Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr. 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_section_title ; A Structural, Magnetic and Moessbauer Spectroscopic Study of an Unusual Angular Jahn-Teller Distortion in a Series of High-Spin Iron(II) Complexes ; loop_ _publ_author_name _publ_author_address 'Jerome Elhaik' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'David J. Evans' ; Department of Biological Chemistry, John Innes Centre, Norwich Research Park, Norwich NR4 7UH, 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\mh87\mh87 _database_code_depnum_ccdc_archive 'CCDC 263420' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-[2,6-dipyrazol-1-ylpyridine]iron(II) diperchlorate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H18 Fe N10, 2[Cl O4]' _chemical_formula_sum 'C22 H18 Cl2 Fe N10 O8' _chemical_formula_weight 677.21 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 14.3860(3) _cell_length_b 9.2460(2) _cell_length_c 20.1033(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.4384(14) _cell_angle_gamma 90.00 _cell_volume 2637.76(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13839 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'Rectamgular prism' _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.844 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 0.913 _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 '/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 13839 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3013 _reflns_number_gt 2524 _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 half a formula unit, with Fe1 lying on the crystallographic C2 axis -x, y, 0.5-z. No disorder was detected during refinement, and no restraints were applied. All non-H atoms were refined anisotropically, while all H atoms were placed in calculated positions and refined using a riding 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^)+(0.0475P)^2^+3.9495P] 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 0.0023(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3013 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.0000 0.69509(4) 0.2500 0.02221(15) Uani 1 2 d S . . N2 N 0.01443(12) 0.74454(19) 0.35660(8) 0.0225(4) Uani 1 1 d . . . C3 C -0.03005(14) 0.6655(2) 0.39681(10) 0.0229(4) Uani 1 1 d . . . C4 C -0.02808(15) 0.6954(2) 0.46449(10) 0.0279(5) Uani 1 1 d . . . H4 H -0.0627 0.6394 0.4916 0.034 Uiso 1 1 calc R . . C5 C 0.02697(16) 0.8113(2) 0.49052(11) 0.0310(5) Uani 1 1 d . . . H5 H 0.0300 0.8363 0.5367 0.037 Uiso 1 1 calc R . . C6 C 0.07796(16) 0.8920(3) 0.45067(11) 0.0300(5) Uani 1 1 d . . . H6 H 0.1179 0.9692 0.4688 0.036 Uiso 1 1 calc R . . C7 C 0.06774(14) 0.8545(2) 0.38342(10) 0.0248(4) Uani 1 1 d . . . N8 N -0.07716(12) 0.54606(19) 0.36366(8) 0.0236(4) Uani 1 1 d . . . N9 N -0.06758(12) 0.5215(2) 0.29792(8) 0.0251(4) Uani 1 1 d . . . C10 C -0.10418(15) 0.3915(2) 0.28340(11) 0.0277(5) Uani 1 1 d . . . H10 H -0.1078 0.3454 0.2408 0.033 Uiso 1 1 calc R . . C11 C -0.13716(16) 0.3305(2) 0.33961(11) 0.0299(5) Uani 1 1 d . . . H11 H -0.1661 0.2387 0.3421 0.036 Uiso 1 1 calc R . . C12 C -0.11854(15) 0.4312(2) 0.38946(11) 0.0279(5) Uani 1 1 d . . . H12 H -0.1320 0.4229 0.4340 0.034 Uiso 1 1 calc R . . N13 N 0.11370(12) 0.92549(19) 0.33611(9) 0.0255(4) Uani 1 1 d . . . N14 N 0.10695(12) 0.8672(2) 0.27286(9) 0.0262(4) Uani 1 1 d . . . C15 C 0.15616(15) 0.9567(2) 0.24009(11) 0.0295(5) Uani 1 1 d . . . H15 H 0.1644 0.9444 0.1945 0.035 Uiso 1 1 calc R . . C16 C 0.19418(16) 1.0715(3) 0.28128(12) 0.0326(5) Uani 1 1 d . . . H16 H 0.2319 1.1487 0.2694 0.039 Uiso 1 1 calc R . . C17 C 0.16578(16) 1.0493(2) 0.34197(12) 0.0314(5) Uani 1 1 d . . . H17 H 0.1796 1.1088 0.3809 0.038 Uiso 1 1 calc R . . Cl18 Cl 0.29743(4) 0.95837(7) 0.08946(3) 0.03291(18) Uani 1 1 d . . . O19 O 0.21843(16) 0.8670(3) 0.09178(12) 0.0763(8) Uani 1 1 d . . . O20 O 0.38256(14) 0.8765(2) 0.10612(9) 0.0470(5) Uani 1 1 d . . . O21 O 0.29790(15) 1.0723(2) 0.13840(12) 0.0561(6) Uani 1 1 d . . . O22 O 0.29469(17) 1.0166(4) 0.02358(11) 0.0870(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0271(2) 0.0235(2) 0.0168(2) 0.000 0.00563(16) 0.000 N2 0.0246(8) 0.0239(9) 0.0191(8) -0.0003(7) 0.0037(6) 0.0008(7) C3 0.0231(9) 0.0263(11) 0.0195(9) 0.0010(8) 0.0038(8) 0.0036(8) C4 0.0326(11) 0.0328(12) 0.0193(10) 0.0018(8) 0.0068(8) 0.0074(9) C5 0.0404(12) 0.0338(12) 0.0182(10) -0.0033(8) 0.0027(9) 0.0102(10) C6 0.0333(11) 0.0309(12) 0.0241(10) -0.0045(9) -0.0001(9) 0.0028(9) C7 0.0239(10) 0.0256(11) 0.0249(10) 0.0007(8) 0.0042(8) 0.0030(8) N8 0.0276(9) 0.0269(9) 0.0171(8) 0.0014(7) 0.0062(7) -0.0003(7) N9 0.0285(9) 0.0293(10) 0.0180(8) 0.0005(7) 0.0051(7) 0.0003(7) C10 0.0309(11) 0.0278(11) 0.0241(10) 0.0000(8) 0.0033(8) -0.0017(9) C11 0.0321(11) 0.0287(12) 0.0291(11) 0.0050(9) 0.0055(9) -0.0038(9) C12 0.0291(11) 0.0324(12) 0.0227(10) 0.0066(9) 0.0057(8) -0.0001(9) N13 0.0283(9) 0.0249(9) 0.0235(9) -0.0027(7) 0.0043(7) 0.0002(7) N14 0.0275(9) 0.0285(10) 0.0233(8) -0.0012(7) 0.0059(7) -0.0001(7) C15 0.0286(11) 0.0307(12) 0.0299(11) 0.0070(9) 0.0067(9) 0.0010(9) C16 0.0294(11) 0.0266(11) 0.0412(13) 0.0055(10) 0.0041(10) -0.0027(9) C17 0.0301(11) 0.0238(11) 0.0388(12) -0.0023(9) 0.0008(9) -0.0016(9) Cl18 0.0307(3) 0.0439(4) 0.0257(3) 0.0045(2) 0.0093(2) 0.0004(2) O19 0.0525(13) 0.111(2) 0.0726(15) -0.0420(15) 0.0308(12) -0.0446(13) O20 0.0477(11) 0.0526(12) 0.0403(10) 0.0034(9) 0.0059(8) 0.0149(9) O21 0.0606(13) 0.0401(11) 0.0762(14) -0.0163(10) 0.0362(11) -0.0047(10) O22 0.0726(16) 0.150(3) 0.0456(12) 0.0538(15) 0.0303(11) 0.0529(17) _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 2.1676(16) . ? Fe1 N9 2.1808(18) . ? Fe1 N14 2.2085(18) . ? N2 C3 1.329(3) . ? N2 C7 1.333(3) . ? C3 C4 1.384(3) . ? C3 N8 1.406(3) . ? C4 C5 1.383(3) . ? C5 C6 1.389(3) . ? C6 C7 1.380(3) . ? C7 N13 1.407(3) . ? N8 C12 1.361(3) . ? N8 N9 1.370(2) . ? N9 C10 1.326(3) . ? C10 C11 1.413(3) . ? C11 C12 1.362(3) . ? N13 C17 1.363(3) . ? N13 N14 1.370(2) . ? N14 C15 1.332(3) . ? C15 C16 1.401(3) . ? C16 C17 1.364(3) . ? Cl18 O19 1.423(2) . ? Cl18 O22 1.424(2) . ? Cl18 O20 1.4320(19) . ? Cl18 O21 1.441(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 N2 155.65(10) . 2 ? N2 Fe1 N9 72.29(6) . . ? N2 Fe1 N9 127.92(6) 2 . ? N9 Fe1 N9 85.24(9) 2 . ? N2 Fe1 N14 72.05(6) . . ? N2 Fe1 N14 90.24(6) 2 . ? N9 Fe1 N14 106.03(6) 2 . ? N9 Fe1 N14 141.63(6) . . ? N14 Fe1 N14 87.83(10) . 2 ? C3 N2 C7 118.41(17) . . ? C3 N2 Fe1 120.52(14) . . ? C7 N2 Fe1 121.07(13) . . ? N2 C3 C4 123.6(2) . . ? N2 C3 N8 112.73(17) . . ? C4 C3 N8 123.63(19) . . ? C5 C4 C3 116.4(2) . . ? C4 C5 C6 121.45(19) . . ? C7 C6 C5 116.6(2) . . ? N2 C7 C6 123.3(2) . . ? N2 C7 N13 112.67(17) . . ? C6 C7 N13 124.0(2) . . ? C12 N8 N9 110.98(17) . . ? C12 N8 C3 129.75(17) . . ? N9 N8 C3 118.08(16) . . ? C10 N9 N8 105.28(16) . . ? C10 N9 Fe1 139.45(14) . . ? N8 N9 Fe1 115.28(13) . . ? N9 C10 C11 111.07(19) . . ? C12 C11 C10 105.29(19) . . ? N8 C12 C11 107.39(18) . . ? C17 N13 N14 111.42(18) . . ? C17 N13 C7 130.26(19) . . ? N14 N13 C7 118.31(17) . . ? C15 N14 N13 104.58(18) . . ? C15 N14 Fe1 138.91(15) . . ? N13 N14 Fe1 114.69(12) . . ? N14 C15 C16 111.5(2) . . ? C17 C16 C15 105.6(2) . . ? N13 C17 C16 106.9(2) . . ? O19 Cl18 O22 110.76(17) . . ? O19 Cl18 O20 109.61(16) . . ? O22 Cl18 O20 108.03(12) . . ? O19 Cl18 O21 109.04(12) . . ? O22 Cl18 O21 110.78(17) . . ? O20 Cl18 O21 108.60(13) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.629 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.205 #=END data_c:\datasets\leeds\mh115\mh115 _database_code_depnum_ccdc_archive 'CCDC 263421' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-[2,6-dipyrazol-1-ylpyridine]iron(II) di(hexafluoroantimonate) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H18 Fe N10, 2[Sb F6]' _chemical_formula_sum 'C22 H18 F12 Fe N10 Sb2' _chemical_formula_weight 949.81 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' 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M '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 14.6737(2) _cell_length_b 9.5610(2) _cell_length_c 21.1182(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.0021(8) _cell_angle_gamma 90.00 _cell_volume 2917.75(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20739 _cell_measurement_theta_min 3.37 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'Rectangular Prism' _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 2.441 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.668 _exptl_absorpt_correction_T_max 0.742 _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 '/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 20739 _diffrn_reflns_av_R_equivalents 0.1207 _diffrn_reflns_av_sigmaI/netI 0.0546 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3330 _reflns_number_gt 3046 _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 half a formula unit, with Fe1 lying on the crystallographic C2 axis -x, y, 0.5-z. No disorder was detected during refinement, and no restraints were applied. All non-H atoms were refined anisotropically, while all H atoms were placed in calculated positions and refined using a riding 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^)+(0.0247P)^2^+4.0634P] 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 0.0018(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3330 _refine_ls_number_parameters 215 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0734 _refine_ls_wR_factor_gt 0.0710 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.0000 0.82756(5) 0.2500 0.02134(13) Uani 1 2 d S . . N2 N 0.00907(13) 0.7772(2) 0.35127(9) 0.0216(4) Uani 1 1 d . . . C3 C -0.03574(16) 0.8539(3) 0.38856(11) 0.0238(5) Uani 1 1 d . . . C4 C -0.03949(17) 0.8201(3) 0.45176(11) 0.0292(5) Uani 1 1 d . . . H4 H -0.0730 0.8759 0.4770 0.035 Uiso 1 1 calc R . . C5 C 0.00800(17) 0.7007(3) 0.47672(11) 0.0294(5) Uani 1 1 d . . . H5 H 0.0066 0.6732 0.5198 0.035 Uiso 1 1 calc R . . C6 C 0.05728(17) 0.6217(3) 0.43915(11) 0.0273(5) Uani 1 1 d . . . H6 H 0.0911 0.5411 0.4558 0.033 Uiso 1 1 calc R . . C7 C 0.05526(16) 0.6647(2) 0.37671(11) 0.0228(5) Uani 1 1 d . . . N8 N -0.07682(15) 0.9741(2) 0.35778(9) 0.0242(4) Uani 1 1 d . . . N9 N -0.06698(15) 0.9964(2) 0.29532(10) 0.0262(4) Uani 1 1 d . . . C10 C -0.10179(18) 1.1238(3) 0.28142(12) 0.0308(5) Uani 1 1 d . . . H10 H -0.1053 1.1681 0.2408 0.037 Uiso 1 1 calc R . . C11 C -0.13264(19) 1.1840(3) 0.33466(12) 0.0355(6) Uani 1 1 d . . . H11 H -0.1597 1.2737 0.3369 0.043 Uiso 1 1 calc R . . C12 C -0.11568(18) 1.0868(3) 0.38215(12) 0.0320(6) Uani 1 1 d . . . H12 H -0.1286 1.0958 0.4245 0.038 Uiso 1 1 calc R . . N13 N 0.10347(14) 0.5970(2) 0.33316(9) 0.0234(4) Uani 1 1 d . . . N14 N 0.10237(14) 0.6560(2) 0.27411(9) 0.0242(4) Uani 1 1 d . . . C15 C 0.15179(18) 0.5703(3) 0.24433(12) 0.0292(5) Uani 1 1 d . . . H15 H 0.1628 0.5841 0.2018 0.035 Uiso 1 1 calc R . . C16 C 0.1859(2) 0.4566(3) 0.28336(14) 0.0307(6) Uani 1 1 d . . . H16 H 0.2231 0.3817 0.2729 0.037 Uiso 1 1 calc R . . C17 C 0.15404(19) 0.4766(2) 0.33968(13) 0.0282(5) Uani 1 1 d . . . H17 H 0.1650 0.4178 0.3765 0.034 Uiso 1 1 calc R . . Sb18 Sb 0.228324(11) 1.035730(18) 0.420511(7) 0.02729(10) Uani 1 1 d . . . F19 F 0.18491(14) 0.95508(17) 0.33978(8) 0.0451(4) Uani 1 1 d . A 1 F20 F 0.27502(12) 1.10802(19) 0.50210(7) 0.0437(4) Uani 1 1 d . A 1 F21 F 0.34455(13) 0.95842(16) 0.41789(9) 0.0424(4) Uani 1 1 d . A 1 F22 F 0.19089(18) 0.8780(3) 0.46056(10) 0.0789(8) Uani 1 1 d . A 1 F23 F 0.11245(13) 1.1177(3) 0.41960(9) 0.0686(7) Uani 1 1 d . A 1 F24 F 0.26327(12) 1.19585(16) 0.37944(8) 0.0392(4) Uani 1 1 d . A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0280(2) 0.0209(2) 0.0155(2) 0.000 0.00478(17) 0.000 N2 0.0238(9) 0.0229(9) 0.0185(9) -0.0017(7) 0.0045(7) -0.0021(7) C3 0.0227(11) 0.0281(11) 0.0204(10) -0.0023(9) 0.0031(8) -0.0017(9) C4 0.0298(12) 0.0366(13) 0.0226(11) -0.0046(10) 0.0087(9) -0.0050(10) C5 0.0314(12) 0.0384(13) 0.0185(10) 0.0031(10) 0.0045(9) -0.0072(10) C6 0.0307(12) 0.0292(12) 0.0214(11) 0.0028(9) 0.0027(9) -0.0032(10) C7 0.0259(11) 0.0226(11) 0.0203(11) -0.0010(9) 0.0048(9) -0.0035(9) N8 0.0269(10) 0.0270(11) 0.0187(10) -0.0036(7) 0.0041(8) 0.0027(8) N9 0.0310(11) 0.0276(10) 0.0195(9) -0.0006(8) 0.0033(8) 0.0041(9) C10 0.0381(13) 0.0256(12) 0.0271(12) -0.0016(10) 0.0014(10) 0.0032(10) C11 0.0401(15) 0.0316(14) 0.0330(13) -0.0102(11) 0.0019(11) 0.0092(12) C12 0.0329(13) 0.0352(14) 0.0275(12) -0.0124(11) 0.0039(10) 0.0038(11) N13 0.0278(10) 0.0232(10) 0.0194(9) 0.0003(8) 0.0047(7) 0.0002(8) N14 0.0279(10) 0.0252(10) 0.0197(9) 0.0022(8) 0.0053(8) 0.0018(8) C15 0.0307(12) 0.0339(13) 0.0238(12) -0.0025(10) 0.0073(10) 0.0012(11) C16 0.0299(13) 0.0254(13) 0.0363(14) -0.0040(10) 0.0042(11) 0.0050(9) C17 0.0322(13) 0.0252(12) 0.0262(12) 0.0031(9) 0.0019(10) 0.0022(10) Sb18 0.02645(13) 0.03727(15) 0.01823(12) 0.00160(6) 0.00412(7) -0.00358(6) F19 0.0529(11) 0.0507(11) 0.0276(8) -0.0041(7) -0.0043(8) -0.0132(8) F20 0.0537(10) 0.0522(10) 0.0225(7) -0.0081(7) -0.0013(7) 0.0161(8) F21 0.0437(10) 0.0442(10) 0.0374(9) -0.0079(7) 0.0017(8) 0.0168(7) F22 0.0927(17) 0.0888(16) 0.0495(12) 0.0312(12) -0.0038(11) -0.0533(14) F23 0.0321(9) 0.137(2) 0.0377(10) 0.0002(12) 0.0096(8) 0.0228(11) F24 0.0518(10) 0.0312(8) 0.0351(8) 0.0046(7) 0.0085(7) 0.0002(7) _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 2.1736(18) . ? Fe1 N9 2.194(2) . ? Fe1 N14 2.223(2) . ? N2 C3 1.330(3) . ? N2 C7 1.334(3) . ? C3 C4 1.384(3) . ? C3 N8 1.404(3) . ? C4 C5 1.392(4) . ? C5 C6 1.387(4) . ? C6 C7 1.377(3) . ? C7 N13 1.411(3) . ? N8 C12 1.361(3) . ? N8 N9 1.368(3) . ? N9 C10 1.333(3) . ? C10 C11 1.406(4) . ? C11 C12 1.358(4) . ? N13 C17 1.363(3) . ? N13 N14 1.366(3) . ? N14 C15 1.323(3) . ? C15 C16 1.403(4) . ? C16 C17 1.365(4) . ? Sb18 F22 1.8583(19) . ? Sb18 F21 1.8684(17) . ? Sb18 F23 1.8694(19) . ? Sb18 F20 1.8724(15) . ? Sb18 F24 1.8744(16) . ? Sb18 F19 1.8787(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 N2 154.41(10) 2 . ? N2 Fe1 N9 71.90(7) . . ? N2 Fe1 N9 129.54(7) . 2 ? N9 Fe1 N9 85.25(12) 2 . ? N2 Fe1 N14 89.16(7) . 2 ? N9 Fe1 N14 107.87(8) . 2 ? N2 Fe1 N14 71.80(7) . . ? N9 Fe1 N14 141.18(7) . . ? N14 Fe1 N14 84.88(10) 2 . ? C3 N2 C7 118.3(2) . . ? C3 N2 Fe1 120.55(15) . . ? C7 N2 Fe1 121.00(15) . . ? N2 C3 C4 123.3(2) . . ? N2 C3 N8 113.2(2) . . ? C4 C3 N8 123.5(2) . . ? C3 C4 C5 117.1(2) . . ? C6 C5 C4 120.4(2) . . ? C7 C6 C5 117.3(2) . . ? N2 C7 C6 123.5(2) . . ? N2 C7 N13 112.6(2) . . ? C6 C7 N13 123.9(2) . . ? C12 N8 N9 111.2(2) . . ? C12 N8 C3 130.3(2) . . ? N9 N8 C3 117.74(19) . . ? C10 N9 N8 104.7(2) . . ? C10 N9 Fe1 139.42(18) . . ? N8 N9 Fe1 115.83(15) . . ? N9 C10 C11 111.2(2) . . ? C12 C11 C10 105.5(2) . . ? C11 C12 N8 107.3(2) . . ? C17 N13 N14 111.1(2) . . ? C17 N13 C7 130.3(2) . . ? N14 N13 C7 118.55(19) . . ? C15 N14 N13 104.94(19) . . ? C15 N14 Fe1 138.79(17) . . ? N13 N14 Fe1 114.47(14) . . ? N14 C15 C16 111.7(2) . . ? C17 C16 C15 105.2(2) . . ? N13 C17 C16 107.1(2) . . ? F22 Sb18 F21 92.05(11) . . ? F22 Sb18 F23 90.28(12) . . ? F21 Sb18 F23 177.31(9) . . ? F22 Sb18 F20 88.32(9) . . ? F21 Sb18 F20 89.04(7) . . ? F23 Sb18 F20 92.38(8) . . ? F22 Sb18 F24 178.71(9) . . ? F21 Sb18 F24 89.14(8) . . ? F23 Sb18 F24 88.52(10) . . ? F20 Sb18 F24 92.21(8) . . ? F22 Sb18 F19 89.97(9) . . ? F21 Sb18 F19 88.75(8) . . ? F23 Sb18 F19 89.91(9) . . ? F20 Sb18 F19 177.15(7) . . ? F24 Sb18 F19 89.55(7) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.543 _refine_diff_density_min -0.847 _refine_diff_density_rms 0.133 #=END data_c:\datasets\leeds\mh44mo~1\mh44mono _database_code_depnum_ccdc_archive 'CCDC 263422' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-bis{3-phenylpyrazol-1-yl}pyridine]iron(II) ditetrafluoroborate, alpha polymorph ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H34 Fe N10, 2[B F4]' _chemical_formula_sum 'C46 H34 B2 F8 Fe N10' _chemical_formula_weight 956.