O 0.9795(4) 0.3203(8) 0.6137(3) 0.051(2) Uiso 0.35 1 d PD C 1 O47A O 0.9200(6) 0.4712(8) 0.6300(5) 0.085(3) Uiso 0.35 1 d PD C 1 Cl43B Cl 0.9336(3) 0.3324(5) 0.62975(19) 0.0427(13) Uiso 0.35 1 d PD D 2 O44B O 0.8778(5) 0.2740(10) 0.6030(4) 0.071(4) Uiso 0.35 1 d PD D 2 O45B O 0.9400(4) 0.3314(8) 0.6804(3) 0.038(2) Uiso 0.35 1 d PD D 2 O46B O 0.9867(4) 0.2735(9) 0.6217(3) 0.043(3) Uiso 0.35 1 d PD D 2 O47B O 0.9354(4) 0.4568(7) 0.6143(3) 0.062(2) Uiso 0.35 1 d PD D 2 Cl43C Cl 0.9346(3) 0.3580(5) 0.63166(18) 0.0422(13) Uiso 0.30 1 d PD E 3 O44C O 0.8764(4) 0.3405(9) 0.5916(4) 0.057(3) Uiso 0.30 1 d PD E 3 O45C O 0.9217(6) 0.3014(13) 0.6736(4) 0.053(4) Uiso 0.30 1 d PD E 3 O46C O 0.9731(5) 0.2778(11) 0.6130(4) 0.039(3) Uiso 0.30 1 d PD E 3 O47C O 0.9474(6) 0.4756(8) 0.6386(5) 0.078(3) Uiso 0.30 1 d PD E 3 C48A C 0.7613(6) 0.6166(13) 0.5711(4) 0.095(4) Uiso 0.50 1 d PD F 1 H48A H 0.7321 0.6033 0.5895 0.143 Uiso 0.50 1 calc PR F 1 H48B H 0.7806 0.6948 0.5799 0.143 Uiso 0.50 1 calc PR F 1 H48C H 0.7922 0.5539 0.5794 0.143 Uiso 0.50 1 calc PR F 1 C49A C 0.7299(4) 0.6133(10) 0.5175(4) 0.067(3) Uiso 0.50 1 d PD F 1 C50A C 0.7588(7) 0.5464(15) 0.4843(5) 0.127(5) Uiso 0.50 1 d PD F 1 H50A H 0.7841 0.6012 0.4721 0.191 Uiso 0.50 1 calc PR F 1 H50B H 0.7273 0.5131 0.4563 0.191 Uiso 0.50 1 calc PR F 1 H50C H 0.7837 0.4814 0.5028 0.191 Uiso 0.50 1 calc PR F 1 O51A O 0.6871(4) 0.6865(8) 0.5036(3) 0.096(3) Uiso 0.50 1 d PD F 1 C48B C 0.7564(7) 0.5697(14) 0.5639(4) 0.108(5) Uiso 0.50 1 d PD G 2 H48D H 0.7270 0.6068 0.5781 0.161 Uiso 0.50 1 calc PR G 2 H48E H 0.7943 0.6146 0.5740 0.161 Uiso 0.50 1 calc PR G 2 H48F H 0.7637 0.4871 0.5756 0.161 Uiso 0.50 1 calc PR G 2 C49B C 0.7321(7) 0.5704(14) 0.5087(5) 0.109(5) Uiso 0.50 1 d PD G 2 C50B C 0.7464(9) 0.4668(16) 0.4813(6) 0.167(8) Uiso 0.50 1 d PD G 2 H50D H 0.7357 0.4861 0.4460 0.250 Uiso 0.50 1 calc PR G 2 H50E H 0.7232 0.3970 0.4861 0.250 Uiso 0.50 1 calc PR G 2 H50F H 0.7896 0.4490 0.4936 0.250 Uiso 0.50 1 calc PR G 2 O51B O 0.6914(4) 0.6412(8) 0.4886(3) 0.090(2) Uiso 0.50 1 d PD G 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 0.0422(3) 0.0375(3) 0.0356(3) -0.00121(17) 0.0146(2) 0.00015(17) N2 0.0432(14) 0.0491(15) 0.0368(14) 0.0076(11) 0.0173(12) 0.0053(12) C3 0.0433(17) 0.0513(19) 0.0411(17) 0.0106(14) 0.0193(15) 0.0084(14) C4 0.065(2) 0.051(2) 0.052(2) 0.0042(16) 0.0316(19) 0.0105(17) C5 0.073(3) 0.053(2) 0.052(2) -0.0023(16) 0.030(2) 0.0015(18) C6 0.053(2) 0.056(2) 0.0428(19) -0.0029(15) 0.0143(16) -0.0036(16) C7 0.0474(18) 0.0496(18) 0.0422(18) 0.0078(14) 0.0206(15) 0.0047(14) N8 0.0451(15) 0.0501(16) 0.0496(16) 0.0076(13) 0.0214(13) 0.0070(12) N9 0.0380(14) 0.0510(16) 0.0525(17) 0.0152(13) 0.0093(13) -0.0002(12) C10 0.0454(19) 0.058(2) 0.061(2) 0.0242(18) 0.0033(18) -0.0081(16) C11 0.0403(19) 0.082(3) 0.071(3) 0.028(2) 0.0184(19) 0.0044(19) C12 0.0415(19) 0.076(3) 0.063(2) 0.015(2) 0.0249(18) 0.0088(18) C13 0.060(2) 0.060(3) 0.100(4) 0.015(2) 0.000(2) -0.009(2) N14 0.0402(14) 0.0560(17) 0.0402(15) 0.0042(12) 0.0128(12) 0.0056(12) N15 0.0511(17) 0.0521(16) 0.0447(16) 0.0074(13) 0.0209(14) 0.0099(13) C16 0.051(2) 0.063(2) 0.047(2) 0.0123(16) 0.0210(17) 0.0177(17) C17 0.046(2) 0.082(3) 0.055(2) 0.010(2) 0.0175(18) 0.0086(19) C18 0.0438(19) 0.069(2) 0.051(2) 0.0032(18) 0.0154(17) 0.0001(17) C19 0.063(2) 0.073(3) 0.077(3) -0.006(2) 0.035(2) 0.012(2) N20 0.0450(15) 0.0420(14) 0.0323(13) -0.0017(11) 0.0114(12) -0.0020(11) C21 0.0510(19) 0.051(2) 0.0351(17) -0.0025(14) 0.0132(15) -0.0045(15) C22 0.082(3) 0.058(2) 0.0403(19) -0.0096(16) 0.0225(19) -0.007(2) C23 0.095(3) 0.054(2) 0.058(2) -0.0169(19) 0.027(2) -0.009(2) C24 0.074(3) 0.044(2) 0.055(2) -0.0042(16) 0.018(2) -0.0031(18) C25 0.0483(18) 0.0441(17) 0.0427(18) 0.0010(14) 0.0138(15) -0.0047(14) N26 0.0503(16) 0.0434(15) 0.0399(15) 0.0053(12) 0.0132(13) 0.0003(12) N27 0.0441(15) 0.0522(16) 0.0345(14) 0.0036(11) 0.0122(12) 0.0006(12) C28 0.0380(17) 0.080(3) 0.0344(18) 0.0048(16) 0.0096(15) 0.0039(16) C29 0.063(2) 0.074(3) 0.046(2) 0.0220(19) 0.0172(18) 0.000(2) C30 0.067(2) 0.052(2) 0.060(2) 0.0160(18) 0.020(2) -0.0012(18) C31 0.061(2) 0.097(3) 0.039(2) -0.006(2) 0.0193(18) 0.000(2) N32 0.0580(18) 0.0516(17) 0.0309(14) 0.0023(12) 0.0125(13) -0.0030(13) N33 0.0507(16) 0.0407(14) 0.0392(15) 0.0008(11) 0.0176(13) -0.0006(12) C34 0.052(2) 0.053(2) 0.0428(18) 0.0087(15) 0.0108(16) -0.0015(16) C35 0.086(3) 0.064(2) 0.043(2) 0.0160(18) 0.019(2) -0.008(2) C36 0.086(3) 0.070(3) 0.0346(19) 0.0063(17) 0.021(2) -0.010(2) C37 0.083(3) 0.048(2) 0.064(3) 0.0078(18) 0.023(2) -0.002(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 N20 2.086(3) . ? Fe1 N2 2.087(3) . ? Fe1 N27 2.139(3) . ? Fe1 N15 2.150(3) . ? Fe1 N9 2.156(3) . ? Fe1 N33 2.170(3) . ? N2 C7 1.335(4) . ? N2 C3 1.344(4) . ? C3 C4 1.380(5) . ? C3 N8 1.391(4) . ? C4 C5 1.374(6) . ? C5 C6 1.400(5) . ? C6 C7 1.380(5) . ? C7 N14 1.399(4) . ? N8 N9 1.367(4) . ? N8 C12 1.370(4) . ? N9 C10 1.332(5) . ? C10 C11 1.410(6) . ? C10 C13 1.482(6) . ? C11 C12 1.339(6) . ? N14 C18 1.346(5) . ? N14 N15 1.378(4) . ? N15 C16 1.334(4) . ? C16 C17 1.396(6) . ? C16 C19 1.474(6) . ? C17 C18 1.360(5) . ? N20 C21 1.334(4) . ? N20 C25 1.337(4) . ? C21 C22 1.381(5) . ? C21 N32 1.401(4) . ? C22 C23 1.388(6) . ? C23 C24 1.390(6) . ? C24 C25 1.373(5) . ? C25 N26 1.401(4) . ? N26 C30 1.353(4) . ? N26 N27 1.363(4) . ? N27 C28 1.347(4) . ? C28 C29 1.396(6) . ? C28 C31 1.491(6) . ? C29 C30 1.355(6) . ? N32 N33 1.363(4) . ? N32 C36 1.366(4) . ? N33 C34 1.327(4) . ? C34 C35 1.397(5) . ? C34 C37 1.479(6) . ? C35 C36 1.356(6) . ? Cl38A O39A 1.372(8) . ? Cl38A O42A 1.384(7) . ? Cl38A O41A 1.484(7) . ? Cl38A O40A 1.560(7) . ? Cl38B O40B 1.319(8) . ? Cl38B O41B 1.459(8) . ? Cl38B O42B 1.479(7) . ? Cl38B O39B 1.508(10) . ? Cl43A O44A 1.356(10) . ? Cl43A O47A 1.446(11) . ? Cl43A O46A 1.459(8) . ? Cl43A O45A 1.501(10) . ? Cl43B O45B 1.400(8) . ? Cl43B O44B 1.449(11) . ? Cl43B O47B 1.464(8) . ? Cl43B O46B 1.471(8) . ? Cl43C O47C 1.351(10) . ? Cl43C O45C 1.452(10) . ? Cl43C O46C 1.470(10) . ? Cl43C O44C 1.497(10) . ? C48A C49A 1.478(13) . ? C49A O51A 1.257(12) . ? C49A C50A 1.506(14) . ? C48B C49B 1.497(14) . ? C49B O51B 1.236(14) . ? C49B C50B 1.487(16) . ? 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 N20 Fe1 N2 176.29(10) . . ? N20 Fe1 N27 74.63(11) . . ? N2 Fe1 N27 108.86(11) . . ? N20 Fe1 N15 103.64(11) . . ? N2 Fe1 N15 74.65(11) . . ? N27 Fe1 N15 101.42(11) . . ? N20 Fe1 N9 107.10(12) . . ? N2 Fe1 N9 74.40(11) . . ? N27 Fe1 N9 91.00(11) . . ? N15 Fe1 N9 148.93(12) . . ? N20 Fe1 N33 74.47(10) . . ? N2 Fe1 N33 102.19(10) . . ? N27 Fe1 N33 148.51(11) . . ? N15 Fe1 N33 91.58(11) . . ? N9 Fe1 N33 92.33(11) . . ? C7 N2 C3 119.0(3) . . ? C7 N2 Fe1 120.5(2) . . ? C3 N2 Fe1 120.5(2) . . ? N2 C3 C4 122.2(3) . . ? N2 C3 N8 112.6(3) . . ? C4 C3 N8 125.3(3) . . ? C5 C4 C3 117.9(3) . . ? C4 C5 C6 121.2(4) . . ? C7 C6 C5 116.3(3) . . ? N2 C7 C6 123.3(3) . . ? N2 C7 N14 112.7(3) . . ? C6 C7 N14 123.9(3) . . ? N9 N8 C12 110.8(3) . . ? N9 N8 C3 118.8(3) . . ? C12 N8 C3 130.4(3) . . ? C10 N9 N8 105.8(3) . . ? C10 N9 Fe1 140.5(3) . . ? N8 N9 Fe1 113.7(2) . . ? N9 C10 C11 109.4(4) . . ? N9 C10 C13 120.6(4) . . ? C11 C10 C13 130.1(4) . . ? C12 C11 C10 107.4(3) . . ? C11 C12 N8 106.6(4) . . ? C18 N14 N15 111.4(3) . . ? C18 N14 C7 130.2(3) . . ? N15 N14 C7 118.2(3) . . ? C16 N15 N14 104.7(3) . . ? C16 N15 Fe1 141.1(3) . . ? N14 N15 Fe1 113.6(2) . . ? N15 C16 C17 110.5(3) . . ? N15 C16 C19 122.1(4) . . ? C17 C16 C19 127.4(4) . . ? C18 C17 C16 106.6(3) . . ? N14 C18 C17 106.8(4) . . ? C21 N20 C25 119.0(3) . . ? C21 N20 Fe1 120.5(2) . . ? C25 N20 Fe1 120.2(2) . . ? N20 C21 C22 123.1(3) . . ? N20 C21 N32 112.5(3) . . ? C22 C21 N32 124.4(3) . . ? C21 C22 C23 116.4(3) . . ? C22 C23 C24 121.7(4) . . ? C25 C24 C23 116.6(4) . . ? N20 C25 C24 123.1(3) . . ? N20 C25 N26 112.3(3) . . ? C24 C25 N26 124.5(3) . . ? C30 N26 N27 111.6(3) . . ? C30 N26 C25 129.7(3) . . ? N27 N26 C25 118.5(3) . . ? C28 N27 N26 104.7(3) . . ? C28 N27 Fe1 141.2(3) . . ? N26 N27 Fe1 113.97(19) . . ? N27 C28 C29 110.3(3) . . ? N27 C28 C31 120.8(4) . . ? C29 C28 C31 128.9(3) . . ? C30 C29 C28 106.4(3) . . ? N26 C30 C29 107.0(4) . . ? N33 N32 C36 110.6(3) . . ? N33 N32 C21 119.1(3) . . ? C36 N32 C21 130.3(3) . . ? C34 N33 N32 106.3(3) . . ? C34 N33 Fe1 140.5(2) . . ? N32 N33 Fe1 112.7(2) . . ? N33 C34 C35 109.6(3) . . ? N33 C34 C37 122.3(3) . . ? C35 C34 C37 128.1(3) . . ? C36 C35 C34 107.1(3) . . ? C35 C36 N32 106.4(4) . . ? O39A Cl38A O42A 115.7(6) . . ? O39A Cl38A O41A 118.6(6) . . ? O42A Cl38A O41A 110.7(5) . . ? O39A Cl38A O40A 106.7(6) . . ? O42A Cl38A O40A 106.2(5) . . ? O41A Cl38A O40A 96.2(5) . . ? O40B Cl38B O41B 123.9(6) . . ? O40B Cl38B O42B 112.1(6) . . ? O41B Cl38B O42B 105.9(5) . . ? O40B Cl38B O39B 109.8(8) . . ? O41B Cl38B O39B 98.8(8) . . ? O42B Cl38B O39B 103.9(7) . . ? O44A Cl43A O47A 111.8(8) . . ? O44A Cl43A O46A 115.3(7) . . ? O47A Cl43A O46A 105.4(7) . . ? O44A Cl43A O45A 114.7(8) . . ? O47A Cl43A O45A 103.2(8) . . ? O46A Cl43A O45A 105.4(7) . . ? O45B Cl43B O44B 110.0(7) . . ? O45B Cl43B O47B 108.1(6) . . ? O44B Cl43B O47B 111.8(7) . . ? O45B Cl43B O46B 108.3(6) . . ? O44B Cl43B O46B 112.0(8) . . ? O47B Cl43B O46B 106.4(6) . . ? O47C Cl43C O45C 113.3(8) . . ? O47C Cl43C O46C 121.1(8) . . ? O45C Cl43C O46C 108.7(8) . . ? O47C Cl43C O44C 110.3(8) . . ? O45C Cl43C O44C 101.9(7) . . ? O46C Cl43C O44C 98.9(7) . . ? O51A C49A C48A 114.4(10) . . ? O51A C49A C50A 125.5(10) . . ? C48A C49A C50A 118.6(10) . . ? O51B C49B C50B 121.0(13) . . ? O51B C49B C48B 119.2(13) . . ? C50B C49B C48B 117.9(12) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.723 _refine_diff_density_min -0.880 _refine_diff_density_rms 0.134 #=END data_je34b _database_code_depnum_ccdc_archive 'CCDC 278903' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-(3-methylpyrazol-1-yl)pyridine]iron(II) diperchlorate acetone solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Fe N10, 2[Cl O4], C3 H6 O' _chemical_formula_sum 'C29 H32 Cl2 Fe N10 O9' _chemical_formula_weight 791.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.8777(2) _cell_length_b 11.0240(1) _cell_length_c 28.3914(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.3318(7) _cell_angle_gamma 90.00 _cell_volume 6871.48(11) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 48139 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 27.55 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour 'Dark brown' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 0.662 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.609 _exptl_absorpt_correction_T_max 0.879 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_ambient_temperature 150(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 diffractometer' _diffrn_measurement_method 'Area detector scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48139 _diffrn_reflns_av_R_equivalents 0.0904 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.55 _reflns_number_total 7909 _reflns_number_gt 6294 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 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 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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. Both the ClO~4~^-^ anions are disordered: Cl38A-O42A (occupancy 0.50) and Cl38B-O42B (occupancy 0.50) and Cl43A-O47A (occupancy 0.35), Cl43B-O47B (occupancy 0.35) and Cl43C-O47C (occupancy 0.30). All disordered Cl-O distances were restrained to 1.44(2)\%A, and O...O distances within a given disorder orientation to 2.35(2)\%A. The acetone molecule is also disordered, over three different orientations: C48A-O51A (occupancy 0.40), C48B-O51B (occupancy 0.40) and C48C-O51C (occupancy 0.20). The following restraints were applied to this molecule: C-C = 1.49(2)\%A, C=O = 1.23(2)\%A and 1,3-C...O = 2.39(2)\%A. All wholly occupied non-H atoms were refined anisotropically. All H atoms were placed in calculated positions and refined using a riding model, except for the solvent methyl groups whose torsions were not allowed to refine. ; _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^)+(0.1040P)^2^+14.0968P] 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 SHELXL _refine_ls_extinction_coef 0.0048(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7909 _refine_ls_number_parameters 491 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1963 _refine_ls_wR_factor_gt 0.1745 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.131 _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 0.59090(2) 0.31997(4) 0.637250(16) 0.03197(17) Uani 1 1 d . . . N2 N 0.59832(12) 0.4637(3) 0.67749(10) 0.0376(6) Uani 1 1 d . . . C3 C 0.54855(15) 0.5195(3) 0.68248(12) 0.0411(8) Uani 1 1 d . . . C4 C 0.55160(18) 0.6201(4) 0.71155(14) 0.0493(9) Uani 1 1 d . . . H4 H 0.5158 0.6601 0.7140 0.059 Uiso 1 1 calc R . . C5 C 0.6088(2) 0.6608(4) 0.73711(14) 0.0516(9) Uani 1 1 d . . . H5 H 0.6122 0.7282 0.7586 0.062 Uiso 1 1 calc R . . C6 C 0.66156(18) 0.6055(3) 0.73229(13) 0.0454(8) Uani 1 1 d . . . H6 H 0.7010 0.6338 0.7495 0.054 Uiso 1 1 calc R . . C7 C 0.65320(15) 0.5070(3) 0.70089(12) 0.0393(7) Uani 1 1 d . . . N8 N 0.49541(13) 0.4605(3) 0.65520(11) 0.0472(7) Uani 1 1 d . . . N9 N 0.50246(13) 0.3580(3) 0.62939(11) 0.0430(7) Uani 1 1 d . . . C10 C 0.44626(17) 0.3185(4) 0.60741(15) 0.0530(10) Uani 1 1 d . . . C11 C 0.40343(18) 0.3962(5) 0.61877(16) 0.0648(13) Uani 1 1 d . . . H11 H 0.3604 0.3888 0.6075 0.078 Uiso 1 1 calc R . . C12 C 0.43500(18) 0.4836(5) 0.64881(15) 0.0596(12) Uani 1 1 d . . . H12 H 0.4183 0.5486 0.6628 0.072 Uiso 1 1 calc R . . C13 C 0.4357(2) 0.2088(4) 0.57525(19) 0.0715(14) Uani 1 1 d . . . H13A H 0.4535 0.2217 0.5480 0.107 Uiso 1 1 calc R . . H13B H 0.3918 0.1945 0.5622 0.107 Uiso 1 1 calc R . . H13C H 0.4549 0.1382 0.5944 0.107 Uiso 1 1 calc R . . N14 N 0.69934(12) 0.4436(3) 0.68845(10) 0.0397(6) Uani 1 1 d . . . N15 N 0.68246(13) 0.3426(3) 0.65862(10) 0.0393(6) Uani 1 1 d . . . C16 C 0.73436(17) 0.3029(4) 0.65089(14) 0.0457(8) Uani 1 1 d . . . C17 C 0.78307(17) 0.3783(4) 0.67516(14) 0.0514(9) Uani 1 1 d . . . H17 H 0.8244 0.3696 0.6752 0.062 Uiso 1 1 calc R . . C18 C 0.75994(16) 0.4665(4) 0.69866(13) 0.0470(8) Uani 1 1 d . . . H18 H 0.7818 0.5307 0.7182 0.056 Uiso 1 1 calc R . . C19 C 0.7367(2) 0.1960(4) 0.61942(17) 0.0577(10) Uani 1 1 d . . . H19A H 0.7218 0.1241 0.6327 0.087 Uiso 1 1 calc R . . H19B H 0.7789 0.1823 0.6189 0.087 Uiso 1 1 calc R . . H19C H 0.7112 0.2112 0.5860 0.087 Uiso 1 1 calc R . . N20 N 0.58627(12) 0.1760(2) 0.59679(10) 0.0348(6) Uani 1 1 d . . . C21 C 0.58486(16) 0.1863(3) 0.54952(12) 0.0392(7) Uani 1 1 d . . . C22 C 0.5852(2) 0.0875(4) 0.52004(14) 0.0504(9) Uani 1 1 d . . . H22 H 0.5845 0.0964 0.4866 0.060 Uiso 1 1 calc R . . C23 C 0.5868(2) -0.0261(4) 0.54164(15) 0.0562(10) Uani 1 1 d . . . H23 H 0.5869 -0.0967 0.5225 0.067 Uiso 1 1 calc R . . C24 C 0.58805(19) -0.0389(4) 0.59074(15) 0.0501(9) Uani 1 1 d . . . H24 H 0.5894 -0.1165 0.6056 0.060 Uiso 1 1 calc R . . C25 C 0.58724(16) 0.0661(3) 0.61671(12) 0.0401(7) Uani 1 1 d . . . N26 N 0.58739(14) 0.0729(3) 0.66552(10) 0.0415(6) Uani 1 1 d . . . N27 N 0.58905(13) 0.1869(3) 0.68620(10) 0.0381(6) Uani 1 1 d . . . C28 C 0.58464(16) 0.1686(4) 0.73173(13) 0.0463(9) Uani 1 1 d . . . C29 C 0.58056(18) 0.0427(4) 0.73971(14) 0.0562(10) Uani 1 1 d . . . H29 H 0.5773 0.0051 0.7690 0.067 Uiso 1 1 calc R . . C30 C 0.58224(19) -0.0145(4) 0.69762(15) 0.0550(10) Uani 1 1 d . . . H30 H 0.5802 -0.0995 0.6919 0.066 Uiso 1 1 calc R . . C31 C 0.58418(18) 0.2687(4) 0.76647(14) 0.0554(10) Uani 1 1 d . . . H31A H 0.6261 0.2939 0.7826 0.083 Uiso 1 1 calc R . . H31B H 0.5648 0.2409 0.7912 0.083 Uiso 1 1 calc R . . H31C H 0.5613 0.3376 0.7485 0.083 Uiso 1 1 calc R . . N32 N 0.58450(14) 0.3081(3) 0.53568(10) 0.0379(6) Uani 1 1 d . . . N33 N 0.58563(12) 0.3948(2) 0.57060(9) 0.0344(6) Uani 1 1 d . . . C34 C 0.58393(15) 0.5008(3) 0.54805(12) 0.0393(7) Uani 1 1 d . . . C35 C 0.58180(18) 0.4817(3) 0.49847(13) 0.0460(8) Uani 1 1 d . . . H35 H 0.5805 0.5426 0.4745 0.055 Uiso 1 1 calc R . . C36 C 0.58197(18) 0.3604(4) 0.49152(12) 0.0463(8) Uani 1 1 d . . . H36 H 0.5806 0.3195 0.4618 0.056 Uiso 1 1 calc R . . C37 C 0.5840(2) 0.6195(3) 0.57374(14) 0.0494(9) Uani 1 1 d . . . H37A H 0.5448 0.6307 0.5808 0.074 Uiso 1 1 calc R . . H37B H 0.5904 0.6857 0.5527 0.074 Uiso 1 1 calc R . . H37C H 0.6168 0.6198 0.6046 0.074 Uiso 1 1 calc R . . Cl38A Cl 0.75972(10) 0.3321(2) 0.82194(8) 0.0379(6) Uiso 0.50 1 d PD A 1 O39A O 0.7276(4) 0.2719(8) 0.7791(3) 0.051(3) Uiso 0.50 1 d PD A 1 O40A O 0.7903(4) 0.4456(7) 0.8103(3) 0.056(2) Uiso 0.50 1 d PD A 1 O41A O 0.7190(3) 0.3889(7) 0.8492(3) 0.0595(18) Uiso 0.50 1 d PD A 1 O42A O 0.8053(3) 0.2628(6) 0.8525(3) 0.061(2) Uiso 0.50 1 d PD A 1 Cl38B Cl 0.76249(11) 0.3591(2) 0.82459(9) 0.0424(7) Uiso 0.50 1 d PD B 2 O39B O 0.7274(4) 0.2953(8) 0.7788(3) 0.056(3) Uiso 0.50 1 d PD B 2 O40B O 0.7794(4) 0.4690(7) 0.8108(3) 0.061(2) Uiso 0.50 1 d PD B 2 O41B O 0.7275(4) 0.3481(7) 0.8578(3) 0.070(2) Uiso 0.50 1 d PD B 2 O42B O 0.8177(3) 0.2809(7) 0.8440(3) 0.068(2) Uiso 0.50 1 d PD B 2 Cl43A Cl 0.9233(2) 0.3476(5) 0.62565(15) 0.0361(11) Uiso 0.35 1 d PD C 1 O44A O 0.8733(4) 0.3223(11) 0.5873(3) 0.045(2) Uiso 0.35 1 d PD C 1 O45A O 0.9156(5) 0.2639(10) 0.6641(4) 0.060(4) Uiso 0.35 1 d PD C 1 O46A O 0.9789(4) 0.3215(8) 0.6128(3) 0.044(2) Uiso 0.35 1 d PD C 1 O47A O 0.9291(6) 0.4691(8) 0.6436(5) 0.075(3) Uiso 0.35 1 d PD C 1 Cl43B Cl 0.9290(2) 0.3239(3) 0.62806(14) 0.0348(10) Uiso 0.35 1 d PD D 2 O44B O 0.8750(4) 0.2787(9) 0.5969(3) 0.062(3) Uiso 0.35 1 d PD D 2 O45B O 0.9350(4) 0.3150(8) 0.6787(3) 0.041(2) Uiso 0.35 1 d PD D 2 O46B O 0.9884(4) 0.2831(10) 0.6217(3) 0.041(3) Uiso 0.35 1 d PD D 2 O47B O 0.9299(6) 0.4602(9) 0.6202(5) 0.091(4) Uiso 0.35 1 d PD D 2 Cl43C Cl 0.93662(19) 0.3522(5) 0.63192(13) 0.0292(9) Uiso 0.30 1 d PD E 3 O44C O 0.8811(5) 0.3585(11) 0.5889(4) 0.055(3) Uiso 0.30 1 d PD E 3 O45C O 0.9237(6) 0.2847(12) 0.6726(4) 0.036(3) Uiso 0.30 1 d PD E 3 O46C O 0.9749(5) 0.2714(9) 0.6123(4) 0.032(2) Uiso 0.30 1 d PD E 3 O47C O 0.9530(6) 0.4670(8) 0.6454(4) 0.062(3) Uiso 0.30 1 d PD E 3 C48A C 0.7593(7) 0.6123(15) 0.5715(4) 0.059(3) Uiso 0.40 1 d PD F 1 H48A H 0.7527 0.6949 0.5817 0.089 Uiso 0.40 1 calc PR F 1 H48B H 0.8031 0.5966 0.5788 0.089 Uiso 0.40 1 calc PR F 1 H48C H 0.7411 0.5541 0.5893 0.089 Uiso 0.40 1 calc PR F 1 C49A C 0.7298(13) 0.599(3) 0.5167(6) 0.056(8) Uiso 0.40 1 d PD F 1 C50A C 0.7661(8) 0.5383(16) 0.4871(6) 0.079(5) Uiso 0.40 1 d PD F 1 H50A H 0.7406 0.5275 0.4533 0.119 Uiso 0.40 1 calc PR F 1 H50B H 0.7801 0.4590 0.5015 0.119 Uiso 0.40 1 calc PR F 1 H50C H 0.8014 0.5889 0.4871 0.119 Uiso 0.40 1 calc PR F 1 O51A O 0.6876(6) 0.6673(13) 0.4971(5) 0.047(3) Uiso 0.40 1 d PD F 1 C48B C 0.7479(7) 0.5724(16) 0.5700(4) 0.057(3) Uiso 0.40 1 d PD G 2 H48D H 0.7278 0.6210 0.5898 0.085 Uiso 0.40 1 calc PR G 2 H48E H 0.7922 0.5817 0.5827 0.085 Uiso 0.40 1 calc PR G 2 H48F H 0.7370 0.4868 0.5716 0.085 Uiso 0.40 1 calc PR G 2 C49B C 0.7277(9) 0.6146(19) 0.5177(5) 0.044(6) Uiso 0.40 1 d PD G 2 C50B C 0.7472(8) 0.5298(15) 0.4823(5) 0.066(4) Uiso 0.40 1 d PD G 2 H50D H 0.7110 0.5009 0.4573 0.099 Uiso 0.40 1 calc PR G 2 H50E H 0.7693 0.4604 0.5005 0.099 Uiso 0.40 1 calc PR G 2 H50F H 0.7737 0.5738 0.4664 0.099 Uiso 0.40 1 calc PR G 2 O51B O 0.6871(5) 0.6918(10) 0.5052(4) 0.060(4) Uiso 0.40 1 d PD G 2 C48C C 0.765(2) 0.575(4) 0.5653(9) 0.093(14) Uiso 0.20 1 d PD H 3 H48G H 0.7491 0.6423 0.5807 0.139 Uiso 0.20 1 calc PR H 3 H48H H 0.8084 0.5856 0.5698 0.139 Uiso 0.20 1 calc PR H 3 H48I H 0.7577 0.4982 0.5804 0.139 Uiso 0.20 1 calc PR H 3 C49C C 0.732(2) 0.572(3) 0.5112(10) 0.080(13) Uiso 0.20 1 d PD H 3 C50C C 0.7429(14) 0.465(2) 0.4825(10) 0.081(8) Uiso 0.20 1 d PD H 3 H50G H 0.7038 0.4311 0.4636 0.121 Uiso 0.20 1 calc PR H 3 H50H H 0.7661 0.4037 0.5050 0.121 Uiso 0.20 1 calc PR H 3 H50I H 0.7660 0.4912 0.4600 0.121 Uiso 0.20 1 calc PR H 3 O51C O 0.6956(14) 0.652(3) 0.4912(10) 0.093(13) Uiso 0.20 1 d PD H 3 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 0.0318(3) 0.0347(3) 0.0307(3) -0.00018(17) 0.01091(18) 0.00102(17) N2 0.0367(14) 0.0454(15) 0.0328(13) 0.0101(11) 0.0136(11) 0.0059(11) C3 0.0373(17) 0.055(2) 0.0345(16) 0.0120(14) 0.0159(13) 0.0102(14) C4 0.055(2) 0.058(2) 0.0427(19) 0.0091(17) 0.0254(17) 0.0172(18) C5 0.069(3) 0.052(2) 0.0397(19) -0.0003(16) 0.0255(18) 0.0084(18) C6 0.052(2) 0.051(2) 0.0354(16) 0.0023(15) 0.0148(15) 0.0012(16) C7 0.0397(17) 0.0487(18) 0.0331(15) 0.0071(14) 0.0163(13) 0.0051(14) N8 0.0366(15) 0.064(2) 0.0447(16) 0.0173(14) 0.0177(13) 0.0092(14) N9 0.0335(14) 0.0530(17) 0.0407(15) 0.0130(13) 0.0074(12) -0.0004(12) C10 0.0350(18) 0.072(3) 0.047(2) 0.0273(19) 0.0026(15) -0.0063(17) C11 0.0343(19) 0.106(4) 0.052(2) 0.032(2) 0.0099(17) -0.002(2) C12 0.041(2) 0.093(3) 0.052(2) 0.029(2) 0.0241(18) 0.021(2) C13 0.052(3) 0.067(3) 0.079(3) 0.014(2) -0.008(2) -0.016(2) N14 0.0339(14) 0.0524(17) 0.0345(13) 0.0036(12) 0.0122(11) 0.0030(12) N15 0.0389(15) 0.0469(16) 0.0356(14) 0.0054(12) 0.0162(12) 0.0079(12) C16 0.0416(18) 0.056(2) 0.0433(18) 0.0135(16) 0.0188(15) 0.0141(16) C17 0.0375(18) 0.075(3) 0.0433(19) 0.0099(18) 0.0137(15) 0.0093(18) C18 0.0362(17) 0.067(2) 0.0377(17) 0.0050(16) 0.0110(14) 0.0022(16) C19 0.054(2) 0.060(2) 0.069(3) 0.000(2) 0.032(2) 0.0144(19) N20 0.0366(14) 0.0378(14) 0.0310(13) -0.0017(10) 0.0112(11) 0.0010(11) C21 0.0403(17) 0.0463(18) 0.0316(15) -0.0030(13) 0.0108(13) -0.0002(14) C22 0.065(2) 0.049(2) 0.0385(18) -0.0103(15) 0.0182(17) -0.0036(18) C23 0.076(3) 0.043(2) 0.051(2) -0.0146(17) 0.021(2) -0.0059(18) C24 0.059(2) 0.0406(19) 0.053(2) -0.0026(16) 0.0196(18) -0.0020(16) C25 0.0391(17) 0.0420(17) 0.0387(17) -0.0013(14) 0.0104(14) -0.0007(13) N26 0.0474(16) 0.0428(15) 0.0357(14) 0.0052(12) 0.0141(12) 0.0017(12) N27 0.0330(13) 0.0520(16) 0.0290(13) -0.0010(11) 0.0083(11) 0.0032(11) C28 0.0323(16) 0.074(3) 0.0331(16) 0.0075(16) 0.0093(13) 0.0100(16) C29 0.049(2) 0.081(3) 0.0413(19) 0.0182(19) 0.0172(16) 0.008(2) C30 0.056(2) 0.057(2) 0.055(2) 0.0190(18) 0.0212(19) 0.0051(18) C31 0.045(2) 0.088(3) 0.0357(18) -0.0086(19) 0.0148(16) -0.001(2) N32 0.0460(16) 0.0432(15) 0.0266(12) -0.0009(11) 0.0138(11) 0.0001(12) N33 0.0347(13) 0.0386(14) 0.0310(13) -0.0001(11) 0.0112(10) 0.0001(11) C34 0.0374(16) 0.0442(18) 0.0365(16) 0.0054(14) 0.0108(13) -0.0013(13) C35 0.056(2) 0.051(2) 0.0327(16) 0.0067(15) 0.0156(15) -0.0050(16) C36 0.056(2) 0.057(2) 0.0270(15) 0.0034(15) 0.0140(15) -0.0032(17) C37 0.061(2) 0.0391(18) 0.048(2) 0.0038(15) 0.0165(18) 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 N2 1.933(3) . ? Fe1 N20 1.945(3) . ? Fe1 N9 2.016(3) . ? Fe1 N15 2.026(3) . ? Fe1 N27 2.029(3) . ? Fe1 N33 2.036(3) . ? N2 C7 1.333(4) . ? N2 C3 1.337(4) . ? C3 C4 1.372(5) . ? C3 N8 1.404(5) . ? C4 C5 1.381(6) . ? C5 C6 1.393(5) . ? C6 C7 1.384(5) . ? C7 N14 1.392(4) . ? N8 C12 1.366(5) . ? N8 N9 1.381(5) . ? N9 C10 1.335(5) . ? C10 C11 1.406(7) . ? C10 C13 1.493(7) . ? C11 C12 1.353(7) . ? N14 C18 1.358(4) . ? N14 N15 1.386(4) . ? N15 C16 1.340(4) . ? C16 C17 1.406(6) . ? C16 C19 1.489(6) . ? C17 C18 1.367(6) . ? N20 C25 1.334(4) . ? N20 C21 1.338(4) . ? C21 C22 1.375(5) . ? C21 N32 1.399(4) . ? C22 C23 1.390(6) . ? C23 C24 1.393(6) . ? C24 C25 1.375(5) . ? C25 N26 1.387(4) . ? N26 C30 1.354(5) . ? N26 N27 1.383(4) . ? N27 C28 1.340(4) . ? C28 C29 1.413(6) . ? C28 C31 1.482(6) . ? C29 C30 1.361(6) . ? N32 C36 1.366(4) . ? N32 N33 1.372(4) . ? N33 C34 1.328(4) . ? C34 C35 1.411(5) . ? C34 C37 1.498(5) . ? C35 C36 1.352(5) . ? Cl38A O42A 1.385(7) . ? Cl38A O39A 1.398(7) . ? Cl38A O41A 1.505(6) . ? Cl38A O40A 1.515(7) . ? Cl38B O40B 1.363(7) . ? Cl38B O41B 1.403(7) . ? Cl38B O39B 1.496(8) . ? Cl38B O42B 1.499(7) . ? Cl43A O44A 1.367(9) . ? Cl43A O47A 1.426(10) . ? Cl43A O46A 1.448(8) . ? Cl43A O45A 1.478(9) . ? Cl43B O44B 1.394(9) . ? Cl43B O45B 1.409(8) . ? Cl43B O46B 1.490(9) . ? Cl43B O47B 1.520(10) . ? Cl43C O47C 1.344(10) . ? Cl43C O46C 1.465(9) . ? Cl43C O45C 1.472(9) . ? Cl43C O44C 1.495(10) . ? C48A C49A 1.517(16) . ? C49A O51A 1.228(15) . ? C49A C50A 1.496(17) . ? C48B C49B 1.498(14) . ? C49B O51B 1.235(14) . ? C49B C50B 1.530(15) . ? C48C C49C 1.506(18) . ? C49C O51C 1.234(19) . ? C49C C50C 1.491(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N20 178.08(12) . . ? N2 Fe1 N9 79.25(12) . . ? N20 Fe1 N9 102.60(12) . . ? N2 Fe1 N15 79.07(12) . . ? N20 Fe1 N15 99.06(12) . . ? N9 Fe1 N15 158.19(13) . . ? N2 Fe1 N27 101.71(11) . . ? N20 Fe1 N27 78.84(11) . . ? N9 Fe1 N27 90.73(11) . . ? N15 Fe1 N27 95.91(11) . . ? N2 Fe1 N33 100.94(11) . . ? N20 Fe1 N33 78.61(11) . . ? N9 Fe1 N33 91.01(11) . . ? N15 Fe1 N33 90.83(11) . . ? N27 Fe1 N33 157.21(11) . . ? C7 N2 C3 119.6(3) . . ? C7 N2 Fe1 120.1(2) . . ? C3 N2 Fe1 120.3(2) . . ? N2 C3 C4 122.4(3) . . ? N2 C3 N8 111.1(3) . . ? C4 C3 N8 126.6(3) . . ? C3 C4 C5 117.3(3) . . ? C4 C5 C6 121.7(4) . . ? C7 C6 C5 116.1(4) . . ? N2 C7 C6 122.9(3) . . ? N2 C7 N14 111.7(3) . . ? C6 C7 N14 125.5(3) . . ? C12 N8 N9 110.3(4) . . ? C12 N8 C3 132.4(4) . . ? N9 N8 C3 117.4(3) . . ? C10 N9 N8 105.9(3) . . ? C10 N9 Fe1 142.0(3) . . ? N8 N9 Fe1 112.0(2) . . ? N9 C10 C11 109.6(4) . . ? N9 C10 C13 121.3(4) . . ? C11 C10 C13 129.1(4) . . ? C12 C11 C10 107.2(4) . . ? C11 C12 N8 107.0(4) . . ? C18 N14 N15 111.8(3) . . ? C18 N14 C7 130.9(3) . . ? N15 N14 C7 117.2(3) . . ? C16 N15 N14 104.8(3) . . ? C16 N15 Fe1 143.1(3) . . ? N14 N15 Fe1 111.7(2) . . ? N15 C16 C17 110.1(3) . . ? N15 C16 C19 122.7(4) . . ? C17 C16 C19 127.2(3) . . ? C18 C17 C16 107.3(3) . . ? N14 C18 C17 106.0(4) . . ? C25 N20 C21 119.7(3) . . ? C25 N20 Fe1 119.9(2) . . ? C21 N20 Fe1 120.3(2) . . ? N20 C21 C22 122.7(3) . . ? N20 C21 N32 111.1(3) . . ? C22 C21 N32 126.2(3) . . ? C21 C22 C23 116.6(3) . . ? C22 C23 C24 121.5(4) . . ? C25 C24 C23 116.8(4) . . ? N20 C25 C24 122.5(3) . . ? N20 C25 N26 111.7(3) . . ? C24 C25 N26 125.8(3) . . ? C30 N26 N27 111.0(3) . . ? C30 N26 C25 131.2(3) . . ? N27 N26 C25 117.7(3) . . ? C28 N27 N26 105.8(3) . . ? C28 N27 Fe1 142.3(3) . . ? N26 N27 Fe1 111.68(19) . . ? N27 C28 C29 109.2(3) . . ? N27 C28 C31 123.1(4) . . ? C29 C28 C31 127.7(3) . . ? C30 C29 C28 107.1(3) . . ? N26 C30 C29 106.9(4) . . ? C36 N32 N33 110.9(3) . . ? C36 N32 C21 131.1(3) . . ? N33 N32 C21 117.9(3) . . ? C34 N33 N32 105.8(3) . . ? C34 N33 Fe1 142.2(2) . . ? N32 N33 Fe1 111.95(19) . . ? N33 C34 C35 109.7(3) . . ? N33 C34 C37 122.6(3) . . ? C35 C34 C37 127.7(3) . . ? C36 C35 C34 107.0(3) . . ? C35 C36 N32 106.5(3) . . ? O42A Cl38A O39A 113.7(5) . . ? O42A Cl38A O41A 111.9(4) . . ? O39A Cl38A O41A 113.2(5) . . ? O42A Cl38A O40A 106.3(5) . . ? O39A Cl38A O40A 111.4(5) . . ? O41A Cl38A O40A 99.2(4) . . ? O40B Cl38B O41B 122.2(5) . . ? O40B Cl38B O39B 107.1(5) . . ? O41B Cl38B O39B 106.0(5) . . ? O40B Cl38B O42B 109.8(5) . . ? O41B Cl38B O42B 106.5(5) . . ? O39B Cl38B O42B 103.9(5) . . ? O44A Cl43A O47A 116.7(8) . . ? O44A Cl43A O46A 110.9(6) . . ? O47A Cl43A O46A 106.1(7) . . ? O44A Cl43A O45A 102.3(7) . . ? O47A Cl43A O45A 109.9(7) . . ? O46A Cl43A O45A 111.0(6) . . ? O44B Cl43B O45B 116.0(6) . . ? O44B Cl43B O46B 119.3(6) . . ? O45B Cl43B O46B 105.8(6) . . ? O44B Cl43B O47B 107.8(7) . . ? O45B Cl43B O47B 102.5(6) . . ? O46B Cl43B O47B 103.3(7) . . ? O47C Cl43C O46C 122.2(7) . . ? O47C Cl43C O45C 110.7(8) . . ? O46C Cl43C O45C 105.3(6) . . ? O47C Cl43C O44C 107.0(7) . . ? O46C Cl43C O44C 100.3(7) . . ? O45C Cl43C O44C 110.7(7) . . ? O51A C49A C50A 120.6(15) . . ? O51A C49A C48A 118.1(15) . . ? C50A C49A C48A 117.5(14) . . ? O51B C49B C48B 119.9(12) . . ? O51B C49B C50B 124.4(12) . . ? C48B C49B C50B 113.3(12) . . ? O51C C49C C50C 120.3(17) . . ? O51C C49C C48C 122.1(18) . . ? C50C C49C C48C 117.6(17) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.841 _refine_diff_density_min -0.752 _refine_diff_density_rms 0.166 #=END data_je34100 _database_code_depnum_ccdc_archive 'CCDC 278904' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-(3-methylpyrazol-1-yl)pyridine]iron(II) diperchlorate acetone solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Fe N10, 2[Cl O4], C3 H6 O' _chemical_formula_sum 'C29 H32 Cl2 Fe N10 O9' _chemical_formula_weight 791.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.7743(3) _cell_length_b 10.9586(2) _cell_length_c 28.4036(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.1525(9) _cell_angle_gamma 90.00 _cell_volume 6809.00(18) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 51437 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 27.56 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour 'Dark brown' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 0.668 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.430 _exptl_absorpt_correction_T_max 0.925 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings The high value of Rint reflects the highly redundant dataset collected for this crystal. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method 'Area detector scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51437 _diffrn_reflns_av_R_equivalents 0.1230 _diffrn_reflns_av_sigmaI/netI 0.0593 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 27.56 _reflns_number_total 7823 _reflns_number_gt 6160 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 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 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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. Both the ClO~4~^-^ anions are disordered: Cl38A-O42A (occupancy 0.50) and Cl38B-O42B (occupancy 0.50) and Cl43A-O47A (occupancy 0.35), Cl43B-O47B (occupancy 0.35) and Cl43C-O47C (occupancy 0.30). All disordered Cl-O distances were restrained to 1.45(2)\%A, and O...O distances within a given disorder orientation to 2.37(2)\%A. The acetone molecule is also disordered, over three different orientations: C48A-O51A (occupancy 0.45), C48B-O51B (occupancy 0.45) and C48C-O51C (occupancy 0.10). The following restraints were applied to this molecule: C-C = 1.49(2)\%A, C=O = 1.26(2)\%A and 1,3-C...O = 2.40(2)\%A. All wholly occupied non-H atoms were refined anisotropically. All H atoms were placed in calculated positions and refined using a riding model, except for the solvent methyl groups whose torsions were not allowed to refine. ; _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^)+(0.0933P)^2^+7.6181P] 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 SHELXL _refine_ls_extinction_coef 0.0015(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7823 _refine_ls_number_parameters 491 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1647 _refine_ls_wR_factor_gt 0.1493 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.002 _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 0.590699(17) 0.31799(3) 0.636482(13) 0.02798(14) Uani 1 1 d . . . N2 N 0.59692(10) 0.4596(2) 0.67620(8) 0.0303(5) Uani 1 1 d . . . C3 C 0.54650(12) 0.5150(3) 0.68097(9) 0.0323(6) Uani 1 1 d . . . C4 C 0.54832(14) 0.6158(3) 0.71009(10) 0.0392(6) Uani 1 1 d . . . H4 H 0.5120 0.6550 0.7124 0.047 Uiso 1 1 calc R . . C5 C 0.60584(15) 0.6576(3) 0.73604(11) 0.0403(7) Uani 1 1 d . . . H5 H 0.6089 0.7258 0.7573 0.048 Uiso 1 1 calc R . . C6 C 0.65880(14) 0.6023(3) 0.73172(10) 0.0375(6) Uani 1 1 d . . . H6 H 0.6981 0.6308 0.7496 0.045 Uiso 1 1 calc R . . C7 C 0.65189(12) 0.5041(2) 0.70027(9) 0.0318(5) Uani 1 1 d . . . N8 N 0.49374(10) 0.4554(2) 0.65295(8) 0.0351(5) Uani 1 1 d . . . N9 N 0.50255(10) 0.3524(2) 0.62759(8) 0.0334(5) Uani 1 1 d . . . C10 C 0.44675(13) 0.3117(3) 0.60493(11) 0.0392(7) Uani 1 1 d . . . C11 C 0.40251(14) 0.3876(3) 0.61588(11) 0.0454(7) Uani 1 1 d . . . H11 H 0.3594 0.3784 0.6044 0.054 Uiso 1 1 calc R . . C12 C 0.43326(13) 0.4765(3) 0.64604(11) 0.0426(7) Uani 1 1 d . . . H12 H 0.4157 0.5414 0.6597 0.051 Uiso 1 1 calc R . . C13 C 0.43742(15) 0.2026(3) 0.57297(13) 0.0502(8) Uani 1 1 d . . . H13A H 0.4594 0.2130 0.5481 0.075 Uiso 1 1 calc R . . H13B H 0.3937 0.1923 0.5569 0.075 Uiso 1 1 calc R . . H13C H 0.4530 0.1303 0.5928 0.075 Uiso 1 1 calc R . . N14 N 0.69817(10) 0.4404(2) 0.68785(8) 0.0317(5) Uani 1 1 d . . . N15 N 0.68176(10) 0.3390(2) 0.65818(8) 0.0320(5) Uani 1 1 d . . . C16 C 0.73400(13) 0.2992(3) 0.65106(10) 0.0350(6) Uani 1 1 d . . . C17 C 0.78307(13) 0.3749(3) 0.67579(10) 0.0392(6) Uani 1 1 d . . . H17 H 0.8247 0.3657 0.6764 0.047 Uiso 1 1 calc R . . C18 C 0.75920(12) 0.4636(3) 0.69866(10) 0.0368(6) Uani 1 1 d . . . H18 H 0.7808 0.5284 0.7182 0.044 Uiso 1 1 calc R . . C19 C 0.73715(15) 0.1916(3) 0.61995(13) 0.0443(7) Uani 1 1 d . . . H19A H 0.7205 0.1199 0.6324 0.066 Uiso 1 1 calc R . . H19B H 0.7798 0.1762 0.6208 0.066 Uiso 1 1 calc R . . H19C H 0.7132 0.2077 0.5861 0.066 Uiso 1 1 calc R . . N20 N 0.58744(11) 0.1750(2) 0.59771(8) 0.0324(5) Uani 1 1 d . . . C21 C 0.58680(14) 0.1840(3) 0.55038(11) 0.0356(6) Uani 1 1 d . . . C22 C 0.58801(16) 0.0839(3) 0.52151(11) 0.0443(7) Uani 1 1 d . . . H22 H 0.5871 0.0920 0.4880 0.053 Uiso 1 1 calc R . . C23 C 0.59058(17) -0.0298(3) 0.54378(12) 0.0511(8) Uani 1 1 d . . . H23 H 0.5920 -0.1011 0.5251 0.061 Uiso 1 1 calc R . . C24 C 0.59118(15) -0.0417(3) 0.59252(12) 0.0446(7) Uani 1 1 d . . . H24 H 0.5932 -0.1195 0.6077 0.053 Uiso 1 1 calc R . . C25 C 0.58873(13) 0.0648(3) 0.61799(10) 0.0355(6) Uani 1 1 d . . . N26 N 0.58859(11) 0.0734(2) 0.66657(8) 0.0348(5) Uani 1 1 d . . . N27 N 0.58932(10) 0.1889(2) 0.68630(8) 0.0322(5) Uani 1 1 d . . . C28 C 0.58450(12) 0.1707(3) 0.73167(10) 0.0341(6) Uani 1 1 d . . . C29 C 0.58099(14) 0.0447(3) 0.74080(11) 0.0424(7) Uani 1 1 d . . . H29 H 0.5772 0.0082 0.7702 0.051 Uiso 1 1 calc R . . C30 C 0.58404(15) -0.0144(3) 0.69933(12) 0.0439(7) Uani 1 1 d . . . H30 H 0.5832 -0.1001 0.6943 0.053 Uiso 1 1 calc R . . C31 C 0.58309(13) 0.2720(3) 0.76614(10) 0.0388(6) Uani 1 1 d . . . H31A H 0.6243 0.3055 0.7791 0.058 Uiso 1 1 calc R . . H31B H 0.5685 0.2411 0.7932 0.058 Uiso 1 1 calc R . . H31C H 0.5555 0.3362 0.7488 0.058 Uiso 1 1 calc R . . N32 N 0.58568(11) 0.3067(2) 0.53629(8) 0.0329(5) Uani 1 1 d . . . N33 N 0.58669(10) 0.3937(2) 0.57151(8) 0.0301(5) Uani 1 1 d . . . C34 C 0.58412(12) 0.5002(3) 0.54891(10) 0.0334(6) Uani 1 1 d . . . C35 C 0.58172(13) 0.4812(3) 0.49903(10) 0.0383(6) Uani 1 1 d . . . H35 H 0.5798 0.5426 0.4750 0.046 Uiso 1 1 calc R . . C36 C 0.58264(14) 0.3597(3) 0.49213(10) 0.0387(6) Uani 1 1 d . . . H36 H 0.5814 0.3188 0.4624 0.046 Uiso 1 1 calc R . . C37 C 0.58370(15) 0.6189(3) 0.57412(11) 0.0407(7) Uani 1 1 d . . . H37A H 0.5455 0.6270 0.5833 0.061 Uiso 1 1 calc R . . H37B H 0.5869 0.6857 0.5520 0.061 Uiso 1 1 calc R . . H37C H 0.6184 0.6223 0.6036 0.061 Uiso 1 1 calc R . . Cl38A Cl 0.75896(8) 0.32766(18) 0.82074(7) 0.0295(5) Uiso 0.50 1 d PD A 1 O39A O 0.7264(3) 0.2668(6) 0.7774(2) 0.0363(19) Uiso 0.50 1 d PD A 1 O40A O 0.7893(3) 0.4427(5) 0.8094(2) 0.0464(18) Uiso 0.50 1 d PD A 1 O41A O 0.7181(2) 0.3830(5) 0.84868(19) 0.0447(13) Uiso 0.50 1 d PD A 1 O42A O 0.8054(3) 0.2556(5) 0.8503(2) 0.0486(16) Uiso 0.50 1 d PD A 1 Cl38B Cl 0.76128(9) 0.35307(19) 0.82283(7) 0.0347(6) Uiso 0.50 1 d PD B 2 O39B O 0.7268(3) 0.2894(6) 0.7770(2) 0.042(2) Uiso 0.50 1 d PD B 2 O40B O 0.7793(3) 0.4635(5) 0.8095(2) 0.0455(18) Uiso 0.50 1 d PD B 2 O41B O 0.7230(3) 0.3442(5) 0.8544(2) 0.0514(15) Uiso 0.50 1 d PD B 2 O42B O 0.8154(3) 0.2745(6) 0.8444(2) 0.0568(19) Uiso 0.50 1 d PD B 2 Cl43A Cl 0.92600(19) 0.3542(3) 0.62680(12) 0.0266(8) Uiso 0.35 1 d PD C 1 O44A O 0.8754(4) 0.3343(10) 0.5852(3) 0.033(2) Uiso 0.35 1 d PD C 1 O45A O 0.9115(4) 0.2570(8) 0.6610(3) 0.046(3) Uiso 0.35 1 d PD C 1 O46A O 0.9794(3) 0.3195(6) 0.6129(3) 0.0321(16) Uiso 0.35 1 d PD C 1 O47A O 0.9310(5) 0.4683(7) 0.6464(4) 0.054(2) Uiso 0.35 1 d PD C 1 Cl43B Cl 0.92571(18) 0.3242(3) 0.62691(11) 0.0285(7) Uiso 0.35 1 d PD D 2 O44B O 0.8738(3) 0.2931(7) 0.5925(3) 0.053(2) Uiso 0.35 1 d PD D 2 O45B O 0.9310(3) 0.3022(7) 0.6770(2) 0.040(2) Uiso 0.35 1 d PD D 2 O46B O 0.9869(4) 0.2854(10) 0.6206(3) 0.032(2) Uiso 0.35 1 d PD D 2 O47B O 0.9332(6) 0.4656(8) 0.6289(4) 0.090(4) Uiso 0.35 1 d PD D 2 Cl43C Cl 0.93666(17) 0.3436(5) 0.63202(13) 0.0287(10) Uiso 0.30 1 d PD E 3 O44C O 0.8805(5) 0.3601(9) 0.5879(3) 0.045(3) Uiso 0.30 1 d PD E 3 O45C O 0.9195(5) 0.2731(9) 0.6697(4) 0.022(2) Uiso 0.30 1 d PD E 3 O46C O 0.9758(4) 0.2705(9) 0.6123(4) 0.033(2) Uiso 0.30 1 d PD E 3 O47C O 0.9520(4) 0.4626(6) 0.6484(3) 0.042(2) Uiso 0.30 1 d PD E 3 C48A C 0.7584(5) 0.6048(10) 0.5717(3) 0.054(3) Uiso 0.45 1 d PD F 1 H48A H 0.7533 0.6863 0.5841 0.082 Uiso 0.45 1 calc PR F 1 H48B H 0.8020 0.5870 0.5778 0.082 Uiso 0.45 1 calc PR F 1 H48C H 0.7397 0.5441 0.5884 0.082 Uiso 0.45 1 calc PR F 1 C49A C 0.7276(8) 0.5999(18) 0.5172(5) 0.054(6) Uiso 0.45 1 d PD F 1 C50A C 0.7589(5) 0.5406(11) 0.4847(4) 0.062(3) Uiso 0.45 1 d PD F 1 H50A H 0.7307 0.5330 0.4518 0.093 Uiso 0.45 1 calc PR F 1 H50B H 0.7727 0.4592 0.4975 0.093 Uiso 0.45 1 calc PR F 1 H50C H 0.7943 0.5897 0.4833 0.093 Uiso 0.45 1 calc PR F 1 O51A O 0.6862(4) 0.6753(9) 0.4985(3) 0.040(2) Uiso 0.45 1 d PD F 1 C48B C 0.7467(5) 0.5735(11) 0.5701(3) 0.049(2) Uiso 0.45 1 d PD G 2 H48D H 0.7263 0.6226 0.5898 0.074 Uiso 0.45 1 calc PR G 2 H48E H 0.7911 0.5839 0.5826 0.074 Uiso 0.45 1 calc PR G 2 H48F H 0.7362 0.4873 0.5721 0.074 Uiso 0.45 1 calc PR G 2 C49B C 0.7259(7) 0.6146(13) 0.5176(4) 0.037(4) Uiso 0.45 1 d PD G 2 C50B C 0.7442(5) 0.5227(10) 0.4825(4) 0.056(3) Uiso 0.45 1 d PD G 2 H50D H 0.7074 0.4948 0.4578 0.084 Uiso 0.45 1 calc PR G 2 H50E H 0.7650 0.4525 0.5013 0.084 Uiso 0.45 1 calc PR G 2 H50F H 0.7717 0.5627 0.4662 0.084 Uiso 0.45 1 calc PR G 2 O51B O 0.6864(4) 0.6952(8) 0.5051(3) 0.059(3) Uiso 0.45 1 d PD G 2 C48C C 0.768(2) 0.548(4) 0.5683(10) 0.064(11) Uiso 0.10 1 d PD H 3 H48G H 0.7529 0.6149 0.5845 0.097 Uiso 0.10 1 calc PR H 3 H48H H 0.8115 0.5606 0.5711 0.097 Uiso 0.10 1 calc PR H 3 H48I H 0.7629 0.4704 0.5841 0.097 Uiso 0.10 1 calc PR H 3 C49C C 0.733(2) 0.544(3) 0.5158(11) 0.078(15) Uiso 0.10 1 d PD H 3 C50C C 0.7413(19) 0.438(3) 0.4856(13) 0.069(11) Uiso 0.10 1 d PD H 3 H50G H 0.7013 0.4065 0.4672 0.103 Uiso 0.10 1 calc PR H 3 H50H H 0.7643 0.3741 0.5069 0.103 Uiso 0.10 1 calc PR H 3 H50I H 0.7639 0.4645 0.4626 0.103 Uiso 0.10 1 calc PR H 3 O51C O 0.6983(17) 0.631(3) 0.4953(12) 0.083(12) Uiso 0.10 1 d PD H 3 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 0.0260(2) 0.0343(2) 0.0241(2) 0.00003(14) 0.00779(15) 0.00083(14) N2 0.0291(11) 0.0377(11) 0.0261(11) 0.0035(9) 0.0112(9) 0.0022(9) C3 0.0318(13) 0.0415(14) 0.0256(13) 0.0055(10) 0.0111(11) 0.0040(11) C4 0.0427(16) 0.0455(16) 0.0333(15) 0.0033(12) 0.0171(12) 0.0106(13) C5 0.0540(19) 0.0408(15) 0.0289(14) -0.0017(11) 0.0161(13) 0.0043(13) C6 0.0419(15) 0.0412(15) 0.0291(14) -0.0018(11) 0.0096(12) -0.0054(12) C7 0.0300(13) 0.0396(14) 0.0257(12) 0.0037(10) 0.0078(10) -0.0001(11) N8 0.0283(11) 0.0479(13) 0.0311(12) 0.0058(10) 0.0113(9) 0.0068(10) N9 0.0283(11) 0.0440(12) 0.0280(11) 0.0043(10) 0.0077(9) -0.0015(10) C10 0.0282(14) 0.0574(18) 0.0307(14) 0.0107(12) 0.0058(11) -0.0043(12) C11 0.0296(14) 0.072(2) 0.0352(16) 0.0147(15) 0.0109(12) -0.0002(14) C12 0.0332(15) 0.0629(19) 0.0351(15) 0.0118(14) 0.0149(12) 0.0131(14) C13 0.0394(17) 0.0573(19) 0.0479(19) 0.0010(15) 0.0024(15) -0.0086(14) N14 0.0270(11) 0.0401(12) 0.0275(11) -0.0007(9) 0.0067(9) -0.0001(9) N15 0.0303(12) 0.0399(12) 0.0267(11) 0.0021(9) 0.0094(9) 0.0037(9) C16 0.0318(14) 0.0427(14) 0.0329(14) 0.0053(11) 0.0129(11) 0.0055(11) C17 0.0288(14) 0.0544(17) 0.0343(15) 0.0078(13) 0.0085(12) 0.0021(12) C18 0.0269(13) 0.0515(16) 0.0313(14) 0.0014(12) 0.0072(11) -0.0026(12) C19 0.0385(16) 0.0465(16) 0.0520(19) -0.0018(14) 0.0196(15) 0.0065(13) N20 0.0326(12) 0.0366(12) 0.0279(11) -0.0010(9) 0.0081(10) 0.0002(9) C21 0.0368(15) 0.0403(15) 0.0294(14) -0.0018(11) 0.0090(12) -0.0016(11) C22 0.0566(19) 0.0465(16) 0.0312(15) -0.0075(12) 0.0146(14) -0.0039(14) C23 0.071(2) 0.0409(16) 0.0423(18) -0.0111(13) 0.0169(16) -0.0055(15) C24 0.0556(19) 0.0369(15) 0.0424(17) -0.0026(12) 0.0154(15) -0.0016(13) C25 0.0346(14) 0.0369(14) 0.0343(15) -0.0016(11) 0.0085(12) -0.0038(11) N26 0.0364(12) 0.0352(12) 0.0326(12) 0.0024(9) 0.0092(10) -0.0003(10) N27 0.0279(11) 0.0395(12) 0.0298(12) -0.0010(9) 0.0093(9) 0.0005(9) C28 0.0253(13) 0.0485(16) 0.0278(14) 0.0051(11) 0.0060(11) 0.0026(11) C29 0.0415(16) 0.0533(17) 0.0343(15) 0.0078(13) 0.0134(13) -0.0001(13) C30 0.0463(17) 0.0415(15) 0.0451(17) 0.0092(13) 0.0149(14) -0.0005(13) C31 0.0340(15) 0.0542(17) 0.0296(14) -0.0010(12) 0.0110(12) -0.0013(13) N32 0.0374(13) 0.0380(12) 0.0237(11) -0.0015(9) 0.0092(10) -0.0005(9) N33 0.0284(11) 0.0369(11) 0.0256(11) -0.0014(9) 0.0083(9) 0.0004(9) C34 0.0298(13) 0.0405(14) 0.0300(13) 0.0035(11) 0.0084(11) 0.0006(11) C35 0.0398(15) 0.0483(16) 0.0277(14) 0.0054(12) 0.0110(12) -0.0004(13) C36 0.0440(16) 0.0501(16) 0.0241(13) 0.0004(12) 0.0126(12) -0.0017(13) C37 0.0490(17) 0.0351(14) 0.0383(16) 0.0023(12) 0.0129(13) 0.0001(13) _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 N2 1.900(2) . ? Fe1 N20 1.905(2) . ? Fe1 N9 1.989(2) . ? Fe1 N33 2.002(2) . ? Fe1 N15 2.006(2) . ? Fe1 N27 2.007(2) . ? N2 C3 1.338(3) . ? N2 C7 1.340(3) . ? C3 C4 1.374(4) . ? C3 N8 1.404(4) . ? C4 C5 1.390(4) . ? C5 C6 1.385(4) . ? C6 C7 1.380(4) . ? C7 N14 1.389(3) . ? N8 C12 1.356(4) . ? N8 N9 1.383(3) . ? N9 C10 1.332(4) . ? C10 C11 1.406(4) . ? C10 C13 1.480(5) . ? C11 C12 1.357(5) . ? N14 C18 1.361(3) . ? N14 N15 1.382(3) . ? N15 C16 1.334(3) . ? C16 C17 1.412(4) . ? C16 C19 1.487(4) . ? C17 C18 1.364(4) . ? N20 C25 1.335(4) . ? N20 C21 1.344(4) . ? C21 C22 1.374(4) . ? C21 N32 1.401(4) . ? C22 C23 1.391(5) . ? C23 C24 1.387(5) . ? C24 C25 1.383(4) . ? C25 N26 1.384(4) . ? N26 C30 1.362(4) . ? N26 N27 1.383(3) . ? N27 C28 1.338(3) . ? C28 C29 1.411(4) . ? C28 C31 1.487(4) . ? C29 C30 1.363(4) . ? N32 C36 1.367(3) . ? N32 N33 1.377(3) . ? N33 C34 1.326(3) . ? C34 C35 1.418(4) . ? C34 C37 1.487(4) . ? C35 C36 1.347(4) . ? Cl38A O42A 1.398(6) . ? Cl38A O39A 1.415(6) . ? Cl38A O41A 1.508(5) . ? Cl38A O40A 1.515(6) . ? Cl38B O40B 1.365(6) . ? Cl38B O41B 1.417(6) . ? Cl38B O42B 1.489(6) . ? Cl38B O39B 1.493(7) . ? Cl43A O47A 1.360(8) . ? Cl43A O44A 1.419(8) . ? Cl43A O46A 1.430(6) . ? Cl43A O45A 1.538(8) . ? Cl43B O44B 1.351(8) . ? Cl43B O45B 1.413(7) . ? Cl43B O46B 1.513(8) . ? Cl43B O47B 1.558(9) . ? Cl43C O47C 1.396(8) . ? Cl43C O46C 1.424(8) . ? Cl43C O45C 1.460(8) . ? Cl43C O44C 1.533(10) . ? C48A C49A 1.513(14) . ? C49A O51A 1.254(14) . ? C49A C50A 1.465(14) . ? C48B C49B 1.501(12) . ? C49B O51B 1.240(12) . ? C49B C50B 1.555(13) . ? C48C C49C 1.486(19) . ? C49C O51C 1.27(2) . ? C49C C50C 1.482(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N20 177.98(10) . . ? N2 Fe1 N9 80.00(9) . . ? N20 Fe1 N9 101.96(10) . . ? N2 Fe1 N33 100.71(9) . . ? N20 Fe1 N33 79.82(9) . . ? N9 Fe1 N33 91.08(9) . . ? N2 Fe1 N15 79.86(9) . . ? N20 Fe1 N15 98.21(10) . . ? N9 Fe1 N15 159.76(10) . . ? N33 Fe1 N15 90.79(9) . . ? N2 Fe1 N27 99.80(9) . . ? N20 Fe1 N27 79.75(10) . . ? N9 Fe1 N27 90.58(9) . . ? N33 Fe1 N27 159.40(9) . . ? N15 Fe1 N27 94.69(9) . . ? C3 N2 C7 119.3(2) . . ? C3 N2 Fe1 120.38(19) . . ? C7 N2 Fe1 120.30(18) . . ? N2 C3 C4 122.8(3) . . ? N2 C3 N8 110.8(2) . . ? C4 C3 N8 126.3(2) . . ? C3 C4 C5 116.8(3) . . ? C6 C5 C4 121.6(3) . . ? C7 C6 C5 117.0(3) . . ? N2 C7 C6 122.4(2) . . ? N2 C7 N14 110.8(2) . . ? C6 C7 N14 126.7(3) . . ? C12 N8 N9 110.6(2) . . ? C12 N8 C3 132.7(3) . . ? N9 N8 C3 116.7(2) . . ? C10 N9 N8 105.5(2) . . ? C10 N9 Fe1 142.3(2) . . ? N8 N9 Fe1 112.11(17) . . ? N9 C10 C11 109.9(3) . . ? N9 C10 C13 121.5(3) . . ? C11 C10 C13 128.6(3) . . ? C12 C11 C10 106.8(3) . . ? N8 C12 C11 107.1(3) . . ? C18 N14 N15 111.9(2) . . ? C18 N14 C7 130.4(2) . . ? N15 N14 C7 117.6(2) . . ? C16 N15 N14 104.7(2) . . ? C16 N15 Fe1 143.6(2) . . ? N14 N15 Fe1 111.14(15) . . ? N15 C16 C17 110.4(3) . . ? N15 C16 C19 122.8(3) . . ? C17 C16 C19 126.8(3) . . ? C18 C17 C16 106.9(2) . . ? N14 C18 C17 106.1(3) . . ? C25 N20 C21 119.4(2) . . ? C25 N20 Fe1 120.13(19) . . ? C21 N20 Fe1 120.37(18) . . ? N20 C21 C22 122.8(3) . . ? N20 C21 N32 110.5(2) . . ? C22 C21 N32 126.7(3) . . ? C21 C22 