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.4920(1) _cell_length_b 25.9500(4) _cell_length_c 22.5016(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.2805(6) _cell_angle_gamma 90.00 _cell_volume 4317.43(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 49571 _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 26.00 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 0.432 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.800 _exptl_absorpt_correction_T_max 0.975 _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 crystal used had a high mosaicity of 0.72 (a well- diffracting crystal gives a mosaicity of 0.4-0.5 under our conditions). This accounts for the poor quality of the data and the refinement. ; _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 49571 _diffrn_reflns_av_R_equivalents 0.1164 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8465 _reflns_number_gt 7174 _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 BF~4~^-^ anions are disordered over two orientations: B58A-F62A (refined occupancy 0.80) and B58B-F62B (0.20) B63A-F67A (refined occupancy 0.74) and B63B-F67B (0.26) All BF distances were restrained to 1.39(2)\%A in the final model, and non-bonded F...F distances within a given disorder orientation to 2.27(2)\%A. All non-H atoms except the two minor anion disorder sites were refined anisotropically, while all H atoms were placed in calculated positions and refined using a riding 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^)+(0.0001P)^2^+52.3169P] 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 8465 _refine_ls_number_parameters 645 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.1410 _refine_ls_R_factor_gt 0.1278 _refine_ls_wR_factor_ref 0.2913 _refine_ls_wR_factor_gt 0.2848 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.166 _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 0.50253(14) 0.12591(4) 0.24559(4) 0.0261(3) Uani 1 1 d . . . N2 N 0.5293(8) 0.0442(2) 0.2532(3) 0.0289(13) Uani 1 1 d . . . C3 C 0.4370(12) 0.0134(3) 0.2114(3) 0.0352(17) Uani 1 1 d . . . C4 C 0.4483(13) -0.0393(3) 0.2135(4) 0.046(2) Uani 1 1 d . . . H4 H 0.3801 -0.0605 0.1838 0.055 Uiso 1 1 calc R . . C5 C 0.5663(14) -0.0599(3) 0.2622(4) 0.053(2) Uani 1 1 d . . . H5 H 0.5783 -0.0963 0.2654 0.063 Uiso 1 1 calc R . . C6 C 0.6657(13) -0.0295(3) 0.3057(4) 0.045(2) Uani 1 1 d . . . H6 H 0.7469 -0.0438 0.3383 0.054 Uiso 1 1 calc R . . C7 C 0.6394(11) 0.0236(3) 0.2986(3) 0.0340(17) Uani 1 1 d . . . N8 N 0.3244(9) 0.0411(2) 0.1659(3) 0.0310(13) Uani 1 1 d . . . N9 N 0.2976(8) 0.0932(2) 0.1749(3) 0.0272(13) Uani 1 1 d . . . C10 C 0.1970(10) 0.1089(3) 0.1227(3) 0.0306(16) Uani 1 1 d . . . C11 C 0.1624(11) 0.0679(3) 0.0805(3) 0.0379(19) Uani 1 1 d . . . H11 H 0.0970 0.0693 0.0407 0.045 Uiso 1 1 calc R . . C12 C 0.2435(11) 0.0263(3) 0.1099(3) 0.0381(19) Uani 1 1 d . . . H12 H 0.2439 -0.0076 0.0940 0.046 Uiso 1 1 calc R . . C13 C 0.1431(10) 0.1635(3) 0.1153(3) 0.0329(16) Uani 1 1 d . . . C14 C 0.1005(10) 0.1920(3) 0.1641(4) 0.0354(17) Uani 1 1 d . . . H14 H 0.1038 0.1759 0.2022 0.043 Uiso 1 1 calc R . . C15 C 0.0539(12) 0.2432(4) 0.1570(4) 0.050(2) Uani 1 1 d . . . H15 H 0.0245 0.2625 0.1899 0.060 Uiso 1 1 calc R . . C16 C 0.0505(14) 0.2661(4) 0.1011(5) 0.061(3) Uani 1 1 d . . . H16 H 0.0216 0.3017 0.0961 0.073 Uiso 1 1 calc R . . C17 C 0.0878(13) 0.2384(4) 0.0533(5) 0.056(3) Uani 1 1 d . . . H17 H 0.0830 0.2548 0.0154 0.067 Uiso 1 1 calc R . . C18 C 0.1333(11) 0.1860(4) 0.0591(4) 0.044(2) Uani 1 1 d . . . H18 H 0.1567 0.1665 0.0254 0.053 Uiso 1 1 calc R . . N19 N 0.7303(9) 0.0596(3) 0.3387(3) 0.0364(15) Uani 1 1 d . . . N20 N 0.7265(9) 0.1103(2) 0.3225(3) 0.0338(14) Uani 1 1 d . . . C21 C 0.8127(10) 0.1353(3) 0.3705(3) 0.0348(17) Uani 1 1 d . . . C22 C 0.8687(11) 0.1009(4) 0.4177(4) 0.045(2) Uani 1 1 d . . . H22 H 0.9317 0.1091 0.4567 0.055 Uiso 1 1 calc R . . C23 C 0.8148(11) 0.0535(4) 0.3967(3) 0.0413(19) Uani 1 1 d . . . H23 H 0.8326 0.0220 0.4183 0.050 Uiso 1 1 calc R . . C24 C 0.8418(11) 0.1917(3) 0.3697(3) 0.0391(19) Uani 1 1 d . . . C25 C 0.8462(12) 0.2201(4) 0.4231(4) 0.048(2) Uani 1 1 d . . . H25 H 0.8290 0.2033 0.4593 0.058 Uiso 1 1 calc R . . C26 C 0.8758(14) 0.2726(4) 0.4225(5) 0.061(3) Uani 1 1 d . . . H26 H 0.8789 0.2921 0.4584 0.073 Uiso 1 1 calc R . . C27 C 0.9011(14) 0.2972(4) 0.3693(5) 0.062(3) Uani 1 1 d . . . H27 H 0.9223 0.3333 0.3694 0.074 Uiso 1 1 calc R . . C28 C 0.8956(13) 0.2699(4) 0.3171(5) 0.057(3) Uani 1 1 d . . . H28 H 0.9104 0.2871 0.2810 0.068 Uiso 1 1 calc R . . C29 C 0.8687(11) 0.2172(3) 0.3171(4) 0.043(2) Uani 1 1 d . . . H29 H 0.8683 0.1982 0.2810 0.052 Uiso 1 1 calc R . . N30 N 0.4757(8) 0.2071(2) 0.2441(3) 0.0292(13) Uani 1 1 d . . . C31 C 0.5241(11) 0.2354(3) 0.1995(4) 0.0367(18) Uani 1 1 d . . . C32 C 0.5139(13) 0.2886(3) 0.1967(5) 0.050(2) Uani 1 1 d . . . H32 H 0.5514 0.3075 0.1648 0.060 Uiso 1 1 calc R . . C33 C 0.4455(15) 0.3127(3) 0.2434(5) 0.058(3) Uani 1 1 d . . . H33 H 0.4354 0.3492 0.2434 0.070 Uiso 1 1 calc R . . C34 C 0.3917(13) 0.2849(3) 0.2899(4) 0.048(2) Uani 1 1 d . . . H34 H 0.3450 0.3014 0.3219 0.057 Uiso 1 1 calc R . . C35 C 0.4095(11) 0.2321(3) 0.2876(3) 0.0350(17) Uani 1 1 d . . . N36 N 0.5929(9) 0.2050(3) 0.1561(3) 0.0359(15) Uani 1 1 d . . . N37 N 0.6301(9) 0.1547(3) 0.1697(3) 0.0354(15) Uani 1 1 d . . . C38 C 0.6764(10) 0.1349(3) 0.1184(3) 0.0367(18) Uani 1 1 d . . . C39 C 0.6673(11) 0.1729(4) 0.0738(4) 0.042(2) Uani 1 1 d . . . H39 H 0.6915 0.1687 0.0339 0.051 Uiso 1 1 calc R . . C40 C 0.6175(12) 0.2165(4) 0.0986(4) 0.051(2) Uani 1 1 d . . . H40 H 0.6022 0.2494 0.0798 0.061 Uiso 1 1 calc R . . C41 C 0.7273(11) 0.0807(4) 0.1176(3) 0.044(2) Uani 1 1 d . . . C42 C 0.8229(11) 0.0564(4) 0.1690(4) 0.044(2) Uani 1 1 d . . . H42 H 0.8608 0.0758 0.2046 0.053 Uiso 1 1 calc R . . C43 C 0.8619(13) 0.0038(4) 0.1677(5) 0.056(2) Uani 1 1 d . . . H43 H 0.9251 -0.0127 0.2026 0.067 Uiso 1 1 calc R . . C44 C 0.8072(15) -0.0245(4) 0.1147(5) 0.064(3) Uani 1 1 d . . . H44 H 0.8334 -0.0602 0.1134 0.076 Uiso 1 1 calc R . . C45 C 0.7171(13) -0.0005(5) 0.0657(5) 0.063(3) Uani 1 1 d . . . H45 H 0.6792 -0.0201 0.0302 0.076 Uiso 1 1 calc R . . C46 C 0.6779(12) 0.0516(4) 0.0654(4) 0.049(2) Uani 1 1 d . . . H46 H 0.6176 0.0675 0.0297 0.058 Uiso 1 1 calc R . . N47 N 0.3584(9) 0.1993(2) 0.3308(3) 0.0344(14) Uani 1 1 d . . . N48 N 0.3475(9) 0.1469(2) 0.3191(3) 0.0304(13) Uani 1 1 d . . . C49 C 0.3069(10) 0.1256(3) 0.3686(3) 0.0348(17) Uani 1 1 d . . . C50 C 0.2946(12) 0.1632(4) 0.4132(4) 0.044(2) Uani 1 1 d . . . H50 H 0.2696 0.1576 0.4528 0.053 Uiso 1 1 calc R . . C51 C 0.3265(12) 0.2095(4) 0.3875(4) 0.045(2) Uani 1 1 d . . . H51 H 0.3263 0.2425 0.4058 0.054 Uiso 1 1 calc R . . C52 C 0.2794(11) 0.0693(3) 0.3732(4) 0.0351(17) Uani 1 1 d . . . C53 C 0.2000(11) 0.0407(3) 0.3237(4) 0.0415(19) Uani 1 1 d . . . H53 H 0.1615 0.0575 0.2863 0.050 Uiso 1 1 calc R . . C54 C 0.1766(13) -0.0120(4) 0.3285(4) 0.052(2) Uani 1 1 d . . . H54 H 0.1281 -0.0317 0.2940 0.062 Uiso 1 1 calc R . . C55 C 0.2244(14) -0.0358(4) 0.3836(5) 0.060(3) Uani 1 1 d . . . H55 H 0.2073 -0.0719 0.3872 0.072 Uiso 1 1 calc R . . C56 C 0.2982(15) -0.0069(4) 0.4344(5) 0.065(3) Uani 1 1 d . . . H56 H 0.3289 -0.0232 0.4725 0.078 Uiso 1 1 calc R . . C57 C 0.3262(12) 0.0457(4) 0.4286(4) 0.046(2) Uani 1 1 d . . . H57 H 0.3774 0.0654 0.4626 0.055 Uiso 1 1 calc R . . B58A B 0.2113(15) 0.1224(4) 0.5752(4) 0.035(2) Uani 0.80 1 d PD A 1 F59A F 0.3782(9) 0.1212(3) 0.5537(3) 0.0583(18) Uani 0.80 1 d PD A 1 F60A F 0.1292(14) 0.0759(3) 0.5643(6) 0.052(3) Uani 0.80 1 d PD A 1 F61A F 0.1107(11) 0.1627(2) 0.5443(3) 0.0527(18) Uani 0.80 1 d PD A 1 F62A F 0.2489(11) 0.1343(3) 0.6363(2) 0.0483(17) Uani 0.80 1 d PD A 1 B58B B 0.119(4) 0.1234(11) 0.5732(12) 0.043(14) Uiso 0.20 1 d PD B 2 F59B F 0.227(5) 0.1571(13) 0.5467(14) 0.081(11) Uiso 0.20 1 d PD B 2 F60B F 0.141(7) 0.0741(12) 0.552(2) 0.08(3) Uiso 0.20 1 d PD B 2 F61B F -0.060(4) 0.1382(16) 0.5591(16) 0.115(14) Uiso 0.20 1 d PD B 2 F62B F 0.164(4) 0.1234(12) 0.6351(10) 0.050(9) Uiso 0.20 1 d PD B 2 B63A B 0.317(2) 0.3789(4) 0.4175(5) 0.033(3) Uani 0.74 1 d PD C 1 F64A F 0.341(2) 0.3840(6) 0.3583(4) 0.065(6) Uani 0.74 1 d PD C 1 F65A F 0.3210(18) 0.3273(3) 0.4339(6) 0.056(4) Uani 0.74 1 d PD C 1 F66A F 0.1479(10) 0.4003(2) 0.4229(3) 0.0547(19) Uani 0.74 1 d PD C 1 F67A F 0.4472(12) 0.4046(3) 0.4553(3) 0.062(2) Uani 0.74 1 d PD C 1 B63B B 0.380(3) 0.3743(10) 0.4186(11) 0.046(16) Uiso 0.26 1 d PD D 2 F64B F 0.348(3) 0.3894(15) 0.3589(9) 0.024(8) Uiso 0.26 1 d PD D 2 F65B F 0.303(4) 0.4098(9) 0.4531(11) 0.080(7) Uiso 0.26 1 d PD D 2 F66B F 0.301(4) 0.3262(9) 0.4240(16) 0.037(9) Uiso 0.26 1 d PD D 2 F67B F 0.562(3) 0.3715(12) 0.4389(13) 0.108(10) Uiso 0.26 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 Fe1 0.0330(6) 0.0218(5) 0.0229(5) -0.0023(4) 0.0026(4) -0.0010(4) N2 0.032(3) 0.023(3) 0.029(3) 0.001(2) -0.002(2) 0.002(2) C3 0.051(5) 0.021(4) 0.034(4) 0.002(3) 0.005(3) -0.002(3) C4 0.069(6) 0.020(4) 0.047(5) -0.003(3) 0.003(4) -0.007(4) C5 0.073(7) 0.030(4) 0.053(5) 0.001(4) 0.002(5) 0.007(4) C6 0.056(5) 0.031(4) 0.045(5) 0.011(4) 0.001(4) 0.005(4) C7 0.039(4) 0.030(4) 0.032(4) -0.002(3) 0.002(3) 0.005(3) N8 0.039(3) 0.025(3) 0.028(3) -0.003(2) 0.001(3) -0.008(3) N9 0.028(3) 0.021(3) 0.032(3) -0.001(2) 0.001(2) -0.004(2) C10 0.029(4) 0.040(4) 0.022(3) 0.002(3) 0.002(3) -0.003(3) C11 0.036(4) 0.058(5) 0.017(3) 0.004(3) -0.003(3) -0.012(4) C12 0.047(5) 0.040(4) 0.026(4) -0.008(3) 0.001(3) -0.017(4) C13 0.027(4) 0.035(4) 0.035(4) 0.004(3) 0.000(3) 0.000(3) C14 0.034(4) 0.032(4) 0.038(4) 0.005(3) 0.001(3) 0.008(3) C15 0.044(5) 0.046(5) 0.058(6) -0.011(4) 0.003(4) 0.015(4) C16 0.051(6) 0.044(5) 0.086(8) 0.028(5) 0.006(5) 0.011(4) C17 0.050(6) 0.060(6) 0.057(6) 0.032(5) 0.007(5) 0.008(5) C18 0.035(4) 0.061(6) 0.034(4) 0.006(4) -0.001(3) -0.001(4) N19 0.035(3) 0.044(4) 0.028(3) 0.001(3) -0.001(3) 0.004(3) N20 0.035(3) 0.035(3) 0.030(3) -0.002(3) 0.001(3) -0.001(3) C21 0.031(4) 0.048(5) 0.024(3) -0.005(3) 0.000(3) 0.002(3) C22 0.037(5) 0.066(6) 0.032(4) -0.008(4) 0.001(3) -0.001(4) C23 0.043(5) 0.054(5) 0.024(4) 0.009(4) 0.000(3) 0.004(4) C24 0.031(4) 0.054(5) 0.031(4) -0.011(4) 0.000(3) -0.008(4) C25 0.051(5) 0.060(6) 0.033(4) -0.023(4) 0.005(4) -0.004(4) C26 0.058(6) 0.060(6) 0.061(6) -0.035(5) 0.000(5) -0.008(5) C27 0.056(6) 0.058(6) 0.068(7) -0.028(5) 0.001(5) -0.014(5) C28 0.042(5) 0.056(6) 0.071(7) -0.013(5) 0.005(5) -0.017(4) C29 0.038(4) 0.050(5) 0.041(5) -0.011(4) 0.002(4) -0.009(4) N30 0.033(3) 0.025(3) 0.028(3) -0.007(2) -0.003(2) -0.005(2) C31 0.044(5) 0.030(4) 0.035(4) 0.007(3) 0.005(3) -0.006(3) C32 0.058(6) 0.030(4) 0.062(6) 0.006(4) 0.010(5) -0.014(4) C33 0.069(7) 0.024(4) 0.077(7) -0.001(4) -0.004(5) -0.009(4) C34 0.052(5) 0.037(5) 0.052(5) -0.015(4) 0.004(4) 0.000(4) C35 0.037(4) 0.030(4) 0.035(4) -0.009(3) -0.005(3) -0.006(3) N36 0.039(4) 0.036(4) 0.032(3) 0.006(3) 0.004(3) -0.010(3) N37 0.034(3) 0.042(4) 0.031(3) -0.004(3) 0.004(3) -0.002(3) C38 0.026(4) 0.061(5) 0.023(3) -0.005(3) 0.002(3) -0.006(4) C39 0.033(4) 0.065(6) 0.028(4) 0.007(4) 0.000(3) -0.001(4) C40 0.042(5) 0.075(7) 0.034(4) 0.015(4) 0.003(4) -0.009(5) C41 0.034(4) 0.072(6) 0.027(4) -0.002(4) 0.011(3) -0.004(4) C42 0.037(4) 0.060(6) 0.035(4) -0.011(4) 0.007(3) 0.001(4) C43 0.048(5) 0.067(7) 0.053(6) 0.000(5) 0.012(4) 0.012(5) C44 0.057(6) 0.052(6) 0.087(8) -0.018(6) 0.027(6) 0.004(5) C45 0.045(5) 0.093(8) 0.050(6) -0.030(6) 0.003(5) -0.002(5) C46 0.042(5) 0.057(6) 0.047(5) -0.017(4) 0.009(4) 0.005(4) N47 0.041(4) 0.031(3) 0.031(3) -0.009(3) 0.006(3) 0.002(3) N48 0.038(3) 0.028(3) 0.025(3) -0.002(2) 0.006(3) 0.005(3) C49 0.031(4) 0.045(4) 0.028(4) -0.003(3) 0.003(3) 0.003(3) C50 0.042(5) 0.064(6) 0.025(4) -0.012(4) 0.000(3) 0.006(4) C51 0.050(5) 0.052(5) 0.035(4) -0.016(4) 0.012(4) 0.007(4) C52 0.034(4) 0.035(4) 0.037(4) 0.010(3) 0.009(3) 0.000(3) C53 0.039(4) 0.049(5) 0.036(4) 0.008(4) 0.003(3) -0.002(4) C54 0.057(6) 0.044(5) 0.055(6) 0.006(4) 0.012(5) -0.013(4) C55 0.060(6) 0.053(6) 0.067(7) 0.019(5) 0.009(5) -0.010(5) C56 0.071(7) 0.062(7) 0.061(7) 0.035(5) 0.008(5) 0.001(5) C57 0.048(5) 0.053(5) 0.036(4) 0.007(4) 0.005(4) 0.003(4) B58A 0.048(8) 0.027(5) 0.029(5) 0.005(4) 0.002(5) -0.006(5) F59A 0.067(5) 0.046(4) 0.066(4) -0.015(3) 0.022(4) -0.013(3) F60A 0.066(6) 0.032(4) 0.054(5) 0.005(3) 0.003(4) -0.006(3) F61A 0.077(5) 0.039(3) 0.036(3) 0.011(3) -0.009(3) 0.017(3) F62A 0.074(6) 0.043(4) 0.027(3) 0.001(3) 0.004(3) 0.013(4) B63A 0.055(10) 0.017(6) 0.028(6) -0.003(4) 0.012(5) 0.000(6) F64A 0.114(11) 0.041(7) 0.038(5) 0.002(3) 0.009(4) 0.022(5) F65A 0.083(8) 0.031(4) 0.044(6) 0.007(3) -0.022(5) -0.009(4) F66A 0.073(5) 0.034(4) 0.062(5) 0.005(3) 0.028(4) 0.012(3) F67A 0.074(6) 0.060(5) 0.044(4) -0.007(3) -0.011(4) -0.035(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 N30 2.117(6) . ? Fe1 N2 2.134(6) . ? Fe1 N9 2.195(6) . ? Fe1 N37 2.217(7) . ? Fe1 N48 2.235(6) . ? Fe1 N20 2.245(6) . ? N2 C7 1.317(9) . ? N2 C3 1.338(9) . ? C3 C4 1.371(10) . ? C3 N8 1.413(10) . ? C4 C5 1.398(13) . ? C5 C6 1.377(13) . ? C6 C7 1.399(11) . ? C7 N19 1.398(10) . ? N8 C12 1.364(9) . ? N8 N9 1.387(8) . ? N9 C10 1.352(9) . ? C10 C11 1.421(11) . ? C10 C13 1.475(11) . ? C11 C12 1.357(12) . ? C13 C18 1.385(11) . ? C13 C14 1.402(11) . ? C14 C15 1.375(11) . ? C15 C16 1.389(14) . ? C16 C17 1.358(15) . ? C17 C18 1.404(13) . ? N19 C23 1.365(9) . ? N19 N20 1.365(9) . ? N20 C21 1.334(9) . ? C21 C22 1.398(12) . ? C21 C24 1.481(12) . ? C22 C23 1.356(13) . ? C24 C29 1.399(12) . ? C24 C25 1.406(11) . ? C25 C26 1.381(14) . ? C26 C27 1.397(16) . ? C27 C28 1.367(14) . ? C28 C29 1.382(13) . ? N30 C35 1.336(10) . ? N30 C31 1.339(10) . ? C31 C32 1.383(11) . ? C31 N36 1.417(11) . ? C32 C33 1.390(14) . ? C33 C34 1.383(14) . ? C34 C35 1.380(11) . ? C35 N47 1.392(10) . ? N36 N37 1.360(9) . ? N36 C40 1.367(10) . ? N37 C38 1.360(10) . ? C38 C39 1.402(12) . ? C38 C41 1.458(13) . ? C39 C40 1.342(14) . ? C41 C46 1.394(12) . ? C41 C42 1.408(12) . ? C42 C43 1.396(13) . ? C43 C44 1.404(14) . ? C44 C45 1.348(16) . ? C45 C46 1.385(15) . ? N47 C51 1.361(10) . ? N47 N48 1.386(8) . ? N48 C49 1.322(10) . ? C49 C50 1.415(11) . ? C49 C52 1.483(11) . ? C50 C51 1.370(13) . ? C52 C57 1.380(11) . ? C52 C53 1.389(12) . ? C53 C54 1.386(12) . ? C54 C55 1.380(13) . ? C55 C56 1.403(15) . ? C56 C57 1.390(14) . ? B58A F60A 1.358(11) . ? B58A F62A 1.393(10) . ? B58A F61A 1.405(10) . ? B58A F59A 1.412(12) . ? B58B F62B 1.379(18) . ? B58B F61B 1.382(18) . ? B58B F60B 1.387(18) . ? B58B F59B 1.388(18) . ? B63A F67A 1.359(12) . ? B63A F64A 1.378(12) . ? B63A F65A 1.388(11) . ? B63A F66A 1.410(14) . ? B63B F67B 1.373(18) . ? B63B F64B 1.384(18) . ? B63B F65B 1.387(18) . ? B63B F66B 1.393(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 N30 Fe1 N2 176.3(2) . . ? N30 Fe1 N9 108.6(2) . . ? N2 Fe1 N9 73.7(2) . . ? N30 Fe1 N37 72.7(2) . . ? N2 Fe1 N37 110.5(2) . . ? N9 Fe1 N37 84.9(2) . . ? N30 Fe1 N48 73.2(2) . . ? N2 Fe1 N48 103.6(2) . . ? N9 Fe1 N48 104.1(2) . . ? N37 Fe1 N48 145.8(2) . . ? N30 Fe1 N20 104.4(2) . . ? N2 Fe1 N20 73.2(2) . . ? N9 Fe1 N20 146.9(2) . . ? N37 Fe1 N20 107.0(2) . . ? N48 Fe1 N20 83.5(2) . . ? C7 N2 C3 119.4(6) . . ? C7 N2 Fe1 120.3(5) . . ? C3 N2 Fe1 120.3(5) . . ? N2 C3 C4 123.3(7) . . ? N2 C3 N8 112.8(6) . . ? C4 C3 N8 124.0(7) . . ? C3 C4 C5 115.9(8) . . ? C6 C5 C4 122.6(8) . . ? C5 C6 C7 115.6(8) . . ? N2 C7 N19 114.1(6) . . ? N2 C7 C6 123.2(7) . . ? N19 C7 C6 122.6(7) . . ? C12 N8 N9 110.9(6) . . ? C12 N8 C3 130.6(7) . . ? N9 N8 C3 118.3(6) . . ? C10 N9 N8 103.9(6) . . ? C10 N9 Fe1 137.7(5) . . ? N8 N9 Fe1 112.4(4) . . ? N9 C10 C11 111.8(7) . . ? N9 C10 C13 119.4(6) . . ? C11 C10 C13 128.8(7) . . ? C12 C11 C10 104.5(6) . . ? C11 C12 N8 108.9(7) . . ? C18 C13 C14 120.5(8) . . ? C18 C13 C10 118.7(7) . . ? C14 C13 C10 120.8(7) . . ? C15 C14 C13 120.3(8) . . ? C14 C15 C16 119.1(9) . . ? C17 C16 C15 120.9(9) . . ? C16 C17 C18 121.2(9) . . ? C13 C18 C17 117.9(9) . . ? C23 N19 N20 110.7(7) . . ? C23 N19 C7 130.0(7) . . ? N20 N19 C7 119.0(6) . . ? C21 N20 N19 105.4(6) . . ? C21 N20 Fe1 137.9(5) . . ? N19 N20 Fe1 111.1(4) . . ? N20 C21 C22 110.6(7) . . ? N20 C21 C24 121.5(7) . . ? C22 C21 C24 127.8(7) . . ? C23 C22 C21 106.1(7) . . ? C22 C23 N19 107.1(8) . . ? C29 C24 C25 119.3(8) . . ? C29 C24 C21 121.3(7) . . ? C25 C24 C21 119.4(8) . . ? C26 C25 C24 119.4(9) . . ? C25 C26 C27 120.3(9) . . ? C28 C27 C26 120.6(10) . . ? C27 C28 C29 119.9(11) . . ? C28 C29 C24 120.5(9) . . ? C35 N30 C31 117.4(7) . . ? C35 N30 Fe1 121.1(5) . . ? C31 N30 Fe1 121.5(5) . . ? N30 C31 C32 124.2(8) . . ? N30 C31 N36 112.6(7) . . ? C32 C31 N36 123.2(8) . . ? C31 C32 C33 116.1(8) . . ? C34 C33 C32 121.7(8) . . ? C35 C34 C33 116.6(9) . . ? N30 C35 C34 124.0(8) . . ? N30 C35 N47 113.1(6) . . ? C34 C35 N47 122.9(8) . . ? N37 N36 C40 111.7(7) . . ? N37 N36 C31 117.5(6) . . ? C40 N36 C31 130.6(8) . . ? C38 N37 N36 104.0(6) . . ? C38 N37 Fe1 136.7(6) . . ? N36 N37 Fe1 113.6(5) . . ? N37 C38 C39 110.6(8) . . ? N37 C38 C41 118.6(7) . . ? C39 C38 C41 130.7(7) . . ? C40 C39 C38 106.3(8) . . ? C39 C40 N36 107.4(8) . . ? C46 C41 C42 118.7(9) . . ? C46 C41 C38 119.9(8) . . ? C42 C41 C38 121.4(8) . . ? C43 C42 C41 120.1(8) . . ? C42 C43 C44 119.6(10) . . ? C45 C44 C43 119.5(10) . . ? C44 C45 C46 122.2(9) . . ? C45 C46 C41 119.8(9) . . ? C51 N47 N48 110.9(7) . . ? C51 N47 C35 130.2(7) . . ? N48 N47 C35 118.8(6) . . ? C49 N48 N47 105.3(6) . . ? C49 N48 Fe1 137.7(5) . . ? N47 N48 Fe1 111.0(4) . . ? N48 C49 C50 111.1(8) . . ? N48 C49 C52 121.6(7) . . ? C50 C49 C52 127.2(7) . . ? C51 C50 C49 105.6(7) . . ? N47 C51 C50 107.1(7) . . ? C57 C52 C53 120.0(8) . . ? C57 C52 C49 118.9(8) . . ? C53 C52 C49 121.0(7) . . ? C54 C53 C52 120.5(8) . . ? C55 C54 C53 119.5(9) . . ? C54 C55 C56 120.3(9) . . ? C57 C56 C55 119.6(9) . . ? C52 C57 C56 120.0(9) . . ? F60A B58A F62A 112.9(9) . . ? F60A B58A F61A 112.4(9) . . ? F62A B58A F61A 109.2(8) . . ? F60A B58A F59A 108.6(9) . . ? F62A B58A F59A 107.1(8) . . ? F61A B58A F59A 106.4(8) . . ? F62B B58B F61B 107.7(17) . . ? F62B B58B F60B 109.4(17) . . ? F61B B58B F60B 109.9(18) . . ? F62B B58B F59B 111.6(17) . . ? F61B B58B F59B 109.6(17) . . ? F60B B58B F59B 108.6(17) . . ? F67A B63A F64A 111.4(11) . . ? F67A B63A F65A 109.0(10) . . ? F64A B63A F65A 110.5(10) . . ? F67A B63A F66A 108.4(9) . . ? F64A B63A F66A 107.7(11) . . ? F65A B63A F66A 109.7(10) . . ? F67B B63B F64B 110.0(17) . . ? F67B B63B F65B 109.2(17) . . ? F64B B63B F65B 109.4(17) . . ? F67B B63B F66B 109.7(17) . . ? F64B B63B F66B 109.3(17) . . ? F65B B63B F66B 109.2(17) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.740 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.127 #================================================================= data_c:\datasets\leeds\mh44\mh44 _database_code_depnum_ccdc_archive 'CCDC 263423' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-bis{3-phenylpyrazol-1-yl}pyridine]iron(II) ditetrafluoroborate, beta polymorph ; _chemical_name_common ; Bis(2,6-bis(3-phenylpyrazol-1-yl)pyridine)iron(ii) ditetrafluoroborate, beta polymorph ; _chemical_melting_point ? _chemical_formula_moiety 'C46 H34 Fe N10, 2[B F4]' _chemical_formula_sum 'C46 H34 B2 F8 Fe N10' _chemical_formula_weight 956.