C23 116.7(3) . . ? C24 C23 C22 121.7(3) . . ? C25 C24 C23 116.9(3) . . ? N20 C25 C24 122.5(3) . . ? N20 C25 N26 111.3(2) . . ? C24 C25 N26 126.2(3) . . ? C30 N26 N27 111.4(2) . . ? C30 N26 C25 130.9(3) . . ? N27 N26 C25 117.6(2) . . ? C28 N27 N26 105.0(2) . . ? C28 N27 Fe1 143.7(2) . . ? N26 N27 Fe1 111.12(16) . . ? N27 C28 C29 110.3(3) . . ? N27 C28 C31 123.0(2) . . ? C29 C28 C31 126.7(3) . . ? C30 C29 C28 106.7(3) . . ? N26 C30 C29 106.7(3) . . ? C36 N32 N33 111.0(2) . . ? C36 N32 C21 131.5(2) . . ? N33 N32 C21 117.5(2) . . ? C34 N33 N32 105.6(2) . . ? C34 N33 Fe1 142.71(19) . . ? N32 N33 Fe1 111.73(16) . . ? N33 C34 C35 109.8(2) . . ? N33 C34 C37 122.9(2) . . ? C35 C34 C37 127.3(3) . . ? C36 C35 C34 107.0(3) . . ? C35 C36 N32 106.6(2) . . ? O42A Cl38A O39A 112.5(4) . . ? O42A Cl38A O41A 112.7(3) . . ? O39A Cl38A O41A 113.4(4) . . ? O42A Cl38A O40A 106.5(4) . . ? O39A Cl38A O40A 111.5(4) . . ? O41A Cl38A O40A 99.3(3) . . ? O40B Cl38B O41B 121.4(4) . . ? O40B Cl38B O42B 110.4(4) . . ? O41B Cl38B O42B 106.5(4) . . ? O40B Cl38B O39B 107.4(4) . . ? O41B Cl38B O39B 104.7(4) . . ? O42B Cl38B O39B 105.2(4) . . ? O47A Cl43A O44A 116.0(7) . . ? O47A Cl43A O46A 112.1(6) . . ? O44A Cl43A O46A 106.6(5) . . ? O47A Cl43A O45A 112.8(5) . . ? O44A Cl43A O45A 98.7(6) . . ? O46A Cl43A O45A 109.7(5) . . ? O44B Cl43B O45B 119.7(5) . . ? O44B Cl43B O46B 119.5(5) . . ? O45B Cl43B O46B 104.3(5) . . ? O44B Cl43B O47B 110.0(6) . . ? O45B Cl43B O47B 98.9(5) . . ? O46B Cl43B O47B 100.9(6) . . ? O47C Cl43C O46C 122.0(6) . . ? O47C Cl43C O45C 110.1(6) . . ? O46C Cl43C O45C 108.4(6) . . ? O47C Cl43C O44C 103.8(6) . . ? O46C Cl43C O44C 102.5(6) . . ? O45C Cl43C O44C 109.2(6) . . ? O51A C49A C50A 117.8(11) . . ? O51A C49A C48A 119.3(12) . . ? C50A C49A C48A 119.4(11) . . ? O51B C49B C48B 120.1(10) . . ? O51B C49B C50B 125.4(10) . . ? C48B C49B C50B 112.1(9) . . ? O51C C49C C50C 119.0(18) . . ? O51C C49C C48C 121.8(19) . . ? C50C C49C C48C 119.1(18) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.637 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.124 data_c:\datasets\leeds\je33bv~1\je33b2~2\je33b250 _database_code_depnum_ccdc_archive 'CCDC 278905' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-bis(3-methylpyrazol-1-yl)pyridine] ditetrafluoroborate tetrakis-acetonitrile solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Fe N10, 2[B F4], 4[C2 H3 N]' _chemical_formula_sum 'C34 H38 B2 F8 Fe N14' _chemical_formula_weight 872.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' 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 11.6508(1) _cell_length_b 13.7476(1) _cell_length_c 26.4113(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4230.31(7) _cell_formula_units_Z 4 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 70076 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'Square prism' _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.435 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.608 _exptl_absorpt_correction_T_max 0.888 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_ambient_temperature 250(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 diffractometer' _diffrn_measurement_method 'Area detector scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70076 _diffrn_reflns_av_R_equivalents 0.0906 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9695 _reflns_number_gt 7479 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 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 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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. Anion B43-F47 is disordered over three sites, labelled 'A' (occupancy 0.4) 'B' (occupancy 0.4) and 'C (occupancy 0.2). These were modelled using the refined restraints B---F = 1.39(2) and 1,3-F...F = 2.27(2)\%A. All non-H atoms except the disordered anion were refined anisotropically. All H atoms were placed in calculated positions and refined using a riding model, with the methyl group torsions allowed to refine freely. ; _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^)+(0.0689P)^2^+0.4468P] 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 -0.014(15) _refine_ls_number_reflns 9695 _refine_ls_number_parameters 556 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1233 _refine_ls_wR_factor_gt 0.1101 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.062 _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 0.25054(3) 0.22140(2) 0.178271(11) 0.04190(10) Uani 1 1 d . . . N2 N 0.30783(18) 0.09397(14) 0.21431(8) 0.0424(4) Uani 1 1 d . . . C3 C 0.3496(2) 0.09770(18) 0.26160(9) 0.0443(5) Uani 1 1 d . . . C4 C 0.3919(3) 0.0173(2) 0.28616(11) 0.0574(7) Uani 1 1 d . . . H4 H 0.4204 0.0213 0.3198 0.069 Uiso 1 1 calc R . . C5 C 0.3913(3) -0.0695(2) 0.25995(12) 0.0647(8) Uani 1 1 d . . . H5 H 0.4209 -0.1263 0.2758 0.078 Uiso 1 1 calc R . . C6 C 0.3487(3) -0.0760(2) 0.21105(12) 0.0593(7) Uani 1 1 d . . . H6 H 0.3483 -0.1357 0.1929 0.071 Uiso 1 1 calc R . . C7 C 0.3066(2) 0.00894(18) 0.19005(10) 0.0467(6) Uani 1 1 d . . . N8 N 0.34601(19) 0.19134(15) 0.28218(8) 0.0465(5) Uani 1 1 d . . . N9 N 0.30851(19) 0.26735(15) 0.25196(8) 0.0474(5) Uani 1 1 d . . . C10 C 0.3172(3) 0.3459(2) 0.28072(11) 0.0555(7) Uani 1 1 d . . . C11 C 0.3605(3) 0.3212(2) 0.32884(12) 0.0665(8) Uani 1 1 d . . . H11 H 0.3758 0.3647 0.3560 0.080 Uiso 1 1 calc R . . C12 C 0.3761(3) 0.2235(2) 0.32898(10) 0.0588(7) Uani 1 1 d . . . H12 H 0.4029 0.1851 0.3564 0.071 Uiso 1 1 calc R . . C13 C 0.2839(4) 0.4433(2) 0.26076(14) 0.0780(10) Uani 1 1 d . . . H13A H 0.2873 0.4425 0.2237 0.117 Uiso 1 1 calc R . . H13B H 0.3369 0.4926 0.2738 0.117 Uiso 1 1 calc R . . H13C H 0.2056 0.4588 0.2717 0.117 Uiso 1 1 calc R . . N14 N 0.2612(2) 0.01518(14) 0.14135(8) 0.0496(5) Uani 1 1 d . . . N15 N 0.22310(18) 0.10425(15) 0.12374(8) 0.0481(5) Uani 1 1 d . . . C16 C 0.1832(2) 0.0869(2) 0.07738(11) 0.0554(6) Uani 1 1 d . . . C17 C 0.1961(3) -0.0124(2) 0.06521(12) 0.0651(8) Uani 1 1 d . . . H17 H 0.1751 -0.0430 0.0343 0.078 Uiso 1 1 calc R . . C18 C 0.2441(3) -0.0554(2) 0.10594(11) 0.0625(7) Uani 1 1 d . . . H18 H 0.2625 -0.1225 0.1093 0.075 Uiso 1 1 calc R . . C19 C 0.1344(3) 0.1653(3) 0.04562(13) 0.0745(9) Uani 1 1 d . . . H19A H 0.1018 0.2159 0.0674 0.112 Uiso 1 1 calc R . . H19B H 0.0741 0.1384 0.0239 0.112 Uiso 1 1 calc R . . H19C H 0.1951 0.1934 0.0245 0.112 Uiso 1 1 calc R . . N20 N 0.19551(19) 0.34541(16) 0.13782(8) 0.0498(5) Uani 1 1 d . . . C21 C 0.0858(3) 0.3740(2) 0.13931(12) 0.0590(7) Uani 1 1 d . . . C22 C 0.0430(3) 0.4488(3) 0.11097(14) 0.0731(9) Uani 1 1 d . . . H22 H -0.0351 0.4681 0.1132 0.088 Uiso 1 1 calc R . . C23 C 0.1192(4) 0.4948(2) 0.07892(15) 0.0806(11) Uani 1 1 d . . . H23 H 0.0925 0.5465 0.0582 0.097 Uiso 1 1 calc R . . C24 C 0.2322(3) 0.4681(2) 0.07618(12) 0.0676(8) Uani 1 1 d . . . H24 H 0.2842 0.4998 0.0540 0.081 Uiso 1 1 calc R . . C25 C 0.2671(2) 0.39236(18) 0.10744(10) 0.0509(6) Uani 1 1 d . . . N26 N 0.0195(2) 0.3159(2) 0.17237(10) 0.0621(6) Uani 1 1 d . . . N27 N 0.07078(19) 0.2387(2) 0.19619(9) 0.0587(6) Uani 1 1 d . . . C28 C -0.0099(3) 0.1982(3) 0.22432(12) 0.0682(9) Uani 1 1 d . . . C29 C -0.1138(3) 0.2488(3) 0.21810(15) 0.0853(11) Uani 1 1 d . . . H29 H -0.1851 0.2340 0.2338 0.102 Uiso 1 1 calc R . . C30 C -0.0928(3) 0.3227(3) 0.18542(16) 0.0833(11) Uani 1 1 d . . . H30 H -0.1463 0.3699 0.1739 0.100 Uiso 1 1 calc R . . C31 C 0.0166(3) 0.1122(3) 0.25631(15) 0.0853(11) Uani 1 1 d . . . H31A H 0.0365 0.0569 0.2346 0.128 Uiso 1 1 calc R . . H31B H -0.0506 0.0957 0.2769 0.128 Uiso 1 1 calc R . . H31C H 0.0815 0.1273 0.2786 0.128 Uiso 1 1 calc R . . N32 N 0.3797(2) 0.35734(15) 0.11000(9) 0.0502(5) Uani 1 1 d . . . N33 N 0.40171(18) 0.27782(16) 0.13976(8) 0.0463(5) Uani 1 1 d . . . C34 C 0.5143(2) 0.2635(2) 0.13702(10) 0.0517(6) Uani 1 1 d . . . C35 C 0.5644(3) 0.3337(2) 0.10554(12) 0.0628(8) Uani 1 1 d . . . H35 H 0.6434 0.3394 0.0972 0.075 Uiso 1 1 calc R . . C36 C 0.4778(3) 0.3919(2) 0.08927(11) 0.0612(7) Uani 1 1 d . . . H36 H 0.4847 0.4466 0.0675 0.073 Uiso 1 1 calc R . . C37 C 0.5704(3) 0.1824(3) 0.16529(13) 0.0645(8) Uani 1 1 d . . . H37A H 0.5488 0.1859 0.2011 0.097 Uiso 1 1 calc R . . H37B H 0.6540 0.1880 0.1621 0.097 Uiso 1 1 calc R . . H37C H 0.5454 0.1199 0.1512 0.097 Uiso 1 1 calc R . . B38 B 0.3219(3) 0.6514(2) 0.16710(13) 0.0535(7) Uani 1 1 d . . . F39 F 0.21787(19) 0.6074(2) 0.17511(10) 0.1060(8) Uani 1 1 d . . . F40 F 0.39471(17) 0.58374(15) 0.14633(9) 0.0889(6) Uani 1 1 d . . . F41 F 0.3104(3) 0.72725(15) 0.13468(9) 0.1207(10) Uani 1 1 d . . . F42 F 0.3655(2) 0.68534(16) 0.21225(8) 0.0882(6) Uani 1 1 d . . . B43A B 0.2332(14) 0.0493(11) 0.4200(6) 0.086(11) Uiso 0.40 1 d PD A 1 F44A F 0.1941(6) 0.0805(5) 0.3730(2) 0.081(2) Uiso 0.40 1 d PD A 1 F45A F 0.2136(5) -0.0491(4) 0.4287(3) 0.086(2) Uiso 0.40 1 d PD A 1 F46A F 0.1752(8) 0.1146(6) 0.4510(3) 0.117(3) Uiso 0.40 1 d PD A 1 F47A F 0.3518(5) 0.0679(4) 0.4249(2) 0.0725(16) Uiso 0.40 1 d PD A 1 B43B B 0.2315(11) 0.0474(10) 0.4238(5) 0.054(7) Uiso 0.40 1 d PD B 2 F44B F 0.2107(6) 0.0503(7) 0.3716(2) 0.0626(18) Uiso 0.40 1 d PD B 2 F45B F 0.2347(6) -0.0389(4) 0.4462(2) 0.0781(17) Uiso 0.40 1 d PD B 2 F46B F 0.1349(6) 0.0924(6) 0.4473(3) 0.0720(18) Uiso 0.40 1 d PD B 2 F47B F 0.3317(6) 0.0977(6) 0.4360(2) 0.0873(19) Uiso 0.40 1 d PD B 2 B43C B 0.2344(12) 0.0661(11) 0.4245(5) 0.033(5) Uiso 0.20 1 d PD C 3 F44C F 0.2256(11) 0.0232(9) 0.3763(4) 0.081(5) Uiso 0.20 1 d PD C 3 F45C F 0.2841(15) 0.1543(10) 0.4310(6) 0.141(6) Uiso 0.20 1 d PD C 3 F46C F 0.1388(9) 0.0629(8) 0.4568(4) 0.066(3) Uiso 0.20 1 d PD C 3 F47C F 0.3087(14) -0.0022(12) 0.4509(6) 0.151(6) Uiso 0.20 1 d PD C 3 C48 C 0.8492(5) 0.0498(4) 0.1014(2) 0.1203(17) Uani 1 1 d . . . H48A H 0.8951 0.0000 0.0842 0.180 Uiso 1 1 calc R . . H48B H 0.7779 0.0206 0.1140 0.180 Uiso 1 1 calc R . . H48C H 0.8929 0.0764 0.1299 0.180 Uiso 1 1 calc R . . C49 C 0.8222(5) 0.1266(4) 0.0664(2) 0.1139(16) Uani 1 1 d . . . N50 N 0.8012(5) 0.1851(4) 0.0386(3) 0.177(3) Uani 1 1 d . . . C51 C 0.4623(4) 0.1275(3) 0.02058(15) 0.0836(11) Uani 1 1 d . . . H51A H 0.5250 0.1612 0.0031 0.125 Uiso 1 1 calc R . . H51B H 0.4211 0.1738 0.0422 0.125 Uiso 1 1 calc R . . H51C H 0.4093 0.1001 -0.0044 0.125 Uiso 1 1 calc R . . C52 C 0.5082(4) 0.0514(3) 0.05089(15) 0.0833(10) Uani 1 1 d . . . N53 N 0.5440(5) -0.0084(3) 0.07494(18) 0.1341(18) Uani 1 1 d . . . C54 C 0.4839(5) 0.7584(3) 0.03337(19) 0.1158(16) Uani 1 1 d . . . H54A H 0.4424 0.8117 0.0168 0.174 Uiso 1 1 calc R . . H54B H 0.5664 0.7659 0.0274 0.174 Uiso 1 1 calc R . . H54C H 0.4687 0.7599 0.0699 0.174 Uiso 1 1 calc R . . C55 C 0.4462(5) 0.6679(4) 0.01310(18) 0.1042(14) Uani 1 1 d . . . N56 N 0.4184(6) 0.5954(4) -0.00196(19) 0.146(2) Uani 1 1 d . . . C57 C -0.0072(6) 0.7558(4) 0.1224(2) 0.134(2) Uani 1 1 d . . . H57A H -0.0086 0.7805 0.0876 0.201 Uiso 1 1 calc R . . H57B H -0.0751 0.7153 0.1283 0.201 Uiso 1 1 calc R . . H57C H 0.0623 0.7168 0.1275 0.201 Uiso 1 1 calc R . . C58 C -0.0073(5) 0.8350(4) 0.1566(2) 0.1001(13) Uani 1 1 d . . . N59 N -0.0022(6) 0.8969(4) 0.1839(2) 0.1488(19) 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 0.04272(17) 0.04016(16) 0.04283(17) 0.00310(13) 0.00091(17) 0.00124(16) N2 0.0450(10) 0.0386(10) 0.0436(11) 0.0022(9) 0.0018(9) -0.0032(9) C3 0.0439(13) 0.0469(13) 0.0421(13) 0.0042(11) -0.0001(10) -0.0025(11) C4 0.0640(17) 0.0551(16) 0.0532(16) 0.0082(13) -0.0099(14) 0.0001(13) C5 0.085(2) 0.0454(15) 0.0638(18) 0.0130(13) -0.0075(15) 0.0092(14) C6 0.0768(19) 0.0406(14) 0.0605(17) 0.0019(12) -0.0023(14) 0.0026(13) C7 0.0503(13) 0.0412(12) 0.0486(15) 0.0007(11) 0.0016(11) -0.0001(11) N8 0.0536(12) 0.0467(11) 0.0391(11) 0.0011(9) -0.0021(9) -0.0013(9) N9 0.0550(12) 0.0396(10) 0.0475(11) -0.0005(9) 0.0015(9) 0.0016(10) C10 0.0590(17) 0.0482(14) 0.0593(17) -0.0052(13) 0.0033(13) -0.0020(13) C11 0.081(2) 0.0636(18) 0.0547(18) -0.0137(14) -0.0018(15) -0.0028(16) C12 0.0656(17) 0.0654(17) 0.0453(15) -0.0035(14) -0.0075(12) 0.0000(15) C13 0.106(3) 0.0461(15) 0.081(2) -0.0063(15) -0.0071(19) 0.0064(16) N14 0.0617(13) 0.0397(9) 0.0473(11) -0.0023(8) -0.0022(11) -0.0026(11) N15 0.0519(13) 0.0465(11) 0.0459(11) 0.0035(9) -0.0038(9) -0.0020(9) C16 0.0553(15) 0.0617(16) 0.0491(15) -0.0002(13) -0.0029(13) -0.0057(13) C17 0.079(2) 0.0666(18) 0.0496(17) -0.0100(14) -0.0066(15) -0.0111(16) C18 0.0797(18) 0.0507(13) 0.0571(15) -0.0100(12) 0.0011(18) -0.0061(17) C19 0.080(2) 0.085(2) 0.0580(18) 0.0034(17) -0.0147(16) 0.0024(18) N20 0.0493(12) 0.0490(11) 0.0511(12) -0.0025(10) -0.0026(10) 0.0036(10) C21 0.0543(17) 0.0635(17) 0.0593(17) -0.0111(14) -0.0093(14) 0.0112(13) C22 0.068(2) 0.071(2) 0.080(2) -0.0057(18) -0.0193(18) 0.0223(17) C23 0.102(3) 0.0572(18) 0.083(2) 0.0011(18) -0.027(2) 0.0142(19) C24 0.094(3) 0.0472(13) 0.0619(17) 0.0035(12) -0.0143(18) -0.0001(17) C25 0.0600(17) 0.0446(12) 0.0482(13) -0.0046(10) -0.0028(13) -0.0005(12) N26 0.0438(12) 0.0795(16) 0.0632(15) -0.0082(13) -0.0026(11) 0.0086(11) N27 0.0457(12) 0.0750(16) 0.0553(13) -0.0059(12) 0.0060(10) -0.0060(11) C28 0.0526(17) 0.092(2) 0.0604(18) -0.0146(16) 0.0071(14) -0.0158(16) C29 0.0538(18) 0.121(3) 0.082(2) -0.015(2) 0.0089(17) -0.005(2) C30 0.0488(17) 0.118(3) 0.083(2) -0.019(2) -0.0019(17) 0.0179(18) C31 0.078(2) 0.099(3) 0.079(2) 0.007(2) 0.0205(19) -0.022(2) N32 0.0573(13) 0.0432(11) 0.0499(13) 0.0027(10) 0.0033(10) -0.0050(10) N33 0.0467(11) 0.0459(10) 0.0463(11) -0.0023(10) 0.0022(9) -0.0008(10) C34 0.0483(14) 0.0605(16) 0.0465(14) -0.0137(12) 0.0009(11) -0.0053(12) C35 0.0593(17) 0.0708(19) 0.0585(17) -0.0110(15) 0.0146(14) -0.0132(15) C36 0.0688(19) 0.0581(17) 0.0568(17) -0.0013(14) 0.0125(14) -0.0168(15) C37 0.0497(15) 0.0780(19) 0.0659(19) 0.0009(15) -0.0009(13) 0.0084(14) B38 0.0590(19) 0.0441(15) 0.0574(19) -0.0027(14) 0.0045(14) 0.0059(14) F39 0.0774(14) 0.135(2) 0.1053(16) -0.0230(16) 0.0228(12) -0.0216(13) F40 0.0703(12) 0.0824(13) 0.1139(17) -0.0388(12) -0.0060(11) 0.0176(10) F41 0.215(3) 0.0614(11) 0.0856(14) 0.0130(11) -0.0114(17) 0.0128(16) F42 0.1099(16) 0.0889(14) 0.0657(12) -0.0177(10) -0.0076(11) 0.0066(12) C48 0.130(4) 0.120(4) 0.111(4) 0.020(3) 0.013(3) 0.034(3) C49 0.099(3) 0.109(3) 0.133(4) 0.023(3) 0.016(3) 0.021(3) N50 0.135(4) 0.154(4) 0.241(7) 0.091(5) 0.008(5) 0.024(4) C51 0.097(3) 0.078(2) 0.075(2) -0.0069(19) -0.002(2) -0.011(2) C52 0.100(3) 0.077(2) 0.073(2) 0.000(2) -0.013(2) -0.021(2) N53 0.171(4) 0.105(3) 0.126(4) 0.018(3) -0.056(3) -0.018(3) C54 0.169(5) 0.083(3) 0.095(3) -0.001(2) -0.008(3) 0.015(3) C55 0.137(4) 0.098(3) 0.078(3) 0.012(3) 0.005(3) -0.018(3) N56 0.196(5) 0.134(4) 0.108(3) 0.004(3) 0.013(3) -0.060(4) C57 0.189(6) 0.095(3) 0.118(4) 0.001(3) -0.046(4) -0.006(4) C58 0.111(3) 0.092(3) 0.098(3) 0.011(3) -0.017(3) 0.006(3) N59 0.193(5) 0.126(4) 0.128(4) -0.009(3) -0.002(4) 0.034(4) _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 N2 2.102(2) . ? Fe1 N20 2.112(2) . ? Fe1 N9 2.155(2) . ? Fe1 N27 2.160(2) . ? Fe1 N33 2.177(2) . ? Fe1 N15 2.184(2) . ? N2 C7 1.333(3) . ? N2 C3 1.342(3) . ? C3 C4 1.373(4) . ? C3 N8 1.398(3) . ? C4 C5 1.380(4) . ? C4 H4 0.9500 . ? C5 C6 1.387(4) . ? C5 H5 0.9500 . ? C6 C7 1.382(4) . ? C6 H6 0.9500 . ? C7 N14 1.394(3) . ? N8 C12 1.359(3) . ? N8 N9 1.386(3) . ? N9 C10 1.324(3) . ? C10 C11 1.409(5) . ? C10 C13 1.490(4) . ? C11 C12 1.355(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? N14 C18 1.363(3) . ? N14 N15 1.383(3) . ? N15 C16 1.331(4) . ? C16 C17 1.410(4) . ? C16 C19 1.479(4) . ? C17 C18 1.349(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? N20 C25 1.326(4) . ? N20 C21 1.338(4) . ? C21 C22 1.366(5) . ? C21 N26 1.412(4) . ? C22 C23 1.380(6) . ? C22 H22 0.9500 . ? C23 C24 1.368(6) . ? C23 H23 0.9500 . ? C24 C25 1.390(4) . ? C24 H24 0.9500 . ? C25 N32 1.398(4) . ? N26 C30 1.357(4) . ? N26 N27 1.371(4) . ? N27 C28 1.321(4) . ? C28 C29 1.406(5) . ? C28 C31 1.486(5) . ? C29 C30 1.355(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? N32 C36 1.354(4) . ? N32 N33 1.371(3) . ? N33 C34 1.328(3) . ? C34 C35 1.401(4) . ? C34 C37 1.493(4) . ? C35 C36 1.358(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? B38 F41 1.356(4) . ? B38 F39 1.371(4) . ? B38 F40 1.373(4) . ? B38 F42 1.378(4) . ? B43A F44A 1.390(15) . ? B43A F46A 1.390(16) . ? B43A F45A 1.392(15) . ? B43A F47A 1.411(15) . ? B43B F45B 1.327(13) . ? B43B F47B 1.395(13) . ? B43B F44B 1.400(13) . ? B43B F46B 1.426(13) . ? B43C F45C 1.355(15) . ? B43C F46C 1.404(14) . ? B43C F44C 1.406(14) . ? B43C F47C 1.455(16) . ? C48 C49 1.439(7) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 N50 1.117(7) . ? C51 C52 1.421(6) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 N53 1.120(5) . ? C54 C55 1.424(7) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 N56 1.122(6) . ? C57 C58 1.415(7) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 N59 1.118(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 N2 Fe1 N20 176.52(8) . . ? N2 Fe1 N9 74.69(8) . . ? N20 Fe1 N9 108.39(8) . . ? N2 Fe1 N27 107.49(9) . . ? N20 Fe1 N27 74.18(10) . . ? N9 Fe1 N27 94.23(9) . . ? N2 Fe1 N33 104.57(8) . . ? N20 Fe1 N33 73.83(8) . . ? N9 Fe1 N33 93.67(8) . . ? N27 Fe1 N33 147.94(9) . . ? N2 Fe1 N15 74.37(8) . . ? N20 Fe1 N15 102.55(8) . . ? N9 Fe1 N15 149.06(8) . . ? N27 Fe1 N15 94.81(9) . . ? N33 Fe1 N15 94.19(8) . . ? C7 N2 C3 119.0(2) . . ? C7 N2 Fe1 120.64(17) . . ? C3 N2 Fe1 120.32(16) . . ? N2 C3 C4 122.6(2) . . ? N2 C3 N8 112.7(2) . . ? C4 C3 N8 124.6(2) . . ? C3 C4 C5 117.2(3) . . ? C3 C4 H4 121.4 . . ? C5 C4 H4 121.4 . . ? C4 C5 C6 121.6(3) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C7 C6 C5 116.5(3) . . ? C7 C6 H6 121.7 . . ? C5 C6 H6 121.7 . . ? N2 C7 C6 123.0(2) . . ? N2 C7 N14 113.2(2) . . ? C6 C7 N14 123.8(2) . . ? C12 N8 N9 111.1(2) . . ? C12 N8 C3 130.2(2) . . ? N9 N8 C3 118.7(2) . . ? C10 N9 N8 105.1(2) . . ? C10 N9 Fe1 141.36(19) . . ? N8 N9 Fe1 113.46(14) . . ? N9 C10 C11 110.4(2) . . ? N9 C10 C13 120.7(3) . . ? C11 C10 C13 129.0(3) . . ? C12 C11 C10 106.8(3) . . ? C12 C11 H11 126.6 . . ? C10 C11 H11 126.6 . . ? C11 C12 N8 106.6(3) . . ? C11 C12 H12 126.7 . . ? N8 C12 H12 126.7 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C18 N14 N15 110.7(2) . . ? C18 N14 C7 130.2(2) . . ? N15 N14 C7 119.12(19) . . ? C16 N15 N14 105.2(2) . . ? C16 N15 Fe1 142.16(19) . . ? N14 N15 Fe1 112.60(15) . . ? N15 C16 C17 110.2(3) . . ? N15 C16 C19 121.7(3) . . ? C17 C16 C19 128.1(3) . . ? C18 C17 C16 106.7(3) . . ? C18 C17 H17 126.6 . . ? C16 C17 H17 126.6 . . ? C17 C18 N14 107.2(3) . . ? C17 C18 H18 126.4 . . ? N14 C18 H18 126.4 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 N20 C21 118.5(2) . . ? C25 N20 Fe1 120.55(18) . . ? C21 N20 Fe1 120.8(2) . . ? N20 C21 C22 123.6(3) . . ? N20 C21 N26 112.0(3) . . ? C22 C21 N26 124.4(3) . . ? C21 C22 C23 116.5(3) . . ? C21 C22 H22 121.8 . . ? C23 C22 H22 121.8 . . ? C24 C23 C22 121.9(3) . . ? C24 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C23 C24 C25 116.9(3) . . ? C23 C24 H24 121.6 . . ? C25 C24 H24 121.6 . . ? N20 C25 C24 122.7(3) . . ? N20 C25 N32 113.2(2) . . ? C24 C25 N32 124.2(3) . . ? C30 N26 N27 110.9(3) . . ? C30 N26 C21 130.2(3) . . ? N27 N26 C21 118.9(2) . . ? C28 N27 N26 105.9(3) . . ? C28 N27 Fe1 140.0(2) . . ? N26 N27 Fe1 114.03(18) . . ? N27 C28 C29 109.8(3) . . ? N27 C28 C31 120.5(3) . . ? C29 C28 C31 129.7(3) . . ? C30 C29 C28 106.8(3) . . ? C30 C29 H29 126.6 . . ? C28 C29 H29 126.6 . . ? C29 C30 N26 106.5(3) . . ? C29 C30 H30 126.7 . . ? N26 C30 H30 126.7 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C36 N32 N33 110.7(2) . . ? C36 N32 C25 130.6(2) . . ? N33 N32 C25 118.6(2) . . ? C34 N33 N32 105.8(2) . . ? C34 N33 Fe1 140.5(2) . . ? N32 N33 Fe1 113.62(15) . . ? N33 C34 C35 110.0(3) . . ? N33 C34 C37 121.1(3) . . ? C35 C34 C37 128.9(3) . . ? C36 C35 C34 106.5(3) . . ? C36 C35 H35 126.7 . . ? C34 C35 H35 126.7 . . ? N32 C36 C35 107.0(3) . . ? N32 C36 H36 126.5 . . ? C35 C36 H36 126.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? F41 B38 F39 110.5(3) . . ? F41 B38 F40 109.2(3) . . ? F39 B38 F40 108.0(3) . . ? F41 B38 F42 108.8(3) . . ? F39 B38 F42 110.0(3) . . ? F40 B38 F42 110.3(3) . . ? F44A B43A F46A 99.7(11) . . ? F44A B43A F45A 113.2(12) . . ? F46A B43A F45A 116.8(12) . . ? F44A B43A F47A 110.2(11) . . ? F46A B43A F47A 107.8(12) . . ? F45A B43A F47A 108.7(11) . . ? F45B B43B F47B 108.5(9) . . ? F45B B43B F44B 117.9(11) . . ? F47B B43B F44B 111.0(10) . . ? F45B B43B F46B 102.5(10) . . ? F47B B43B F46B 110.2(10) . . ? F44B B43B F46B 106.3(9) . . ? F45C B43C F46C 106.9(12) . . ? F45C B43C F44C 121.5(13) . . ? F46C B43C F44C 118.6(12) . . ? F45C B43C F47C 105.2(12) . . ? F46C B43C F47C 99.2(11) . . ? F44C B43C F47C 101.9(11) . . ? C49 C48 H48A 109.5 . . ? C49 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C49 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N50 C49 C48 178.9(7) . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N53 C52 C51 179.7(6) . . ? C55 C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C55 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N56 C55 C54 178.1(7) . . ? C58 C57 H57A 109.5 . . ? C58 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C58 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N59 C58 C57 176.9(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.453 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.123 #=END data_c:\datasets\leeds\je33bv~1\je33b2~1\je33b200 _database_code_depnum_ccdc_archive 'CCDC 278906' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-bis(3-methylpyrazol-1-yl)pyridine] ditetrafluoroborate tetrakis-acetonitrile solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Fe N10, 2[B F4], 4[C2 H3 N]' _chemical_formula_sum 'C34 H38 B2 F8 Fe N14' _chemical_formula_weight 872.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' 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 11.5476(1) _cell_length_b 13.6803(1) _cell_length_c 26.3236(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4158.46(6) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 80961 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 27.51 _exptl_crystal_description 'Square prism' _exptl_crystal_colour Brown _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.443 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.715 _exptl_absorpt_correction_T_max 0.902 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _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 'Nonius KappaCCD diffractometer' _diffrn_measurement_method 'Area detector scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 80961 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 27.51 _reflns_number_total 9499 _reflns_number_gt 8630 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 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 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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. Anion B43-F47 is disordered over three sites, labelled 'A' (occupancy 0.4) 'B' (occupancy 0.4) and 'C (occupancy 0.2). These were modelled using the refined restraints B---F = 1.39(2) and 1,3-F...F = 2.27(2)\%A. All non-H atoms except the disordered anion were refined anisotropically. All H atoms were placed in calculated positions and refined using a riding model, with the methyl group torsions allowed to refine freely. ; _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^)+(0.0664P)^2^+0.7215P] 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 -0.013(12) _refine_ls_number_reflns 9499 _refine_ls_number_parameters 556 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.0998 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.003 _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 0.25013(2) 0.218421(17) 0.178263(9) 0.03394(8) Uani 1 1 d . . . N2 N 0.30694(14) 0.09273(11) 0.21365(6) 0.0349(3) Uani 1 1 d . . . C3 C 0.34921(16) 0.09620(15) 0.26107(7) 0.0368(4) Uani 1 1 d . . . C4 C 0.3924(2) 0.01553(16) 0.28581(8) 0.0459(5) Uani 1 1 d . . . H4 H 0.4212 0.0195 0.3196 0.055 Uiso 1 1 calc R . . C5 C 0.3920(2) -0.07165(17) 0.25926(9) 0.0524(5) Uani 1 1 d . . . H5 H 0.4226 -0.1286 0.2750 0.063 Uiso 1 1 calc R . . C6 C 0.3481(2) -0.07826(16) 0.21016(9) 0.0488(5) Uani 1 1 d . . . H6 H 0.3470 -0.1383 0.1920 0.059 Uiso 1 1 calc R . . C7 C 0.30598(17) 0.00758(14) 0.18921(7) 0.0383(4) Uani 1 1 d . . . N8 N 0.34458(15) 0.19059(12) 0.28148(6) 0.0391(3) Uani 1 1 d . . . N9 N 0.30678(15) 0.26600(12) 0.25085(6) 0.0395(3) Uani 1 1 d . . . C10 C 0.3150(2) 0.34577(16) 0.27944(10) 0.0492(5) Uani 1 1 d . . . C11 C 0.3583(2) 0.32234(19) 0.32788(10) 0.0566(6) Uani 1 1 d . . . H11 H 0.3727 0.3666 0.3550 0.068 Uiso 1 1 calc R . . C12 C 0.3757(2) 0.22402(18) 0.32833(8) 0.0500(5) Uani 1 1 d . . . H12 H 0.4039 0.1861 0.3559 0.060 Uiso 1 1 calc R . . C13 C 0.2813(3) 0.44309(17) 0.25889(12) 0.0663(7) Uani 1 1 d . . . H13A H 0.2852 0.4417 0.2217 0.100 Uiso 1 1 calc R . . H13B H 0.3345 0.4930 0.2719 0.100 Uiso 1 1 calc R . . H13C H 0.2021 0.4586 0.2696 0.100 Uiso 1 1 calc R . . N14 N 0.25956(17) 0.01459(11) 0.14022(6) 0.0405(3) Uani 1 1 d . . . N15 N 0.22140(14) 0.10443(13) 0.12346(6) 0.0394(4) Uani 1 1 d . . . C16 C 0.18014(19) 0.08778(18) 0.07706(8) 0.0467(5) Uani 1 1 d . . . C17 C 0.1926(2) -0.01129(19) 0.06390(9) 0.0542(6) Uani 1 1 d . . . H17 H 0.1708 -0.0411 0.0328 0.065 Uiso 1 1 calc R . . C18 C 0.2420(2) -0.05580(15) 0.10446(8) 0.0512(5) Uani 1 1 d . . . H18 H 0.2607 -0.1232 0.1074 0.061 Uiso 1 1 calc R . . C19 C 0.1316(3) 0.1684(2) 0.04534(10) 0.0613(6) Uani 1 1 d . . . H19A H 0.0843 0.2114 0.0666 0.092 Uiso 1 1 calc R . . H19B H 0.0836 0.1406 0.0183 0.092 Uiso 1 1 calc R . . H19C H 0.1951 0.2060 0.0303 0.092 Uiso 1 1 calc R . . N20 N 0.19493(16) 0.34077(14) 0.13840(7) 0.0459(4) Uani 1 1 d . . . C21 C 0.0837(2) 0.3687(2) 0.13986(10) 0.0568(6) Uani 1 1 d . . . C22 C 0.0398(3) 0.4440(2) 0.11129(12) 0.0692(8) Uani 1 1 d . . . H22 H -0.0391 0.4632 0.1136 0.083 Uiso 1 1 calc R . . C23 C 0.1164(3) 0.4906(2) 0.07896(13) 0.0705(8) Uani 1 1 d . . . H23 H 0.0892 0.5425 0.0582 0.085 Uiso 1 1 calc R . . C24 C 0.2315(3) 0.46361(17) 0.07607(10) 0.0588(6) Uani 1 1 d . . . H24 H 0.2839 0.4955 0.0537 0.071 Uiso 1 1 calc R . . C25 C 0.2668(2) 0.38786(15) 0.10734(8) 0.0458(5) Uani 1 1 d . . . N26 N 0.01814(16) 0.31073(19) 0.17310(8) 0.0597(5) Uani 1 1 d . . . N27 N 0.07167(17) 0.23365(19) 0.19695(8) 0.0589(6) Uani 1 1 d . . . C28 C -0.0086(2) 0.1920(3) 0.22616(10) 0.0737(10) Uani 1 1 d . . . C29 C -0.1148(3) 0.2431(4) 0.22003(13) 0.0954(14) Uani 1 1 d . . . H29 H -0.1862 0.2282 0.2362 0.114 Uiso 1 1 calc R . . C30 C -0.0954(2) 0.3169(3) 0.18701(14) 0.0871(12) Uani 1 1 d . . . H30 H -0.1502 0.3638 0.1757 0.105 Uiso 1 1 calc R . . C31 C 0.0198(3) 0.1069(3) 0.25805(13) 0.0882(11) Uani 1 1 d . . . H31A H 0.0363 0.0505 0.2363 0.132 Uiso 1 1 calc R . . H31B H -0.0460 0.0919 0.2802 0.132 Uiso 1 1 calc R . . H31C H 0.0879 0.1218 0.2788 0.132 Uiso 1 1 calc R . . N32 N 0.38053(16) 0.35262(13) 0.11027(7) 0.0446(4) Uani 1 1 d . . . N33 N 0.40143(15) 0.27276(14) 0.14076(7) 0.0431(4) Uani 1 1 d . . . C34 C 0.51540(18) 0.25805(18) 0.13815(8) 0.0481(5) Uani 1 1 d . . . C35 C 0.5672(2) 0.3280(2) 0.10659(10) 0.0570(6) Uani 1 1 d . . . H35 H 0.6471 0.3330 0.0984 0.068 Uiso 1 1 calc R . . C36 C 0.4805(2) 0.38753(19) 0.08989(9) 0.0538(6) Uani 1 1 d . . . H36 H 0.4883 0.4427 0.0682 0.065 Uiso 1 1 calc R . . C37 C 0.5714(2) 0.1768(2) 0.16685(10) 0.0588(6) Uani 1 1 d . . . H37A H 0.5561 0.1848 0.2032 0.088 Uiso 1 1 calc R . . H37B H 0.6552 0.1780 0.1609 0.088 Uiso 1 1 calc R . . H37C H 0.5398 0.1141 0.1553 0.088 Uiso 1 1 calc R . . B38 B 0.3225(2) 0.64969(18) 0.16475(9) 0.0434(5) Uani 1 1 d . . . F39 F 0.21675(15) 0.60530(17) 0.17296(8) 0.0854(5) Uani 1 1 d . . . F40 F 0.39716(13) 0.58230(12) 0.14403(7) 0.0682(4) Uani 1 1 d . . . F41 F 0.3108(3) 0.72689(13) 0.13257(7) 0.1008(7) Uani 1 1 d . . . F42 F 0.36606(16) 0.68356(12) 0.21085(6) 0.0671(4) Uani 1 1 d . . . B43A B 0.2355(10) 0.0437(10) 0.4223(4) 0.051(7) Uiso 0.40 1 d PD A 1 F44A F 0.1973(5) 0.0758(4) 0.37254(19) 0.0614(16) Uiso 0.40 1 d PD A 1 F45A F 0.2172(5) -0.0520(4) 0.4291(2) 0.0779(17) Uiso 0.40 1 d PD A 1 F46A F 0.1730(6) 0.1118(5) 0.4511(2) 0.0887(18) Uiso 0.40 1 d PD A 1 F47A F 0.3543(4) 0.0682(4) 0.4251(2) 0.0691(14) Uiso 0.40 1 d PD A 1 B43B B 0.2319(13) 0.0521(11) 0.4231(6) 0.060(12) Uiso 0.40 1 d PD B 2 F44B F 0.2115(6) 0.0494(6) 0.3712(2) 0.0545(17) Uiso 0.40 1 d PD B 2 F45B F 0.2352(5) -0.0415(3) 0.4441(2) 0.0594(11) Uiso 0.40 1 d PD B 2 F46B F 0.1344(5) 0.0914(5) 0.4476(2) 0.0641(15) Uiso 0.40 1 d PD B 2 F47B F 0.3368(5) 0.0951(5) 0.4353(2) 0.0701(14) Uiso 0.40 1 d PD B 2 B43C B 0.2353(12) 0.0651(10) 0.4243(4) 0.029(5) Uiso 0.20 1 d PD C 3 F44C F 0.2242(10) 0.0269(8) 0.3746(3) 0.063(4) Uiso 0.20 1 d PD C 3 F45C F 0.3006(9) 0.1428(8) 0.4339(4) 0.086(3) Uiso 0.20 1 d PD C 3 F46C F 0.1385(8) 0.0665(7) 0.4560(4) 0.055(3) Uiso 0.20 1 d PD C 3 F47C F 0.2917(12) -0.0186(9) 0.4505(5) 0.109(4) Uiso 0.20 1 d PD C 3 C48 C 0.8504(4) 0.0479(3) 0.10197(15) 0.0906(10) Uani 1 1 d . . . H48A H 0.9125 0.0072 0.0880 0.136 Uiso 1 1 calc R . . H48B H 0.7819 0.0073 0.1083 0.136 Uiso 1 1 calc R . . H48C H 0.8763 0.0773 0.1339 0.136 Uiso 1 1 calc R . . C49 C 0.8216(3) 0.1241(3) 0.06617(16) 0.0871(10) Uani 1 1 d . . . N50 N 0.7999(4) 0.1833(3) 0.0383(2) 0.1385(17) Uani 1 1 d . . . C51 C 0.4604(3) 0.1274(2) 0.02117(11) 0.0640(7) Uani 1 1 d . . . H51A H 0.5237 