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 'F d d d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, -y+1/4, z' 'x, -y+1/4, -z+1/4' '-x+1/4, y, -z+1/4' 'x, y+1/2, z+1/2' '-x+1/4, -y+3/4, z+1/2' 'x, -y+3/4, -z+3/4' '-x+1/4, y+1/2, -z+3/4' 'x+1/2, y, z+1/2' '-x+3/4, -y+1/4, z+1/2' 'x+1/2, -y+1/4, -z+3/4' '-x+3/4, y, -z+3/4' 'x+1/2, y+1/2, z' '-x+3/4, -y+3/4, z' 'x+1/2, -y+3/4, -z+1/4' '-x+3/4, y+1/2, -z+1/4' '-x, -y, -z' 'x-1/4, y-1/4, -z' '-x, y-1/4, z-1/4' 'x-1/4, -y, z-1/4' '-x, -y+1/2, -z+1/2' 'x-1/4, y+1/4, -z+1/2' '-x, y+1/4, z+1/4' 'x-1/4, -y+1/2, z+1/4' '-x+1/2, -y, -z+1/2' 'x+1/4, y-1/4, -z+1/2' '-x+1/2, y-1/4, z+1/4' 'x+1/4, -y, z+1/4' '-x+1/2, -y+1/2, -z' 'x+1/4, y+1/4, -z' '-x+1/2, y+1/4, z-1/4' 'x+1/4, -y+1/2, z-1/4' _cell_length_a 7.6246(15) _cell_length_b 26.370(4) _cell_length_c 44.091(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8865(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10080 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 27.49 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3904 _exptl_absorpt_coefficient_mu 0.421 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 0.971 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 293(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 10080 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2539 _reflns_number_gt 1955 _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 asymmetric unit contains a quarter of a complex dication with Fe1 lying on the 222 site 0.125, 0.125, 0.125 and N2 and C5 on the C2 axis 0.125, y, 0.125; and, half a BF~4~^-^ anion lying on the ?? site 0.375, 0.375, z. The BF~4~^-^ ion is badly disordered. Three equally occupied orientations of F atoms were refined, labelled 'A', 'B' and 'C', using the restraints B---F = 1.39(2) and F...F = 2.27(2)\%A. Attempts to refine different partial B sites to go with these disorder orientations led to at least one partial B atom in all cases having a high thermal parameter of >0.3. Hence, only one fully occupied B atom was included in the final model. The rather non-tetrahedral geometries of the final partial BF~4~^-^ environments mean that this model is only an approximation of the true positioning of this anion in the crystal, however. All non-disordered non-H atoms were refined anisotropically, and all H atoms were placed in calculated positions and refined using a riding model. The non-sequential atom numbering scheme has been chosen to correspond with the numbering used in the alpha polymorph of the same compound. ; _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^)+(0.0646P)^2^+6.5066P] 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 2539 _refine_ls_number_parameters 183 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1226 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.150 _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 0.1250 0.1250 0.1250 0.0452(2) Uani 1 4 d S . . N2 N 0.1250 0.20516(9) 0.1250 0.0535(6) Uani 1 2 d S . . C3 C 0.2043(3) 0.23112(8) 0.14683(5) 0.0680(6) Uani 1 1 d . . . C4 C 0.2078(5) 0.28326(10) 0.14768(8) 0.1014(10) Uani 1 1 d . . . H4 H 0.2648 0.3006 0.1632 0.122 Uiso 1 1 calc R . . C5 C 0.1250 0.30847(16) 0.1250 0.1170(18) Uani 1 2 d S . . H5 H 0.1250 0.3437 0.1250 0.140 Uiso 1 2 calc SR . . N8 N 0.2850(3) 0.20012(7) 0.16837(4) 0.0638(5) Uani 1 1 d . . . N9 N 0.3013(2) 0.14941(7) 0.16225(4) 0.0554(4) Uani 1 1 d . . . C10 C 0.3711(3) 0.12935(10) 0.18731(4) 0.0624(6) Uani 1 1 d . . . C11 C 0.3963(3) 0.16753(14) 0.20939(5) 0.0818(8) Uani 1 1 d . . . H11 H 0.4411 0.1633 0.2288 0.098 Uiso 1 1 calc R . . C12 C 0.3430(4) 0.21095(13) 0.19673(6) 0.0830(8) Uani 1 1 d . . . H12 H 0.3452 0.2428 0.2057 0.100 Uiso 1 1 calc R . . C13 C 0.4106(3) 0.07543(11) 0.18907(5) 0.0695(6) Uani 1 1 d . . . C14 C 0.4710(3) 0.04894(11) 0.16404(6) 0.0806(7) Uani 1 1 d . . . H14 H 0.4879 0.0658 0.1457 0.097 Uiso 1 1 calc R . . C15 C 0.5064(5) -0.00214(14) 0.16608(8) 0.1039(10) Uani 1 1 d . . . H15 H 0.5462 -0.0197 0.1491 0.125 Uiso 1 1 calc R . . C16 C 0.4830(5) -0.02733(15) 0.19317(11) 0.1203(13) Uani 1 1 d . . . H16 H 0.5052 -0.0619 0.1945 0.144 Uiso 1 1 calc R . . C17 C 0.4268(5) -0.00099(18) 0.21796(9) 0.1192(13) Uani 1 1 d . . . H17 H 0.4127 -0.0178 0.2363 0.143 Uiso 1 1 calc R . . C18 C 0.3907(4) 0.04997(15) 0.21629(7) 0.0905(9) Uani 1 1 d . . . H18 H 0.3530 0.0673 0.2334 0.109 Uiso 1 1 calc R . . B19 B 0.3750 0.3750 0.20828(9) 0.0953(17) Uani 1 2 d SD . . F20A F 0.3296(19) 0.4216(4) 0.2221(3) 0.049(2) Uiso 0.17 1 d PD . 1 F21A F 0.5872(11) 0.3903(4) 0.2139(3) 0.074(2) Uiso 0.17 1 d PD . 1 F22A F 0.3750 0.3750 0.17912(13) 0.0607(18) Uiso 0.33 2 d SPD . 1 F23A F 0.3562(17) 0.3373(3) 0.2274(2) 0.057(2) Uiso 0.17 1 d PD . 1 F20B F 0.300(2) 0.4094(5) 0.2276(3) 0.085(5) Uiso 0.17 1 d PD . 2 F21B F 0.5555(18) 0.3864(7) 0.2016(5) 0.170(8) Uiso 0.17 1 d PD . 2 F22B F 0.2715(17) 0.3860(6) 0.1813(3) 0.085(5) Uiso 0.17 1 d PD . 2 F23B F 0.3604(19) 0.3268(3) 0.2176(2) 0.049(2) Uiso 0.17 1 d PD . 2 F20C F 0.1937(18) 0.3802(7) 0.2236(3) 0.128(5) Uiso 0.17 1 d PD . 3 F21C F 0.479(2) 0.4125(5) 0.2185(3) 0.094(3) Uiso 0.17 1 d PD . 3 F22C F 0.3101(18) 0.3871(4) 0.1785(2) 0.057(3) Uiso 0.17 1 d PD . 3 F23C F 0.429(2) 0.3295(4) 0.2110(3) 0.107(5) Uiso 0.17 1 d PD . 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 0.0466(3) 0.0453(3) 0.0437(3) 0.000 0.000 0.000 N2 0.0585(15) 0.0470(12) 0.0549(12) 0.000 0.0054(10) 0.000 C3 0.0749(16) 0.0567(12) 0.0723(13) -0.0117(10) 0.0125(12) -0.0128(11) C4 0.133(3) 0.0572(15) 0.114(2) -0.0208(15) 0.014(2) -0.0225(16) C5 0.171(6) 0.048(2) 0.133(4) 0.000 0.026(4) 0.000 N8 0.0634(12) 0.0693(11) 0.0586(10) -0.0149(8) 0.0000(8) -0.0175(9) N9 0.0475(10) 0.0683(11) 0.0505(8) -0.0013(7) -0.0024(7) -0.0090(8) C10 0.0398(11) 0.0999(17) 0.0475(10) 0.0028(10) -0.0015(8) -0.0070(11) C11 0.0639(16) 0.129(3) 0.0524(12) -0.0142(14) -0.0060(10) -0.0193(15) C12 0.0752(18) 0.107(2) 0.0664(14) -0.0299(15) 0.0020(12) -0.0279(15) C13 0.0429(12) 0.1066(19) 0.0590(12) 0.0134(12) -0.0084(9) 0.0009(11) C14 0.0604(15) 0.110(2) 0.0718(14) 0.0118(14) -0.0059(12) 0.0160(15) C15 0.082(2) 0.118(2) 0.111(2) 0.002(2) -0.0107(17) 0.0352(19) C16 0.100(3) 0.117(3) 0.145(3) 0.037(3) -0.024(2) 0.025(2) C17 0.102(3) 0.150(4) 0.106(3) 0.054(3) -0.010(2) 0.012(2) C18 0.0733(18) 0.127(3) 0.0716(15) 0.0287(16) -0.0045(13) 0.0038(16) B19 0.159(6) 0.065(3) 0.062(2) 0.000 0.000 0.003(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 2.114(2) . ? Fe1 N9 2.2178(16) . ? N2 C3 1.327(3) . ? C3 C4 1.376(3) . ? C3 N8 1.396(3) . ? C4 C5 1.357(4) . ? N8 C12 1.357(3) . ? N8 N9 1.370(2) . ? N9 C10 1.336(3) . ? C10 C11 1.414(3) . ? C10 C13 1.455(4) . ? C11 C12 1.337(4) . ? C13 C18 1.383(3) . ? C13 C14 1.385(4) . ? C14 C15 1.377(4) . ? C15 C16 1.378(5) . ? C16 C17 1.364(6) . ? C17 C18 1.374(6) . ? B19 F20A 1.416(8) . ? B19 F20B 1.369(10) . ? B19 F20C 1.544(12) . ? B19 F21A 1.686(9) . ? B19 F21B 1.439(13) . ? B19 F21C 1.346(9) . ? B19 F22A 1.286(7) . ? B19 F22B 1.457(11) . ? B19 F22C 1.437(10) . ? B19 F23A 1.313(8) . ? B19 F23B 1.340(7) . ? B19 F23C 1.272(11) . ? 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 N2 180.0 2 . ? N2 Fe1 N9 73.13(5) . . ? N9 Fe1 N9 146.25(9) . 4 ? N9 Fe1 N9 105.38(9) . 3 ? N2 Fe1 N9 106.87(5) . 2 ? N9 Fe1 N9 84.45(9) . 2 ? C3 N2 C3 117.9(3) . 4 ? C3 N2 Fe1 121.06(14) . . ? N2 C3 C4 123.0(3) . . ? N2 C3 N8 113.09(18) . . ? C4 C3 N8 123.9(2) . . ? C5 C4 C3 117.4(3) . . ? C4 C5 C4 121.3(4) 4 . ? C12 N8 N9 110.9(2) . . ? C12 N8 C3 130.3(2) . . ? N9 N8 C3 118.53(16) . . ? C10 N9 N8 105.06(17) . . ? C10 N9 Fe1 137.66(16) . . ? N8 N9 Fe1 111.98(13) . . ? N9 C10 C11 110.0(2) . . ? N9 C10 C13 120.9(2) . . ? C11 C10 C13 129.1(2) . . ? C12 C11 C10 106.3(2) . . ? C11 C12 N8 107.7(2) . . ? C18 C13 C14 118.9(3) . . ? C18 C13 C10 119.9(3) . . ? C14 C13 C10 121.3(2) . . ? C15 C14 C13 120.4(3) . . ? C14 C15 C16 120.2(3) . . ? C17 C16 C15 119.3(4) . . ? C16 C17 C18 121.2(3) . . ? C17 C18 C13 120.0(3) . . ? F22A B19 F23A 130.0(5) . . ? F22A B19 F20A 115.5(6) . . ? F22A B19 F21A 98.4(4) . . ? F23A B19 F21A 101.1(6) . . ? F20A B19 F21A 87.9(6) . . ? F23A B19 F20A 110.7(8) . . ? F23B B19 F20B 113.8(7) . . ? F23B B19 F21B 109.9(9) . . ? F20B B19 F21B 112.7(10) . . ? F23B B19 F22B 113.3(7) . . ? F20B B19 F22B 98.7(8) . . ? F21B B19 F22B 108.0(10) . . ? F23C B19 F21C 118.0(10) . . ? F23C B19 F22C 114.0(8) . . ? F21C B19 F22C 110.3(7) . . ? F23C B19 F20C 109.3(9) . . ? F21C B19 F20C 108.5(8) . . ? F22C B19 F20C 94.0(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.296 _refine_diff_density_min -0.210 _refine_diff_density_rms 0.037 #=END data_c:\datasets\leeds\mh49\mh49 _database_code_depnum_ccdc_archive 'CCDC 263424' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-bis(3-isopropylpyrazol-1-yl)pyridine]iron(II) dihexafluorophosphate hemi-diethyl ether acetonitrile solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H42 Fe N10, 2[P F6], 0.5 [C4 H10 O], 0.59[C2 H3 N]' _chemical_formula_sum 'C37.17 H48.76 F12 Fe N10.59 O0.50 P2' _chemical_formula_weight 997.75 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' P P 0.1023 0.0942 '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 '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 22.7463(1) _cell_length_b 13.2037(1) _cell_length_c 63.9493(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.5942(2) _cell_angle_gamma 90.00 _cell_volume 18814.36(19) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 165650 _cell_measurement_theta_min 1.01 _cell_measurement_theta_max 26.00 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8223 _exptl_absorpt_coefficient_mu 0.477 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.810 _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 The high R~int~ value of 0.11 reflects the highly redundant dataset arising from the very high number of reflections collected. ; _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 165650 _diffrn_reflns_av_R_equivalents 0.1063 _diffrn_reflns_av_sigmaI/netI 0.0704 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -67 _diffrn_reflns_limit_l_max 78 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 26.00 _reflns_number_total 36173 _reflns_number_gt 23679 _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: four complex cations (labelled A-D); eight PF~6~^-^ anions; two molecules of diethyl ether; and four acetonitrile environments (three of which are only partially occupied, see below). Three isopropyl groups in the model were disordered, and were each modelled over two orientations: C43B-C45B (occupancy 0.63) and C43E-C45E (occupancy 0.37) C13C-C15C (occupancy 0.75) and C13E-C15E (occupancy 0.25) C43D-C45D (occupancy 0.63) and C43F-C45F (occupancy 0.37). All disordered isopropyl C-C bonds were restrained to 1.52(2)\%A, and non-bonded 1,3-C...C distances within each disorder orientation to 2.48(2)\%A. Four of the eight PF~6~^-^ anions were also modelled as disordered: P4A, F19A-F24A (occupancy 0.50) and P4B, F19B-F24B (occupancy 0.50) P6A, F31A-F36A (occupancy 0.50) and P6B, F31B-F36B (occupancy 0.50) P7A, F37A-F42A (occupancy 0.40), P7B, F37B-F42B (occupancy 0.40) and P7A, F37C-F42C (occupancy 0.20, so that P7A has total occupancy 0.60) P8A, F43A-F48A (occupancy 0.50) and P4B, F43B-F48B (occupancy 0.50) All disordered P---F bonds were restrained to 1.60(2)\%A, cis-F...F distances to 2.26(2)\%A and trans-F...F distances to 3.20(2)\%A. One of the four acetonitrile molecules in the lattice (C11S-N13S) is wholly occupied, one is half occupied (C14S-N16S) and another was modelled as quarter-occupied (C20S-N22S). The remaining molecule was refined over two different orientations (C17S-N19S and C17E-N19E) with an occupancy ratio of 0.40:0.20. This gives a total content of acetonitrile in the asymmetric unit of 2.35 molecules, or 0.59 per formula unit. The C-C bonds in the disordered molecule were restrained to 1.46(2)\%A, the C-N bonds to 1.13(2)\%A and the 1,3-C...N distances to 2.59(2)\%A. All non-H atoms with occupancies >0.5 were refined anisotropically, while all H atoms were placed in calculate dpositions and refined using a riding model. The torsions of wholly occupied methyl groups were allowed to refine, while those of partially occupied methyl groups were fixed. The largest residual electron hole of -1.1 e.\%A^-3^ lies within the disordered anion P8, F43-F48. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0984P)^2^+45.8141P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 36173 _refine_ls_number_parameters 2339 _refine_ls_number_restraints 231 _refine_ls_R_factor_all 0.1216 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.2285 _refine_ls_wR_factor_gt 0.1979 _refine_ls_goodness_of_fit_ref 1.030 _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 Fe1A Fe 0.59484(3) 0.50981(5) 0.307735(10) 0.03006(14) Uani 1 1 d . . . N2A N 0.50644(15) 0.4491(3) 0.30303(6) 0.0324(8) Uani 1 1 d . . . C3A C 0.47082(18) 0.4488(3) 0.28375(8) 0.0341(10) Uani 1 1 d . . . C4A C 0.4099(2) 0.4304(4) 0.28017(9) 0.0431(12) Uani 1 1 d . . . H4A H 0.3858 0.4314 0.2662 0.052 Uiso 1 1 calc R . . C5A C 0.3862(2) 0.4104(4) 0.29774(10) 0.0521(14) Uani 1 1 d . . . H5A H 0.3445 0.3968 0.2959 0.062 Uiso 1 1 calc R . . C6A C 0.4215(2) 0.4095(4) 0.31827(9) 0.0474(13) Uani 1 1 d . . . H6A H 0.4049 0.3956 0.3305 0.057 Uiso 1 1 calc R . . C7A C 0.4816(2) 0.4298(3) 0.31985(8) 0.0352(10) Uani 1 1 d . . . N8A N 0.50167(15) 0.4744(3) 0.26751(6) 0.0326(8) Uani 1 1 d . . . N9A N 0.56029(15) 0.5068(3) 0.27302(6) 0.0329(8) Uani 1 1 d . . . C10A C 0.5778(2) 0.5211(3) 0.25472(8) 0.0365(10) Uani 1 1 d . . . C11A C 0.5306(2) 0.4999(4) 0.23745(8) 0.0409(11) Uani 1 1 d . . . H11A H 0.5315 0.5053 0.2227 0.049 Uiso 1 1 calc R . . C12A C 0.4838(2) 0.4704(4) 0.24607(8) 0.0401(11) Uani 1 1 d . . . H12A H 0.4453 0.4505 0.2384 0.048 Uiso 1 1 calc R . . C13A C 0.6408(2) 0.5538(4) 0.25422(8) 0.0448(12) Uani 1 1 d . . . H13A H 0.6625 0.5663 0.2692 0.054 Uiso 1 1 calc R . . C14A C 0.6414(3) 0.6510(5) 0.24157(11) 0.0709(18) Uani 1 1 d . . . H14A H 0.6214 0.6394 0.2267 0.106 Uiso 1 1 calc R . . H14B H 0.6829 0.6721 0.2421 0.106 Uiso 1 1 calc R . . H14C H 0.6201 0.7042 0.2478 0.106 Uiso 1 1 calc R . . C15A C 0.6725(3) 0.4663(6) 0.24494(12) 0.078(2) Uani 1 1 d . . . H15A H 0.6769 0.4085 0.2547 0.117 Uiso 1 1 calc R . . H15B H 0.7122 0.4887 0.2431 0.117 Uiso 1 1 calc R . . H15C H 0.6484 0.4460 0.2311 0.117 Uiso 1 1 calc R . . N16A N 0.52257(17) 0.4366(3) 0.33932(6) 0.0396(9) Uiso 1 1 d . . . N17A N 0.57919(17) 0.4722(3) 0.33934(6) 0.0382(9) Uiso 1 1 d . . . C18A C 0.6061(2) 0.4756(4) 0.35967(9) 0.0496(13) Uiso 1 1 d . . . C19A C 0.5677(3) 0.4386(5) 0.37282(11) 0.0644(16) Uiso 1 1 d . . . H19A H 0.5768 0.4309 0.3879 0.077 Uiso 1 1 calc R . . C20A C 0.5156(3) 0.4167(5) 0.35949(9) 0.0582(15) Uani 1 1 d . . . H20A H 0.4802 0.3919 0.3635 0.070 Uiso 1 1 calc R . . C21A C 0.6679(3) 0.5193(5) 0.36635(9) 0.0580(15) Uani 1 1 d . . . H21A H 0.6913 0.5045 0.3550 0.070 Uiso 1 1 calc R . . C22A C 0.7001(3) 0.4728(6) 0.38707(11) 0.078(2) Uani 1 1 d . . . H22A H 0.6785 0.4893 0.3984 0.117 Uiso 1 1 calc R . . H22B H 0.7410 0.4999 0.3908 0.117 Uiso 1 1 calc R . . H22C H 0.7018 0.3991 0.3855 0.117 Uiso 1 1 calc R . . C23A C 0.6648(3) 0.6337(5) 0.36910(10) 0.0681(17) Uani 1 1 d . . . H23A H 0.6412 0.6637 0.3561 0.102 Uiso 1 1 calc R . . H23B H 0.7054 0.6619 0.3718 0.102 Uiso 1 1 calc R . . H23C H 0.6457 0.6489 0.3812 0.102 Uiso 1 1 calc R . . N24A N 0.67964(15) 0.5831(3) 0.31210(6) 0.0322(8) Uani 1 1 d . . . C25A C 0.72938(19) 0.5300(4) 0.31221(8) 0.0375(11) Uani 1 1 d . . . C26A C 0.7863(2) 0.5710(4) 0.31688(9) 0.0471(13) Uani 1 1 d . . . H26A H 0.8210 0.5310 0.3169 0.057 Uiso 1 1 calc R . . C27A C 0.7902(2) 0.6738(4) 0.32155(9) 0.0522(14) Uani 1 1 d . . . H27A H 0.8285 0.7051 0.3249 0.063 Uiso 1 1 calc R . . C28A C 0.7398(2) 0.7312(4) 0.32141(9) 0.0502(13) Uani 1 1 d . . . H28A H 0.7425 0.8015 0.3246 0.060 Uiso 1 1 calc R . . C29A C 0.68488(19) 0.6824(4) 0.31635(7) 0.0355(10) Uani 1 1 d . . . N30A N 0.71812(16) 0.4271(3) 0.30715(7) 0.0413(10) Uani 1 1 d . . . N31A N 0.66083(15) 0.3903(3) 0.30491(6) 0.0339(8) Uani 1 1 d . . . C32A C 0.6633(2) 0.2936(3) 0.29976(8) 0.0407(11) Uani 1 1 d . . . C33A C 0.7223(2) 0.2688(5) 0.29815(12) 0.075(2) Uani 1 1 d . . . H33A H 0.7363 0.2046 0.2945 0.089 Uiso 1 1 calc R . . C34A C 0.7557(2) 0.3545(5) 0.30281(12) 0.074(2) Uani 1 1 d . . . H34A H 0.7974 0.3618 0.3030 0.088 Uiso 1 1 calc R . . C35A C 0.6085(2) 0.2281(4) 0.29527(9) 0.0432(12) Uani 1 1 d . . . H35A H 0.5791 0.2556 0.3035 0.052 Uiso 1 1 calc R . . C36A C 0.5797(3) 0.2319(4) 0.27177(10) 0.0605(16) Uani 1 1 d . . . H36A H 0.5731 0.3026 0.2673 0.091 Uiso 1 1 calc R . . H36B H 0.5411 0.1962 0.2694 0.091 Uiso 1 1 calc R . . H36C H 0.6062 0.1993 0.2634 0.091 Uiso 1 1 calc R . . C37A C 0.6239(2) 0.1196(4) 0.30282(10) 0.0531(14) Uani 1 1 d . . . H37A H 0.6508 0.0895 0.2943 0.080 Uiso 1 1 calc R . . H37B H 0.5870 0.0795 0.3011 0.080 Uiso 1 1 calc R . . H37C H 0.6439 0.1202 0.3179 0.080 Uiso 1 1 calc R . . N38A N 0.62985(16) 0.7306(3) 0.31569(6) 0.0370(9) Uani 1 1 d . . . N39A N 0.57797(16) 0.6730(3) 0.31156(6) 0.0335(8) Uani 1 1 d . . . C40A C 0.5337(2) 0.7384(3) 0.31249(8) 0.0370(10) Uani 1 1 d . . . C41A C 0.5570(2) 0.8372(4) 0.31717(9) 0.0453(12) Uani 1 1 d . . . H41A H 0.5350 0.8968 0.3188 0.054 Uiso 1 1 calc R . . C42A C 0.6172(2) 0.8293(4) 0.31893(8) 0.0467(12) Uani 1 1 d . . . H42A H 0.6454 0.8830 0.3219 0.056 Uiso 1 1 calc R . . C43A C 0.4698(2) 0.7051(4) 0.30843(9) 0.0441(12) Uani 1 1 d . . . H43A H 0.4689 0.6296 0.3095 0.053 Uiso 1 1 calc R . . C44A C 0.4369(3) 0.7491(6) 0.32485(13) 0.088(2) Uani 1 1 d . . . H44A H 0.4545 0.7222 0.3390 0.132 Uiso 1 1 calc R . . H44B H 0.3944 0.7305 0.3211 0.132 Uiso 1 1 calc R . . H44C H 0.4407 0.8231 0.3250 0.132 Uiso 1 1 calc R . . C45A C 0.4391(3) 0.7348(8) 0.28621(12) 0.110(3) Uani 1 1 d . . . H45A H 0.4341 0.8085 0.2854 0.165 Uiso 1 1 calc R . . H45B H 0.3996 0.7023 0.2827 0.165 Uiso 1 1 calc R . . H45C H 0.4635 0.7130 0.2760 0.165 Uiso 1 1 calc R . . Fe1B Fe 0.70630(3) 1.00114(5) 0.443180(10) 0.03539(15) Uani 1 1 d . . . N2B N 0.76728(17) 0.9311(3) 0.42629(6) 0.0378(9) Uani 1 1 d . . . C3B C 0.7643(2) 0.8322(4) 0.42205(8) 0.0418(11) Uani 1 1 d . . . C4B C 0.8008(3) 0.7845(4) 0.41049(9) 0.0549(14) Uani 1 1 d . . . H4B H 0.7970 0.7141 0.4074 0.066 Uiso 1 1 calc R . . C5B C 0.8431(3) 0.8423(5) 0.40352(10) 0.0658(17) Uani 1 1 d . . . H5B H 0.8693 0.8111 0.3956 0.079 Uiso 1 1 calc R . . C6B C 0.8484(2) 0.9459(4) 0.40776(9) 0.0526(14) Uani 1 1 d . . . H6B H 0.8777 0.9863 0.4030 0.063 Uiso 1 1 calc R . . C7B C 0.8087(2) 0.9864(4) 0.41924(8) 0.0415(11) Uani 1 1 d . . . N8B N 0.71963(18) 0.7823(3) 0.43052(7) 0.0419(10) Uani 1 1 d . . . N9B N 0.68201(18) 0.8379(3) 0.44038(6) 0.0397(9) Uani 1 1 d . . . C10B C 0.6434(2) 0.7711(4) 0.44592(8) 0.0434(12) Uani 1 1 d . . . C11B C 0.6568(2) 0.6724(4) 0.43947(9) 0.0503(13) Uani 1 1 d . . . H11B H 0.6363 0.6114 0.4413 0.060 Uiso 1 1 calc R . . C12B C 0.7050(2) 0.6830(4) 0.43016(9) 0.0494(13) Uani 1 1 d . . . H12B H 0.7250 0.6299 0.4244 0.059 Uiso 1 1 calc R . . C13B C 0.5962(2) 0.8033(4) 0.45797(10) 0.0531(14) Uani 1 1 d . . . H13B H 0.5829 0.8733 0.4533 0.064 Uiso 1 1 calc R . . C14B C 0.5413(3) 0.7335(5) 0.45359(13) 0.076(2) Uani 1 1 d . . . H14D H 0.5245 0.7321 0.4382 0.114 Uiso 1 1 calc R . . H14E H 0.5109 0.7589 0.4612 0.114 Uiso 1 1 calc R . . H14F H 0.5533 0.6649 0.4585 0.114 Uiso 1 1 calc R . . C15B C 0.6233(3) 0.8061(5) 0.48186(10) 0.0720(18) Uani 1 1 d . . . H15D H 0.6329 0.7370 0.4871 0.108 Uiso 1 1 calc R . . H15E H 0.5943 0.8361 0.4895 0.108 Uiso 1 1 calc R . . H15F H 0.6600 0.8470 0.4843 0.108 Uiso 1 1 calc R . . N16B N 0.80720(17) 1.0894(3) 0.42482(7) 0.0412(9) Uani 1 1 d . . . N17B N 0.76428(17) 1.1204(3) 0.43567(6) 0.0387(9) Uani 1 1 d . . . C18B C 0.7736(2) 1.2191(4) 0.43937(8) 0.0423(11) Uani 1 1 d . . . C19B C 0.8228(2) 1.2506(4) 