0.1615 0.0038 0.096 Uiso 1 1 calc R . . H51B H 0.4185 0.1736 0.0429 0.096 Uiso 1 1 calc R . . H51C H 0.4072 0.1001 -0.0041 0.096 Uiso 1 1 calc R . . C52 C 0.5066(3) 0.0506(2) 0.05151(11) 0.0645(7) Uani 1 1 d . . . N53 N 0.5434(4) -0.0095(2) 0.07569(14) 0.1050(11) Uani 1 1 d . . . C54 C 0.4843(4) 0.7584(3) 0.03304(14) 0.0895(10) Uani 1 1 d . . . H54A H 0.4402 0.8112 0.0169 0.134 Uiso 1 1 calc R . . H54B H 0.5669 0.7668 0.0257 0.134 Uiso 1 1 calc R . . H54C H 0.4720 0.7603 0.0699 0.134 Uiso 1 1 calc R . . C55 C 0.4457(4) 0.6657(3) 0.01339(13) 0.0821(9) Uani 1 1 d . . . N56 N 0.4170(4) 0.5927(3) -0.00161(14) 0.1148(13) Uani 1 1 d . . . C57 C -0.0073(5) 0.7528(3) 0.12147(18) 0.1139(16) Uani 1 1 d . . . H57A H 0.0161 0.7767 0.0879 0.171 Uiso 1 1 calc R . . H57B H -0.0854 0.7252 0.1194 0.171 Uiso 1 1 calc R . . H57C H 0.0470 0.7023 0.1328 0.171 Uiso 1 1 calc R . . C58 C -0.0066(3) 0.8320(3) 0.15688(15) 0.0806(9) Uani 1 1 d . . . N59 N -0.0015(4) 0.8948(3) 0.18365(17) 0.1214(13) 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 0.03417(12) 0.03396(12) 0.03368(13) 0.00144(9) 0.00076(12) 0.00026(12) N2 0.0368(7) 0.0324(7) 0.0353(8) 0.0024(6) 0.0005(6) -0.0013(6) C3 0.0358(9) 0.0392(10) 0.0355(9) 0.0016(8) 0.0013(7) -0.0026(7) C4 0.0521(11) 0.0457(11) 0.0398(10) 0.0041(9) -0.0053(9) 0.0014(9) C5 0.0651(14) 0.0400(11) 0.0521(13) 0.0081(9) -0.0082(10) 0.0063(10) C6 0.0625(13) 0.0334(10) 0.0505(12) 0.0004(9) -0.0026(10) 0.0013(9) C7 0.0415(10) 0.0338(9) 0.0397(10) 0.0010(7) 0.0018(8) -0.0015(7) N8 0.0430(8) 0.0392(8) 0.0350(8) -0.0011(6) -0.0009(7) -0.0023(7) N9 0.0434(9) 0.0334(8) 0.0417(8) -0.0005(7) 0.0041(7) -0.0007(7) C10 0.0486(12) 0.0397(10) 0.0592(13) -0.0097(10) 0.0081(10) -0.0044(9) C11 0.0616(13) 0.0577(13) 0.0506(13) -0.0182(11) 0.0003(11) -0.0041(11) C12 0.0537(12) 0.0588(13) 0.0374(10) -0.0083(10) -0.0028(9) -0.0013(10) C13 0.0814(19) 0.0383(11) 0.0793(18) -0.0102(11) 0.0027(14) 0.0026(11) N14 0.0486(9) 0.0347(7) 0.0381(8) -0.0020(6) -0.0022(8) -0.0016(8) N15 0.0401(9) 0.0409(8) 0.0374(8) 0.0033(7) -0.0021(6) -0.0013(6) C16 0.0435(11) 0.0563(12) 0.0402(11) 0.0028(9) -0.0027(9) -0.0056(9) C17 0.0634(14) 0.0594(14) 0.0399(11) -0.0063(10) -0.0048(10) -0.0097(11) C18 0.0658(13) 0.0428(10) 0.0449(10) -0.0083(8) 0.0003(12) -0.0066(12) C19 0.0668(15) 0.0710(16) 0.0462(13) 0.0085(12) -0.0129(11) 0.0013(13) N20 0.0407(9) 0.0520(10) 0.0452(9) -0.0109(8) -0.0013(8) 0.0023(8) C21 0.0445(12) 0.0699(16) 0.0561(14) -0.0198(12) -0.0056(10) 0.0074(11) C22 0.0587(15) 0.0700(17) 0.0789(19) -0.0184(15) -0.0178(14) 0.0207(13) C23 0.0799(19) 0.0528(14) 0.0789(19) -0.0110(14) -0.0240(16) 0.0125(13) C24 0.0735(17) 0.0442(11) 0.0586(13) -0.0046(9) -0.0124(13) 0.0022(11) C25 0.0492(12) 0.0439(10) 0.0443(10) -0.0117(8) -0.0022(9) -0.0004(9) N26 0.0357(9) 0.0880(16) 0.0555(12) -0.0156(11) 0.0004(8) 0.0036(9) N27 0.0456(10) 0.0856(15) 0.0457(10) -0.0170(11) 0.0104(8) -0.0201(10) C28 0.0531(14) 0.121(3) 0.0471(13) -0.0220(15) 0.0123(11) -0.0381(16) C29 0.0450(14) 0.169(4) 0.072(2) -0.039(2) 0.0148(14) -0.027(2) C30 0.0369(12) 0.150(3) 0.074(2) -0.040(2) 0.0058(12) 0.0002(16) C31 0.079(2) 0.125(3) 0.0606(17) -0.0010(19) 0.0229(15) -0.044(2) N32 0.0455(9) 0.0434(9) 0.0450(10) -0.0049(8) 0.0030(7) -0.0040(8) N33 0.0384(8) 0.0488(9) 0.0421(9) -0.0109(8) 0.0002(7) 0.0028(7) C34 0.0392(10) 0.0624(14) 0.0427(11) -0.0206(10) -0.0003(8) 0.0010(9) C35 0.0461(11) 0.0710(16) 0.0540(13) -0.0184(12) 0.0107(10) -0.0115(11) C36 0.0555(13) 0.0555(13) 0.0505(13) -0.0098(11) 0.0113(10) -0.0126(10) C37 0.0394(11) 0.0801(17) 0.0568(14) -0.0082(12) -0.0015(10) 0.0101(11) B38 0.0474(12) 0.0371(11) 0.0458(13) -0.0027(9) 0.0041(10) 0.0042(9) F39 0.0585(9) 0.1148(15) 0.0828(11) -0.0224(11) 0.0157(8) -0.0163(9) F40 0.0544(8) 0.0672(9) 0.0830(11) -0.0296(8) -0.0035(7) 0.0124(7) F41 0.183(2) 0.0538(9) 0.0656(10) 0.0089(8) -0.0104(12) 0.0152(12) F42 0.0808(10) 0.0695(9) 0.0510(8) -0.0141(7) -0.0046(7) 0.0047(8) C48 0.098(2) 0.092(2) 0.081(2) 0.0135(19) 0.0114(19) 0.025(2) C49 0.072(2) 0.082(2) 0.108(3) 0.017(2) 0.0121(19) 0.0145(17) N50 0.109(3) 0.122(3) 0.184(4) 0.070(3) 0.004(3) 0.022(2) C51 0.0731(17) 0.0642(16) 0.0547(14) -0.0033(12) -0.0014(12) -0.0075(13) C52 0.0779(18) 0.0610(15) 0.0545(14) -0.0012(13) -0.0057(13) -0.0173(14) N53 0.137(3) 0.0792(19) 0.099(2) 0.0146(19) -0.041(2) -0.0112(19) C54 0.127(3) 0.0671(19) 0.074(2) 0.0051(16) -0.005(2) 0.0098(19) C55 0.102(3) 0.085(2) 0.0595(17) 0.0107(16) 0.0049(17) -0.012(2) N56 0.153(4) 0.102(2) 0.090(2) 0.001(2) 0.007(2) -0.039(3) C57 0.151(4) 0.080(2) 0.110(3) -0.001(2) -0.043(3) -0.009(3) C58 0.082(2) 0.073(2) 0.087(2) 0.0109(18) -0.0138(18) 0.0036(17) N59 0.152(4) 0.102(3) 0.110(3) -0.011(2) -0.001(3) 0.025(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.0627(16) . ? Fe1 N20 2.076(2) . ? Fe1 N9 2.1220(17) . ? Fe1 N27 2.129(2) . ? Fe1 N33 2.1401(18) . ? Fe1 N15 2.1501(17) . ? N2 C7 1.331(3) . ? N2 C3 1.341(3) . ? C3 C4 1.375(3) . ? C3 N8 1.400(3) . ? C4 C5 1.382(3) . ? C5 C6 1.391(3) . ? C6 C7 1.385(3) . ? C7 N14 1.400(3) . ? N8 C12 1.364(3) . ? N8 N9 1.380(2) . ? N9 C10 1.329(3) . ? C10 C11 1.407(4) . ? C10 C13 1.489(4) . ? C11 C12 1.360(4) . ? N14 C18 1.362(3) . ? N14 N15 1.378(2) . ? N15 C16 1.331(3) . ? C16 C17 1.406(4) . ? C16 C19 1.492(3) . ? C17 C18 1.355(3) . ? N20 C25 1.331(3) . ? N20 C21 1.341(3) . ? C21 C22 1.373(4) . ? C21 N26 1.402(4) . ? C22 C23 1.383(5) . ? C23 C24 1.381(4) . ? C24 C25 1.385(3) . ? C25 N32 1.401(3) . ? N26 C30 1.364(3) . ? N26 N27 1.374(4) . ? N27 C28 1.332(3) . ? C28 C29 1.422(5) . ? C28 C31 1.471(5) . ? C29 C30 1.350(6) . ? N32 C36 1.359(3) . ? N32 N33 1.377(3) . ? N33 C34 1.333(3) . ? C34 C35 1.401(4) . ? C34 C37 1.492(4) . ? C35 C36 1.364(4) . ? B38 F41 1.361(3) . ? B38 F40 1.375(3) . ? B38 F39 1.380(3) . ? B38 F42 1.393(3) . ? B43A F45A 1.339(13) . ? B43A F46A 1.402(13) . ? B43A F47A 1.415(12) . ? B43A F44A 1.449(12) . ? B43B F47B 1.384(14) . ? B43B F44B 1.387(14) . ? B43B F45B 1.396(15) . ? B43B F46B 1.405(15) . ? B43C F45C 1.328(14) . ? B43C F46C 1.395(13) . ? B43C F44C 1.416(13) . ? B43C F47C 1.486(14) . ? C48 C49 1.445(5) . ? C49 N50 1.121(5) . ? C51 C52 1.424(4) . ? C52 N53 1.123(4) . ? C54 C55 1.440(5) . ? C55 N56 1.123(5) . ? C57 C58 1.429(6) . ? C58 N59 1.113(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 N2 Fe1 N20 176.48(7) . . ? N2 Fe1 N9 75.58(6) . . ? N20 Fe1 N9 107.61(7) . . ? N2 Fe1 N27 106.57(8) . . ? N20 Fe1 N27 74.97(9) . . ? N9 Fe1 N27 93.46(7) . . ? N2 Fe1 N33 103.78(7) . . ? N20 Fe1 N33 74.78(7) . . ? N9 Fe1 N33 93.28(7) . . ? N27 Fe1 N33 149.64(9) . . ? N2 Fe1 N15 75.37(6) . . ? N20 Fe1 N15 101.44(7) . . ? N9 Fe1 N15 150.95(6) . . ? N27 Fe1 N15 94.40(7) . . ? N33 Fe1 N15 93.93(6) . . ? C7 N2 C3 118.94(17) . . ? C7 N2 Fe1 120.58(13) . . ? C3 N2 Fe1 120.43(13) . . ? N2 C3 C4 122.99(19) . . ? N2 C3 N8 112.09(17) . . ? C4 C3 N8 124.92(18) . . ? C3 C4 C5 116.9(2) . . ? C4 C5 C6 121.8(2) . . ? C7 C6 C5 116.3(2) . . ? N2 C7 C6 123.14(19) . . ? N2 C7 N14 112.86(16) . . ? C6 C7 N14 124.00(18) . . ? C12 N8 N9 111.15(17) . . ? C12 N8 C3 130.29(19) . . ? N9 N8 C3 118.52(16) . . ? C10 N9 N8 105.10(17) . . ? C10 N9 Fe1 141.61(16) . . ? N8 N9 Fe1 113.22(12) . . ? N9 C10 C11 110.6(2) . . ? N9 C10 C13 120.7(2) . . ? C11 C10 C13 128.7(2) . . ? C12 C11 C10 106.6(2) . . ? C11 C12 N8 106.6(2) . . ? C18 N14 N15 111.20(17) . . ? C18 N14 C7 130.19(17) . . ? N15 N14 C7 118.59(15) . . ? C16 N15 N14 104.82(17) . . ? C16 N15 Fe1 142.67(15) . . ? N14 N15 Fe1 112.50(11) . . ? N15 C16 C17 110.7(2) . . ? N15 C16 C19 121.4(2) . . ? C17 C16 C19 127.8(2) . . ? C18 C17 C16 106.4(2) . . ? C17 C18 N14 106.8(2) . . ? C25 N20 C21 118.5(2) . . ? C25 N20 Fe1 120.62(15) . . ? C21 N20 Fe1 120.62(18) . . ? N20 C21 C22 123.5(3) . . ? N20 C21 N26 112.0(2) . . ? C22 C21 N26 124.5(2) . . ? C21 C22 C23 116.5(3) . . ? C24 C23 C22 121.8(3) . . ? C23 C24 C25 116.8(3) . . ? N20 C25 C24 122.9(2) . . ? N20 C25 N32 112.57(19) . . ? C24 C25 N32 124.5(2) . . ? C30 N26 N27 110.9(3) . . ? C30 N26 C21 130.6(3) . . ? N27 N26 C21 118.44(19) . . ? C28 N27 N26 106.2(2) . . ? C28 N27 Fe1 139.9(2) . . ? N26 N27 Fe1 113.89(15) . . ? N27 C28 C29 108.9(3) . . ? N27 C28 C31 120.9(3) . . ? C29 C28 C31 130.3(3) . . ? C30 C29 C28 107.3(3) . . ? C29 C30 N26 106.6(3) . . ? C36 N32 N33 111.10(19) . . ? C36 N32 C25 130.8(2) . . ? N33 N32 C25 118.00(17) . . ? C34 N33 N32 105.24(19) . . ? C34 N33 Fe1 141.01(18) . . ? N32 N33 Fe1 113.66(12) . . ? N33 C34 C35 110.4(2) . . ? N33 C34 C37 121.0(2) . . ? C35 C34 C37 128.6(2) . . ? C36 C35 C34 106.6(2) . . ? N32 C36 C35 106.6(2) . . ? F41 B38 F40 109.6(2) . . ? F41 B38 F39 110.6(2) . . ? F40 B38 F39 108.8(2) . . ? F41 B38 F42 108.7(2) . . ? F40 B38 F42 110.0(2) . . ? F39 B38 F42 109.2(2) . . ? F45A B43A F46A 119.7(9) . . ? F45A B43A F47A 112.2(9) . . ? F46A B43A F47A 108.3(9) . . ? F45A B43A F44A 111.7(9) . . ? F46A B43A F44A 97.6(8) . . ? F47A B43A F44A 105.8(8) . . ? F47B B43B F44B 113.0(11) . . ? F47B B43B F45B 105.9(11) . . ? F44B B43B F45B 111.7(11) . . ? F47B B43B F46B 115.6(12) . . ? F44B B43B F46B 109.0(11) . . ? F45B B43B F46B 101.0(10) . . ? F45C B43C F46C 109.3(11) . . ? F45C B43C F44C 121.5(11) . . ? F46C B43C F44C 119.1(11) . . ? F45C B43C F47C 106.3(11) . . ? F46C B43C F47C 94.9(9) . . ? F44C B43C F47C 100.6(10) . . ? N50 C49 C48 179.6(5) . . ? N53 C52 C51 179.4(4) . . ? N56 C55 C54 179.0(5) . . ? N59 C58 C57 177.0(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.298 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.058 #=END data_c:\datasets\leeds\je33bv~1\je33b1~2\je33b150 _database_code_depnum_ccdc_archive 'CCDC 278907' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-bis(3-methylpyrazol-1-yl)pyridine] ditetrafluoroborate tetrakis-acetonitrile solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Fe N10, 2[B F4], 4[C2 H3 N]' _chemical_formula_sum 'C34 H38 B2 F8 Fe N14' _chemical_formula_weight 872.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' 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 11.3871(1) _cell_length_b 13.6181(1) _cell_length_c 26.2355(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4068.36(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 67255 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 27.49 _exptl_crystal_description 'Square prism' _exptl_crystal_colour Brown _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.453 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.630 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_ambient_temperature 150(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 diffractometer' _diffrn_measurement_method 'Area detector scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67255 _diffrn_reflns_av_R_equivalents 0.0723 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 27.49 _reflns_number_total 9331 _reflns_number_gt 7497 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 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 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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. Anion B43-F47 is disordered over two sites, labelled 'A' (occupancy 0.6) and 'B' (occupancy 0.4). These were modelled using the refined restraints B---F = 1.38(2) and 1,3-F...F = 2.25(2)\%A. All non-H atoms except the minor disorder orientation were refined anisotropically. All H atoms were placed in calculated positions and refined using a riding model, with the methyl group torsions allowed to refine freely. ; _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^)+(0.0558P)^2^+1.1338P] 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 -0.017(14) _refine_ls_number_reflns 9331 _refine_ls_number_parameters 561 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1074 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 1.026 _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 0.25016(3) 0.21251(2) 0.178581(11) 0.02633(9) Uani 1 1 d . . . N2 N 0.30583(18) 0.09244(14) 0.21275(7) 0.0273(4) Uani 1 1 d . . . C3 C 0.3486(2) 0.09610(18) 0.26024(9) 0.0288(5) Uani 1 1 d . . . C4 C 0.3922(2) 0.01497(19) 0.28524(10) 0.0362(6) Uani 1 1 d . . . H4 H 0.4215 0.0191 0.3191 0.043 Uiso 1 1 calc R . . C5 C 0.3913(3) -0.07317(19) 0.25853(11) 0.0397(6) Uani 1 1 d . . . H5 H 0.4221 -0.1304 0.2743 0.048 Uiso 1 1 calc R . . C6 C 0.3466(2) -0.07976(18) 0.20950(10) 0.0366(6) Uani 1 1 d . . . H6 H 0.3451 -0.1402 0.1914 0.044 Uiso 1 1 calc R . . C7 C 0.3041(2) 0.00650(17) 0.18829(9) 0.0294(5) Uani 1 1 d . . . N8 N 0.34329(18) 0.19138(14) 0.27996(8) 0.0307(4) Uani 1 1 d . . . N9 N 0.30375(19) 0.26506(14) 0.24788(8) 0.0308(4) Uani 1 1 d . . . C10 C 0.3106(2) 0.34724(19) 0.27542(11) 0.0390(6) Uani 1 1 d . . . C11 C 0.3544(3) 0.3273(2) 0.32414(12) 0.0460(7) Uani 1 1 d . . . H11 H 0.3680 0.3735 0.3506 0.055 Uiso 1 1 calc R . . C12 C 0.3740(2) 0.2282(2) 0.32618(10) 0.0394(6) Uani 1 1 d . . . H12 H 0.4033 0.1921 0.3544 0.047 Uiso 1 1 calc R . . C13 C 0.2742(3) 0.44369(19) 0.25305(13) 0.0529(8) Uani 1 1 d . . . H13A H 0.3013 0.4477 0.2177 0.079 Uiso 1 1 calc R . . H13B H 0.3090 0.4973 0.2729 0.079 Uiso 1 1 calc R . . H13C H 0.1884 0.4492 0.2540 0.079 Uiso 1 1 calc R . . N14 N 0.2567(2) 0.01501(13) 0.13946(7) 0.0311(4) Uani 1 1 d . . . N15 N 0.21964(18) 0.10676(14) 0.12372(8) 0.0304(5) Uani 1 1 d . . . C16 C 0.1773(2) 0.0932(2) 0.07668(10) 0.0359(6) Uani 1 1 d . . . C17 C 0.1873(3) -0.0065(2) 0.06276(10) 0.0414(7) Uani 1 1 d . . . H17 H 0.1635 -0.0352 0.0314 0.050 Uiso 1 1 calc R . . C18 C 0.2375(3) -0.05354(18) 0.10288(9) 0.0381(6) Uani 1 1 d . . . H18 H 0.2558 -0.1215 0.1049 0.046 Uiso 1 1 calc R . . C19 C 0.1291(3) 0.1747(2) 0.04553(11) 0.0475(7) Uani 1 1 d . . . H19A H 0.0714 0.2115 0.0657 0.071 Uiso 1 1 calc R . . H19B H 0.0910 0.1478 0.0151 0.071 Uiso 1 1 calc R . . H19C H 0.1930 0.2187 0.0353 0.071 Uiso 1 1 calc R . . N20 N 0.1954(2) 0.32834(17) 0.14137(8) 0.0373(5) Uani 1 1 d . . . C21 C 0.0813(3) 0.3538(2) 0.14292(12) 0.0470(7) Uani 1 1 d . . . C22 C 0.0362(3) 0.4301(3) 0.11472(14) 0.0567(9) Uani 1 1 d . . . H22 H -0.0440 0.4486 0.1173 0.068 Uiso 1 1 calc R . . C23 C 0.1125(3) 0.4787(2) 0.08251(14) 0.0577(9) Uani 1 1 d . . . H23 H 0.0831 0.5309 0.0622 0.069 Uiso 1 1 calc R . . C24 C 0.2313(3) 0.4540(2) 0.07872(12) 0.0478(7) Uani 1 1 d . . . H24 H 0.2835 0.4869 0.0562 0.057 Uiso 1 1 calc R . . C25 C 0.2674(3) 0.37758(18) 0.11027(10) 0.0367(6) Uani 1 1 d . . . N26 N 0.0190(2) 0.2924(2) 0.17661(10) 0.0536(7) Uani 1 1 d . . . N27 N 0.0793(2) 0.2171(2) 0.19999(9) 0.0473(6) Uani 1 1 d . . . C28 C 0.0007(3) 0.1719(3) 0.23036(12) 0.0654(11) Uani 1 1 d . . . C29 C -0.1095(3) 0.2186(4) 0.22566(14) 0.0810(13) Uani 1 1 d . . . H29 H -0.1798 0.2008 0.2428 0.097 Uiso 1 1 calc R . . C30 