0.43070(10) 0.0589(15) Uani 1 1 d . . . H19B H 0.8386 1.3173 0.4310 0.071 Uiso 1 1 calc R . . C20B C 0.8432(2) 1.1675(4) 0.42187(10) 0.0583(15) Uani 1 1 d . . . H20B H 0.8765 1.1647 0.4150 0.070 Uiso 1 1 calc R . . C21B C 0.7354(2) 1.2754(4) 0.45183(9) 0.0474(13) Uani 1 1 d . . . H21B H 0.6988 1.2340 0.4521 0.057 Uiso 1 1 calc R . . C22B C 0.7155(2) 1.3775(4) 0.44153(9) 0.0508(13) Uani 1 1 d . . . H22D H 0.7509 1.4201 0.4415 0.076 Uiso 1 1 calc R . . H22E H 0.6889 1.4112 0.4496 0.076 Uiso 1 1 calc R . . H22F H 0.6941 1.3668 0.4268 0.076 Uiso 1 1 calc R . . C23B C 0.7702(3) 1.2886(4) 0.47505(9) 0.0603(15) Uani 1 1 d . . . H23D H 0.7826 1.2221 0.4812 0.090 Uiso 1 1 calc R . . H23E H 0.7442 1.3215 0.4835 0.090 Uiso 1 1 calc R . . H23F H 0.8057 1.3307 0.4752 0.090 Uiso 1 1 calc R . . N24B N 0.64425(17) 1.0596(3) 0.46104(6) 0.0355(9) Uani 1 1 d . . . C25B C 0.5881(2) 1.0842(3) 0.45125(7) 0.0356(10) Uani 1 1 d . . . C26B C 0.5442(2) 1.1116(4) 0.46199(8) 0.0444(12) Uani 1 1 d . . . H26B H 0.5047 1.1277 0.4547 0.053 Uiso 1 1 calc R . . C27B C 0.5601(2) 1.1148(4) 0.48413(9) 0.0502(13) Uani 1 1 d . . . H27B H 0.5310 1.1334 0.4922 0.060 Uiso 1 1 calc R . . C28B C 0.6175(2) 1.0915(4) 0.49457(8) 0.0480(13) Uani 1 1 d . . . H28B H 0.6285 1.0940 0.5097 0.058 Uiso 1 1 calc R . . C29B C 0.6586(2) 1.0645(3) 0.48234(8) 0.0387(11) Uani 1 1 d . . . N30B N 0.58016(16) 1.0782(3) 0.42881(6) 0.0371(9) Uani 1 1 d . . . N31B N 0.62923(17) 1.0551(3) 0.42003(6) 0.0370(9) Uani 1 1 d . . . C32B C 0.6108(2) 1.0669(4) 0.39920(7) 0.0399(11) Uani 1 1 d . . . C33B C 0.5500(2) 1.0967(4) 0.39439(9) 0.0507(13) Uani 1 1 d . . . H33B H 0.5262 1.1093 0.3806 0.061 Uiso 1 1 calc R . . C34B C 0.5325(2) 1.1039(4) 0.41342(8) 0.0493(13) Uani 1 1 d . . . H34B H 0.4939 1.1233 0.4155 0.059 Uiso 1 1 calc R . . C35B C 0.6531(2) 1.0516(4) 0.38430(8) 0.0480(13) Uani 1 1 d . . . H35B H 0.6949 1.0508 0.3930 0.058 Uiso 1 1 calc R . . C36B C 0.6412(3) 0.9492(6) 0.37321(12) 0.082(2) Uani 1 1 d . . . H36D H 0.6424 0.8959 0.3839 0.122 Uiso 1 1 calc R . . H36E H 0.6721 0.9359 0.3648 0.122 Uiso 1 1 calc R . . H36F H 0.6016 0.9500 0.3637 0.122 Uiso 1 1 calc R . . C37B C 0.6486(3) 1.1381(6) 0.36832(10) 0.076(2) Uani 1 1 d . . . H37D H 0.6087 1.1378 0.3590 0.113 Uiso 1 1 calc R . . H37E H 0.6792 1.1295 0.3596 0.113 Uiso 1 1 calc R . . H37F H 0.6550 1.2026 0.3760 0.113 Uiso 1 1 calc R . . N38B N 0.71851(18) 1.0393(3) 0.49054(6) 0.0399(9) Uani 1 1 d . A . N39B N 0.75391(18) 1.0051(3) 0.47698(6) 0.0405(9) Uani 1 1 d . A . C40B C 0.8084(2) 0.9953(4) 0.48853(8) 0.0435(11) Uani 1 1 d D . . C41B C 0.8089(2) 1.0227(4) 0.50996(8) 0.0482(13) Uani 1 1 d . A . H41B H 0.8424 1.0216 0.5215 0.058 Uiso 1 1 calc R . . C42B C 0.7520(2) 1.0506(4) 0.51063(8) 0.0451(12) Uani 1 1 d . . . H42B H 0.7380 1.0738 0.5228 0.054 Uiso 1 1 calc R A . C43B C 0.8598(7) 0.9573(14) 0.4791(4) 0.061(14) Uani 0.63 1 d PD A 1 H43B H 0.8480 0.9617 0.4632 0.073 Uiso 0.63 1 calc PR A 1 C44B C 0.8725(8) 0.8466(10) 0.4853(4) 0.104(7) Uani 0.63 1 d PD A 1 H44D H 0.9063 0.8224 0.4793 0.156 Uiso 0.63 1 calc PR A 1 H44E H 0.8368 0.8057 0.4797 0.156 Uiso 0.63 1 calc PR A 1 H44F H 0.8824 0.8406 0.5009 0.156 Uiso 0.63 1 calc PR A 1 C45B C 0.9157(6) 1.0213(15) 0.4864(4) 0.096(6) Uani 0.63 1 d PD A 1 H45D H 0.9486 0.9944 0.4803 0.144 Uiso 0.63 1 calc PR A 1 H45E H 0.9271 1.0193 0.5020 0.144 Uiso 0.63 1 calc PR A 1 H45F H 0.9074 1.0914 0.4817 0.144 Uiso 0.63 1 calc PR A 1 C43E C 0.8602(10) 0.9604(18) 0.4787(6) 0.044(18) Uiso 0.37 1 d PD A 2 H43E H 0.8450 0.9465 0.4632 0.053 Uiso 0.37 1 calc PR A 2 C44E C 0.8870(11) 0.8631(16) 0.4896(6) 0.066(7) Uiso 0.37 1 d PD A 2 H44G H 0.9198 0.8399 0.4830 0.099 Uiso 0.37 1 calc PR A 2 H44H H 0.8559 0.8107 0.4881 0.099 Uiso 0.37 1 calc PR A 2 H44I H 0.9025 0.8764 0.5048 0.099 Uiso 0.37 1 calc PR A 2 C45E C 0.9085(9) 1.042(2) 0.4810(5) 0.060(7) Uiso 0.37 1 d PD A 2 H45G H 0.9410 1.0191 0.4742 0.090 Uiso 0.37 1 calc PR A 2 H45H H 0.9245 1.0544 0.4962 0.090 Uiso 0.37 1 calc PR A 2 H45I H 0.8911 1.1045 0.4742 0.090 Uiso 0.37 1 calc PR A 2 Fe1C Fe 0.20438(3) 0.50319(5) 0.442607(10) 0.03467(15) Uani 1 1 d . . . N2C N 0.26989(17) 0.5700(3) 0.42703(6) 0.0378(9) Uani 1 1 d . . . C3C C 0.2692(2) 0.6699(4) 0.42322(8) 0.0399(11) Uani 1 1 d . . . C4C C 0.3102(2) 0.7169(4) 0.41316(8) 0.0494(13) Uani 1 1 d . . . H4C H 0.3081 0.7876 0.4103 0.059 Uiso 1 1 calc R . . C5C C 0.3541(2) 0.6577(4) 0.40739(9) 0.0540(14) Uani 1 1 d . . . H5C H 0.3834 0.6881 0.4007 0.065 Uiso 1 1 calc R . . C6C C 0.3561(2) 0.5536(4) 0.41118(8) 0.0473(12) Uani 1 1 d . . . H6C H 0.3857 0.5116 0.4070 0.057 Uiso 1 1 calc R . . C7C C 0.3128(2) 0.5146(4) 0.42130(7) 0.0378(11) Uani 1 1 d . . . N8C N 0.22294(18) 0.7211(3) 0.43060(6) 0.0404(9) Uani 1 1 d . B . N9C N 0.18254(17) 0.6655(3) 0.43921(6) 0.0376(9) Uani 1 1 d . B . C10C C 0.1424(2) 0.7322(4) 0.44327(8) 0.0409(11) Uani 1 1 d D . . C11C C 0.1577(2) 0.8314(4) 0.43749(9) 0.0465(12) Uani 1 1 d . B . H11C H 0.1366 0.8924 0.4388 0.056 Uiso 1 1 calc R . . C12C C 0.2083(2) 0.8210(4) 0.42972(8) 0.0454(12) Uani 1 1 d . . . H12C H 0.2298 0.8740 0.4246 0.055 Uiso 1 1 calc R B . C13C C 0.0903(4) 0.7010(10) 0.4531(2) 0.052(8) Uani 0.75 1 d PD B 1 H13C H 0.0780 0.6311 0.4480 0.062 Uiso 0.75 1 calc PR B 1 C14C C 0.1089(4) 0.6984(7) 0.47733(13) 0.070(2) Uani 0.75 1 d PD B 1 H14G H 0.0745 0.6779 0.4835 0.104 Uiso 0.75 1 calc PR B 1 H14H H 0.1224 0.7659 0.4826 0.104 Uiso 0.75 1 calc PR B 1 H14I H 0.1417 0.6497 0.4815 0.104 Uiso 0.75 1 calc PR B 1 C15C C 0.0352(3) 0.7715(7) 0.44688(19) 0.087(3) Uani 0.75 1 d PD B 1 H15G H 0.0029 0.7473 0.4537 0.130 Uiso 0.75 1 calc PR B 1 H15H H 0.0215 0.7713 0.4313 0.130 Uiso 0.75 1 calc PR B 1 H15I H 0.0464 0.8406 0.4517 0.130 Uiso 0.75 1 calc PR B 1 C13E C 0.0882(10) 0.695(3) 0.4517(4) 0.05(2) Uiso 0.25 1 d PD B 2 H13E H 0.0945 0.6238 0.4571 0.056 Uiso 0.25 1 calc PR B 2 C14E C 0.0791(9) 0.7673(18) 0.4695(3) 0.055(6) Uiso 0.25 1 d PD B 2 H14J H 0.0445 0.7451 0.4753 0.082 Uiso 0.25 1 calc PR B 2 H14K H 0.0719 0.8358 0.4637 0.082 Uiso 0.25 1 calc PR B 2 H14L H 0.1151 0.7672 0.4808 0.082 Uiso 0.25 1 calc PR B 2 C15E C 0.0355(8) 0.701(3) 0.4327(4) 0.093(9) Uiso 0.25 1 d PD B 2 H15J H -0.0011 0.6775 0.4371 0.140 Uiso 0.25 1 calc PR B 2 H15K H 0.0436 0.6573 0.4212 0.140 Uiso 0.25 1 calc PR B 2 H15L H 0.0302 0.7708 0.4277 0.140 Uiso 0.25 1 calc PR B 2 N16C N 0.30874(17) 0.4111(3) 0.42654(6) 0.0391(9) Uani 1 1 d . . . N17C N 0.26044(16) 0.3805(3) 0.43480(6) 0.0360(9) Uani 1 1 d . . . C18C C 0.2685(2) 0.2820(4) 0.43843(8) 0.0424(11) Uani 1 1 d . . . C19C C 0.3219(2) 0.2496(4) 0.43247(9) 0.0515(14) Uani 1 1 d . . . H19C H 0.3375 0.1826 0.4334 0.062 Uiso 1 1 calc R . . C20C C 0.3465(2) 0.3331(4) 0.42518(9) 0.0492(13) Uani 1 1 d . . . H20C H 0.3830 0.3361 0.4201 0.059 Uiso 1 1 calc R . . C21C C 0.2253(2) 0.2240(4) 0.44872(9) 0.0477(13) Uani 1 1 d . . . H21C H 0.1873 0.2640 0.4471 0.057 Uiso 1 1 calc R . . C22C C 0.2103(2) 0.1214(4) 0.43829(10) 0.0542(14) Uani 1 1 d . . . H22G H 0.1914 0.1309 0.4232 0.081 Uiso 1 1 calc R . . H22H H 0.1825 0.0854 0.4456 0.081 Uiso 1 1 calc R . . H22I H 0.2472 0.0817 0.4393 0.081 Uiso 1 1 calc R . . C23C C 0.2516(3) 0.2127(4) 0.47259(10) 0.0640(17) Uani 1 1 d . . . H23G H 0.2866 0.1679 0.4746 0.096 Uiso 1 1 calc R . . H23H H 0.2212 0.1836 0.4797 0.096 Uiso 1 1 calc R . . H23I H 0.2637 0.2793 0.4787 0.096 Uiso 1 1 calc R . . N24C N 0.14199(17) 0.4432(3) 0.45997(6) 0.0356(9) Uani 1 1 d . . . C25C C 0.1552(2) 0.4380(4) 0.48129(8) 0.0383(11) Uani 1 1 d . . . C26C C 0.1142(2) 0.4096(4) 0.49329(9) 0.0494(13) Uani 1 1 d . . . H26C H 0.1247 0.4072 0.5084 0.059 Uiso 1 1 calc R . . C27C C 0.0573(2) 0.3848(5) 0.48257(9) 0.0539(14) Uani 1 1 d . . . H27C H 0.0277 0.3665 0.4905 0.065 Uiso 1 1 calc R . . C28C C 0.0426(2) 0.3861(4) 0.46058(9) 0.0470(13) Uani 1 1 d . . . H28C H 0.0038 0.3670 0.4531 0.056 Uiso 1 1 calc R . . C29C C 0.0866(2) 0.4161(4) 0.44997(8) 0.0403(11) Uani 1 1 d . . . N30C N 0.07928(16) 0.4215(3) 0.42763(6) 0.0407(9) Uani 1 1 d . . . N31C N 0.12768(16) 0.4516(3) 0.41911(6) 0.0400(9) Uani 1 1 d . . . C32C C 0.1099(2) 0.4410(5) 0.39818(8) 0.0500(13) Uani 1 1 d . . . C33C C 0.0505(2) 0.4052(5) 0.39315(9) 0.0624(17) Uani 1 1 d . . . H33C H 0.0273 0.3925 0.3793 0.075 Uiso 1 1 calc R . . C34C C 0.0332(2) 0.3927(5) 0.41191(9) 0.0562(15) Uani 1 1 d . . . H34C H -0.0047 0.3680 0.4138 0.067 Uiso 1 1 calc R . . C35C C 0.1519(3) 0.4657(6) 0.38362(9) 0.0645(17) Uani 1 1 d . . . H35C H 0.1938 0.4628 0.3922 0.077 Uiso 1 1 calc R . . C36C C 0.1464(3) 0.3887(6) 0.36576(10) 0.079(2) Uani 1 1 d . . . H36G H 0.1546 0.3208 0.3718 0.119 Uiso 1 1 calc R . . H36H H 0.1755 0.4048 0.3568 0.119 Uiso 1 1 calc R . . H36I H 0.1057 0.3908 0.3571 0.119 Uiso 1 1 calc R . . C37C C 0.1406(3) 0.5722(6) 0.37479(12) 0.089(2) Uani 1 1 d . . . H37G H 0.1002 0.5760 0.3658 0.133 Uiso 1 1 calc R . . H37H H 0.1704 0.5890 0.3662 0.133 Uiso 1 1 calc R . . H37I H 0.1437 0.6204 0.3866 0.133 Uiso 1 1 calc R . . N38C N 0.21534(17) 0.4644(3) 0.48994(6) 0.0378(9) Uani 1 1 d . . . N39C N 0.25109(17) 0.4979(3) 0.47646(6) 0.0380(9) Uani 1 1 d . . . C40C C 0.3060(2) 0.5060(4) 0.48834(8) 0.0410(11) Uani 1 1 d . . . C41C C 0.3054(2) 0.4774(4) 0.50949(8) 0.0446(12) Uani 1 1 d . . . H41C H 0.3387 0.4767 0.5212 0.054 Uiso 1 1 calc R . . C42C C 0.2485(2) 0.4513(4) 0.50992(8) 0.0439(12) Uani 1 1 d . . . H42C H 0.2341 0.4280 0.5220 0.053 Uiso 1 1 calc R . . C43C C 0.3580(2) 0.5428(5) 0.47935(9) 0.0536(14) Uani 1 1 d . . . H43C H 0.3455 0.5441 0.4634 0.064 Uiso 1 1 calc R . . C44C C 0.4112(3) 0.4718(6) 0.48518(14) 0.092(2) Uani 1 1 d . . . H44J H 0.4239 0.4688 0.5007 0.137 Uiso 1 1 calc R . . H44K H 0.4444 0.4969 0.4789 0.137 Uiso 1 1 calc R . . H44L H 0.3996 0.4040 0.4796 0.137 Uiso 1 1 calc R . . C45C C 0.3752(4) 0.6507(6) 0.48701(14) 0.094(2) Uani 1 1 d . . . H45J H 0.3409 0.6959 0.4823 0.141 Uiso 1 1 calc R . . H45K H 0.4092 0.6737 0.4810 0.141 Uiso 1 1 calc R . . H45L H 0.3864 0.6515 0.5026 0.141 Uiso 1 1 calc R . . Fe1D Fe 0.09701(3) 0.05972(5) 0.307117(11) 0.03340(15) Uani 1 1 d . . . N2D N 0.18208(15) -0.0103(3) 0.30819(6) 0.0332(8) Uani 1 1 d . . . C3D C 0.23085(19) 0.0464(4) 0.30788(8) 0.0359(10) Uani 1 1 d . . . C4D C 0.2872(2) 0.0061(4) 0.30849(9) 0.0482(13) Uani 1 1 d . . . H4D H 0.3211 0.0479 0.3085 0.058 Uiso 1 1 calc R . . C5D C 0.2914(2) -0.0973(4) 0.30913(10) 0.0563(15) Uani 1 1 d . . . H5D H 0.3293 -0.1282 0.3093 0.068 Uiso 1 1 calc R . . C6D C 0.2422(2) -0.1581(4) 0.30950(9) 0.0488(13) Uani 1 1 d . . . H6D H 0.2455 -0.2298 0.3100 0.059 Uiso 1 1 calc R . . C7D C 0.1885(2) -0.1104(4) 0.30913(7) 0.0368(10) Uani 1 1 d . . . N8D N 0.21841(15) 0.1504(3) 0.30554(7) 0.0383(9) Uani 1 1 d . . . N9D N 0.16024(15) 0.1834(3) 0.30384(6) 0.0349(9) Uani 1 1 d . . . C10D C 0.1615(2) 0.2817(4) 0.30021(8) 0.0414(11) Uani 1 1 d . . . C11D C 0.2204(2) 0.3133(4) 0.29963(10) 0.0578(16) Uani 1 1 d . . . H11D H 0.2332 0.3801 0.2973 0.069 Uiso 1 1 calc R . . C12D C 0.2550(2) 0.2291(4) 0.30303(10) 0.0533(14) Uani 1 1 d . . . H12D H 0.2970 0.2256 0.3036 0.064 Uiso 1 1 calc R . . C13D C 0.1053(2) 0.3453(4) 0.29600(10) 0.0510(14) Uani 1 1 d . . . H13D H 0.0760 0.3144 0.3039 0.061 Uiso 1 1 calc R . . C14D C 0.0773(3) 0.3444(4) 0.27232(11) 0.0646(17) Uani 1 1 d . . . H14M H 0.1041 0.3786 0.2644 0.097 Uiso 1 1 calc R . . H14N H 0.0386 0.3797 0.2700 0.097 Uiso 1 1 calc R . . H14O H 0.0711 0.2742 0.2674 0.097 Uiso 1 1 calc R . . C15D C 0.1176(2) 0.4538(4) 0.30399(10) 0.0539(14) Uani 1 1 d . . . H15M H 0.1365 0.4527 0.3192 0.081 Uiso 1 1 calc R . . H15N H 0.0797 0.4912 0.3020 0.081 Uiso 1 1 calc R . . H15O H 0.1445 0.4869 0.2959 0.081 Uiso 1 1 calc R . . N16D N 0.13465(16) -0.1613(3) 0.30971(7) 0.0395(9) Uani 1 1 d . . . N17D N 0.08360(16) -0.1066(3) 0.30968(7) 0.0386(9) Uani 1 1 d . . . C18D C 0.0418(2) -0.1729(4) 0.31179(9) 0.0480(13) Uani 1 1 d . . . C19D C 0.0655(2) -0.2717(4) 0.31316(9) 0.0514(14) Uani 1 1 d . . . H19D H 0.0448 -0.3328 0.3148 0.062 Uiso 1 1 calc R . . C20D C 0.1237(2) -0.2620(4) 0.31172(9) 0.0450(12) Uani 1 1 d . . . H20D H 0.1518 -0.3154 0.3120 0.054 Uiso 1 1 calc R . . C21D C -0.0211(3) -0.1401(4) 0.31178(14) 0.078(2) Uani 1 1 d . . . H21D H -0.0203 -0.0675 0.3163 0.094 Uiso 1 1 calc R . . C22D C -0.0473(6) -0.2006(8) 0.3270(3) 0.270(12) Uani 1 1 d . . . H22J H -0.0911 -0.1958 0.3233 0.406 Uiso 1 1 calc R . . H22K H -0.0330 -0.1748 0.3415 0.406 Uiso 1 1 calc R . . H22L H -0.0351 -0.2715 0.3263 0.406 Uiso 1 1 calc R . . C23D C -0.0583(4) -0.1481(10) 0.2898(3) 0.241(10) Uani 1 1 d . . . H23J H -0.0672 -0.2195 0.2863 0.361 Uiso 1 1 calc R . . H23K H -0.0361 -0.1193 0.2795 0.361 Uiso 1 1 calc R . . H23L H -0.0959 -0.1108 0.2890 0.361 Uiso 1 1 calc R . . N24D N 0.00967(16) 0.1212(3) 0.30522(7) 0.0386(9) Uani 1 1 d . . . C25D C -0.0107(2) 0.1384(3) 0.32293(9) 0.0399(11) Uani 1 1 d . . . C26D C -0.0702(2) 0.1634(4) 0.32270(10) 0.0536(14) Uani 1 1 d . . . H26D H -0.0842 0.1756 0.3355 0.064 Uiso 1 1 calc R . . C27D C -0.1078(2) 0.1695(4) 0.30300(11) 0.0584(16) Uani 1 1 d . . . H27D H -0.1488 0.1861 0.3022 0.070 Uiso 1 1 calc R . . C28D C -0.0877(2) 0.1525(4) 0.28454(11) 0.0572(15) Uani 1 1 d . . . H28D H -0.1139 0.1576 0.2710 0.069 Uiso 1 1 calc R . . C29D C -0.0279(2) 0.1274(4) 0.28635(9) 0.0425(12) Uani 1 1 d . . . N30D N -0.00141(16) 0.1049(3) 0.26899(7) 0.0439(10) Uani 1 1 d . . . N31D N 0.05709(16) 0.0713(3) 0.27289(7) 0.0393(9) Uani 1 1 d . . . C32D C 0.0712(2) 0.0576(4) 0.25383(8) 0.0454(12) Uani 1 1 d . . . C33D C 0.0214(2) 0.0837(4) 0.23756(9) 0.0536(14) Uani 1 1 d . . . H33D H 0.0194 0.0817 0.2226 0.064 Uiso 1 1 calc R . . C34D C -0.0229(2) 0.1121(4) 0.24771(9) 0.0552(15) Uani 1 1 d . . . H34D H -0.0621 0.1333 0.2411 0.066 Uiso 1 1 calc R . . C35D C 0.1322(2) 0.0220(4) 0.25182(9) 0.0526(14) Uani 1 1 d . . . H35D H 0.1587 0.0228 0.2663 0.063 Uiso 1 1 calc R . . C36D C 0.1285(3) -0.0861(5) 0.24350(11) 0.078(2) Uani 1 1 d . . . H36J H 0.1108 -0.1296 0.2530 0.118 Uiso 1 1 calc R . . H36K H 0.1689 -0.1105 0.2430 0.118 Uiso 1 1 calc R . . H36L H 0.1034 -0.0880 0.2291 0.118 Uiso 1 1 calc R . . C37D C 0.1589(3) 0.0947(6) 0.23727(11) 0.0747(19) Uani 1 1 d . . . H37J H 0.1347 0.0919 0.2228 0.112 Uiso 1 1 calc R . . H37K H 0.2002 0.0743 0.2370 0.112 Uiso 1 1 calc R . . H37L H 0.1588 0.1639 0.2428 0.112 Uiso 1 1 calc R . . N38D N 0.03293(17) 0.1251(3) 0.34155(7) 0.0426(10) Uani 1 1 d . C . N39D N 0.08809(16) 0.0873(3) 0.33982(6) 0.0392(9) Uani 1 1 d . C . C40D C 0.1184(2) 0.0762(4) 0.35967(9) 0.0514(13) Uani 1 1 d D . . C41D C 0.0833(3) 0.1067(5) 0.37409(10) 0.0632(16) Uani 1 1 d . C . H41D H 0.0946 0.1062 0.3892 0.076 Uiso 1 1 calc R . . C42D C 0.0301(3) 0.1371(5) 0.36225(10) 0.0577(15) Uani 1 1 d . . . H42D H -0.0032 0.1622 0.3676 0.069 Uiso 1 1 calc R C . C43D C 0.1820(5) 0.0383(12) 0.3638(3) 0.071(9) Uani 0.63 1 d PD C 1 H43D H 0.1878 0.0004 0.3508 0.086 Uiso 0.63 1 calc PR C 1 C44D C 0.1924(5) -0.0359(9) 0.38254(17) 0.087(4) Uani 0.63 1 d PD C 1 H44M H 0.2339 -0.0603 0.3851 0.130 Uiso 0.63 1 calc PR C 1 H44N H 0.1649 -0.0934 0.3792 0.130 Uiso 0.63 1 calc PR C 1 H44O H 0.1850 -0.0015 0.3953 0.130 Uiso 0.63 1 calc PR C 1 C45D C 0.2268(4) 0.1238(8) 0.3674(3) 0.103(5) Uani 0.63 1 d PD C 1 H45M H 0.2675 0.0960 0.3700 0.155 Uiso 0.63 1 calc PR C 1 H45N H 0.2212 0.1635 0.3798 0.155 Uiso 0.63 1 calc PR C 1 H45O H 0.2207 0.1675 0.3548 0.155 Uiso 0.63 1 calc PR C 1 C43F C 0.1805(8) 0.0280(14) 0.3634(4) 0.044(10) Uiso 0.37 1 d PD C 2 H43F H 0.1978 0.0360 0.3504 0.053 Uiso 0.37 1 calc PR C 2 C44F C 0.1758(10) -0.0855(12) 0.3684(4) 0.113(8) Uiso 0.37 1 d PD C 2 H44P H 0.2159 -0.1161 0.3708 0.170 Uiso 0.37 1 calc PR C 2 H44Q H 0.1497 -0.1190 0.3564 0.170 Uiso 0.37 1 calc PR C 2 H44R H 0.1589 -0.0935 0.3813 0.170 Uiso 0.37 1 calc PR C 2 C45F C 0.2221(9) 0.0778(19) 0.3824(4) 0.120(10) Uiso 0.37 1 d PD C 2 H45P H 0.2617 0.0459 0.3845 0.180 Uiso 0.37 1 calc PR C 2 H45Q H 0.2054 0.0694 0.3952 0.180 Uiso 0.37 1 calc PR C 2 H45R H 0.2258 0.1502 0.3794 0.180 Uiso 0.37 1 calc PR C 2 P1 P 0.88497(6) 0.55677(11) 0.44406(2) 0.0459(3) Uani 1 1 d . . . F1 F 0.9213(2) 0.4766(4) 0.43381(7) 0.1117(17) Uani 1 1 d . . . F2 F 0.93985(14) 0.5813(3) 0.46284(5) 0.0707(10) Uani 1 1 d . . . F3 F 0.84473(17) 0.6352(3) 0.45423(6) 0.0773(11) Uani 1 1 d . . . F4 F 0.82774(15) 0.5347(3) 0.42558(5) 0.0662(9) Uani 1 1 d . . . F5 F 0.86389(18) 0.4710(3) 0.45850(6) 0.0814(11) Uani 1 1 d . . . F6 F 0.90245(16) 0.6454(3) 0.43010(6) 0.0802(11) Uani 1 1 d . . . P2 P 0.18958(6) 0.50423(11) 0.15536(3) 0.0521(4) Uani 1 1 d . . . F7 F 0.16394(19) 0.4689(3) 0.17556(6) 0.0912(13) Uani 1 1 d . . . F8 F 0.19605(15) 0.6162(2) 0.16488(6) 0.0681(9) Uani 1 1 d . . . F9 F 0.21557(17) 0.5409(3) 0.13547(6) 0.0787(11) Uani 1 1 d . . . F10 F 0.18250(18) 0.3924(3) 0.14625(7) 0.0848(12) Uani 1 1 d . . . F11 F 0.25607(15) 0.4791(3) 0.16810(6) 0.0763(11) Uani 1 1 d . . . F12 F 0.12383(15) 0.5298(3) 0.14279(6) 0.0786(11) Uani 1 1 d . . . P3 P 0.45554(5) 1.11749(10) 0.32529(2) 0.0394(3) Uani 1 1 d . . . F13 F 0.42790(13) 1.0251(2) 0.30998(5) 0.0526(8) Uani 1 1 d . . . F14 F 0.47985(16) 1.1671(3) 0.30609(6) 0.0782(11) Uani 1 1 d . . . F15 F 0.48275(15) 1.2095(2) 0.34001(6) 0.0674(9) Uani 1 1 d . . . F16 F 0.4293(2) 1.0689(3) 0.34376(6) 0.0946(14) Uani 1 1 d . . . F17 F 0.51570(16) 1.0565(3) 0.33213(8) 0.0979(15) Uani 1 1 d . . . F18 F 0.39449(12) 1.1790(2) 0.31796(6) 0.0603(9) Uani 1 1 d . . . P4A P 0.2337(3) 0.6183(4) 0.26849(10) 0.047(2) Uiso 0.50 1 d PD D 1 F19A F 0.2331(3) 0.5943(5) 0.29248(9) 0.0505(18) Uiso 0.50 1 d PD D 1 F20A F 0.1779(3) 0.5369(5) 0.26104(10) 0.0474(15) Uiso 0.50 1 d PD D 1 F21A F 0.2291(4) 0.6246(7) 0.24220(11) 0.061(3) Uiso 0.50 1 d PD D 1 F22A F 0.2856(3) 0.6938(6) 0.27405(12) 0.068(2) Uiso 0.50 1 d PD D 1 F23A F 0.2782(3) 0.5243(5) 0.26726(11) 0.0651(19) Uiso 0.50 1 d PD D 1 F24A F 0.1840(3) 0.7033(6) 0.26778(13) 0.069(3) Uiso 0.50 1 d PD D 1 P4B P 0.2369(3) 0.6164(5) 0.26603(10) 0.050(2) Uiso 0.50 1 d PD E 2 F19B F 0.2539(4) 0.5986(8) 0.29184(13) 0.097(4) Uiso 0.50 1 d PD E 2 F20B F 0.2018(4) 0.5136(6) 0.26328(16) 0.107(4) Uiso 0.50 1 d PD E 2 F21B F 0.2219(4) 0.6505(7) 0.24256(12) 0.070(3) Uiso 0.50 1 d PD E 2 F22B F 0.2710(4) 0.7262(6) 0.27051(15) 0.089(3) Uiso 0.50 1 d PD E 2 F23B F 0.2971(3) 0.5665(7) 0.26376(14) 0.091(3) Uiso 0.50 1 d PD E 2 F24B F 0.1769(3) 0.6735(7) 0.27046(15) 0.078(3) Uiso 0.50 1 d PD E 2 P5 P 0.38553(6) 0.95110(10) 0.44321(2) 0.0416(3) Uani 1 1 d . . . F25 F 0.41324(15) 0.8746(3) 0.42878(5) 0.0647(9) Uani 1 1 d . . . F26 F 0.44194(13) 0.9385(3) 0.46224(5) 0.0608(8) Uani 1 1 d . . . F27 F 0.35593(14) 1.0280(2) 0.45773(5) 0.0551(8) Uani 1 1 d . . . F28 F 0.32760(13) 0.9641(2) 0.42429(5) 0.0505(7) Uani 1 1 d . . . F29 F 0.35268(14) 0.8593(2) 0.45265(5) 0.0569(8) Uani 1 1 d . . . F30 F 0.41584(14) 1.0451(3) 0.43369(5) 0.0605(8) Uani 1 1 d . . . P6A P 0.5293(2) 1.3968(4) 0.43348(8) 0.0510(18) Uiso 0.50 1 d PD F 1 F31A F 0.5689(3) 1.3169(5) 0.42517(13) 0.073(2) Uiso 0.50 1 d PD F 1 F32A F 0.5694(4) 1.3926(8) 0.45671(13) 0.117(4) Uiso 0.50 1 d PD F 1 F33A F 0.4844(4) 1.4778(7) 0.44165(17) 0.096(4) Uiso 0.50 1 d PD F 1 F34A F 0.4847(3) 1.4042(7) 0.41063(11) 0.071(2) Uiso 0.50 1 d PD F 1 F35A F 0.5671(4) 1.4868(6) 0.42713(16) 0.075(4) Uiso 0.50 1 d PD F 1 F36A F 0.4870(3) 1.3071(6) 0.43895(13) 0.079(2) Uiso 0.50 1 d PD F 1 P6B P 0.5278(2) 1.4046(4) 0.43702(8) 0.0447(16) Uiso 0.50 1 d PD G 2 F31B F 0.5744(3) 1.3129(5) 0.43738(13) 0.0661(19) Uiso 0.50 1 d PD G 2 F32B F 0.5682(3) 1.4480(5) 0.45790(10) 0.0597(17) Uiso 0.50 1 d PD G 2 F33B F 0.4828(4) 1.4953(6) 0.43597(15) 0.068(3) Uiso 0.50 1 d PD G 2 F34B F 0.4895(4) 1.3639(7) 0.41428(13) 0.089(3) Uiso 0.50 1 d PD G 2 F35B F 0.5696(4) 1.4685(6) 0.42342(15) 0.065(3) Uiso 0.50 1 d PD G 2 F36B F 0.4896(3) 1.3381(5) 0.44919(11) 0.0624(18) Uiso 0.50 1 d PD G 2 P7A P -0.04207(16) 0.4487(3) 0.32533(6) 0.0385(12) Uiso 0.60 1 d PD . . F37A F -0.0213(3) 0.3892(6) 0.30657(12) 0.0352(16) Uiso 0.40 1 d PD H 1 F38A F 0.0204(4) 0.5066(8) 0.32992(17) 0.055(4) Uiso 0.40 1 d PD H 1 F39A F -0.0673(3) 0.5102(7) 0.34350(13) 0.047(2) Uiso 0.40 1 d PD H 1 F40A F -0.1055(3) 0.3908(7) 0.32107(16) 0.045(3) Uiso 0.40 1 d PD H 1 F41A F -0.0175(4) 0.3621(5) 0.34189(12) 0.0393(19) Uiso 0.40 1 d PD H 1 F42A F -0.0701(4) 0.5375(5) 0.30858(12) 0.041(2) Uiso 0.40 1 d PD H 1 P7B P -0.0435(2) 0.4661(4) 0.32664(9) 0.0395(19) Uiso 0.40 1 d PD I 2 F37B F -0.0066(4) 0.3725(7) 0.31829(19) 0.084(3) Uiso 0.40 1 d PD I 2 F38B F 0.0173(3) 0.5100(7) 0.34001(15) 0.062(3) Uiso 0.40 1 d PD I 2 F39B F -0.0799(4) 0.5537(7) 0.33409(18) 0.082(3) Uiso 0.40 1 d PD I 2 F40B F -0.1038(3) 0.4163(6) 0.31281(13) 0.046(2) Uiso 0.40 1 d PD I 2 F41B F -0.0490(5) 0.3959(9) 0.34640(15) 0.102(3) Uiso 0.40 1 d PD I 2 F42B F -0.0342(5) 0.5275(7) 0.30633(13) 0.082(3) Uiso 0.40 1 d PD I 2 F37C F -0.0059(5) 0.3553(8) 0.3358(2) 0.033(4) Uiso 0.20 1 d PD H 3 F38C F 0.0162(6) 0.5219(12) 0.3331(3) 0.041(6) Uiso 0.20 1 d PD H 3 F39C F -0.0762(6) 0.5523(10) 0.3153(3) 0.057(5) Uiso 0.20 1 d PD H 3 F40C F -0.1009(6) 0.3852(13) 0.3171(3) 0.044(7) Uiso 0.20 1 d PD H 3 F41C F -0.0622(7) 0.4740(14) 0.3474(2) 0.062(6) Uiso 0.20 1 d PD H 3 F42C F -0.0200(7) 0.4303(13) 0.30375(19) 0.060(5) Uiso 0.20 1 d PD H 3 P8A P 0.0242(2) 1.0949(4) 0.43133(8) 0.0561(16) Uiso 0.50 1 d PD J 1 F43A F 0.0618(5) 1.0106(8) 0.42360(19) 0.092(5) Uiso 0.50 1 d PD J 1 F44A F 0.0644(5) 1.0903(9) 0.45531(15) 0.132(5) Uiso 0.50 1 d PD J 1 F45A F -0.0153(3) 1.1867(6) 0.43950(14) 0.080(2) Uiso 0.50 1 d PD J 1 F46A F -0.0188(3) 1.1065(7) 0.40896(12) 0.073(2) Uiso 0.50 1 d PD J 1 F47A F 0.0674(3) 1.1802(5) 0.42563(13) 0.072(2) Uiso 0.50 1 d PD J 1 F48A F -0.0216(5) 1.0156(8) 0.43840(19) 0.097(5) Uiso 0.50 1 d PD J 1 P8B P 0.0261(2) 1.0960(4) 0.43643(9) 0.0599(17) Uiso 0.50 1 d PD K 2 F43B F 0.0644(4) 1.0294(8) 0.42113(16) 0.072(4) Uiso 0.50 1 d PD K 2 F44B F 0.0660(3) 1.0440(6) 0.45550(11) 0.068(2) Uiso 0.50 1 d PD K 2 F45B F -0.0111(3) 1.1584(6) 0.44843(13) 0.075(2) Uiso 0.50 1 d PD K 2 F46B F -0.0105(4) 1.1413(8) 0.41306(14) 0.109(4) Uiso 0.50 1 d PD K 2 F47B F 0.0735(3) 1.1841(5) 0.43647(14) 0.074(2) Uiso 0.50 1 d PD K 2 F48B F -0.0219(4) 1.0058(7) 0.43332(18) 0.076(4) Uiso 0.50 1 d PD K 2 C1S C 0.5163(4) 0.6665(9) 0.39245(18) 0.140(4) Uani 1 1 d . . . H1S1 H 0.4938 0.6404 0.4028 0.209 Uiso 1 1 calc R . . H1S2 H 0.5594 0.6571 0.3980 0.209 Uiso 1 1 calc R . . H1S3 H 0.5044 0.6298 0.3789 0.209 Uiso 1 1 calc R . . C2S C 0.5033(4) 0.7759(8) 0.38883(15) 0.111(3) Uani 1 1 d . . . H2S1 H 0.5149 0.8135 0.4024 0.133 Uiso 1 1 calc R . . H2S2 H 0.5266 0.8033 0.3786 0.133 Uiso 1 1 calc R . . O3S O 0.4392(2) 0.7882(3) 0.38033(7) 0.0689(11) Uani 1 1 d . . . C4S C 0.4219(5) 0.8903(5) 0.37635(14) 0.109(3) Uani 1 1 d . . . H4S1 H 0.4438 0.9205 0.3660 0.130 Uiso 1 1 calc R . . H4S2 H 0.4311 0.9300 0.3897 0.130 Uiso 1 1 calc R . . C5S C 0.3561(4) 0.8914(7) 0.36754(16) 0.124(4) Uani 1 1 d . . . H5S1 H 0.3460 0.8376 0.3569 0.185 Uiso 1 1 calc R . . H5S2 H 0.3446 0.9572 0.3608 0.185 Uiso 1 1 calc R . . H5S3 H 0.3344 0.8802 0.3791 0.185 Uiso 1 1 calc R . . C6S C 0.3805(4) 0.2550(7) 0.37488(16) 0.115(3) Uani 1 1 d . . . H6S1 H 0.3960 0.2291 0.3627 0.172 Uiso 1 1 calc R . . H6S2 H 0.3673 0.1983 0.3826 0.172 Uiso 1 1 calc R . . H6S3 H 0.4123 0.2923 0.3844 0.172 Uiso 1 1 calc R . . C7S C 0.3285(4) 0.3245(8) 0.36707(13) 0.103(3) Uani 1 1 d . . . H7S1 H 0.3001 0.2924 0.3552 0.123 Uiso 1 1 calc R . . H7S2 H 0.3070 0.3390 0.3787 0.123 Uiso 1 1 calc R . . O8S O 0.3509(3) 0.4140(5) 0.36014(9) 0.0974(17) Uani 1 1 d . . . C9S C 0.3040(4) 0.4898(9) 0.35420(14) 0.112(3) Uani 1 1 d . . . H9S1 H 0.2854 0.5046 0.3666 0.134 Uiso 1 1 calc R . . H9S2 H 0.2724 0.4633 0.3425 0.134 Uiso 1 1 calc R . . C10S C 0.3291(5) 0.5831(7) 0.34720(15) 0.113(3) Uani 1 1 d . . . H10A H 0.3673 0.5985 0.3568 0.170 Uiso 1 1 calc R . . H10B H 0.3010 0.6390 0.3474 0.170 Uiso 1 1 calc R . . H10C H 0.3359 0.5740 0.3327 0.170 Uiso 1 1 calc R . . C11S C 0.7721(3) 0.8898(6) 0.27714(11) 0.081(2) Uani 1 1 d . . . H11E H 0.7887 0.8212 0.2790 0.121 Uiso 1 1 calc R . . H11F H 0.7896 0.9313 0.2895 0.121 Uiso 1 1 calc R . . H11G H 0.7817 0.9198 0.2642 0.121 Uiso 1 1 calc R . . C12S C 0.7088(3) 0.8856(5) 0.27516(9) 0.0590(15) Uani 1 1 d . . . N13S N 0.6588(2) 0.8805(5) 0.27341(8) 0.0724(15) Uani 1 1 d . . . C14S C -0.0616(5) 0.6107(10) 0.3849(2) 0.069(3) Uiso 0.50 1 d P . . H14P H -0.0494 0.6807 0.3830 0.103 Uiso 0.50 1 calc PR . . H14Q H -0.0403 0.5651 0.3769 0.103 Uiso 0.50 1 calc PR . . H14R H -0.0518 0.5929 0.4001 0.103 Uiso 0.50 1 calc PR . . C15S C -0.1267(4) 0.6006(7) 0.37700(15) 0.036(2) Uiso 0.50 1 d P . . N16S N -0.1714(5) 0.5986(8) 0.37153(17) 0.063(3) Uiso 0.50 1 d P . . C17S C -0.1892(7) 0.3426(14) 0.3583(3) 0.071(5) Uiso 0.40 1 d PD L 1 H17A H -0.1920 0.4152 0.3611 0.106 Uiso 0.40 1 calc PR L 1 H17B H -0.2241 0.3077 0.3617 0.106 Uiso 0.40 1 calc PR L 1 H17C H -0.1881 0.3319 0.3432 0.106 Uiso 0.40 1 calc PR L 1 C18S C -0.1352(8) 0.3025(18) 0.3714(3) 0.056(7) Uiso 0.40 1 d PD L 1 N19S N -0.0901(7) 0.2848(16) 0.3802(3) 0.082(7) Uiso 0.40 1 d PD L 1 C17E C -0.1930(8) 0.3182(18) 0.3672(4) 0.037(5) Uiso 0.20 1 d PD M 2 H17D H -0.1936 0.3892 0.3627 0.055 Uiso 0.20 1 calc PR M 2 H17E H -0.2139 0.3115 0.3791 0.055 Uiso 0.20 1 calc PR M 2 H17F H -0.2130 0.2764 0.3553 0.055 Uiso 0.20 1 calc PR M 2 C18E C -0.1309(9) 0.285(3) 0.3741(6) 0.033(9) Uiso 0.20 1 d PD M 2 N19E N -0.0828(9) 0.264(2) 0.3773(5) 0.047(8) Uiso 0.20 1 d PD M 2 C20S C -0.0165(8) 0.8886(14) 0.3841(3) 0.038(4) Uiso 0.25 1 d P . . H20E H -0.0294 0.9395 0.3730 0.057 Uiso 0.25 1 calc PR . . H20F H -0.0066 0.9221 0.3980 0.057 Uiso 0.25 1 calc PR . . H20G H -0.0489 0.8398 0.3841 0.057 Uiso 0.25 1 calc PR . . C21S C 0.0226(18) 0.850(3) 0.3810(7) 0.117(12) Uiso 0.25 1 d P . . N22S N 0.0636(14) 0.835(3) 0.3661(5) 0.120(10) Uiso 0.25 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 0.0264(3) 0.0303(3) 0.0331(3) -0.0021(3) 0.0052(3) -0.0020(2) N2A 0.0282(18) 0.0278(19) 0.042(2) -0.0024(16) 0.0100(17) -0.0002(15) C3A 0.027(2) 0.030(2) 0.045(3) 0.000(2) 0.006(2) 0.0011(18) C4A 0.027(2) 0.043(3) 0.057(3) 0.008(2) 0.003(2) -0.002(2) C5A 0.032(3) 0.052(3) 0.073(4) 0.010(3) 0.012(3) -0.006(2) C6A 0.043(3) 0.042(3) 0.063(4) 0.009(2) 0.025(3) 0.001(2) C7A 0.038(2) 0.026(2) 0.043(3) -0.0007(19) 0.012(2) -0.0006(18) N8A 0.0235(18) 0.035(2) 0.037(2) -0.0003(16) 0.0008(16) 0.0006(15) N9A 0.0263(18) 0.036(2) 0.035(2) -0.0001(17) 0.0038(16) -0.0025(15) C10A 0.034(2) 0.036(3) 0.038(3) 0.000(2) 0.005(2) -0.0001(19) C11A 0.039(3) 0.051(3) 0.030(3) 0.001(2) -0.001(2) -0.001(2) C12A 0.036(3) 0.042(3) 0.038(3) -0.003(2) -0.003(2) -0.001(2) C13A 0.040(3) 0.062(3) 0.033(3) 0.000(2) 0.007(2) -0.014(2) C14A 0.067(4) 0.075(4) 0.068(4) 0.010(3) 0.007(3) -0.034(3) C15A 0.037(3) 0.095(5) 0.108(6) -0.014(4) 0.029(3) -0.001(3) C20A 0.070(4) 0.070(4) 0.040(3) -0.008(3) 0.024(3) -0.028(3) C21A 0.063(4) 0.068(4) 0.040(3) 0.000(3) 0.002(3) -0.008(3) C22A 0.081(5) 0.085(5) 0.060(4) -0.001(4) -0.009(4) 0.000(4) C23A 0.077(4) 0.066(4) 0.056(4) 0.001(3) 0.002(3) -0.018(3) N24A 0.0280(18) 0.031(2) 0.037(2) -0.0011(16) 0.0045(16) -0.0017(15) C25A 0.029(2) 0.041(3) 0.041(3) 0.000(2) 0.004(2) -0.0007(19) C26A 0.029(2) 0.050(3) 0.061(4) -0.003(3) 0.004(2) -0.002(2) C27A 0.033(3) 0.052(3) 0.069(4) 0.001(3) 0.006(2) -0.014(2) C28A 0.041(3) 0.045(3) 0.062(4) -0.004(3) 0.005(3) -0.011(2) C29A 0.031(2) 0.039(3) 0.035(3) 0.001(2) 0.0038(19) -0.0019(19) N30A 0.0241(19) 0.037(2) 0.060(3) -0.0090(19) 0.0027(18) -0.0004(16) N31A 0.0236(18) 0.036(2) 0.039(2) -0.0022(17) 0.0004(16) -0.0029(15) C32A 0.030(2) 0.031(3) 0.058(3) -0.006(2) 0.002(2) 0.0019(19) C33A 0.035(3) 0.045(3) 0.140(7) -0.033(4) 0.012(3) 0.005(2) C34A 0.028(3) 0.054(4) 0.139(7) -0.028(4) 0.015(3) 0.006(2) C35A 0.032(2) 0.031(3) 0.065(4) -0.005(2) 0.008(2) 0.0025(19) C36A 0.059(3) 0.045(3) 0.067(4) 0.005(3) -0.013(3) -0.009(3) C37A 0.055(3) 0.039(3) 0.063(4) 0.003(3) 0.006(3) 0.001(2) N38A 0.036(2) 0.028(2) 0.045(2) -0.0038(17) 0.0049(18) -0.0060(16) N39A 0.0318(19) 0.028(2) 0.040(2) -0.0021(16) 0.0043(16) -0.0057(15) C40A 0.043(3) 0.031(2) 0.039(3) 0.004(2) 0.011(2) 0.004(2) C41A 0.048(3) 0.028(3) 0.061(4) -0.004(2) 0.014(3) 0.003(2) C42A 0.053(3) 0.035(3) 0.051(3) -0.009(2) 0.007(2) -0.007(2) C43A 0.038(3) 0.035(3) 0.060(3) 0.008(2) 0.013(2) 0.004(2) C44A 0.053(4) 0.098(6) 0.124(7) -0.012(5) 0.040(4) -0.002(4) C45A 0.065(4) 0.164(9) 0.084(6) 0.043(6) -0.027(4) -0.047(5) Fe1B 0.0402(4) 0.0315(3) 0.0334(4) -0.0026(3) 0.0049(3) 0.0006(3) N2B 0.040(2) 0.036(2) 0.035(2) -0.0009(17) 0.0026(17) 0.0045(17) C3B 0.048(3) 0.038(3) 0.035(3) -0.001(2) 0.000(2) 0.006(2) C4B 0.068(4) 0.040(3) 0.058(4) -0.002(3) 0.018(3) 0.011(3) C5B 0.081(4) 0.059(4) 0.063(4) -0.002(3) 0.029(3) 0.022(3) C6B 0.052(3) 0.054(3) 0.054(3) 0.005(3) 0.019(3) 0.011(3) C7B 0.040(3) 0.045(3) 0.038(3) 0.002(2) 0.003(2) 0.003(2) N8B 0.050(2) 0.033(2) 0.042(2) -0.0002(18) 0.0066(19) 0.0046(18) N9B 0.047(2) 0.031(2) 0.039(2) -0.0025(17) 0.0042(19) 0.0048(18) C10B 0.049(3) 0.030(3) 0.046(3) 0.000(2) -0.001(2) -0.003(2) C11B 0.057(3) 0.034(3) 0.054(3) 0.003(2) -0.002(3) -0.002(2) C12B 0.063(3) 0.033(3) 0.047(3) -0.008(2) -0.003(3) 0.005(2) C13B 0.057(3) 0.037(3) 0.066(4) 0.004(3) 0.015(3) -0.002(2) C14B 0.064(4) 0.053(4) 0.113(6) 0.002(4) 0.025(4) -0.008(3) C15B 0.094(5) 0.057(4) 0.072(5) -0.003(3) 0.034(4) -0.006(3) N16B 0.038(2) 0.038(2) 0.048(3) -0.0017(19) 0.0103(19) 0.0025(17) N17B 0.039(2) 0.036(2) 0.041(2) -0.0014(18) 0.0080(18) 0.0018(17) C18B 0.042(3) 0.037(3) 0.048(3) -0.004(2) 0.008(2) -0.004(2) C19B 0.048(3) 0.044(3) 0.088(5) -0.008(3) 0.022(3) -0.007(2) C20B 0.045(3) 0.054(3) 0.082(4) -0.001(3) 0.026(3) -0.004(3) C21B 0.050(3) 0.035(3) 0.060(4) -0.002(2) 0.017(3) -0.003(2) C22B 0.051(3) 0.046(3) 0.054(3) 0.000(3) 0.007(3) 0.006(2) C23B 0.089(4) 0.042(3) 0.050(4) 0.004(3) 0.014(3) 0.010(3) N24B 0.044(2) 0.031(2) 0.031(2) 0.0006(16) 0.0076(17) -0.0062(17) C25B 0.038(3) 0.032(2) 0.036(3) -0.0013(19) 0.007(2) -0.0056(19) C26B 0.044(3) 0.043(3) 0.047(3) -0.005(2) 0.013(2) -0.004(2) C27B 0.054(3) 0.052(3) 0.049(3) -0.004(3) 0.019(3) -0.005(3) C28B 0.060(3) 0.050(3) 0.037(3) -0.005(2) 0.015(3) -0.006(3) C29B 0.047(3) 0.031(3) 0.038(3) -0.002(2) 0.008(2) -0.005(2) N30B 0.034(2) 0.037(2) 0.041(2) -0.0005(17) 0.0080(18) -0.0006(16) N31B 0.038(2) 0.037(2) 0.036(2) -0.0032(17) 0.0079(18) -0.0020(17) C32B 0.040(3) 0.048(3) 0.030(3) 0.000(2) 0.003(2) -0.004(2) C33B 0.035(3) 0.075(4) 0.039(3) 0.001(3) 0.001(2) 0.001(3) C34B 0.031(3) 0.069(4) 0.047(3) -0.003(3) 0.005(2) -0.001(2) C35B 0.035(3) 0.076(4) 0.031(3) 0.000(3) 0.003(2) -0.003(2) C36B 0.075(4) 0.094(5) 0.086(5) -0.041(4) 0.041(4) -0.021(4) C37B 0.063(4) 0.109(6) 0.060(4) 0.026(4) 0.025(3) 0.006(4) N38B 0.048(2) 0.038(2) 0.032(2) -0.0021(17) 0.0034(19) -0.0034(18) N39B 0.047(2) 0.039(2) 0.034(2) 0.0009(18) 0.0052(19) 0.0009(18) C40B 0.048(3) 0.040(3) 0.039(3) 0.006(2) 0.001(2) 0.000(2) C41B 0.055(3) 0.046(3) 0.038(3) 0.003(2) -0.004(2) -0.006(2) C42B 0.061(3) 0.043(3) 0.029(3) 0.001(2) 0.004(2) -0.009(2) C43B 0.056(14) 0.08(2) 0.038(11) 0.000(5) -0.002(4) 0.018(6) C44B 0.091(11) 0.058(8) 0.17(2) -0.016(10) 0.036(13) 0.019(8) C45B 0.062(8) 0.115(15) 0.114(18) 0.000(12) 0.028(10) -0.007(9) Fe1C 0.0359(3) 0.0339(4) 0.0338(4) 0.0028(3) 0.0059(3) -0.0011(3) N2C 0.042(2) 0.038(2) 0.032(2) 0.0029(17) 0.0033(17) -0.0032(17) C3C 0.043(3) 0.041(3) 0.035(3) 0.001(2) 0.005(2) 0.001(2) C4C 0.062(3) 0.041(3) 0.048(3) 0.001(2) 0.018(3) -0.009(2) C5C 0.055(3) 0.061(4) 0.050(3) 0.005(3) 0.019(3) -0.014(3) C6C 0.049(3) 0.049(3) 0.046(3) 0.004(2) 0.016(2) -0.002(2) C7C 0.037(2) 0.044(3) 0.032(3) 0.002(2) 0.006(2) 0.000(2) N8C 0.047(2) 0.037(2) 0.038(2) 0.0028(17) 0.0111(19) -0.0026(18) N9C 0.041(2) 0.032(2) 0.039(2) -0.0002(17) 0.0077(18) -0.0054(17) C10C 0.040(3) 0.040(3) 0.039(3) -0.004(2) -0.001(2) 0.000(2) C11C 0.054(3) 0.030(3) 0.054(3) 0.001(2) 0.006(3) -0.001(2) C12C 0.059(3) 0.031(3) 0.046(3) 0.006(2) 0.010(3) -0.005(2) C13C 0.045(8) 0.028(6) 0.084(14) -0.007(4) 0.017(4) -0.002(3) C14C 0.088(6) 0.062(5) 0.070(6) -0.001(4) 0.043(5) -0.007(5) C15C 0.043(5) 0.060(6) 0.159(11) 0.029(6) 0.026(5) 0.006(4) N16C 0.035(2) 0.039(2) 0.044(2) 0.0049(18) 0.0095(18) -0.0007(17) N17C 0.0311(19) 0.039(2) 0.038(2) 0.0027(17) 0.0069(17) -0.0007(16) C18C 0.039(3) 0.040(3) 0.048(3) 0.001(2) 0.008(2) 0.004(2) C19C 0.049(3) 0.040(3) 0.070(4) 0.008(3) 0.023(3) 0.009(2) C20C 0.043(3) 0.052(3) 0.057(3) 0.002(3) 0.019(3) 0.007(2) C21C 0.047(3) 0.031(3) 0.069(4) 0.002(2) 0.021(3) 0.003(2) C22C 0.045(3) 0.046(3) 0.071(4) -0.005(3) 0.011(3) -0.005(2) C23C 0.097(5) 0.038(3) 0.064(4) -0.005(3) 0.033(4) -0.011(3) N24C 0.039(2) 0.034(2) 0.034(2) 0.0006(17) 0.0075(17) 0.0029(16) C25C 0.042(3) 0.037(3) 0.037(3) 0.000(2) 0.008(2) 0.005(2) C26C 0.050(3) 0.062(4) 0.037(3) 0.006(2) 0.011(2) 0.004(3) C27C 0.044(3) 0.071(4) 0.051(4) 0.007(3) 0.018(3) 0.000(3) C28C 0.035(3) 0.054(3) 0.052(3) 0.008(3) 0.010(2) 0.002(2) C29C 0.035(2) 0.041(3) 0.045(3) 0.004(2) 0.007(2) 0.007(2) N30C 0.031(2) 0.054(3) 0.035(2) 0.0055(19) 0.0033(17) 0.0008(18) N31C 0.032(2) 0.049(2) 0.039(2) 0.0016(19) 0.0075(18) -0.0014(18) C32C 0.038(3) 0.076(4) 0.034(3) 0.003(3) 0.002(2) -0.003(3) C33C 0.043(3) 0.103(5) 0.037(3) 0.006(3) -0.001(2) -0.006(3) C34C 0.034(3) 0.089(4) 0.043(3) 0.005(3) 0.000(2) -0.007(3) C35C 0.042(3) 0.109(5) 0.040(3) 0.010(3) 0.003(3) -0.011(3) C36C 0.062(4) 0.120(6) 0.057(4) -0.008(4) 0.016(3) 0.011(4) C37C 0.083(5) 0.107(6) 0.078(5) 0.010(4) 0.021(4) -0.035(4) N38C 0.042(2) 0.037(2) 0.033(2) 0.0014(17) 0.0044(18) 0.0019(17) N39C 0.042(2) 0.038(2) 0.033(2) -0.0006(17) 0.0055(18) -0.0041(18) C40C 0.046(3) 0.039(3) 0.035(3) -0.004(2) 0.001(2) 0.000(2) C41C 0.048(3) 0.049(3) 0.032(3) -0.002(2) -0.003(2) 0.005(2) C42C 0.051(3) 0.045(3) 0.035(3) 0.001(2) 0.007(2) 0.004(2) C43C 0.044(3) 0.074(4) 0.040(3) 0.005(3) 0.001(2) -0.013(3) C44C 0.058(4) 0.110(6) 0.116(7) 0.015(5) 0.040(4) 0.014(4) C45C 0.102(6) 0.071(5) 0.113(7) 0.003(4) 0.030(5) -0.035(4) Fe1D 0.0238(3) 0.0344(4) 0.0407(4) 0.0045(3) 0.0035(3) 0.0002(3) N2D 0.0245(18) 0.038(2) 0.037(2) 0.0009(17) 0.0035(16) 0.0001(15) C3D 0.029(2) 0.036(3) 0.041(3) 0.000(2) 0.005(2) -0.0006(19) C4D 0.024(2) 0.046(3) 0.074(4) 0.002(3) 0.008(2) 0.000(2) C5D 0.033(3) 0.049(3) 0.089(5) 0.001(3) 0.017(3) 0.008(2) C6D 0.037(3) 0.041(3) 0.067(4) -0.001(3) 0.008(2) 0.006(2) C7D 0.037(2) 0.037(3) 0.035(3) 0.002(2) 0.004(2) 0.000(2) N8D 0.0236(18) 0.038(2) 0.053(3) 0.0045(18) 0.0071(17) -0.0028(16) N9D 0.0240(18) 0.036(2) 0.045(2) 0.0021(17) 0.0065(16) -0.0007(15) C10D 0.029(2) 0.040(3) 0.055(3) 0.002(2) 0.008(2) -0.003(2) C11D 0.038(3) 0.043(3) 0.096(5) 0.012(3) 0.021(3) -0.002(2) C12D 0.029(2) 0.050(3) 0.082(4) 0.009(3) 0.012(3) -0.008(2) C13D 0.031(3) 0.039(3) 0.085(4) 0.013(3) 0.015(3) 0.006(2) C14D 0.049(3) 0.043(3) 0.090(5) -0.004(3) -0.012(3) 0.008(3) C15D 0.052(3) 0.046(3) 0.068(4) 0.005(3) 0.020(3) 0.005(3) N16D 0.0277(19) 0.038(2) 0.051(3) 0.0005(18) 0.0030(18) -0.0022(16) N17D 0.031(2) 0.028(2) 0.057(3) 0.0028(18) 0.0082(18) -0.0047(16) C18D 0.035(3) 0.042(3) 0.068(4) -0.003(3) 0.013(2) -0.007(2) C19D 0.048(3) 0.032(3) 0.077(4) -0.001(3) 0.018(3) -0.006(2) C20D 0.044(3) 0.027(2) 0.062(4) -0.003(2) 0.005(2) -0.002(2) C21D 0.044(3) 0.038(3) 0.161(7) -0.013(4) 0.041(4) -0.009(3) C22D 0.213(13) 0.110(8) 0.59(3) 0.150(14) 0.315(19) 0.084(9) C23D 0.046(5) 0.212(14) 0.41(2) -0.194(16) -0.084(9) 0.044(6) N24D 0.029(2) 0.032(2) 0.052(3) 0.0071(18) 0.0034(19) 0.0000(16) C25D 0.030(2) 0.031(2) 0.059(3) 0.007(2) 0.011(2) -0.0012(19) C26D 0.033(3) 0.049(3) 0.082(4) 0.007(3) 0.019(3) -0.001(2) C27D 0.030(3) 0.053(3) 0.092(5) 0.013(3) 0.012(3) 0.006(2) C28D 0.030(3) 0.057(4) 0.078(4) 0.016(3) -0.004(3) 0.002(2) C29D 0.029(2) 0.038(3) 0.058(3) 0.012(2) 0.004(2) -0.002(2) N30D 0.029(2) 0.050(3) 0.047(3) 0.010(2) -0.0067(18) -0.0024(18) N31D 0.0251(19) 0.042(2) 0.047(3) 0.0038(19) -0.0019(17) -0.0046(16) C32D 0.046(3) 0.043(3) 0.042(3) 0.003(2) -0.002(2) -0.007(2) C33D 0.046(3) 0.065(4) 0.042(3) 0.006(3) -0.009(3) -0.010(3) C34D 0.039(3) 0.059(4) 0.058(4) 0.014(3) -0.014(3) -0.009(2) C35D 0.050(3) 0.068(4) 0.036(3) -0.002(3) 0.000(2) 0.004(3) C36D 0.089(5) 0.064(4) 0.074(5) -0.005(4) -0.001(4) 0.023(4) C37D 0.059(4) 0.095(5) 0.074(5) 0.018(4) 0.023(3) 0.002(4) N38D 0.034(2) 0.041(2) 0.055(3) 0.003(2) 0.013(2) 0.0023(17) N39D 0.032(2) 0.041(2) 0.045(3) 0.0023(18) 0.0086(18) 0.0038(17) C40D 0.047(3) 0.063(4) 0.043(3) 0.003(3) 0.005(2) 0.007(3) C41D 0.062(4) 0.083(5) 0.045(3) -0.002(3) 0.013(3) 0.009(3) C42D 0.056(3) 0.064(4) 0.059(4) 0.001(3) 0.027(3) 0.006(3) C43D 0.057(9) 0.112(15) 0.038(7) -0.012(6) -0.007(5) 0.029(7) C44D 0.096(8) 0.112(10) 0.049(6) 0.020(6) 0.010(6) 0.060(8) C45D 0.027(5) 0.081(8) 0.189(16) -0.017(9) -0.009(7) 0.006(5) P1 0.0477(8) 