C -0.0964(3) 0.2940(4) 0.19201(14) 0.0730(12) Uani 1 1 d . . . H30 H -0.1554 0.3388 0.1813 0.088 Uiso 1 1 calc R . . C31 C 0.0343(4) 0.0875(3) 0.26300(13) 0.0741(13) Uani 1 1 d . . . H31A H 0.0495 0.0300 0.2415 0.111 Uiso 1 1 calc R . . H31B H -0.0297 0.0727 0.2867 0.111 Uiso 1 1 calc R . . H31C H 0.1054 0.1039 0.2823 0.111 Uiso 1 1 calc R . . N32 N 0.3825(2) 0.34131(16) 0.11326(9) 0.0379(5) Uani 1 1 d . . . N33 N 0.4010(2) 0.26002(16) 0.14369(8) 0.0360(5) Uani 1 1 d . . . C34 C 0.5166(2) 0.2439(2) 0.14201(10) 0.0402(7) Uani 1 1 d . . . C35 C 0.5709(3) 0.3143(2) 0.11046(11) 0.0485(8) Uani 1 1 d . . . H35 H 0.6522 0.3185 0.1026 0.058 Uiso 1 1 calc R . . C36 C 0.4847(3) 0.3751(2) 0.09342(11) 0.0453(7) Uani 1 1 d . . . H36 H 0.4943 0.4305 0.0718 0.054 Uiso 1 1 calc R . . C37 C 0.5714(3) 0.1624(2) 0.17067(12) 0.0498(8) Uani 1 1 d . . . H37A H 0.5627 0.1742 0.2073 0.075 Uiso 1 1 calc R . . H37B H 0.6550 0.1586 0.1621 0.075 Uiso 1 1 calc R . . H37C H 0.5329 0.1005 0.1616 0.075 Uiso 1 1 calc R . . B38 B 0.3222(3) 0.6496(2) 0.16129(11) 0.0333(6) Uani 1 1 d . . . F39 F 0.21422(17) 0.60682(16) 0.16924(8) 0.0685(6) Uani 1 1 d . . . F40 F 0.39885(15) 0.58132(12) 0.14070(7) 0.0506(4) Uani 1 1 d . . . F41 F 0.3126(3) 0.72852(13) 0.12942(7) 0.0806(7) Uani 1 1 d . . . F42 F 0.36597(16) 0.68238(12) 0.20818(6) 0.0479(4) Uani 1 1 d . . . B43A B 0.2381(9) 0.0468(8) 0.4224(4) 0.038(5) Uani 0.60 1 d PD A 1 F44A F 0.2044(4) 0.0635(4) 0.37157(15) 0.0506(10) Uani 0.60 1 d PD A 1 F45A F 0.2328(4) -0.0534(3) 0.43500(16) 0.0589(9) Uani 0.60 1 d PD A 1 F46A F 0.1564(7) 0.0917(6) 0.4521(3) 0.083(2) Uani 0.60 1 d PD A 1 F47A F 0.3500(3) 0.0788(3) 0.42994(15) 0.0671(10) Uani 0.60 1 d PD A 1 B43B B 0.2313(15) 0.0521(13) 0.4243(7) 0.049(9) Uiso 0.40 1 d PD B 2 F44B F 0.2183(8) 0.0330(5) 0.3723(3) 0.056(3) Uiso 0.40 1 d PD B 2 F45B F 0.2757(7) -0.0327(6) 0.4449(3) 0.086(3) Uiso 0.40 1 d PD B 2 F46B F 0.1286(9) 0.0788(9) 0.4477(5) 0.061(3) Uiso 0.40 1 d PD B 2 F47B F 0.3118(7) 0.1258(5) 0.4337(3) 0.092(2) Uiso 0.40 1 d PD B 2 C48 C 0.8521(4) 0.0425(3) 0.10217(15) 0.0674(10) Uani 1 1 d . . . H48A H 0.9183 0.0044 0.0888 0.101 Uiso 1 1 calc R . . H48B H 0.7839 -0.0006 0.1064 0.101 Uiso 1 1 calc R . . H48C H 0.8736 0.0709 0.1352 0.101 Uiso 1 1 calc R . . C49 C 0.8234(3) 0.1202(3) 0.06697(17) 0.0691(10) Uani 1 1 d . . . N50 N 0.8008(4) 0.1804(3) 0.0382(2) 0.1126(16) Uani 1 1 d . . . C51 C 0.4571(3) 0.1257(2) 0.02147(11) 0.0480(7) Uani 1 1 d . . . H51A H 0.5209 0.1605 0.0041 0.072 Uiso 1 1 calc R . . H51B H 0.4138 0.1717 0.0432 0.072 Uiso 1 1 calc R . . H51C H 0.4037 0.0975 -0.0039 0.072 Uiso 1 1 calc R . . C52 C 0.5056(3) 0.0480(2) 0.05255(12) 0.0498(8) Uani 1 1 d . . . N53 N 0.5445(4) -0.0131(2) 0.07663(14) 0.0802(11) Uani 1 1 d . . . C54 C 0.4880(4) 0.7583(3) 0.03143(15) 0.0748(11) Uani 1 1 d . . . H54A H 0.4449 0.8112 0.0143 0.112 Uiso 1 1 calc R . . H54B H 0.5717 0.7634 0.0232 0.112 Uiso 1 1 calc R . . H54C H 0.4774 0.7641 0.0684 0.112 Uiso 1 1 calc R . . C55 C 0.4439(4) 0.6649(3) 0.01451(15) 0.0712(11) Uani 1 1 d . . . N56 N 0.4125(5) 0.5898(3) 0.00035(15) 0.1048(15) Uani 1 1 d . . . C57 C -0.0115(5) 0.7494(3) 0.12087(17) 0.0868(14) Uani 1 1 d . . . H57A H 0.0047 0.7755 0.0868 0.130 Uiso 1 1 calc R . . H57B H -0.0895 0.7190 0.1212 0.130 Uiso 1 1 calc R . . H57C H 0.0478 0.7002 0.1297 0.130 Uiso 1 1 calc R . . C58 C -0.0082(3) 0.8267(3) 0.15671(16) 0.0619(9) Uani 1 1 d . . . N59 N -0.0028(4) 0.8890(3) 0.18492(16) 0.0943(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 0.02723(16) 0.02658(14) 0.02518(15) -0.00010(12) 0.00068(16) -0.00046(16) N2 0.0281(10) 0.0266(9) 0.0270(10) 0.0006(8) -0.0001(9) -0.0011(8) C3 0.0276(13) 0.0304(12) 0.0285(12) 0.0001(10) 0.0004(10) -0.0012(10) C4 0.0386(15) 0.0406(14) 0.0294(13) 0.0052(11) -0.0033(11) 0.0015(12) C5 0.0468(16) 0.0308(13) 0.0413(15) 0.0041(11) -0.0050(13) 0.0033(12) C6 0.0456(16) 0.0288(12) 0.0352(14) -0.0006(10) -0.0011(12) 0.0022(11) C7 0.0290(12) 0.0282(11) 0.0308(13) 0.0010(10) 0.0009(10) -0.0005(10) N8 0.0322(11) 0.0309(11) 0.0290(10) -0.0018(8) -0.0014(9) 0.0011(8) N9 0.0326(11) 0.0251(10) 0.0346(11) -0.0011(8) 0.0026(9) -0.0009(8) C10 0.0337(15) 0.0339(13) 0.0493(17) -0.0099(12) 0.0060(13) -0.0032(11) C11 0.0447(16) 0.0465(15) 0.0470(16) -0.0224(14) 0.0005(15) -0.0019(13) C12 0.0358(14) 0.0521(16) 0.0303(13) -0.0092(12) -0.0027(11) -0.0006(12) C13 0.055(2) 0.0298(13) 0.074(2) -0.0097(13) 0.0037(16) 0.0041(13) N14 0.0369(11) 0.0269(9) 0.0295(9) -0.0017(7) -0.0003(11) 0.0003(10) N15 0.0315(12) 0.0299(9) 0.0298(10) 0.0039(8) -0.0015(8) -0.0007(8) C16 0.0302(14) 0.0460(14) 0.0314(13) 0.0023(12) -0.0006(11) -0.0019(11) C17 0.0465(17) 0.0483(16) 0.0295(14) -0.0065(12) -0.0031(12) -0.0085(13) C18 0.0462(16) 0.0344(11) 0.0335(12) -0.0092(10) -0.0001(14) -0.0047(13) C19 0.0514(18) 0.0554(17) 0.0358(15) 0.0039(13) -0.0102(13) 0.0020(14) N20 0.0302(12) 0.0463(12) 0.0353(12) -0.0135(10) 0.0024(10) -0.0028(10) C21 0.0346(16) 0.0566(18) 0.0498(18) -0.0221(15) -0.0083(14) 0.0072(14) C22 0.0404(17) 0.065(2) 0.065(2) -0.0264(18) -0.0064(16) 0.0110(16) C23 0.062(2) 0.0438(16) 0.067(2) -0.0185(16) -0.0237(19) 0.0113(16) C24 0.056(2) 0.0390(14) 0.0487(16) -0.0122(12) -0.0045(15) -0.0019(14) C25 0.0370(16) 0.0353(12) 0.0378(13) -0.0139(10) -0.0033(12) -0.0002(12) N26 0.0306(12) 0.0863(19) 0.0440(14) -0.0232(15) 0.0093(11) -0.0110(13) N27 0.0388(13) 0.0696(16) 0.0335(12) -0.0111(12) 0.0032(10) -0.0142(13) C28 0.0423(19) 0.115(3) 0.0387(17) -0.0268(19) 0.0114(15) -0.0411(19) C29 0.050(2) 0.147(4) 0.046(2) -0.026(2) 0.0144(16) -0.038(3) C30 0.0312(16) 0.130(3) 0.058(2) -0.041(2) 0.0016(15) -0.002(2) C31 0.069(3) 0.113(3) 0.0404(18) 0.003(2) 0.0122(17) -0.049(2) N32 0.0375(13) 0.0395(12) 0.0368(12) -0.0086(10) 0.0020(10) -0.0045(10) N33 0.0337(12) 0.0426(12) 0.0317(11) -0.0097(9) -0.0001(9) 0.0026(10) C34 0.0286(14) 0.0590(18) 0.0332(14) -0.0177(13) -0.0007(11) 0.0001(12) C35 0.0369(16) 0.065(2) 0.0434(16) -0.0201(14) 0.0038(13) -0.0055(14) C36 0.0434(17) 0.0505(16) 0.0420(16) -0.0154(13) 0.0065(13) -0.0116(14) C37 0.0302(15) 0.075(2) 0.0440(17) -0.0102(15) -0.0010(13) 0.0075(14) B38 0.0396(18) 0.0278(13) 0.0325(15) -0.0040(11) 0.0019(13) 0.0019(12) F39 0.0474(11) 0.0916(14) 0.0666(12) -0.0263(11) 0.0099(9) -0.0131(10) F40 0.0436(10) 0.0500(9) 0.0582(11) -0.0195(8) -0.0011(8) 0.0093(8) F41 0.152(2) 0.0417(10) 0.0479(10) 0.0045(8) -0.0062(12) 0.0177(12) F42 0.0559(10) 0.0502(9) 0.0377(9) -0.0094(7) -0.0031(8) -0.0002(8) B43A 0.035(5) 0.046(6) 0.032(5) 0.003(2) -0.005(3) -0.013(3) F44A 0.057(2) 0.063(3) 0.0321(18) 0.0059(18) -0.0022(13) -0.007(2) F45A 0.053(2) 0.0482(18) 0.076(2) 0.0073(17) 0.0138(19) -0.0035(17) F46A 0.088(5) 0.107(5) 0.055(3) -0.022(3) 0.004(3) 0.045(4) F47A 0.0427(19) 0.077(2) 0.082(3) 0.007(2) -0.0179(18) -0.0136(19) C48 0.069(2) 0.071(2) 0.063(2) 0.0109(19) 0.0091(19) 0.0174(19) C49 0.057(2) 0.064(2) 0.087(3) 0.008(2) 0.013(2) 0.0121(18) N50 0.088(3) 0.089(3) 0.160(4) 0.051(3) 0.007(3) 0.022(2) C51 0.0538(19) 0.0502(17) 0.0398(16) -0.0031(13) -0.0002(14) -0.0062(15) C52 0.056(2) 0.0474(17) 0.0455(17) -0.0032(14) -0.0045(15) -0.0118(15) N53 0.106(3) 0.0604(19) 0.075(2) 0.0088(18) -0.032(2) -0.0091(19) C54 0.101(3) 0.057(2) 0.067(2) 0.0070(18) -0.009(2) 0.006(2) C55 0.090(3) 0.072(3) 0.051(2) 0.0022(19) 0.005(2) -0.007(2) N56 0.146(4) 0.099(3) 0.069(2) -0.012(2) 0.018(2) -0.043(3) C57 0.114(4) 0.060(2) 0.087(3) -0.002(2) -0.036(3) -0.004(2) C58 0.059(2) 0.060(2) 0.067(2) 0.0100(19) -0.0069(18) 0.0036(18) N59 0.111(3) 0.081(2) 0.091(3) -0.003(2) -0.006(2) 0.015(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 N20 1.957(2) . ? Fe1 N2 1.9696(19) . ? Fe1 N27 2.026(2) . ? Fe1 N9 2.047(2) . ? Fe1 N33 2.051(2) . ? Fe1 N15 2.066(2) . ? N2 C7 1.335(3) . ? N2 C3 1.338(3) . ? C3 C4 1.378(4) . ? C3 N8 1.398(3) . ? C4 C5 1.390(4) . ? C5 C6 1.386(4) . ? C6 C7 1.387(3) . ? C7 N14 1.395(3) . ? N8 C12 1.358(3) . ? N8 N9 1.385(3) . ? N9 C10 1.334(3) . ? C10 C11 1.399(4) . ? C10 C13 1.497(4) . ? C11 C12 1.369(4) . ? N14 C18 1.357(3) . ? N14 N15 1.382(3) . ? N15 C16 1.338(3) . ? C16 C17 1.411(4) . ? C16 C19 1.483(4) . ? C17 C18 1.358(4) . ? N20 C25 1.337(4) . ? N20 C21 1.346(4) . ? C21 C22 1.375(5) . ? C21 N26 1.408(4) . ? C22 C23 1.381(5) . ? C23 C24 1.397(5) . ? C24 C25 1.392(4) . ? C25 N32 1.403(4) . ? N26 C30 1.375(4) . ? N26 N27 1.378(4) . ? N27 C28 1.347(4) . ? C28 C29 1.412(6) . ? C28 C31 1.484(6) . ? C29 C30 1.362(6) . ? N32 C36 1.356(4) . ? N32 N33 1.381(3) . ? N33 C34 1.335(4) . ? C34 C35 1.410(4) . ? C34 C37 1.479(4) . ? C35 C36 1.360(5) . ? B38 F41 1.367(3) . ? B38 F39 1.376(4) . ? B38 F40 1.385(3) . ? B38 F42 1.401(3) . ? B43A F46A 1.359(12) . ? B43A F47A 1.362(10) . ? B43A F45A 1.405(10) . ? B43A F44A 1.406(9) . ? B43B F46B 1.370(16) . ? B43B F45B 1.371(16) . ? B43B F47B 1.381(16) . ? B43B F44B 1.397(16) . ? C48 C49 1.442(5) . ? C49 N50 1.144(5) . ? C51 C52 1.445(5) . ? C52 N53 1.134(4) . ? C54 C55 1.438(6) . ? C55 N56 1.146(5) . ? C57 C58 1.412(6) . ? C58 N59 1.128(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 N20 Fe1 N2 177.13(9) . . ? N20 Fe1 N27 78.90(11) . . ? N2 Fe1 N27 102.04(10) . . ? N20 Fe1 N9 104.85(8) . . ? N2 Fe1 N9 77.88(8) . . ? N27 Fe1 N9 91.68(9) . . ? N20 Fe1 N33 77.87(9) . . ? N2 Fe1 N33 101.27(9) . . ? N27 Fe1 N33 156.66(10) . . ? N9 Fe1 N33 92.09(8) . . ? N20 Fe1 N15 99.26(8) . . ? N2 Fe1 N15 78.02(8) . . ? N27 Fe1 N15 93.04(9) . . ? N9 Fe1 N15 155.90(8) . . ? N33 Fe1 N15 92.86(8) . . ? C7 N2 C3 119.0(2) . . ? C7 N2 Fe1 120.30(16) . . ? C3 N2 Fe1 120.64(16) . . ? N2 C3 C4 123.0(2) . . ? N2 C3 N8 111.3(2) . . ? C4 C3 N8 125.7(2) . . ? C3 C4 C5 116.7(2) . . ? C6 C5 C4 121.8(2) . . ? C5 C6 C7 116.5(2) . . ? N2 C7 C6 123.0(2) . . ? N2 C7 N14 111.97(19) . . ? C6 C7 N14 125.0(2) . . ? C12 N8 N9 111.0(2) . . ? C12 N8 C3 131.4(2) . . ? N9 N8 C3 117.48(19) . . ? C10 N9 N8 105.0(2) . . ? C10 N9 Fe1 142.33(19) . . ? N8 N9 Fe1 112.55(14) . . ? N9 C10 C11 110.7(2) . . ? N9 C10 C13 120.5(3) . . ? C11 C10 C13 128.9(3) . . ? C12 C11 C10 106.6(2) . . ? N8 C12 C11 106.7(2) . . ? C18 N14 N15 111.21(19) . . ? C18 N14 C7 130.9(2) . . ? N15 N14 C7 117.89(18) . . ? C16 N15 N14 105.13(19) . . ? C16 N15 Fe1 143.10(18) . . ? N14 N15 Fe1 111.77(14) . . ? N15 C16 C17 110.0(2) . . ? N15 C16 C19 122.6(2) . . ? C17 C16 C19 127.4(3) . . ? C18 C17 C16 106.7(2) . . ? N14 C18 C17 106.9(2) . . ? C25 N20 C21 118.8(3) . . ? C25 N20 Fe1 120.90(18) . . ? C21 N20 Fe1 120.0(2) . . ? N20 C21 C22 122.6(3) . . ? N20 C21 N26 110.6(3) . . ? C22 C21 N26 126.7(3) . . ? C21 C22 C23 117.2(3) . . ? C22 C23 C24 122.5(3) . . ? C25 C24 C23 115.1(3) . . ? N20 C25 C24 123.8(3) . . ? N20 C25 N32 111.2(2) . . ? C24 C25 N32 124.9(3) . . ? C30 N26 N27 110.9(3) . . ? C30 N26 C21 131.0(4) . . ? N27 N26 C21 118.1(2) . . ? C28 N27 N26 105.8(3) . . ? C28 N27 Fe1 142.0(3) . . ? N26 N27 Fe1 112.20(18) . . ? N27 C28 C29 109.4(4) . . ? N27 C28 C31 121.6(3) . . ? C29 C28 C31 129.0(3) . . ? C30 C29 C28 107.4(3) . . ? C29 C30 N26 106.5(4) . . ? C36 N32 N33 111.3(2) . . ? C36 N32 C25 131.4(3) . . ? N33 N32 C25 117.2(2) . . ? C34 N33 N32 105.3(2) . . ? C34 N33 Fe1 142.0(2) . . ? N32 N33 Fe1 112.53(16) . . ? N33 C34 C35 109.9(3) . . ? N33 C34 C37 121.6(3) . . ? C35 C34 C37 128.6(3) . . ? C36 C35 C34 106.9(3) . . ? N32 C36 C35 106.7(3) . . ? F41 B38 F39 110.7(3) . . ? F41 B38 F40 109.9(2) . . ? F39 B38 F40 109.8(2) . . ? F41 B38 F42 108.3(2) . . ? F39 B38 F42 108.7(2) . . ? F40 B38 F42 109.4(2) . . ? F46A B43A F47A 114.4(9) . . ? F46A B43A F45A 105.8(8) . . ? F47A B43A F45A 108.5(8) . . ? F46A B43A F44A 106.5(8) . . ? F47A B43A F44A 109.9(7) . . ? F45A B43A F44A 111.6(7) . . ? F46B B43B F45B 111.3(13) . . ? F46B B43B F47B 107.1(12) . . ? F45B B43B F47B 107.4(12) . . ? F46B B43B F44B 113.3(13) . . ? F45B B43B F44B 105.4(12) . . ? F47B B43B F44B 112.3(13) . . ? N50 C49 C48 178.6(5) . . ? N53 C52 C51 179.4(4) . . ? N56 C55 C54 177.7(6) . . ? N59 C58 C57 178.3(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.300 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.065 #=END data_c:\datasets\leeds\je33bv~1\je33b1~1\je33b100 _database_code_depnum_ccdc_archive 'CCDC 278908' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-bis(3-methylpyrazol-1-yl)pyridine] ditetrafluoroborate tetrakis-acetonitrile solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Fe N10, 2[B F4], 4[C2 H3 N]' _chemical_formula_sum 'C34 H38 B2 F8 Fe N14' _chemical_formula_weight 872.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' 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 11.2572(1) _cell_length_b 13.5578(1) _cell_length_c 26.1701(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3994.16(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 65112 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 27.51 _exptl_crystal_description 'Square prism' _exptl_crystal_colour Brown _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.461 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.661 _exptl_absorpt_correction_T_max 0.898 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method 'Area detector scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65112 _diffrn_reflns_av_R_equivalents 0.0780 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 27.51 _reflns_number_total 9152 _reflns_number_gt 8165 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 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 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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. Anion B43-F47 is disordered over two sites, labelled 'A' (occupancy 0.6) and 'B' (occupancy 0.4). These were modelled using the refined restraints B---F = 1.39(2) and 1,3-F...F = 2.27(2)\%A. All non-H atoms except the minor disorder orientation were refined anisotropically. All H atoms were placed in calculated positions and refined using a riding model, with the methyl group torsions allowed to refine freely. ; _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^)+(0.0467P)^2^+1.1029P] 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 -0.025(11) _refine_ls_number_reflns 9152 _refine_ls_number_parameters 561 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0885 _refine_ls_wR_factor_gt 0.0834 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.034 _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 0.25027(2) 0.207284(17) 0.178904(9) 0.02040(7) Uani 1 1 d . . . N2 N 0.30521(14) 0.09035(12) 0.21211(6) 0.0220(3) Uani 1 1 d . . . C3 C 0.34901(18) 0.09417(15) 0.25990(8) 0.0234(4) Uani 1 1 d . . . C4 C 0.39298(18) 0.01236(15) 0.28488(8) 0.0265(4) Uani 1 1 d . . . H4 H 0.4235 0.0165 0.3187 0.032 Uiso 1 1 calc R . . C5 C 0.3905(2) -0.07667(16) 0.25818(8) 