0.0495(8) 0.0398(8) 0.0036(6) 0.0068(6) -0.0034(6) F1 0.122(4) 0.144(4) 0.067(3) -0.005(3) 0.012(2) 0.083(3) F2 0.0489(18) 0.101(3) 0.055(2) 0.0120(19) -0.0049(15) -0.0202(18) F3 0.087(3) 0.090(3) 0.054(2) -0.0057(19) 0.0122(19) 0.024(2) F4 0.071(2) 0.070(2) 0.049(2) -0.0014(16) -0.0065(16) -0.0128(18) F5 0.110(3) 0.064(2) 0.062(2) 0.0190(18) -0.002(2) -0.030(2) F6 0.076(2) 0.097(3) 0.063(2) 0.031(2) 0.0008(18) -0.030(2) P2 0.0449(8) 0.0455(8) 0.0632(10) 0.0009(7) 0.0042(7) 0.0030(6) F7 0.102(3) 0.102(3) 0.071(3) 0.010(2) 0.020(2) -0.031(2) F8 0.063(2) 0.0499(19) 0.089(3) -0.0113(18) 0.0102(18) 0.0032(16) F9 0.078(2) 0.090(3) 0.073(3) 0.006(2) 0.026(2) -0.001(2) F10 0.094(3) 0.052(2) 0.095(3) -0.013(2) -0.015(2) 0.0034(19) F11 0.055(2) 0.061(2) 0.100(3) -0.003(2) -0.0137(19) 0.0122(16) F12 0.0496(19) 0.081(3) 0.097(3) 0.002(2) -0.0045(19) 0.0105(18) P3 0.0363(6) 0.0360(7) 0.0432(8) -0.0046(5) 0.0014(6) 0.0041(5) F13 0.0468(17) 0.0465(17) 0.063(2) -0.0169(14) 0.0063(14) -0.0046(13) F14 0.077(2) 0.088(3) 0.081(3) -0.013(2) 0.041(2) -0.032(2) F15 0.072(2) 0.0453(18) 0.073(2) -0.0204(16) -0.0161(17) 0.0083(16) F16 0.174(4) 0.057(2) 0.063(2) 0.0111(18) 0.047(3) -0.003(2) F17 0.066(2) 0.060(2) 0.144(4) -0.040(2) -0.038(2) 0.0297(18) F18 0.0340(15) 0.0427(17) 0.098(3) 0.0014(17) -0.0007(16) 0.0007(13) P5 0.0417(7) 0.0435(7) 0.0402(7) 0.0016(6) 0.0095(6) 0.0017(6) F25 0.070(2) 0.069(2) 0.058(2) -0.0070(17) 0.0201(17) 0.0194(17) F26 0.0486(18) 0.073(2) 0.055(2) 0.0018(16) -0.0042(15) 0.0081(16) F27 0.066(2) 0.0510(18) 0.0501(19) -0.0041(14) 0.0160(15) 0.0095(15) F28 0.0487(17) 0.0548(18) 0.0452(18) 0.0047(14) 0.0029(14) -0.0023(14) F29 0.075(2) 0.0477(18) 0.0477(19) 0.0068(14) 0.0114(16) -0.0107(15) F30 0.0569(19) 0.067(2) 0.059(2) 0.0070(16) 0.0139(16) -0.0177(16) C1S 0.102(7) 0.151(10) 0.156(10) 0.040(8) 0.002(6) 0.045(7) C2S 0.081(6) 0.133(8) 0.109(7) 0.039(6) -0.003(5) -0.036(5) O3S 0.082(3) 0.057(3) 0.069(3) 0.009(2) 0.020(2) -0.003(2) C4S 0.203(11) 0.050(4) 0.080(6) 0.014(4) 0.046(6) 0.004(5) C5S 0.136(8) 0.119(8) 0.136(8) 0.067(6) 0.077(7) 0.072(7) C6S 0.127(8) 0.111(7) 0.129(8) -0.046(6) 0.081(7) -0.038(6) C7S 0.115(7) 0.130(8) 0.070(5) -0.015(5) 0.035(5) -0.051(6) O8S 0.098(4) 0.116(5) 0.094(4) -0.019(3) 0.057(3) -0.024(4) C9S 0.090(6) 0.163(10) 0.079(6) -0.036(6) 0.012(5) -0.016(7) C10S 0.150(9) 0.102(7) 0.100(7) 0.007(5) 0.055(6) 0.011(6) C11S 0.048(4) 0.115(6) 0.072(5) 0.025(4) -0.003(3) 0.003(4) C12S 0.052(4) 0.072(4) 0.048(4) 0.002(3) -0.003(3) 0.015(3) N13S 0.058(3) 0.099(4) 0.054(3) -0.001(3) -0.003(3) 0.020(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 N24A 2.126(3) . ? Fe1A N2A 2.129(3) . ? Fe1A N17A 2.179(4) . ? Fe1A N9A 2.201(4) . ? Fe1A N31A 2.210(4) . ? Fe1A N39A 2.211(4) . ? N2A C3A 1.332(6) . ? N2A C7A 1.336(6) . ? C3A C4A 1.379(6) . ? C3A N8A 1.406(6) . ? C4A C5A 1.367(7) . ? C5A C6A 1.394(8) . ? C6A C7A 1.379(6) . ? C7A N16A 1.400(6) . ? N8A C12A 1.351(6) . ? N8A N9A 1.377(5) . ? N9A C10A 1.324(6) . ? C10A C11A 1.405(6) . ? C10A C13A 1.503(6) . ? C11A C12A 1.352(7) . ? C13A C14A 1.519(8) . ? C13A C15A 1.541(8) . ? N16A C20A 1.356(6) . ? N16A N17A 1.371(5) . ? N17A C18A 1.322(7) . ? C18A C19A 1.416(8) . ? C18A C21A 1.500(8) . ? C19A C20A 1.345(8) . ? C21A C22A 1.510(8) . ? C21A C23A 1.524(9) . ? N24A C25A 1.330(6) . ? N24A C29A 1.339(6) . ? C25A C26A 1.379(6) . ? C25A N30A 1.409(6) . ? C26A C27A 1.388(7) . ? C27A C28A 1.372(7) . ? C28A C29A 1.385(6) . ? C29A N38A 1.398(6) . ? N30A C34A 1.350(6) . ? N30A N31A 1.371(5) . ? N31A C32A 1.323(6) . ? C32A C33A 1.406(7) . ? C32A C35A 1.496(6) . ? C33A C34A 1.362(8) . ? C35A C36A 1.515(8) . ? C35A C37A 1.530(7) . ? N38A C42A 1.359(6) . ? N38A N39A 1.384(5) . ? N39A C40A 1.337(6) . ? C40A C41A 1.418(7) . ? C40A C43A 1.490(6) . ? C41A C42A 1.354(7) . ? C43A C45A 1.504(8) . ? C43A C44A 1.522(8) . ? Fe1B N24B 2.131(4) . ? Fe1B N2B 2.132(4) . ? Fe1B N17B 2.169(4) . ? Fe1B N31B 2.175(4) . ? Fe1B N39B 2.215(4) . ? Fe1B N9B 2.223(4) . ? N2B C3B 1.333(6) . ? N2B C7B 1.340(6) . ? C3B C4B 1.371(7) . ? C3B N8B 1.407(6) . ? C4B C5B 1.370(8) . ? C5B C6B 1.395(8) . ? C6B C7B 1.380(7) . ? C7B N16B 1.407(6) . ? N8B C12B 1.352(6) . ? N8B N9B 1.373(5) . ? N9B C10B 1.342(6) . ? C10B C11B 1.419(7) . ? C10B C13B 1.502(7) . ? C11B C12B 1.356(8) . ? C13B C15B 1.529(9) . ? C13B C14B 1.532(8) . ? N16B C20B 1.354(7) . ? N16B N17B 1.369(5) . ? N17B C18B 1.333(6) . ? C18B C19B 1.408(7) . ? C18B C21B 1.489(7) . ? C19B C20B 1.359(8) . ? C21B C22B 1.529(7) . ? C21B C23B 1.545(8) . ? N24B C29B 1.337(6) . ? N24B C25B 1.343(6) . ? C25B C26B 1.370(6) . ? C25B N30B 1.412(6) . ? C26B C27B 1.390(7) . ? C27B C28B 1.376(8) . ? C28B C29B 1.380(7) . ? C29B N38B 1.399(6) . ? N30B C34B 1.353(6) . ? N30B N31B 1.380(5) . ? N31B C32B 1.323(6) . ? C32B C33B 1.410(7) . ? C32B C35B 1.499(7) . ? C33B C34B 1.358(7) . ? C35B C37B 1.522(8) . ? C35B C36B 1.525(8) . ? N38B C42B 1.364(6) . ? N38B N39B 1.373(5) . ? N39B C40B 1.316(6) . ? C40B C41B 1.416(7) . ? C40B C43B 1.504(14) . ? C40B C43E 1.514(18) . ? C41B C42B 1.355(7) . ? C43B C45B 1.521(15) . ? C43B C44B 1.526(14) . ? C43E C45E 1.524(17) . ? C43E C44E 1.528(19) . ? Fe1C N24C 2.123(4) . ? Fe1C N2C 2.142(4) . ? Fe1C N31C 2.171(4) . ? Fe1C N17C 2.181(4) . ? Fe1C N9C 2.200(4) . ? Fe1C N39C 2.212(4) . ? N2C C7C 1.328(6) . ? N2C C3C 1.342(6) . ? C3C C4C 1.382(7) . ? C3C N8C 1.409(6) . ? C4C C5C 1.375(7) . ? C5C C6C 1.396(8) . ? C6C C7C 1.382(7) . ? C7C N16C 1.414(6) . ? N8C C12C 1.360(6) . ? N8C N9C 1.375(5) . ? N9C C10C 1.331(6) . ? C10C C11C 1.423(7) . ? C10C C13C 1.503(10) . ? C10C C13E 1.52(2) . ? C11C C12C 1.350(7) . ? C13C C14C 1.525(12) . ? C13C C15C 1.547(11) . ? C13E C15E 1.53(2) . ? C13E C14E 1.53(2) . ? N16C C20C 1.356(6) . ? N16C N17C 1.372(5) . ? N17C C18C 1.327(6) . ? C18C C19C 1.410(7) . ? C18C C21C 1.499(7) . ? C19C C20C 1.361(7) . ? C21C C22C 1.518(7) . ? C21C C23C 1.530(8) . ? N24C C25C 1.338(6) . ? N24C C29C 1.342(6) . ? C25C C26C 1.373(7) . ? C25C N38C 1.413(6) . ? C26C C27C 1.376(7) . ? C27C C28C 1.378(7) . ? C28C C29C 1.376(7) . ? C29C N30C 1.406(6) . ? N30C C34C 1.354(6) . ? N30C N31C 1.381(5) . ? N31C C32C 1.325(6) . ? C32C C33C 1.405(7) . ? C32C C35C 1.498(7) . ? C33C C34C 1.346(8) . ? C35C C36C 1.515(9) . ? C35C C37C 1.519(10) . ? N38C C42C 1.358(6) . ? N38C N39C 1.372(5) . ? N39C C40C 1.329(6) . ? C40C C41C 1.407(7) . ? C40C C43C 1.497(7) . ? C41C C42C 1.347(7) . ? C43C C44C 1.515(9) . ? C43C C45C 1.531(9) . ? Fe1D N24D 2.127(4) . ? Fe1D N2D 2.133(3) . ? Fe1D N39D 2.172(4) . ? Fe1D N31D 2.200(4) . ? Fe1D N9D 2.214(4) . ? Fe1D N17D 2.228(4) . ? N2D C7D 1.330(6) . ? N2D C3D 1.342(5) . ? C3D C4D 1.380(6) . ? C3D N8D 1.404(6) . ? C4D C5D 1.369(7) . ? C5D C6D 1.381(7) . ? C6D C7D 1.371(6) . ? C7D N16D 1.403(6) . ? N8D C12D 1.361(6) . ? N8D N9D 1.376(5) . ? N9D C10D 1.320(6) . ? C10D C11D 1.411(6) . ? C10D C13D 1.508(6) . ? C11D C12D 1.355(7) . ? C13D C14D 1.520(8) . ? C13D C15D 1.528(8) . ? N16D C20D 1.363(6) . ? N16D N17D 1.367(5) . ? N17D C18D 1.319(6) . ? C18D C19D 1.407(7) . ? C18D C21D 1.495(7) . ? C19D C20D 1.351(7) . ? C21D C22D 1.473(12) . ? C21D C23D 1.493(15) . ? N24D C25D 1.327(6) . ? N24D C29D 1.334(6) . ? C25D C26D 1.391(6) . ? C25D N38D 1.399(6) . ? C26D C27D 1.376(8) . ? C27D C28D 1.367(8) . ? C28D C29D 1.382(7) . ? C29D N30D 1.398(7) . ? N30D C34D 1.354(7) . ? N30D N31D 1.377(5) . ? N31D C32D 1.334(6) . ? C32D C33D 1.419(7) . ? C32D C35D 1.494(7) . ? C33D C34D 1.356(8) . ? C35D C36D 1.520(8) . ? C35D C37D 1.544(8) . ? N38D C42D 1.347(7) . ? N38D N39D 1.375(5) . ? N39D C40D 1.326(6) . ? C40D C41D 1.395(7) . ? C40D C43D 1.502(13) . ? C40D C43F 1.522(17) . ? C41D C42D 1.354(8) . ? C43D C45D 1.508(15) . ? C43D C44D 1.531(15) . ? C43F C45F 1.527(19) . ? C43F C44F 1.539(17) . ? P1 F1 1.566(4) . ? P1 F6 1.570(4) . ? P1 F2 1.582(3) . ? P1 F5 1.594(4) . ? P1 F4 1.599(3) . ? P1 F3 1.604(4) . ? P2 F9 1.582(4) . ? P2 F10 1.584(4) . ? P2 F12 1.585(4) . ? P2 F7 1.591(4) . ? P2 F8 1.594(4) . ? P2 F11 1.602(3) . ? P3 F16 1.564(4) . ? P3 F17 1.572(3) . ? P3 F15 1.584(3) . ? P3 F14 1.586(4) . ? P3 F18 1.596(3) . ? P3 F13 1.610(3) . ? P4A F22A 1.531(8) . ? P4A F19A 1.570(8) . ? P4A F24A 1.587(8) . ? P4A F23A 1.613(8) . ? P4A F20A 1.659(8) . ? P4A F21A 1.665(8) . ? P4B F21B 1.538(9) . ? P4B F23B 1.552(8) . ? P4B F20B 1.567(9) . ? P4B F24B 1.633(9) . ? P4B F19B 1.635(9) . ? P4B F22B 1.642(9) . ? P5 F25 1.582(3) . ? P5 F26 1.590(3) . ? P5 F30 1.599(3) . ? P5 F29 1.605(3) . ? P5 F28 1.609(3) . ? P5 F27 1.612(3) . ? P6A F31A 1.549(8) . ? P6A F35A 1.567(8) . ? P6A F32A 1.580(9) . ? P6A F34A 1.607(8) . ? P6A F36A 1.609(8) . ? P6A F33A 1.635(9) . ? P6B F36B 1.551(7) . ? P6B F33B 1.567(8) . ? P6B F32B 1.569(7) . ? P6B F31B 1.607(7) . ? P6B F34B 1.629(8) . ? P6B F35B 1.644(8) . ? P7A F37C 1.558(10) . ? P7A F40C 1.577(11) . ? P7A F42C 1.579(10) . ? P7A F41A 1.582(7) . ? P7A F37A 1.584(7) . ? P7A F38A 1.589(8) . ? P7A F41C 1.606(11) . ? P7A F40A 1.606(8) . ? P7A F39A 1.615(7) . ? P7A F42A 1.629(7) . ? P7A F38C 1.634(11) . ? P7A F39C 1.640(11) . ? P7B F39B 1.552(9) . ? P7B F42B 1.581(9) . ? P7B F38B 1.582(8) . ? P7B F41B 1.592(9) . ? P7B F40B 1.616(8) . ? P7B F37B 1.642(9) . ? P8A F43A 1.545(9) . ? P8A F46A 1.569(8) . ? P8A F47A 1.584(7) . ? P8A F48A 1.604(9) . ? P8A F44A 1.621(10) . ? P8A F45A 1.655(8) . ? P8B F45B 1.498(8) . ? P8B F44B 1.529(8) . ? P8B F47B 1.584(8) . ? P8B F48B 1.601(8) . ? P8B F46B 1.668(9) . ? P8B F43B 1.683(8) . ? C1S C2S 1.483(13) . ? C2S O3S 1.459(9) . ? O3S C4S 1.413(8) . ? C4S C5S 1.489(12) . ? C6S C7S 1.502(12) . ? C7S O8S 1.393(9) . ? O8S C9S 1.456(11) . ? C9S C10S 1.465(12) . ? C11S C12S 1.421(8) . ? C12S N13S 1.122(7) . ? C14S C15S 1.470(15) . ? C15S N16S 1.007(12) . ? C17S C18S 1.441(14) . ? C18S N19S 1.091(14) . ? C17E C18E 1.461(16) . ? C18E N19E 1.105(16) . ? C20S C21S 1.08(4) . ? C21S N22S 1.48(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 N24A Fe1A N2A 175.00(14) . . ? N24A Fe1A N17A 107.16(14) . . ? N2A Fe1A N17A 73.72(15) . . ? N24A Fe1A N9A 105.74(14) . . ? N2A Fe1A N9A 73.44(14) . . ? N17A Fe1A N9A 147.09(14) . . ? N24A Fe1A N31A 73.89(13) . . ? N2A Fe1A N31A 110.95(13) . . ? N17A Fe1A N31A 98.83(14) . . ? N9A Fe1A N31A 90.88(14) . . ? N24A Fe1A N39A 73.42(13) . . ? N2A Fe1A N39A 101.68(13) . . ? N17A Fe1A N39A 93.16(14) . . ? N9A Fe1A N39A 95.42(14) . . ? N31A Fe1A N39A 147.21(13) . . ? C3A N2A C7A 117.9(4) . . ? C3A N2A Fe1A 120.9(3) . . ? C7A N2A Fe1A 119.8(3) . . ? N2A C3A C4A 123.9(4) . . ? N2A C3A N8A 112.4(4) . . ? C4A C3A N8A 123.6(4) . . ? C5A C4A C3A 116.6(5) . . ? C4A C5A C6A 121.9(5) . . ? C7A C6A C5A 116.3(5) . . ? N2A C7A C6A 123.5(5) . . ? N2A C7A N16A 113.0(4) . . ? C6A C7A N16A 123.4(4) . . ? C12A N8A N9A 110.6(4) . . ? C12A N8A C3A 130.3(4) . . ? N9A N8A C3A 119.1(4) . . ? C10A N9A N8A 105.5(4) . . ? C10A N9A Fe1A 141.2(3) . . ? N8A N9A Fe1A 113.2(3) . . ? N9A C10A C11A 110.4(4) . . ? N9A C10A C13A 121.2(4) . . ? C11A C10A C13A 128.4(4) . . ? C12A C11A C10A 106.1(4) . . ? N8A C12A C11A 107.5(4) . . ? C10A C13A C14A 111.3(4) . . ? C10A C13A C15A 108.3(4) . . ? C14A C13A C15A 112.0(5) . . ? C20A N16A N17A 110.8(4) . . ? C20A N16A C7A 130.5(4) . . ? N17A N16A C7A 118.6(4) . . ? C18A N17A N16A 105.2(4) . . ? C18A N17A Fe1A 140.8(3) . . ? N16A N17A Fe1A 114.0(3) . . ? N17A C18A C19A 110.6(5) . . ? N17A C18A C21A 121.1(5) . . ? C19A C18A C21A 128.2(5) . . ? C20A C19A C18A 105.6(6) . . ? C19A C20A N16A 107.7(5) . . ? C18A C21A C22A 110.8(5) . . ? C18A C21A C23A 110.6(5) . . ? C22A C21A C23A 109.1(5) . . ? C25A N24A C29A 118.3(4) . . ? C25A N24A Fe1A 120.6(3) . . ? C29A N24A Fe1A 120.9(3) . . ? N24A C25A C26A 123.7(4) . . ? N24A C25A N30A 113.1(4) . . ? C26A C25A N30A 123.2(4) . . ? C25A C26A C27A 116.5(5) . . ? C28A C27A C26A 121.5(5) . . ? C27A C28A C29A 117.2(5) . . ? N24A C29A C28A 122.9(4) . . ? N24A C29A N38A 113.4(4) . . ? C28A C29A N38A 123.7(4) . . ? C34A N30A N31A 110.8(4) . . ? C34A N30A C25A 129.7(4) . . ? N31A N30A C25A 119.4(4) . . ? C32A N31A N30A 106.3(3) . . ? C32A N31A Fe1A 140.6(3) . . ? N30A N31A Fe1A 112.7(3) . . ? N31A C32A C33A 109.4(4) . . ? N31A C32A C35A 122.1(4) . . ? C33A C32A C35A 128.4(4) . . ? C34A C33A C32A 106.8(5) . . ? N30A C34A C33A 106.6(5) . . ? C32A C35A C36A 110.4(4) . . ? C32A C35A C37A 110.6(4) . . ? C36A C35A C37A 111.7(4) . . ? C42A N38A N39A 110.9(4) . . ? C42A N38A C29A 130.4(4) . . ? N39A N38A C29A 118.7(4) . . ? C40A N39A N38A 105.0(4) . . ? C40A N39A Fe1A 141.5(3) . . ? N38A N39A Fe1A 113.4(3) . . ? N39A C40A C41A 110.4(4) . . ? N39A C40A C43A 121.3(4) . . ? C41A C40A C43A 128.2(4) . . ? C42A C41A C40A 106.0(4) . . ? C41A C42A N38A 107.7(4) . . ? C40A C43A C45A 109.9(4) . . ? C40A C43A C44A 111.4(5) . . ? C45A C43A C44A 110.7(6) . . ? N24B Fe1B N2B 175.48(15) . . ? N24B Fe1B N17B 110.69(14) . . ? N2B Fe1B N17B 73.52(15) . . ? N24B Fe1B N31B 73.50(14) . . ? N2B Fe1B N31B 108.35(15) . . ? N17B Fe1B N31B 93.10(15) . . ? N24B Fe1B N39B 73.44(15) . . ? N2B Fe1B N39B 105.32(15) . . ? N17B Fe1B N39B 89.95(15) . . ? N31B Fe1B N39B 145.65(15) . . ? N24B Fe1B N9B 102.34(14) . . ? N2B Fe1B N9B 73.47(15) . . ? N17B Fe1B N9B 146.97(15) . . ? N31B Fe1B N9B 96.29(15) . . ? N39B Fe1B N9B 99.58(15) . . ? C3B N2B C7B 118.4(4) . . ? C3B N2B Fe1B 121.1(3) . . ? C7B N2B Fe1B 120.5(3) . . ? N2B C3B C4B 123.2(5) . . ? N2B C3B N8B 113.1(4) . . ? C4B C3B N8B 123.7(5) . . ? C5B C4B C3B 117.4(5) . . ? C4B C5B C6B 121.5(5) . . ? C7B C6B C5B 116.3(5) . . ? N2B C7B C6B 123.1(5) . . ? N2B C7B N16B 112.7(4) . . ? C6B C7B N16B 124.2(5) . . ? C12B N8B N9B 110.7(4) . . ? C12B N8B C3B 129.9(4) . . ? N9B N8B C3B 119.4(4) . . ? C10B N9B N8B 105.7(4) . . ? C10B N9B Fe1B 141.4(3) . . ? N8B N9B Fe1B 112.8(3) . . ? N9B C10B C11B 109.6(5) . . ? N9B C10B C13B 121.5(4) . . ? C11B C10B C13B 128.8(5) . . ? C12B C11B C10B 105.9(5) . . ? N8B C12B C11B 108.1(5) . . ? C10B C13B C15B 109.5(5) . . ? C10B C13B C14B 112.1(5) . . ? C15B C13B C14B 110.3(5) . . ? C20B N16B N17B 110.8(4) . . ? C20B N16B C7B 130.8(4) . . ? N17B N16B C7B 118.3(4) . . ? C18B N17B N16B 106.2(4) . . ? C18B N17B Fe1B 138.7(3) . . ? N16B N17B Fe1B 115.0(3) . . ? N17B C18B C19B 109.2(4) . . ? N17B C18B C21B 119.6(4) . . ? C19B C18B C21B 131.1(5) . . ? C20B C19B C18B 106.9(5) . . ? N16B C20B C19B 106.9(5) . . ? C18B C21B C22B 111.3(4) . . ? C18B C21B C23B 109.3(4) . . ? C22B C21B C23B 111.4(4) . . ? C29B N24B C25B 118.5(4) . . ? C29B N24B Fe1B 120.8(3) . . ? C25B N24B Fe1B 120.5(3) . . ? N24B C25B C26B 123.4(5) . . ? N24B C25B N30B 112.1(4) . . ? C26B C25B N30B 124.5(4) . . ? C25B C26B C27B 116.9(5) . . ? C28B C27B C26B 121.0(5) . . ? C27B C28B C29B 117.8(5) . . ? N24B C29B C28B 122.4(5) . . ? N24B C29B N38B 112.9(4) . . ? C28B C29B N38B 124.6(5) . . ? C34B N30B N31B 110.8(4) . . ? C34B N30B C25B 130.2(4) . . ? N31B N30B C25B 118.4(4) . . ? C32B N31B N30B 105.3(4) . . ? C32B N31B Fe1B 140.7(3) . . ? N30B N31B Fe1B 113.8(3) . . ? N31B C32B C33B 110.6(4) . . ? N31B C32B C35B 120.6(4) . . ? C33B C32B C35B 128.8(5) . . ? C34B C33B C32B 106.0(5) . . ? N30B C34B C33B 107.3(4) . . ? C32B C35B C37B 111.1(5) . . ? C32B C35B C36B 109.8(5) . . ? C37B C35B C36B 111.8(5) . . ? C42B N38B N39B 110.1(4) . . ? C42B N38B C29B 130.2(4) . . ? N39B N38B C29B 119.5(4) . . ? C40B N39B N38B 106.5(4) . . ? C40B N39B Fe1B 140.0(3) . . ? N38B N39B Fe1B 113.0(3) . . ? N39B C40B C41B 110.0(4) . . ? N39B C40B C43B 121.9(10) . . ? C41B C40B C43B 128.1(10) . . ? N39B C40B C43E 121.4(14) . . ? C41B C40B C43E 128.6(14) . . ? C42B C41B C40B 106.2(5) . . ? C41B C42B N38B 107.3(5) . . ? C40B C43B C45B 111.1(12) . . ? C40B C43B C44B 109.7(12) . . ? C45B C43B C44B 110.5(12) . . ? C40B C43E C45E 110.5(16) . . ? C40B C43E C44E 109.8(17) . . ? C45E C43E C44E 109.6(17) . . ? N24C Fe1C N2C 175.97(15) . . ? N24C Fe1C N31C 73.51(15) . . ? N2C Fe1C N31C 110.17(15) . . ? N24C Fe1C N17C 109.02(14) . . ? N2C Fe1C N17C 72.88(14) . . ? N31C Fe1C N17C 91.95(15) . . ? N24C Fe1C N9C 104.69(14) . . ? N2C Fe1C N9C 73.59(15) . . ? N31C Fe1C N9C 95.92(15) . . ? N17C Fe1C N9C 146.25(14) . . ? N24C Fe1C N39C 73.54(14) . . ? N2C Fe1C N39C 103.05(14) . . ? N31C Fe1C N39C 145.95(15) . . ? N17C Fe1C N39C 90.73(15) . . ? N9C Fe1C N39C 100.48(15) . . ? C7C N2C C3C 118.3(4) . . ? C7C N2C Fe1C 121.3(3) . . ? C3C N2C Fe1C 120.4(3) . . ? N2C C3C C4C 122.8(5) . . ? N2C C3C N8C 113.1(4) . . ? C4C C3C N8C 124.1(5) . . ? C5C C4C C3C 117.6(5) . . ? C4C C5C C6C 120.9(5) . . ? C7C C6C C5C 116.5(5) . . ? N2C C7C C6C 123.8(5) . . ? N2C C7C N16C 112.3(4) . . ? C6C C7C N16C 123.8(4) . . ? C12C N8C N9C 110.9(4) . . ? C12C N8C C3C 130.1(4) . . ? N9C N8C C3C 118.8(4) . . ? C10C N9C N8C 105.4(4) . . ? C10C N9C Fe1C 140.8(3) . . ? N8C N9C Fe1C 113.8(3) . . ? N9C C10C C11C 110.2(4) . . ? N9C C10C C13C 121.9(6) . . ? C11C C10C C13C 127.8(6) . . ? N9C C10C C13E 119.3(13) . . ? C11C C10C C13E 130.4(13) . . ? C12C C11C C10C 105.9(4) . . ? C11C C12C N8C 107.6(4) . . ? C10C C13C C14C 110.5(8) . . ? C10C C13C C15C 113.2(8) . . ? C14C C13C C15C 108.5(9) . . ? C10C C13E C15E 105.3(16) . . ? C10C C13E C14E 107.4(17) . . ? C15E C13E C14E 110.9(18) . . ? C20C N16C N17C 111.6(4) . . ? C20C N16C C7C 130.3(4) . . ? N17C N16C C7C 118.1(4) . . ? C18C N17C N16C 105.2(4) . . ? C18C N17C Fe1C 139.0(3) . . ? N16C N17C Fe1C 114.8(3) . . ? N17C C18C C19C 110.3(4) . . ? N17C C18C C21C 119.9(4) . . ? C19C C18C C21C 129.8(5) . . ? C20C C19C C18C 106.4(5) . . ? N16C C20C C19C 106.5(4) . . ? C18C C21C C22C 111.9(4) . . ? C18C C21C C23C 109.2(5) . . ? C22C C21C C23C 111.1(4) . . ? C25C N24C C29C 118.0(4) . . ? C25C N24C Fe1C 121.0(3) . . ? C29C N24C Fe1C 120.8(3) . . ? N24C C25C C26C 123.0(5) . . ? N24C C25C N38C 112.8(4) . . ? C26C C25C N38C 124.1(5) . . ? C25C C26C C27C 117.5(5) . . ? C26C C27C C28C 121.1(5) . . ? C29C C28C C27C 117.1(5) . . ? N24C C29C C28C 123.3(5) . . ? N24C C29C N30C 112.2(4) . . ? C28C C29C N30C 124.5(5) . . ? C34C N30C N31C 110.4(4) . . ? C34C N30C C29C 131.0(4) . . ? N31C N30C C29C 118.3(4) . . ? C32C N31C N30C 105.2(4) . . ? C32C N31C Fe1C 140.5(3) . . ? N30C N31C Fe1C 114.2(3) . . ? N31C C32C C33C 110.6(5) . . ? N31C C32C C35C 120.1(5) . . ? C33C C32C C35C 129.4(5) . . ? C34C C33C C32C 106.1(5) . . ? C33C C34C N30C 107.7(5) . . ? C32C C35C C36C 111.0(5) . . ? C32C C35C C37C 110.6(6) . . ? C36C C35C C37C 111.0(6) . . ? C42C N38C N39C 110.2(4) . . ? C42C N38C C25C 130.4(4) . . ? N39C N38C C25C 118.9(4) . . ? C40C N39C N38C 105.9(4) . . ? C40C N39C Fe1C 140.2(3) . . ? N38C N39C Fe1C 113.4(3) . . ? N39C C40C C41C 109.9(4) . . ? N39C C40C C43C 122.1(4) . . ? C41C C40C C43C 128.0(5) . . ? C42C C41C C40C 106.4(4) . . ? C41C C42C N38C 107.6(4) . . ? C40C C43C C44C 111.0(5) . . ? C40C C43C C45C 110.5(5) . . ? C44C C43C C45C 110.9(6) . . ? N24D Fe1D N2D 176.51(15) . . ? N24D Fe1D N39D 73.98(15) . . ? N2D Fe1D N39D 107.54(14) . . ? N24D Fe1D N31D 73.90(15) . . ? N2D Fe1D N31D 104.62(14) . . ? N39D Fe1D N31D 147.84(14) . . ? N24D Fe1D N9D 109.27(14) . . ? N2D Fe1D N9D 73.75(14) . . ? N39D Fe1D N9D 98.94(15) . . ? N31D Fe1D N9D 90.05(14) . . ? N24D Fe1D N17D 103.92(14) . . ? N2D Fe1D N17D 72.98(14) . . ? N39D Fe1D N17D 93.10(15) . . ? N31D Fe1D N17D 96.10(15) . . ? N9D Fe1D N17D 146.65(13) . . ? C7D N2D C3D 118.2(4) . . ? C7D N2D Fe1D 121.5(3) . . ? C3D N2D Fe1D 120.3(3) . . ? N2D C3D C4D 123.3(4) . . ? N2D C3D N8D 113.4(4) . . ? C4D C3D N8D 123.1(4) . . ? C5D C4D C3D 116.4(5) . . ? C4D C5D C6D 121.8(5) . . ? C7D C6D C5D 117.1(5) . . ? N2D C7D C6D 123.1(4) . . ? N2D C7D N16D 112.9(4) . . ? C6D C7D N16D 124.0(4) . . ? C12D N8D N9D 110.5(4) . . ? C12D N8D C3D 130.1(4) . . ? N9D N8D C3D 119.2(3) . . ? C10D N9D N8D 105.7(3) . . ? C10D N9D Fe1D 141.2(3) . . ? N8D N9D Fe1D 113.1(3) . . ? N9D C10D C11D 110.5(4) . . ? N9D C10D C13D 122.1(4) . . ? C11D C10D C13D 127.3(5) . . ? C12D C11D C10D 106.1(5) . . ? C11D C12D N8D 107.2(4) . . ? C10D C13D C14D 110.1(5) . . ? C10D C13D C15D 111.7(4) . . ? C14D C13D C15D 110.7(5) . . ? C20D N16D N17D 110.1(4) . . ? C20D N16D C7D 130.3(4) . . ? N17D N16D C7D 119.5(4) . . ? C18D N17D N16D 106.2(4) . . ? C18D N17D Fe1D 140.7(3) . . ? N16D N17D Fe1D 113.1(3) . . ? N17D C18D C19D 110.3(4) . . ? N17D C18D C21D 121.1(5) . . ? C19D C18D C21D 128.6(5) . . ? C20D C19D C18D 106.0(4) . . ? C19D C20D N16D 107.4(4) . . ? C22D C21D C23D 110.9(10) . . ? C22D C21D C18D 110.9(7) . . ? C23D C21D C18D 109.9(7) . . ? C25D N24D C29D 119.4(4) . . ? C25D N24D Fe1D 119.9(3) . . ? C29D N24D Fe1D 119.8(3) . . ? N24D C25D C26D 122.5(5) . . ? N24D C25D N38D 113.3(4) . . ? C26D C25D N38D 124.1(5) . . ? C27D C26D C25D 116.6(5) . . ? C28D C27D C26D 121.8(5) . . ? C27D C28D C29D 117.5(5) . . ? N24D C29D C28D 122.1(5) . . ? N24D C29D N30D 113.9(4) . . ? C28D C29D N30D 124.0(5) . . ? C34D N30D N31D 110.2(4) . . ? C34D N30D C29D 131.1(4) . . ? N31D N30D C29D 118.7(4) . . ? C32D N31D N30D 106.3(4) . . ? C32D N31D Fe1D 140.6(3) . . ? N30D N31D Fe1D 113.1(3) . . ? N31D C32D C33D 109.5(5) . . ? N31D C32D C35D 121.3(4) . . ? C33D C32D C35D 129.2(5) . . ? C34D C33D C32D 106.1(5) . . ? N30D C34D C33D 108.0(5) . . ? C32D C35D C36D 109.8(5) . . ? C32D C35D C37D 110.0(5) . . ? C36D C35D C37D 111.9(5) . . ? C42D N38D N39D 110.3(4) . . ? C42D N38D C25D 130.9(4) . . ? N39D N38D C25D 118.6(4) . . ? C40D N39D N38D 105.7(4) . . ? C40D N39D Fe1D 140.5(3) . . ? N38D N39D Fe1D 113.7(3) . . ? N39D C40D C41D 110.1(5) . . ? N39D C40D C43D 120.1(8) . . ? C41D C40D C43D 129.8(9) . . ? N39D C40D C43F 119.1(11) . . ? C41D C40D C43F 130.6(11) . . ? C42D C41D C40D 106.4(5) . . ? N38D C42D C41D 107.5(5) . . ? C40D C43D C45D 111.9(11) . . ? C40D C43D C44D 110.0(11) . . ? C45D C43D C44D 111.3(11) . . ? C40D C43F C45F 110.6(16) . . ? C40D C43F C44F 109.9(14) . . ? C45F C43F C44F 108.2(15) . . ? F1 P1 F6 92.9(3) . . ? F1 P1 F2 93.1(2) . . ? F6 P1 F2 91.6(2) . . ? F1 P1 F5 90.5(3) . . ? F6 P1 F5 176.5(2) . . ? F2 P1 F5 89.4(2) . . ? F1 P1 F4 89.3(2) . . ? F6 P1 F4 88.71(19) . . ? F2 P1 F4 177.6(2) . . ? F5 P1 F4 90.2(2) . . ? F1 P1 F3 177.0(3) . . ? F6 P1 F3 88.8(2) . . ? F2 P1 F3 89.3(2) . . ? F5 P1 F3 87.8(2) . . ? F4 P1 F3 88.3(2) . . ? F9 P2 F10 91.0(2) . . ? F9 P2 F12 89.7(2) . . ? F10 P2 F12 89.8(2) . . ? F9 P2 F7 179.1(3) . . ? F10 P2 F7 89.9(2) . . ? F12 P2 F7 90.7(2) . . ? F9 P2 F8 90.1(2) . . ? F10 P2 F8 178.9(3) . . ? F12 P2 F8 90.1(2) . . ? F7 P2 F8 89.0(2) . . ? F9 P2 F11 90.3(2) . . ? F10 P2 F11 90.6(2) . . ? F12 P2 F11 179.6(3) . . ? F7 P2 F11 89.4(2) . . ? F8 P2 F11 89.57(19) . . ? F16 P3 F17 91.3(3) . . ? F16 P3 F15 91.6(2) . . ? F17 P3 F15 90.75(18) . . ? F16 P3 F14 178.0(3) . . ? F17 P3 F14 90.4(3) . . ? F15 P3 F14 89.3(2) . . ? F16 P3 F18 89.4(2) . . ? F17 P3 F18 179.1(2) . . ? F15 P3 F18 89.85(17) . . ? F14 P3 F18 88.9(2) . . ? F16 P3 F13 89.3(2) . . ? F17 P3 F13 89.59(18) . . ? F15 P3 F13 179.0(2) . . ? F14 P3 F13 89.79(19) . . ? F18 P3 F13 89.79(17) . . ? F22A P4A F19A 93.6(5) . . ? F22A P4A F24A 93.4(5) . . ? F19A P4A F24A 91.4(5) . . ? F22A P4A F23A 92.9(5) . . ? F19A P4A F23A 91.2(5) . . ? F24A P4A F23A 173.1(6) . . ? F22A P4A F20A 176.8(5) . . ? F19A P4A F20A 89.6(4) . . ? F24A P4A F20A 87.1(5) . . ? F23A P4A F20A 86.5(4) . . ? F22A P4A F21A 95.3(5) . . ? F19A P4A F21A 170.3(6) . . ? F24A P4A F21A 92.1(5) . . ? F23A P4A F21A 84.4(5) . . ? F20A P4A F21A 81.5(4) . . ? F21B P4B F23B 93.5(5) . . ? F21B P4B F20B 97.8(6) . . ? F23B P4B F20B 93.5(6) . . ? F21B P4B F24B 90.3(5) . . ? F23B P4B F24B 174.7(6) . . ? F20B P4B F24B 89.7(5) . . ? F21B P4B F19B 171.2(7) . . ? F23B P4B F19B 90.0(5) . . ? F20B P4B F19B 90.0(6) . . ? F24B P4B F19B 85.8(5) . . ? F21B P4B F22B 85.2(5) . . ? F23B P4B F22B 89.8(5) . . ? F20B P4B F22B 175.4(6) . . ? F24B P4B F22B 86.8(5) . . ? F19B P4B F22B 86.8(5) . . ? F25 P5 F26 91.41(18) . . ? F25 P5 F30 91.21(19) . . ? F26 P5 F30 91.69(18) . . ? F25 P5 F29 90.39(19) . . ? F26 P5 F29 89.89(18) . . ? F30 P5 F29 177.72(19) . . ? F25 P5 F28 89.51(18) . . ? F26 P5 F28 178.87(18) . . ? F30 P5 F28 88.96(17) . . ? F29 P5 F28 89.44(17) . . ? F25 P5 F27 178.8(2) . . ? F26 P5 F27 89.51(18) . . ? F30 P5 F27 89.55(18) . . ? F29 P5 F27 88.82(17) . . ? F28 P5 F27 89.56(17) . . ? F31A P6A F35A 92.4(5) . . ? F31A P6A F32A 91.9(5) . . ? F35A P6A F32A 91.6(6) . . ? F31A P6A F34A 92.0(5) . . ? F35A P6A F34A 89.9(5) . . ? F32A P6A F34A 175.8(6) . . ? F31A P6A F36A 89.3(5) . . ? F35A P6A F36A 176.4(6) . . ? F32A P6A F36A 91.6(5) . . ? F34A P6A F36A 86.9(5) . . ? F31A P6A F33A 177.0(6) . . ? F35A P6A F33A 89.8(5) . . ? F32A P6A F33A 90.1(6) . . ? F34A P6A F33A 85.9(5) . . ? F36A P6A F33A 88.4(5) . . ? F36B P6B F33B 91.6(5) . . ? F36B P6B F32B 94.1(4) . . ? F33B P6B F32B 91.3(5) . . ? F36B P6B F31B 90.1(4) . . ? F33B P6B F31B 178.1(6) . . ? F32B P6B F31B 89.5(4) . . ? F36B P6B F34B 90.5(5) . . ? F33B P6B F34B 89.2(5) . . ? F32B P6B F34B 175.4(5) . . ? F31B P6B F34B 89.8(5) . . ? F36B P6B F35B 176.3(6) . . ? F33B P6B F35B 91.6(5) . . ? F32B P6B F35B 87.8(5) . . ? F31B P6B F35B 86.8(4) . . ? F34B P6B F35B 87.7(5) . . ? F37C P7A F40C 93.6(8) . . ? F37C P7A F42C 91.2(7) . . ? F40C P7A F42C 91.4(8) . . ? F37C P7A F41A 19.0(5) . . ? F40C P7A F41A 90.0(8) . . ? F42C P7A F41A 110.0(7) . . ? F37C P7A F37A 73.8(6) . . ? F40C P7A F37A 81.2(8) . . ? F42C P7A F37A 20.9(6) . . ? F41A P7A F37A 91.7(4) . . ? F37C P7A F38A 85.7(7) . . ? F40C P7A F38A 170.2(8) . . ? F42C P7A F38A 78.8(8) . . ? F41A P7A F38A 92.4(5) . . ? F37A P7A F38A 89.2(5) . . ? F37C P7A F41C 90.3(7) . . ? F40C P7A F41C 91.7(8) . . ? F42C P7A F41C 176.4(9) . . ? F41A P7A F41C 71.7(7) . . ? F37A P7A F41C 162.0(8) . . ? F38A P7A F41C 98.1(8) . . ? F37C P7A F40A 94.3(7) . . ? F40C P7A F40A 10.8(8) . . ? F42C P7A F40A 102.1(7) . . ? F41A P7A F40A 87.4(5) . . ? F37A P7A F40A 91.7(5) . . ? F38A P7A F40A 179.0(6) . . ? F41C P7A F40A 81.0(7) . . ? F37C P7A F39A 108.8(6) . . ? F40C P7A F39A 96.1(8) . . ? F42C P7A F39A 158.0(7) . . ? F41A P7A F39A 90.7(5) . . ? F37A P7A F39A 176.4(5) . . ? F38A P7A F39A 93.4(5) . . ? F41C P7A F39A 19.4(6) . . ? F40A P7A F39A 85.6(5) . . ? F37C P7A F42A 163.0(7) . . ? F40C P7A F42A 88.3(8) . . ? F42C P7A F42A 71.8(7) . . ? F41A P7A F42A 177.6(5) . . ? F37A P7A F42A 89.8(4) . . ? F38A P7A F42A 89.6(5) . . ? F41C P7A F42A 106.6(7) . . ? F40A P7A F42A 90.6(4) . . ? F39A P7A F42A 87.8(5) . . ? F37C P7A F38C 90.7(7) . . ? F40C P7A F38C 175.8(10) . . ? F42C P7A F38C 88.6(8) . . ? F41A P7A F38C 94.0(8) . . ? F37A P7A F38C 100.1(8) . . ? F38A P7A F38C 11.0(8) . . ? F41C P7A F38C 88.2(8) . . ? F40A P7A F38C 168.0(8) . . ? F39A P7A F38C 82.5(8) . . ? F42A P7A F38C 87.7(8) . . ? F37C P7A F39C 175.8(8) . . ? F40C P7A F39C 90.6(8) . . ? F42C P7A F39C 89.7(7) . . ? F41A P7A F39C 160.3(7) . . ? F37A P7A F39C 107.9(7) . . ? F38A P7A F39C 90.4(7) . . ? F41C P7A F39C 88.6(7) . . ? F40A P7A F39C 89.5(7) . . ? F39A P7A F39C 69.7(7) . . ? F42A P7A F39C 18.1(6) . . ? F38C P7A F39C 85.2(7) . . ? F39B P7B F42B 92.1(6) . . ? F39B P7B F38B 91.4(6) . . ? F42B P7B F38B 90.6(5) . . ? F39B P7B F41B 93.4(6) . . ? F42B P7B F41B 174.5(7) . . ? F38B P7B F41B 89.1(6) . . ? F39B P7B F40B 91.4(5) . . ? F42B P7B F40B 89.9(5) . . ? F38B P7B F40B 177.2(6) . . ? F41B P7B F40B 90.2(5) . . ? F39B P7B F37B 178.4(7) . . ? F42B P7B F37B 87.6(6) . . ? F38B P7B F37B 90.2(5) . . ? F41B P7B F37B 86.9(6) . . ? F40B P7B F37B 87.0(5) . . ? F43A P8A F46A 93.6(6) . . ? F43A P8A F47A 91.7(6) . . ? F46A P8A F47A 91.3(5) . . ? F43A P8A F48A 93.0(6) . . ? F46A P8A F48A 90.0(6) . . ? F47A P8A F48A 175.0(6) . . ? F43A P8A F44A 91.8(6) . . ? F46A P8A F44A 174.5(6) . . ? F47A P8A F44A 89.2(5) . . ? F48A P8A F44A 89.1(6) . . ? F43A P8A F45A 178.9(7) . . ? F46A P8A F45A 86.5(5) . . ? F47A P8A F45A 87.3(4) . . ? F48A P8A F45A 88.0(5) . . ? F44A P8A F45A 88.1(5) . . ? F45B P8B F44B 98.3(5) . . ? F45B P8B F47B 92.8(5) . . ? F44B P8B F47B 92.0(5) . . ? F45B P8B F48B 91.8(5) . . ? F44B P8B F48B 92.6(5) . . ? F47B P8B F48B 173.0(6) . . ? F45B P8B F46B 91.7(5) . . ? F44B P8B F46B 170.0(6) . . ? F47B P8B F46B 87.5(5) . . ? F48B P8B F46B 87.1(6) . . ? F45B P8B F43B 175.4(6) . . ? F44B P8B F43B 86.3(5) . . ? F47B P8B F43B 87.4(5) . . ? F48B P8B F43B 87.6(5) . . ? F46B P8B F43B 83.7(5) . . ? O3S C2S C1S 108.7(7) . . ? C4S O3S C2S 113.3(7) . . ? O3S C4S C5S 107.5(7) . . ? O8S C7S C6S 108.1(7) . . ? C7S O8S C9S 111.7(7) . . ? O8S C9S C10S 110.3(8) . . ? N13S C12S C11S 178.7(8) . . ? N16S C15S C14S 176.3(12) . . ? N19S C18S C17S 169(3) . . ? N19E C18E C17E 172(4) . . ? C20S C21S N22S 146(4) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.935 _refine_diff_density_min -1.076 _refine_diff_density_rms 0.102 #=END data_je1 _database_code_depnum_ccdc_archive 'CCDC 263425' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-bis(3-{ethylcarboxy}pyrazol-1-yl)pyridine]iron(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H34 Fe N10 O8, 2[B F4]' _chemical_formula_sum 'C34 H34 B2 F8 Fe N10 O8' _chemical_formula_weight 940.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 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 18.2200(3) _cell_length_b 9.5176(2) _cell_length_c 23.8513(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.2193(6) _cell_angle_gamma 90.00 _cell_volume 4009.36(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 26369 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'Rectangular Prism' _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.477 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.898 _exptl_absorpt_correction_T_max 0.954 _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 '\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 26369 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0634 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9135 _reflns_number_gt 6328 _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. Two of the four ethylcarboxy substituents in the molecule are disordered: C23, O24A-C27A (occupancy 0.70) and C23, O24B-C27B (occupancy 0.30) - C23 is common to both orientations and has total occupancy 1.0 C49, O50A-C52A, C53 (occupancy 0.60) and C49, O50B-C52B, C53 (occupancy 0.40) - C49 and C53 are common to both orientations and have total occupancy 1.0. These were modelled using the following restraints: C=O = 1.21(1)\%A C-O = 1.47(1)\%A C-C = 1.49(1)\%A 1,3-O...O = 2.25(1)\%A 1,3-O...C = 2.42(1)\%A. Both BF~4~^-^ anions are also disordered: B54A-F58A (occupancy 0.70) and B54B-F58B (occupancy 0.30) B59A-F63A (occupancy 0.70) and B59B-F63B (occupancy 0.30). These were modelled using the restraints B-F = 1.38(2)\%A and F...F = 2.25(2)\%A. All non-H atoms with occupancy >0.5 were modelled anisotropically, and all H atoms were placed and calculated positions and refined using a riding 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^)+(0.0480P)^2^+1.9248P] 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_number_reflns 9135 _refine_ls_number_parameters 638 _refine_ls_number_restraints 64 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1229 _refine_ls_wR_factor_gt 0.1073 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.056 _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 0.248907(18) 0.99191(3) 0.493728(13) 0.02742(11) Uani 1 1 d . . . N2 N 0.31657(11) 0.99501(19) 0.57967(8) 0.0285(4) Uani 1 1 d . . . C3 C 0.35686(13) 1.1084(2) 0.60064(10) 0.0301(5) Uani 1 1 d . . . C4 C 0.40160(13) 1.1190(3) 0.65628(10) 0.0364(6) Uani 1 1 d . . . H4 H 0.4304 1.2010 0.6695 0.044 Uiso 1 1 calc R . . C5 C 0.40222(15) 1.0036(3) 0.69184(11) 0.0425(7) Uani 1 1 d . . . H5 H 0.4320 1.0062 0.7306 0.051 Uiso 1 1 calc R . . C6 C 0.36017(15) 0.8848(3) 0.67189(11) 0.0408(6) Uani 1 1 d . . . H6 H 0.3602 0.8055 0.6961 0.049 Uiso 1 1 calc R . . C7 C 0.31831(13) 0.8865(3) 0.61546(10) 0.0325(5) Uani 1 1 d . . . N8 N 0.34953(10) 1.2187(2) 0.55977(8) 0.0291(4) Uani 1 1 d . . . N9 N 0.30978(10) 1.1949(2) 0.50461(8) 0.0288(4) Uani 1 1 d . . . C10 C 0.31470(13) 1.3161(2) 0.47699(10) 0.0312(5) Uani 1 1 d . . . C11 C 0.35705(14) 1.4156(3) 0.51482(11) 0.0371(6) Uani 1 1 d . . . H11 H 0.3684 1.5092 0.5059 0.045 Uiso 1 1 calc R . . C12 C 0.37853(14) 1.3497(3) 0.56700(11) 0.0360(6) Uani 1 1 d . . . H12 H 0.4083 1.3887 0.6019 0.043 Uiso 1 1 calc R . . C13 C 0.27915(14) 1.3291(3) 0.41452(11) 0.0370(6) Uani 1 1 d . . . O14 O 0.25005(12) 1.2330(2) 0.38423(8) 0.0521(5) Uani 1 1 d . . . O15 O 0.28391(11) 1.46097(19) 0.39712(8) 0.0455(5) Uani 1 1 d . . . C16 C 0.25302(18) 1.4901(3) 0.33517(12) 0.0525(8) Uani 1 1 d . . . H16A H 0.2369 1.5895 0.3300 0.063 Uiso 1 1 calc R . . H16B H 0.2081 1.4302 0.3201 0.063 Uiso 1 1 calc R . . C17 C 0.3111(2) 1.4617(4) 0.30201(15) 0.0704(10) Uani 1 1 d . . . H17A H 0.3597 1.5016 0.3228 0.106 Uiso 1 1 calc R . . H17B H 0.2951 1.5049 0.2636 0.106 Uiso 1 1 calc R . . H17C H 0.3164 1.3600 0.2978 0.106 Uiso 1 1 calc R . . N18 N 0.27307(12) 0.7723(2) 0.58892(9) 0.0348(5) Uani 1 1 d . . . N19 N 0.23151(11) 0.7845(2) 0.53332(9) 0.0324(5) Uani 1 1 d . . . C20 C 0.19499(15) 0.6612(3) 0.52246(12) 0.0389(6) Uani 1 1 d . A . C21 C 0.21394(18) 0.5728(3) 0.57063(13) 0.0505(7) Uani 1 1 d . . . H21 H 0.1958 0.4802 0.5736 0.061 Uiso 1 1 calc R . . C22 C 0.26323(17) 0.6455(3) 0.61211(12) 0.0454(7) Uani 1 1 d . . . H22 H 0.2865 0.6140 0.6501 0.055 Uiso 1 1 calc R . . C23 C 0.14242(17) 0.6358(3) 0.46556(13) 0.0474(7) Uani 1 1 d D . . O24A O 0.1353(6) 0.7116(7) 0.4254(3) 0.073(3) Uani 0.70 1 d PD A 1 O25A O 0.09712(17) 0.5217(3) 0.46723(12) 0.0445(7) Uani 0.70 1 d PD A 1 C26A C 0.0399(3) 0.4876(4) 0.4138(2) 0.0470(10) Uani 0.70 1 d PD A 1 H26A H 0.0145 0.5752 0.3968 0.056 Uiso 0.70 1 calc PR A 1 H26B H 0.0010 0.4255 0.4233 0.056 Uiso 0.70 1 calc PR A 1 C27A C 0.0740(2) 0.4164(5) 0.3704(2) 0.0571(12) Uani 0.70 1 d PD A 1 H27A H 0.1014 0.4855 0.3528 0.086 Uiso 0.70 1 calc PR A 1 H27B H 0.0338 0.3737 0.3402 0.086 Uiso 0.70 1 calc PR A 1 H27C H 0.1092 0.3432 0.3896 0.086 Uiso 0.70 1 calc PR A 1 O24B O 0.1246(12) 0.7129(13) 0.4252(6) 0.041(4) Uiso 0.30 1 d PD A 2 O25B O 0.1336(5) 0.4915(7) 0.4612(3) 0.060(2) Uiso 0.30 1 d PD A 2 C26B C 0.0815(7) 0.4504(15) 0.4062(5) 0.074(4) Uiso 0.30 1 d PD A 2 H26C H 0.0844 0.3477 0.4005 0.089 Uiso 0.30 1 calc PR A 2 H26D H 0.0958 0.4983 0.3736 0.089 Uiso 0.30 1 calc PR A 2 C27B C 0.0031(6) 0.4907(18) 0.4080(7) 0.086(5) Uiso 0.30 1 d PD A 2 H27D H -0.0167 0.4221 0.4312 0.129 Uiso 0.30 1 calc PR A 2 H27E H -0.0293 0.4923 0.3685 0.129 Uiso 0.30 1 calc PR A 2 H27F H 0.0038 0.5841 0.4253 0.129 Uiso 0.30 1 calc PR A 2 N28 N 0.17196(10) 0.98904(18) 0.41079(8) 0.0271(4) Uani 1 1 d . . . C29 C 0.19361(13) 0.9365(2) 0.36597(10) 0.0308(5) Uani 1 1 d . . . C30 C 0.14510(15) 0.9147(3) 0.31226(11) 0.0413(6) Uani 1 1 d . . . H30 H 0.1627 0.8775 0.2810 0.050 Uiso 1 1 calc R . . C31 C 0.07037(16) 0.9491(3) 0.30615(12) 0.0483(7) Uani 1 1 d . . . H31 H 0.0353 0.9354 0.2699 0.058 Uiso 1 1 calc R . . C32 C 0.04546(15) 1.0032(3) 0.35189(11) 0.0427(6) Uani 1 1 d . . . H32 H -0.0062 1.0267 0.3481 0.051 Uiso 1 1 calc R . . C33 C 0.09914(14) 1.0216(2) 0.40329(10) 0.0321(5) Uani 1 1 d . . . N34 N 0.27108(11) 0.9020(2) 0.37794(8) 0.0310(4) Uani 1 1 d . . . N35 N 0.31241(11) 0.90139(19) 0.43408(8) 0.0294(4) Uani 1 1 d . . . C36 C 0.38242(13) 0.8658(3) 0.43035(10) 0.0326(5) Uani 1 1 d . . . C37 C 0.38541(15) 0.8471(3) 0.37281(11) 0.0409(6) Uani 1 1 d . . . H37 H 0.4285 0.8232 0.3591 0.049 Uiso 1 1 calc R . . C38 C 0.31404(15) 0.8701(3) 0.34076(11) 0.0403(6) Uani 1 1 d . . . H38 H 0.2973 0.8649 0.2998 0.048 Uiso 1 1 calc R . . C39 C 0.44765(14) 0.8497(3) 0.48075(11) 0.0351(6) Uani 1 1 d . . . O40 O 0.51159(10) 0.8450(2) 0.47470(8) 0.0496(5) Uani 1 1 d . . . O41 O 0.42874(9) 0.84023(19) 0.53073(7) 0.0387(4) Uani 1 1 d . . . C42 C 0.49120(14) 0.8244(3) 0.58294(11) 0.0402(6) Uani 1 1 d . . . H42A H 0.4831 0.8886 0.6135 0.048 Uiso 1 1 calc R . . H42B H 0.5397 0.8499 0.5739 0.048 Uiso 1 1 calc R . . C43 C 0.49489(19) 0.6770(3) 0.60398(14) 0.0621(9) Uani 1 1 d . . . H43A H 0.4448 0.6480 0.6080 0.093 Uiso 1 1 calc R . . H43B H 0.5316 0.6704 0.6416 0.093 Uiso 1 1 calc R . . H43C H 0.5107 0.6153 0.5762 0.093 Uiso 1 1 calc R . . N44 N 0.08200(11) 1.0796(2) 0.45307(8) 0.0314(4) Uani 1 1 d . . . N45 N 0.13840(11) 1.0921(2) 0.50245(8) 0.0306(4) Uani 1 1 d . . . C46 C 0.10584(14) 1.1569(3) 0.53956(11) 0.0352(6) Uani 1 1 d . B . C47 C 0.02918(15) 1.1844(3) 0.51424(12) 0.0450(7) Uani 1 1 d . . . H47 H -0.0061 1.2287 0.5320 0.054 Uiso 1 1 calc R . . C48 C 0.01583(15) 1.1353(3) 0.45968(12) 0.0416(6) Uani 1 1 d . . . H48 H -0.0309 1.1389 0.4312 0.050 Uiso 1 1 calc R . . C49 C 0.15217(14) 1.1981(3) 0.59707(11) 0.0366(6) Uani 1 1 d D . . O50A O 0.2186(2) 1.1852(9) 0.6127(4) 0.067(2) Uani 0.70 1 d PD B 1 O51A O 0.1095(2) 1.2635(5) 0.62834(14) 0.0572(11) Uani 0.70 1 d PD B 1 C52A C 0.1475(3) 1.3155(7) 0.68653(19) 0.0653(17) Uani 0.70 1 d PD B 1 H52A H 0.1454 1.4194 0.6871 0.078 Uiso 0.70 1 calc PR B 1 H52B H 0.2014 1.2867 0.6963 0.078 Uiso 0.70 1 calc