0.0305(5) Uani 1 1 d . . . H5 H 0.4207 -0.1345 0.2740 0.037 Uiso 1 1 calc R . . C6 C 0.34500(19) -0.08271(16) 0.20885(8) 0.0283(4) Uani 1 1 d . . . H6 H 0.3429 -0.1434 0.1907 0.034 Uiso 1 1 calc R . . C7 C 0.30310(17) 0.00360(14) 0.18754(7) 0.0236(4) Uani 1 1 d . . . N8 N 0.34277(14) 0.18979(12) 0.27912(6) 0.0231(3) Uani 1 1 d . . . N9 N 0.30234(14) 0.26292(12) 0.24644(6) 0.0227(3) Uani 1 1 d . . . C10 C 0.30842(18) 0.34613(15) 0.27322(8) 0.0261(4) Uani 1 1 d . . . C11 C 0.35274(18) 0.32701(16) 0.32259(9) 0.0294(4) Uani 1 1 d . . . H11 H 0.3658 0.3740 0.3489 0.035 Uiso 1 1 calc R . . C12 C 0.37316(18) 0.22811(15) 0.32526(8) 0.0269(4) Uani 1 1 d . . . H12 H 0.4029 0.1928 0.3539 0.032 Uiso 1 1 calc R . . C13 C 0.2712(2) 0.44245(14) 0.25058(9) 0.0327(5) Uani 1 1 d . . . H13A H 0.2973 0.4457 0.2149 0.049 Uiso 1 1 calc R . . H13B H 0.3074 0.4966 0.2699 0.049 Uiso 1 1 calc R . . H13C H 0.1845 0.4482 0.2521 0.049 Uiso 1 1 calc R . . N14 N 0.25416(17) 0.01377(11) 0.13887(6) 0.0241(3) Uani 1 1 d . . . N15 N 0.21812(14) 0.10700(12) 0.12387(6) 0.0237(4) Uani 1 1 d . . . C16 C 0.17513(18) 0.09484(15) 0.07657(8) 0.0260(4) Uani 1 1 d . . . C17 C 0.18374(19) -0.00492(16) 0.06162(8) 0.0292(5) Uani 1 1 d . . . H17 H 0.1591 -0.0324 0.0300 0.035 Uiso 1 1 calc R . . C18 C 0.2343(2) -0.05397(14) 0.10145(7) 0.0286(4) Uani 1 1 d . . . H18 H 0.2524 -0.1224 0.1029 0.034 Uiso 1 1 calc R . . C19 C 0.1269(2) 0.17820(17) 0.04565(8) 0.0334(5) Uani 1 1 d . . . H19A H 0.0677 0.2143 0.0658 0.050 Uiso 1 1 calc R . . H19B H 0.0895 0.1522 0.0146 0.050 Uiso 1 1 calc R . . H19C H 0.1917 0.2229 0.0362 0.050 Uiso 1 1 calc R . . N20 N 0.19507(15) 0.32053(12) 0.14268(6) 0.0236(3) Uani 1 1 d . . . C21 C 0.07971(18) 0.34567(15) 0.14448(8) 0.0265(4) Uani 1 1 d . . . C22 C 0.0323(2) 0.42163(17) 0.11600(8) 0.0322(5) Uani 1 1 d . . . H22 H -0.0492 0.4392 0.1184 0.039 Uiso 1 1 calc R . . C23 C 0.1100(2) 0.47116(16) 0.08369(9) 0.0335(5) Uani 1 1 d . . . H23 H 0.0804 0.5237 0.0633 0.040 Uiso 1 1 calc R . . C24 C 0.2297(2) 0.44632(14) 0.08024(8) 0.0298(5) Uani 1 1 d . . . H24 H 0.2824 0.4796 0.0577 0.036 Uiso 1 1 calc R . . C25 C 0.26757(19) 0.37024(14) 0.11156(7) 0.0248(4) Uani 1 1 d . . . N26 N 0.01751(14) 0.28332(13) 0.17779(7) 0.0284(4) Uani 1 1 d . . . N27 N 0.08055(14) 0.20856(13) 0.20125(6) 0.0256(3) Uani 1 1 d . . . C28 C 0.00336(19) 0.16310(17) 0.23222(8) 0.0291(4) Uani 1 1 d . . . C29 C -0.1095(2) 0.20817(19) 0.22791(8) 0.0352(5) Uani 1 1 d . . . H29 H -0.1800 0.1894 0.2453 0.042 Uiso 1 1 calc R . . C30 C -0.0976(2) 0.28371(19) 0.19400(8) 0.0350(5) Uani 1 1 d . . . H30 H -0.1581 0.3282 0.1836 0.042 Uiso 1 1 calc R . . C31 C 0.0391(2) 0.07923(18) 0.26547(8) 0.0341(5) Uani 1 1 d . . . H31A H 0.0616 0.0228 0.2441 0.051 Uiso 1 1 calc R . . H31B H -0.0276 0.0607 0.2875 0.051 Uiso 1 1 calc R . . H31C H 0.1069 0.0989 0.2867 0.051 Uiso 1 1 calc R . . N32 N 0.38355(16) 0.33343(12) 0.11483(7) 0.0256(4) Uani 1 1 d . . . N33 N 0.40127(15) 0.25147(12) 0.14528(6) 0.0236(3) Uani 1 1 d . . . C34 C 0.51793(18) 0.23414(15) 0.14367(7) 0.0254(4) Uani 1 1 d . . . C35 C 0.57440(19) 0.30504(16) 0.11231(8) 0.0302(5) Uani 1 1 d . . . H35 H 0.6568 0.3087 0.1047 0.036 Uiso 1 1 calc R . . C36 C 0.4880(2) 0.36714(16) 0.09507(8) 0.0294(5) Uani 1 1 d . . . H36 H 0.4985 0.4229 0.0735 0.035 Uiso 1 1 calc R . . C37 C 0.57316(18) 0.15189(17) 0.17298(8) 0.0312(5) Uani 1 1 d . . . H37A H 0.5634 0.1639 0.2097 0.047 Uiso 1 1 calc R . . H37B H 0.6580 0.1480 0.1648 0.047 Uiso 1 1 calc R . . H37C H 0.5345 0.0896 0.1638 0.047 Uiso 1 1 calc R . . B38 B 0.3227(2) 0.64726(16) 0.15905(9) 0.0235(5) Uani 1 1 d . . . F39 F 0.21217(12) 0.60508(11) 0.16716(5) 0.0425(3) Uani 1 1 d . . . F40 F 0.39998(11) 0.57799(10) 0.13851(5) 0.0354(3) Uani 1 1 d . . . F41 F 0.31234(16) 0.72725(10) 0.12680(5) 0.0516(4) Uani 1 1 d . . . F42 F 0.36753(11) 0.68006(9) 0.20641(5) 0.0336(3) Uani 1 1 d . . . B43A B 0.2379(10) 0.0433(8) 0.4236(4) 0.031(5) Uani 0.60 1 d PD A 1 F44A F 0.2077(3) 0.0583(3) 0.37154(13) 0.0355(8) Uani 0.60 1 d PD A 1 F45A F 0.2428(3) -0.05663(19) 0.43592(11) 0.0393(6) Uani 0.60 1 d PD A 1 F46A F 0.1490(6) 0.0871(5) 0.4519(3) 0.0539(15) Uani 0.60 1 d PD A 1 F47A F 0.3481(3) 0.0854(3) 0.43155(12) 0.0530(7) Uani 0.60 1 d PD A 1 B43B B 0.2365(14) 0.0495(11) 0.4238(6) 0.026(7) Uiso 0.40 1 d PD B 2 F44B F 0.2192(6) 0.0307(4) 0.3715(3) 0.0380(19) Uiso 0.40 1 d PD B 2 F45B F 0.2813(5) -0.0368(4) 0.4439(2) 0.0451(15) Uiso 0.40 1 d PD B 2 F46B F 0.1298(8) 0.0703(8) 0.4483(4) 0.0373(18) Uiso 0.40 1 d PD B 2 F47B F 0.3137(5) 0.1261(4) 0.4340(2) 0.0511(14) Uiso 0.40 1 d PD B 2 C48 C 0.8535(3) 0.0389(2) 0.10186(11) 0.0490(6) Uani 1 1 d . . . H48A H 0.9212 0.0012 0.0887 0.073 Uiso 1 1 calc R . . H48B H 0.7852 -0.0050 0.1061 0.073 Uiso 1 1 calc R . . H48C H 0.8745 0.0680 0.1349 0.073 Uiso 1 1 calc R . . C49 C 0.8237(2) 0.1166(2) 0.06618(12) 0.0509(7) Uani 1 1 d . . . N50 N 0.8006(3) 0.1775(2) 0.03756(13) 0.0756(9) Uani 1 1 d . . . C51 C 0.4555(2) 0.12485(17) 0.02164(9) 0.0351(5) Uani 1 1 d . . . H51A H 0.5203 0.1596 0.0043 0.053 Uiso 1 1 calc R . . H51B H 0.4122 0.1712 0.0435 0.053 Uiso 1 1 calc R . . H51C H 0.4012 0.0970 -0.0038 0.053 Uiso 1 1 calc R . . C52 C 0.5042(2) 0.04597(18) 0.05275(9) 0.0376(5) Uani 1 1 d . . . N53 N 0.5435(3) -0.01528(18) 0.07755(9) 0.0563(6) Uani 1 1 d . . . C54 C 0.4874(3) 0.7588(2) 0.03065(11) 0.0529(7) Uani 1 1 d . . . H54A H 0.4429 0.8110 0.0132 0.079 Uiso 1 1 calc R . . H54B H 0.5717 0.7636 0.0216 0.079 Uiso 1 1 calc R . . H54C H 0.4784 0.7664 0.0677 0.079 Uiso 1 1 calc R . . C55 C 0.4416(3) 0.6629(2) 0.01509(11) 0.0528(7) Uani 1 1 d . . . N56 N 0.4093(3) 0.5864(2) 0.00244(11) 0.0795(10) Uani 1 1 d . . . C57 C -0.0138(3) 0.7454(2) 0.11926(12) 0.0601(8) Uani 1 1 d . . . H57A H -0.0144 0.7742 0.0849 0.090 Uiso 1 1 calc R . . H57B H -0.0861 0.7063 0.1243 0.090 Uiso 1 1 calc R . . H57C H 0.0560 0.7029 0.1231 0.090 Uiso 1 1 calc R . . C58 C -0.0094(2) 0.8230(2) 0.15669(10) 0.0430(6) Uani 1 1 d . . . N59 N -0.0044(3) 0.8846(2) 0.18529(10) 0.0658(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02221(12) 0.02026(12) 0.01872(12) 0.00036(10) -0.00015(12) 0.00025(12) N2 0.0233(8) 0.0221(8) 0.0205(8) -0.0007(7) -0.0003(6) 0.0004(6) C3 0.0230(9) 0.0235(10) 0.0239(10) -0.0007(8) 0.0010(8) -0.0017(8) C4 0.0277(10) 0.0294(10) 0.0223(9) 0.0042(8) -0.0025(8) 0.0010(8) C5 0.0357(11) 0.0255(10) 0.0303(11) 0.0057(9) -0.0018(9) 0.0028(9) C6 0.0337(11) 0.0231(10) 0.0282(11) -0.0015(8) -0.0001(9) -0.0011(8) C7 0.0240(9) 0.0228(9) 0.0242(10) 0.0006(8) 0.0010(8) -0.0019(7) N8 0.0256(8) 0.0226(8) 0.0211(8) 0.0002(6) -0.0020(6) 0.0011(6) N9 0.0238(8) 0.0212(8) 0.0232(8) 0.0016(7) 0.0009(6) 0.0003(6) C10 0.0271(10) 0.0238(10) 0.0273(11) -0.0027(8) 0.0015(8) -0.0013(8) C11 0.0319(11) 0.0297(10) 0.0267(10) -0.0063(9) -0.0021(9) -0.0004(8) C12 0.0279(10) 0.0337(11) 0.0191(9) -0.0020(8) -0.0022(8) -0.0016(8) C13 0.0396(13) 0.0226(10) 0.0358(11) -0.0012(8) -0.0027(9) 0.0016(9) N14 0.0299(8) 0.0206(7) 0.0219(7) -0.0003(6) 0.0014(8) 0.0002(8) N15 0.0257(9) 0.0230(8) 0.0224(8) 0.0017(6) -0.0005(6) -0.0002(6) C16 0.0261(10) 0.0294(11) 0.0226(10) -0.0013(8) 0.0006(8) -0.0012(8) C17 0.0332(11) 0.0316(11) 0.0229(10) -0.0040(9) -0.0002(8) -0.0055(9) C18 0.0350(12) 0.0248(9) 0.0259(10) -0.0049(8) 0.0015(9) -0.0045(9) C19 0.0404(12) 0.0354(12) 0.0243(11) -0.0001(9) -0.0060(9) 0.0027(10) N20 0.0258(8) 0.0249(8) 0.0203(8) -0.0016(7) -0.0004(7) 0.0007(7) C21 0.0285(10) 0.0262(10) 0.0248(10) -0.0043(8) -0.0024(8) 0.0025(8) C22 0.0322(11) 0.0331(11) 0.0312(11) -0.0045(9) -0.0044(9) 0.0069(9) C23 0.0461(13) 0.0229(10) 0.0315(11) -0.0013(9) -0.0111(10) 0.0030(9) C24 0.0420(13) 0.0233(10) 0.0242(10) -0.0009(8) -0.0025(9) -0.0023(9) C25 0.0295(11) 0.0225(9) 0.0224(9) -0.0042(7) -0.0006(8) -0.0005(8) N26 0.0238(8) 0.0339(9) 0.0274(8) -0.0004(8) 0.0005(7) 0.0020(7) N27 0.0258(8) 0.0293(8) 0.0217(8) -0.0008(7) -0.0002(6) 0.0000(7) C28 0.0284(10) 0.0362(11) 0.0229(10) -0.0033(9) 0.0006(8) -0.0085(9) C29 0.0277(10) 0.0487(13) 0.0292(11) -0.0025(11) 0.0018(8) -0.0038(11) C30 0.0263(10) 0.0462(13) 0.0326(11) -0.0035(10) -0.0001(8) 0.0011(10) C31 0.0318(11) 0.0421(13) 0.0285(11) 0.0044(10) 0.0029(9) -0.0078(10) N32 0.0296(9) 0.0223(8) 0.0247(9) -0.0002(7) 0.0026(7) -0.0013(7) N33 0.0280(8) 0.0217(8) 0.0211(8) -0.0003(7) 0.0002(7) -0.0001(7) C34 0.0258(10) 0.0296(10) 0.0208(10) -0.0058(8) 0.0005(7) -0.0006(8) C35 0.0287(10) 0.0354(12) 0.0266(10) -0.0039(9) 0.0039(8) -0.0048(9) C36 0.0345(11) 0.0281(11) 0.0255(11) -0.0021(9) 0.0054(8) -0.0050(9) C37 0.0253(10) 0.0395(12) 0.0289(11) -0.0008(10) -0.0002(8) 0.0036(8) B38 0.0287(11) 0.0188(10) 0.0229(11) -0.0032(8) 0.0001(9) 0.0025(8) F39 0.0326(7) 0.0511(9) 0.0436(8) -0.0136(7) 0.0037(6) -0.0058(6) F40 0.0322(6) 0.0366(7) 0.0372(7) -0.0109(6) -0.0004(5) 0.0049(5) F41 0.0917(12) 0.0301(7) 0.0329(7) 0.0045(6) -0.0031(7) 0.0073(7) F42 0.0379(7) 0.0359(7) 0.0269(6) -0.0054(5) -0.0014(5) -0.0010(5) B43A 0.030(5) 0.040(7) 0.024(5) 0.0040(19) -0.0054(18) -0.009(2) F44A 0.0397(17) 0.045(2) 0.0217(13) 0.0043(14) 0.0000(9) -0.0005(16) F45A 0.0374(15) 0.0321(13) 0.0483(15) 0.0011(11) 0.0102(13) 0.0020(13) F46A 0.074(4) 0.048(3) 0.040(2) -0.007(2) 0.011(2) 0.025(3) F47A 0.0395(16) 0.065(2) 0.0551(18) 0.0090(16) -0.0136(13) -0.0181(16) C48 0.0480(15) 0.0524(16) 0.0465(15) 0.0045(13) 0.0072(12) 0.0089(13) C49 0.0393(14) 0.0506(16) 0.0627(18) 0.0012(15) 0.0078(13) 0.0060(12) N50 0.0638(17) 0.0622(17) 0.101(2) 0.0277(17) 0.0069(16) 0.0124(14) C51 0.0416(13) 0.0350(12) 0.0287(11) -0.0020(10) 0.0013(10) -0.0034(10) C52 0.0422(13) 0.0381(13) 0.0323(12) -0.0035(10) -0.0010(10) -0.0098(11) N53 0.0724(17) 0.0465(13) 0.0499(14) 0.0059(12) -0.0197(12) -0.0061(12) C54 0.0668(19) 0.0454(15) 0.0466(16) 0.0038(13) -0.0034(14) 0.0058(13) C55 0.0623(18) 0.0586(18) 0.0374(14) 0.0022(13) 0.0042(13) -0.0042(15) N56 0.109(3) 0.0759(19) 0.0538(16) -0.0094(15) 0.0210(16) -0.0405(19) C57 0.079(2) 0.0430(16) 0.0579(18) -0.0067(14) -0.0217(16) -0.0011(15) C58 0.0448(14) 0.0423(14) 0.0417(14) 0.0045(12) -0.0051(11) 0.0014(11) N59 0.0796(19) 0.0603(16) 0.0576(16) -0.0101(14) -0.0041(14) 0.0099(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 N20 1.9084(17) . ? Fe1 N2 1.9107(16) . ? Fe1 N27 1.9982(16) . ? Fe1 N33 2.0055(17) . ? Fe1 N9 2.0090(17) . ? Fe1 N15 2.0134(17) . ? N2 C7 1.341(2) . ? N2 C3 1.345(3) . ? C3 C4 1.379(3) . ? C3 N8 1.392(3) . ? C4 C5 1.395(3) . ? C5 C6 1.392(3) . ? C6 C7 1.379(3) . ? C7 N14 1.395(2) . ? N8 C12 1.358(3) . ? N8 N9 1.386(2) . ? N9 C10 1.330(3) . ? C10 C11 1.409(3) . ? C10 C13 1.494(3) . ? C11 C12 1.362(3) . ? N14 C18 1.361(2) . ? N14 N15 1.384(2) . ? N15 C16 1.339(3) . ? C16 C17 1.411(3) . ? C16 C19 1.492(3) . ? C17 C18 1.361(3) . ? N20 C25 1.336(3) . ? N20 C21 1.343(3) . ? C21 C22 1.379(3) . ? C21 N26 1.402(3) . ? C22 C23 1.389(3) . ? C23 C24 1.393(3) . ? C24 C25 1.384(3) . ? C25 N32 1.400(3) . ? N26 C30 1.364(3) . ? N26 N27 1.381(2) . ? N27 C28 1.338(3) . ? C28 C29 1.414(3) . ? C28 C31 1.487(3) . ? C29 C30 1.362(3) . ? N32 C36 1.363(3) . ? N32 N33 1.382(2) . ? N33 C34 1.335(3) . ? C34 C35 1.415(3) . ? C34 C37 1.490(3) . ? C35 C36 1.363(3) . ? B38 F41 1.379(3) . ? B38 F39 1.386(3) . ? B38 F40 1.388(3) . ? B38 F42 1.410(3) . ? B43A F46A 1.380(11) . ? B43A F47A 1.381(11) . ? B43A F45A 1.394(11) . ? B43A F44A 1.418(10) . ? B43B F45B 1.379(15) . ? B43B F47B 1.380(15) . ? B43B F46B 1.390(15) . ? B43B F44B 1.405(15) . ? C48 C49 1.447(4) . ? C49 N50 1.145(4) . ? C51 C52 1.452(3) . ? C52 N53 1.143(3) . ? C54 C55 1.457(4) . ? C55 N56 1.147(4) . ? C57 C58 1.438(4) . ? C58 N59 1.123(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 N20 Fe1 N2 177.20(7) . . ? N20 Fe1 N27 80.04(7) . . ? N2 Fe1 N27 100.58(7) . . ? N20 Fe1 N33 79.50(7) . . ? N2 Fe1 N33 99.97(7) . . ? N27 Fe1 N33 159.42(7) . . ? N20 Fe1 N9 103.29(7) . . ? N2 Fe1 N9 79.45(7) . . ? N27 Fe1 N9 91.05(7) . . ? N33 Fe1 N9 91.52(7) . . ? N20 Fe1 N15 97.44(7) . . ? N2 Fe1 N15 79.82(7) . . ? N27 Fe1 N15 92.48(7) . . ? N33 Fe1 N15 92.31(7) . . ? N9 Fe1 N15 159.27(7) . . ? C7 N2 C3 119.09(17) . . ? C7 N2 Fe1 120.26(13) . . ? C3 N2 Fe1 120.63(13) . . ? N2 C3 C4 122.76(18) . . ? N2 C3 N8 110.68(17) . . ? C4 C3 N8 126.56(18) . . ? C3 C4 C5 116.83(19) . . ? C6 C5 C4 121.53(19) . . ? C7 C6 C5 116.82(19) . . ? N2 C7 C6 122.97(18) . . ? N2 C7 N14 111.00(16) . . ? C6 C7 N14 126.03(17) . . ? C12 N8 N9 110.95(15) . . ? C12 N8 C3 131.64(17) . . ? N9 N8 C3 117.37(15) . . ? C10 N9 N8 105.35(15) . . ? C10 N9 Fe1 142.85(14) . . ? N8 N9 Fe1 111.72(12) . . ? N9 C10 C11 110.21(18) . . ? N9 C10 C13 121.21(18) . . ? C11 C10 C13 128.58(19) . . ? C12 C11 C10 106.73(19) . . ? N8 C12 C11 106.76(18) . . ? C18 N14 N15 111.35(15) . . ? C18 N14 C7 130.94(16) . . ? N15 N14 C7 117.72(15) . . ? C16 N15 N14 104.81(15) . . ? C16 N15 Fe1 144.02(15) . . ? N14 N15 Fe1 111.16(11) . . ? N15 C16 C17 110.45(18) . . ? N15 C16 C19 122.65(18) . . ? C17 C16 C19 126.90(19) . . ? C18 C17 C16 106.53(18) . . ? N14 C18 C17 106.86(18) . . ? C25 N20 C21 118.94(18) . . ? C25 N20 Fe1 120.66(14) . . ? C21 N20 Fe1 120.10(15) . . ? N20 C21 C22 123.0(2) . . ? N20 C21 N26 110.59(18) . . ? C22 C21 N26 126.40(19) . . ? C21 C22 C23 116.5(2) . . ? C22 C23 C24 122.1(2) . . ? C25 C24 C23 116.1(2) . . ? N20 C25 C24 123.3(2) . . ? N20 C25 N32 110.64(17) . . ? C24 C25 N32 126.06(19) . . ? C30 N26 N27 110.67(17) . . ? C30 N26 C21 131.75(19) . . ? N27 N26 C21 117.53(16) . . ? C28 N27 N26 105.87(16) . . ? C28 N27 Fe1 142.55(15) . . ? N26 N27 Fe1 111.57(12) . . ? N27 C28 C29 109.6(2) . . ? N27 C28 C31 122.05(19) . . ? C29 C28 C31 128.3(2) . . ? C30 C29 C28 106.79(19) . . ? C29 C30 N26 107.0(2) . . ? C36 N32 N33 111.34(17) . . ? C36 N32 C25 131.40(18) . . ? N33 N32 C25 117.16(16) . . ? C34 N33 N32 105.39(16) . . ? C34 N33 Fe1 142.67(15) . . ? N32 N33 Fe1 111.77(12) . . ? N33 C34 C35 109.93(19) . . ? N33 C34 C37 121.75(18) . . ? C35 C34 C37 128.30(18) . . ? C36 C35 C34 106.91(19) . . ? N32 C36 C35 106.42(19) . . ? F41 B38 F39 110.02(19) . . ? F41 B38 F40 110.37(18) . . ? F39 B38 F40 110.04(17) . . ? F41 B38 F42 108.67(17) . . ? F39 B38 F42 108.47(17) . . ? F40 B38 F42 109.23(17) . . ? F46A B43A F47A 113.1(9) . . ? F46A B43A F45A 108.8(8) . . ? F47A B43A F45A 109.3(8) . . ? F46A B43A F44A 106.2(8) . . ? F47A B43A F44A 107.6(8) . . ? F45A B43A F44A 111.8(8) . . ? F45B B43B F47B 109.5(11) . . ? F45B B43B F46B 108.2(12) . . ? F47B B43B F46B 107.6(11) . . ? F45B B43B F44B 105.6(11) . . ? F47B B43B F44B 114.3(11) . . ? F46B B43B F44B 111.5(12) . . ? N50 C49 C48 179.3(3) . . ? N53 C52 C51 179.1(3) . . ? N56 C55 C54 177.8(4) . . ? N59 C58 C57 178.6(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.357 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.112