PR B 1 O50B O 0.2188(5) 1.2163(18) 0.6090(7) 0.031(2) Uiso 0.30 1 d PD B 2 O51B O 0.1075(5) 1.2085(8) 0.6344(3) 0.035(2) Uiso 0.30 1 d PD B 2 C52B C 0.1572(6) 1.2511(15) 0.6911(4) 0.068(5) Uiso 0.30 1 d PD B 2 H52C H 0.1983 1.1816 0.7042 0.082 Uiso 0.30 1 calc PR B 2 H52D H 0.1802 1.3442 0.6880 0.082 Uiso 0.30 1 calc PR B 2 C53 C 0.1091(3) 1.2566(4) 0.73051(15) 0.0989(15) Uani 1 1 d D . . H53A H 0.0559 1.2854 0.7208 0.148 Uiso 0.70 1 d PR B . H53B H 0.1343 1.2922 0.7690 0.148 Uiso 0.70 1 d PR . . H53C H 0.1122 1.1538 0.7304 0.148 Uiso 0.70 1 d PR . . H53D H 0.0700 1.3281 0.7175 0.148 Uiso 0.30 1 d PR . . H53E H 0.1395 1.2806 0.7693 0.148 Uiso 0.30 1 d PR . . H53F H 0.0852 1.1648 0.7316 0.148 Uiso 0.30 1 d PR . . B54A B 0.4044(3) 0.0393(9) 0.2358(3) 0.036(2) Uani 0.70 1 d PD C 1 F55A F 0.4279(4) 0.1146(7) 0.2860(3) 0.053(2) Uani 0.70 1 d PD C 1 F56A F 0.4053(3) -0.1027(4) 0.2473(2) 0.0593(11) Uani 0.70 1 d PD C 1 F57A F 0.4548(2) 0.0673(4) 0.20016(14) 0.0507(9) Uani 0.70 1 d PD C 1 F58A F 0.33246(15) 0.0801(4) 0.20591(15) 0.0730(9) Uani 0.70 1 d PD C 1 B54B B 0.4027(11) 0.020(2) 0.2395(9) 0.074(12) Uiso 0.30 1 d PD D 2 F55B F 0.4272(12) 0.120(2) 0.2820(8) 0.083(8) Uiso 0.30 1 d PD D 2 F56B F 0.4271(7) -0.1112(13) 0.2604(5) 0.060(4) Uiso 0.30 1 d PD D 2 F57B F 0.4325(6) 0.0464(12) 0.1930(5) 0.064(4) Uiso 0.30 1 d PD D 2 F58B F 0.3250(5) 0.0217(8) 0.2229(4) 0.064(3) Uiso 0.30 1 d PD D 2 B59A B 0.1416(3) 0.6881(7) 0.1898(2) 0.032(2) Uani 0.70 1 d PD E 1 F60A F 0.2143(4) 0.7318(8) 0.2167(4) 0.062(3) Uani 0.70 1 d PD E 1 F61A F 0.1405(5) 0.6102(8) 0.1417(3) 0.079(3) Uani 0.70 1 d PD E 1 F62A F 0.1090(2) 0.6217(4) 0.22904(13) 0.0649(9) Uani 0.70 1 d PD E 1 F63A F 0.1007(2) 0.8103(4) 0.17061(18) 0.0761(11) Uani 0.70 1 d PD E 1 B59B B 0.1438(11) 0.677(2) 0.1889(9) 0.081(13) Uiso 0.30 1 d PD F 2 F60B F 0.2143(7) 0.7293(14) 0.2155(8) 0.038(5) Uiso 0.30 1 d PD F 2 F61B F 0.1420(11) 0.6082(15) 0.1381(6) 0.054(5) Uiso 0.30 1 d PD F 2 F62B F 0.1281(5) 0.5720(8) 0.2246(4) 0.063(3) Uiso 0.30 1 d PD F 2 F63B F 0.0866(6) 0.7737(10) 0.1844(4) 0.067(3) Uiso 0.30 1 d PD F 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 0.02604(19) 0.03137(19) 0.02369(18) 0.00033(13) 0.00389(13) 0.00082(14) N2 0.0258(10) 0.0337(10) 0.0263(10) 0.0020(8) 0.0069(8) 0.0046(8) C3 0.0253(12) 0.0388(13) 0.0266(12) 0.0003(10) 0.0073(9) 0.0047(10) C4 0.0283(13) 0.0540(16) 0.0265(13) -0.0039(11) 0.0057(10) -0.0003(11) C5 0.0304(14) 0.0712(19) 0.0246(12) 0.0045(13) 0.0044(10) 0.0077(13) C6 0.0383(15) 0.0560(17) 0.0294(13) 0.0129(12) 0.0107(11) 0.0123(13) C7 0.0298(13) 0.0393(13) 0.0303(13) 0.0070(10) 0.0114(10) 0.0078(11) N8 0.0256(10) 0.0342(11) 0.0266(10) -0.0020(8) 0.0045(8) 0.0008(8) N9 0.0258(10) 0.0348(11) 0.0248(10) -0.0005(8) 0.0042(8) 0.0005(8) C10 0.0287(13) 0.0340(13) 0.0316(13) 0.0011(10) 0.0088(10) -0.0004(10) C11 0.0398(15) 0.0320(13) 0.0404(15) -0.0009(11) 0.0114(12) -0.0051(11) C12 0.0350(14) 0.0387(14) 0.0340(14) -0.0093(11) 0.0078(11) -0.0041(11) C13 0.0348(14) 0.0383(14) 0.0368(14) 0.0061(11) 0.0068(11) -0.0036(11) O14 0.0684(14) 0.0460(11) 0.0347(11) 0.0058(9) -0.0013(9) -0.0158(10) O15 0.0511(12) 0.0398(10) 0.0423(11) 0.0120(8) 0.0051(9) -0.0045(9) C16 0.0548(19) 0.0551(18) 0.0440(16) 0.0220(14) 0.0050(14) -0.0004(14) C17 0.066(2) 0.095(3) 0.053(2) 0.0293(19) 0.0210(17) 0.0108(19) N18 0.0384(12) 0.0356(11) 0.0328(11) 0.0074(9) 0.0131(9) 0.0065(9) N19 0.0319(11) 0.0324(11) 0.0339(11) 0.0031(9) 0.0102(9) 0.0021(9) C20 0.0459(16) 0.0303(13) 0.0456(16) 0.0001(11) 0.0206(13) -0.0001(12) C21 0.069(2) 0.0332(14) 0.0543(18) 0.0077(13) 0.0254(16) -0.0006(14) C22 0.0598(18) 0.0372(14) 0.0433(16) 0.0139(12) 0.0205(14) 0.0081(13) C23 0.0572(19) 0.0298(14) 0.0564(19) -0.0029(13) 0.0163(15) -0.0022(13) O24A 0.087(6) 0.047(3) 0.067(3) 0.0173(17) -0.014(2) -0.030(2) O25A 0.0442(18) 0.0338(14) 0.0561(18) -0.0035(12) 0.0134(14) -0.0133(13) C26A 0.037(3) 0.038(2) 0.068(3) -0.0103(19) 0.016(2) -0.008(2) C27A 0.048(3) 0.057(3) 0.067(3) -0.015(2) 0.016(2) -0.009(2) N28 0.0261(10) 0.0279(10) 0.0260(10) 0.0011(8) 0.0037(8) -0.0011(8) C29 0.0301(13) 0.0319(12) 0.0293(13) 0.0011(10) 0.0051(10) 0.0000(10) C30 0.0408(16) 0.0513(16) 0.0292(13) -0.0064(11) 0.0038(11) -0.0003(12) C31 0.0441(17) 0.0614(18) 0.0317(15) -0.0032(13) -0.0056(12) 0.0017(14) C32 0.0309(14) 0.0543(17) 0.0368(14) -0.0015(12) -0.0031(11) 0.0048(12) C33 0.0307(13) 0.0327(13) 0.0327(13) 0.0027(10) 0.0070(10) 0.0001(10) N34 0.0309(11) 0.0366(11) 0.0248(10) -0.0022(8) 0.0059(8) -0.0025(9) N35 0.0281(11) 0.0332(10) 0.0265(10) -0.0022(8) 0.0060(8) -0.0024(8) C36 0.0286(13) 0.0360(13) 0.0350(14) -0.0033(10) 0.0112(10) -0.0004(10) C37 0.0338(14) 0.0551(16) 0.0374(15) -0.0075(12) 0.0158(12) -0.0011(12) C38 0.0422(16) 0.0524(16) 0.0285(13) -0.0063(11) 0.0130(11) -0.0031(12) C39 0.0304(14) 0.0375(14) 0.0392(15) -0.0047(11) 0.0123(11) 0.0023(11) O40 0.0318(10) 0.0713(13) 0.0470(12) -0.0059(10) 0.0123(9) 0.0046(9) O41 0.0274(9) 0.0547(11) 0.0330(10) -0.0010(8) 0.0052(7) 0.0016(8) C42 0.0311(14) 0.0509(16) 0.0356(14) -0.0068(12) 0.0025(11) -0.0012(12) C43 0.062(2) 0.0490(18) 0.063(2) 0.0000(15) -0.0088(16) 0.0038(15) N44 0.0241(10) 0.0366(11) 0.0321(11) 0.0008(9) 0.0040(8) 0.0026(8) N45 0.0269(10) 0.0337(11) 0.0301(11) 0.0005(8) 0.0051(8) 0.0007(8) C46 0.0318(13) 0.0373(13) 0.0379(14) 0.0002(11) 0.0112(11) 0.0022(11) C47 0.0327(14) 0.0547(17) 0.0479(17) -0.0056(13) 0.0104(12) 0.0127(13) C48 0.0300(14) 0.0494(16) 0.0438(16) -0.0008(12) 0.0059(11) 0.0082(12) C49 0.0336(15) 0.0394(14) 0.0408(15) -0.0038(11) 0.0169(12) 0.0027(11) O50A 0.032(2) 0.089(6) 0.075(4) -0.039(4) 0.0076(16) 0.007(2) O51A 0.0380(18) 0.087(4) 0.047(2) -0.027(2) 0.0114(14) 0.005(2) C52A 0.037(3) 0.108(5) 0.050(3) -0.045(3) 0.011(2) 0.008(3) C53 0.149(4) 0.084(3) 0.054(2) -0.006(2) 0.006(3) -0.020(3) B54A 0.033(3) 0.045(3) 0.023(3) -0.0114(19) -0.0040(17) -0.006(2) F55A 0.056(3) 0.050(2) 0.042(2) -0.0248(14) -0.0055(12) -0.0073(12) F56A 0.088(4) 0.0384(18) 0.058(3) -0.0090(16) 0.032(3) -0.0129(19) F57A 0.052(2) 0.065(2) 0.0327(15) 0.0169(13) 0.0043(15) 0.0001(18) F58A 0.0405(16) 0.084(2) 0.079(2) -0.0194(19) -0.0150(15) 0.0041(16) B59A 0.022(3) 0.044(3) 0.025(3) -0.0071(17) -0.0047(15) -0.0042(18) F60A 0.036(2) 0.100(5) 0.047(3) -0.0227(16) 0.0013(11) -0.0196(15) F61A 0.066(3) 0.105(5) 0.059(3) -0.051(2) 0.0056(16) -0.0206(17) F62A 0.060(2) 0.083(2) 0.0546(18) -0.0148(17) 0.0197(15) -0.0310(19) F63A 0.057(2) 0.078(2) 0.087(3) 0.020(2) 0.0077(19) 0.0285(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.1169(19) . ? Fe1 N28 2.1252(18) . ? Fe1 N9 2.2110(19) . ? Fe1 N35 2.217(2) . ? Fe1 N19 2.2442(19) . ? Fe1 N45 2.283(2) . ? N2 C3 1.332(3) . ? N2 C7 1.335(3) . ? C3 C4 1.380(3) . ? C3 N8 1.416(3) . ? C4 C5 1.386(4) . ? C5 C6 1.384(4) . ? C6 C7 1.374(3) . ? C7 N18 1.416(3) . ? N8 C12 1.349(3) . ? N8 N9 1.356(2) . ? N9 C10 1.342(3) . ? C10 C11 1.402(3) . ? C10 C13 1.477(3) . ? C11 C12 1.362(3) . ? C13 O14 1.204(3) . ? C13 O15 1.332(3) . ? O15 C16 1.473(3) . ? C16 C17 1.492(4) . ? N18 C22 1.358(3) . ? N18 N19 1.361(3) . ? N19 C20 1.343(3) . ? C20 C21 1.397(4) . ? C20 C23 1.476(4) . ? C21 C22 1.352(4) . ? C23 O24A 1.180(5) . ? C23 O24B 1.190(9) . ? C23 O25A 1.371(4) . ? C23 O25B 1.384(6) . ? O25A C26A 1.471(5) . ? C26A C27A 1.496(5) . ? O25B C26B 1.470(9) . ? C26B C27B 1.490(9) . ? N28 C29 1.325(3) . ? N28 C33 1.331(3) . ? C29 C30 1.382(3) . ? C29 N34 1.408(3) . ? C30 C31 1.373(4) . ? C31 C32 1.380(4) . ? C32 C33 1.379(3) . ? C33 N44 1.412(3) . ? N34 C38 1.354(3) . ? N34 N35 1.365(3) . ? N35 C36 1.344(3) . ? C36 C37 1.398(3) . ? C36 C39 1.476(3) . ? C37 C38 1.355(4) . ? C39 O40 1.209(3) . ? C39 O41 1.323(3) . ? O41 C42 1.474(3) . ? C42 C43 1.486(4) . ? N44 C48 1.361(3) . ? N44 N45 1.365(3) . ? N45 C46 1.332(3) . ? C46 C47 1.403(4) . ? C46 C49 1.476(3) . ? C47 C48 1.348(4) . ? C49 O50A 1.182(5) . ? C49 O50B 1.190(8) . ? C49 O51B 1.349(6) . ? C49 O51A 1.354(4) . ? O51A C52A 1.476(5) . ? C52A C53 1.505(6) . ? O51B C52B 1.487(9) . ? C52B C53 1.436(9) . ? B54A F55A 1.370(6) . ? B54A F56A 1.378(9) . ? B54A F58A 1.386(6) . ? B54A F57A 1.422(7) . ? B54B F56B 1.374(18) . ? B54B F58B 1.375(17) . ? B54B F57B 1.375(18) . ? B54B F55B 1.384(17) . ? B59A F61A 1.361(7) . ? B59A F62A 1.380(6) . ? B59A F60A 1.387(6) . ? B59A F63A 1.396(7) . ? B59B F61B 1.369(17) . ? B59B F63B 1.376(17) . ? B59B F60B 1.380(17) . ? B59B F62B 1.386(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 N2 Fe1 N28 174.62(7) . . ? N2 Fe1 N9 73.63(7) . . ? N28 Fe1 N9 108.52(7) . . ? N2 Fe1 N35 110.81(7) . . ? N28 Fe1 N35 74.13(7) . . ? N9 Fe1 N35 95.11(7) . . ? N2 Fe1 N19 73.36(7) . . ? N28 Fe1 N19 104.55(7) . . ? N9 Fe1 N19 146.92(7) . . ? N35 Fe1 N19 94.48(7) . . ? N2 Fe1 N45 102.88(7) . . ? N28 Fe1 N45 72.26(7) . . ? N9 Fe1 N45 93.02(7) . . ? N35 Fe1 N45 146.29(7) . . ? N19 Fe1 N45 96.32(7) . . ? C3 N2 C7 117.5(2) . . ? C3 N2 Fe1 120.74(15) . . ? C7 N2 Fe1 121.67(16) . . ? N2 C3 C4 124.2(2) . . ? N2 C3 N8 113.07(19) . . ? C4 C3 N8 122.8(2) . . ? C3 C4 C5 116.4(2) . . ? C6 C5 C4 121.1(2) . . ? C7 C6 C5 117.0(2) . . ? N2 C7 C6 123.8(2) . . ? N2 C7 N18 112.8(2) . . ? C6 C7 N18 123.4(2) . . ? C12 N8 N9 112.16(19) . . ? C12 N8 C3 129.0(2) . . ? N9 N8 C3 118.82(18) . . ? C10 N9 N8 104.41(18) . . ? C10 N9 Fe1 141.76(15) . . ? N8 N9 Fe1 113.11(13) . . ? N9 C10 C11 110.9(2) . . ? N9 C10 C13 120.1(2) . . ? C11 C10 C13 128.9(2) . . ? C12 C11 C10 105.5(2) . . ? N8 C12 C11 107.0(2) . . ? O14 C13 O15 125.5(2) . . ? O14 C13 C10 124.1(2) . . ? O15 C13 C10 110.3(2) . . ? C13 O15 C16 116.9(2) . . ? O15 C16 C17 110.6(2) . . ? C22 N18 N19 112.0(2) . . ? C22 N18 C7 128.4(2) . . ? N19 N18 C7 119.60(19) . . ? C20 N19 N18 104.15(19) . . ? C20 N19 Fe1 143.36(17) . . ? N18 N19 Fe1 112.48(14) . . ? N19 C20 C21 110.9(2) . . ? N19 C20 C23 119.9(2) . . ? C21 C20 C23 129.1(2) . . ? C22 C21 C20 106.2(2) . . ? C21 C22 N18 106.7(2) . . ? O24A C23 O25A 124.1(5) . . ? O24B C23 O25B 123.2(9) . . ? O24A C23 C20 124.3(5) . . ? O24B C23 C20 129.0(10) . . ? O25A C23 C20 111.2(2) . . ? O25B C23 C20 105.6(4) . . ? C23 O25A C26A 117.0(3) . . ? O25A C26A C27A 111.9(4) . . ? C23 O25B C26B 111.6(8) . . ? O25B C26B C27B 108.7(8) . . ? C29 N28 C33 117.6(2) . . ? C29 N28 Fe1 119.79(15) . . ? C33 N28 Fe1 122.01(16) . . ? N28 C29 C30 123.7(2) . . ? N28 C29 N34 114.0(2) . . ? C30 C29 N34 122.3(2) . . ? C31 C30 C29 117.0(2) . . ? C30 C31 C32 121.0(2) . . ? C33 C32 C31 116.8(2) . . ? N28 C33 C32 123.8(2) . . ? N28 C33 N44 113.4(2) . . ? C32 C33 N44 122.8(2) . . ? C38 N34 N35 111.9(2) . . ? C38 N34 C29 129.2(2) . . ? N35 N34 C29 118.93(19) . . ? C36 N35 N34 103.89(19) . . ? C36 N35 Fe1 142.57(16) . . ? N34 N35 Fe1 112.25(14) . . ? N35 C36 C37 111.3(2) . . ? N35 C36 C39 124.0(2) . . ? C37 C36 C39 124.6(2) . . ? C38 C37 C36 105.7(2) . . ? N34 C38 C37 107.2(2) . . ? O40 C39 O41 125.2(2) . . ? O40 C39 C36 120.9(2) . . ? O41 C39 C36 113.9(2) . . ? C39 O41 C42 116.77(19) . . ? O41 C42 C43 110.1(2) . . ? C48 N44 N45 111.5(2) . . ? C48 N44 C33 129.4(2) . . ? N45 N44 C33 118.97(19) . . ? C46 N45 N44 104.47(19) . . ? C46 N45 Fe1 143.20(16) . . ? N44 N45 Fe1 112.28(14) . . ? N45 C46 C47 111.0(2) . . ? N45 C46 C49 119.6(2) . . ? C47 C46 C49 129.2(2) . . ? C48 C47 C46 106.0(2) . . ? C47 C48 N44 107.0(2) . . ? O50B C49 O51B 125.3(8) . . ? O50A C49 O51A 123.8(5) . . ? O50A C49 C46 124.9(5) . . ? O50B C49 C46 125.3(8) . . ? O51B C49 C46 109.4(4) . . ? O51A C49 C46 111.0(2) . . ? C49 O51A C52A 118.1(3) . . ? O51A C52A C53 109.8(4) . . ? C49 O51B C52B 106.7(6) . . ? C53 C52B O51B 105.8(7) . . ? F55A B54A F56A 110.7(6) . . ? F55A B54A F58A 110.9(5) . . ? F56A B54A F58A 109.9(5) . . ? F55A B54A F57A 108.3(6) . . ? F56A B54A F57A 109.0(5) . . ? F58A B54A F57A 107.9(5) . . ? F56B B54B F58B 109.6(14) . . ? F56B B54B F57B 107.7(15) . . ? F58B B54B F57B 110.4(14) . . ? F56B B54B F55B 110.1(16) . . ? F58B B54B F55B 109.0(16) . . ? F57B B54B F55B 110.1(16) . . ? F61A B59A F62A 113.7(6) . . ? F61A B59A F60A 111.6(6) . . ? F62A B59A F60A 110.1(5) . . ? F61A B59A F63A 106.4(5) . . ? F62A B59A F63A 108.7(5) . . ? F60A B59A F63A 105.9(6) . . ? F61B B59B F63B 113.4(15) . . ? F61B B59B F60B 113.5(16) . . ? F63B B59B F60B 113.3(15) . . ? F61B B59B F62B 103.7(14) . . ? F63B B59B F62B 105.2(14) . . ? F60B B59B F62B 106.7(14) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.479 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.083 #=END data_je36 _database_code_depnum_ccdc_archive 'CCDC 263426' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-bis{3-(hydroxymethyl)pyrazol-1-yl}pyridine]iron(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Fe N10 O4, 2[B F4]' _chemical_formula_sum 'C26 H26 B2 F8 Fe N10 O4' _chemical_formula_weight 772.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 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 20.0482(3) _cell_length_b 9.9323(1) _cell_length_c 16.4584(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.2730(7) _cell_angle_gamma 90.00 _cell_volume 3093.60(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 27162 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.49 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.589 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.723 _exptl_absorpt_correction_T_max 0.862 _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 27162 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7049 _reflns_number_gt 5930 _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 BF~4~^-^ anions are disordered over three orientations: B42A-F46A (occupancy 0.60), B42B-F46B (occupancy 0.30) and B42C-F46C (occupancy 0.10). and B47A-F51A (occupancy 0.33), B47B-F51B (occupancy 0.33) and B47C-F51C (occupancy 0.33). All B-F distances were restrained to 1.39(2)\%A, and non-bonded F...F distances within a given disorder orientation to 2.27(2)\%A. All four hydroxymethyl substituents on the complex dication are also disordered, each over two orientations: C13A, O14A (occupancy 0.75) and C13B, O14B (occupancy 0.25) C20A, O21A (occupancy 0.75) and C20B, O21B (occupancy 0.25) C33A, O34A (occupancy 0.75) and C33B, O34B (occupancy 0.25) C40A, O41A (occupancy 0.75) and C40B, O41B (occupancy 0.25). All disordered C-O bonds were restrained to 1.40(2)\%A, and non-bonded 1,3-C...O distances to 2.38(2)\%A. All non-H atoms with occupancy >=0.75 were refined anisotropically, while all H atoms were placed in calculated positions and refined using a riding model. The largest residual Fourier peak of 0.97 e.\%A^-3^ lies within the disordered hydroxymethyl group C13, O14. There is no apparent hydrogen bond acceptor for the minor partial hydroxyl group O21B. ; _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^)+(0.1244P)^2^+3.3066P] 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 0.020(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7049 _refine_ls_number_parameters 534 _refine_ls_number_restraints 76 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.2054 _refine_ls_wR_factor_gt 0.1929 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.012 _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 0.25142(2) 0.45188(4) 0.54904(3) 0.0372(2) Uani 1 1 d . . . N2 N 0.36272(13) 0.4730(2) 0.58044(17) 0.0373(5) Uani 1 1 d . . . C3 C 0.39010(17) 0.5867(3) 0.5608(2) 0.0431(7) Uani 1 1 d . . . C4 C 0.46158(19) 0.6050(4) 0.5757(3) 0.0567(9) Uani 1 1 d . . . H4 H 0.4795 0.6871 0.5616 0.068 Uiso 1 1 calc R . . C5 C 0.50539(19) 0.4990(5) 0.6117(3) 0.0627(10) Uani 1 1 d . . . H5 H 0.5547 0.5073 0.6222 0.075 Uiso 1 1 calc R . . C6 C 0.47899(18) 0.3803(4) 0.6332(3) 0.0584(9) Uani 1 1 d . . . H6 H 0.5092 0.3069 0.6583 0.070 Uiso 1 1 calc R . . C7 C 0.40693(16) 0.3733(3) 0.6164(2) 0.0414(6) Uani 1 1 d . . . N8 N 0.33876(15) 0.6849(3) 0.52376(18) 0.0434(6) Uani 1 1 d . A . N9 N 0.26937(14) 0.6523(3) 0.50726(17) 0.0414(6) Uani 1 1 d . A . C10 C 0.2338(2) 0.7649(3) 0.4757(2) 0.0492(8) Uani 1 1 d D . . C11 C 0.2805(2) 0.8687(4) 0.4724(3) 0.0599(10) Uani 1 1 d . A . H11 H 0.2684 0.9583 0.4528 0.072 Uiso 1 1 calc R . . C12 C 0.3461(2) 0.8148(4) 0.5029(3) 0.0568(9) Uani 1 1 d . . . H12 H 0.3893 0.8596 0.5086 0.068 Uiso 1 1 calc R A . C13A C 0.1590(3) 0.7780(7) 0.4563(5) 0.0522(15) Uani 0.75 1 d PD A 1 H13A H 0.1491 0.8324 0.5014 0.063 Uiso 0.75 1 calc PR A 1 H13B H 0.1384 0.8249 0.4005 0.063 Uiso 0.75 1 calc PR A 1 O14A O 0.12787(18) 0.6494(4) 0.4520(2) 0.0575(8) Uani 0.75 1 d PD A 1 H14A H 0.1149 0.6215 0.4009 0.086 Uiso 0.75 1 calc PR A 1 C13B C 0.1458(9) 0.7449(16) 0.4436(12) 0.033(4) Uiso 0.25 1 d PD A 2 H13C H 0.1277 0.7098 0.3840 0.039 Uiso 0.25 1 calc PR A 2 H13D H 0.1321 0.6823 0.4822 0.039 Uiso 0.25 1 calc PR A 2 O14B O 0.1199(6) 0.8757(12) 0.4483(8) 0.068(3) Uiso 0.25 1 d PD A 2 H14B H 0.1489 0.9180 0.4890 0.102 Uiso 0.25 1 calc PR A 2 N15 N 0.37282(13) 0.2589(3) 0.63407(18) 0.0400(6) Uani 1 1 d . B . N16 N 0.30220(12) 0.2646(2) 0.62319(16) 0.0360(5) Uani 1 1 d . B . C17 C 0.28707(16) 0.1455(3) 0.6486(2) 0.0406(6) Uani 1 1 d D . . C18 C 0.3478(2) 0.0640(4) 0.6765(3) 0.0570(9) Uani 1 1 d . B . H18 H 0.3509 -0.0253 0.6981 0.068 Uiso 1 1 calc R . . C19 C 0.40087(19) 0.1386(4) 0.6664(3) 0.0534(8) Uani 1 1 d . . . H19 H 0.4487 0.1117 0.6795 0.064 Uiso 1 1 calc R B . C20A C 0.2122(4) 0.1115(7) 0.6425(6) 0.0416(15) Uani 0.75 1 d PD B 1 H20A H 0.1884 0.1915 0.6562 0.050 Uiso 0.75 1 calc PR B 1 H20B H 0.1850 0.0805 0.5837 0.050 Uiso 0.75 1 calc PR B 1 O21A O 0.21697(15) 0.0067(3) 0.7037(2) 0.0477(7) Uani 0.75 1 d PD B 1 H21A H 0.1764 -0.0115 0.7048 0.072 Uiso 0.75 1 calc PR B 1 C20B C 0.2201(16) 0.110(3) 0.6634(16) 0.045(7) Uiso 0.25 1 d PD B 2 H20C H 0.2304 0.0615 0.7189 0.055 Uiso 0.25 1 calc PR B 2 H20D H 0.1932 0.1923 0.6659 0.055 Uiso 0.25 1 calc PR B 2 O21B O 0.1806(8) 0.0282(16) 0.5966(11) 0.092(4) Uiso 0.25 1 d PD B 2 H21B H 0.2000 0.0245 0.5586 0.137 Uiso 0.25 1 calc PR B 2 N22 N 0.14649(12) 0.3748(3) 0.52280(16) 0.0357(5) Uani 1 1 d . . . C23 C 0.10771(16) 0.4122(3) 0.5717(2) 0.0419(7) Uani 1 1 d . . . C24 C 0.04225(17) 0.3562(4) 0.5619(3) 0.0553(9) Uani 1 1 d . . . H24 H 0.0161 0.3812 0.5983 0.066 Uiso 1 1 calc R . . C25 C 0.01690(18) 0.2632(5) 0.4975(3) 0.0606(10) Uani 1 1 d . . . H25 H -0.0283 0.2245 0.4886 0.073 Uiso 1 1 calc R . . C26 C 0.05513(17) 0.2237(4) 0.4449(2) 0.0526(8) Uani 1 1 d . . . H26 H 0.0373 0.1596 0.4002 0.063 Uiso 1 1 calc R . . C27 C 0.12082(15) 0.2835(3) 0.46150(19) 0.0383(6) Uani 1 1 d . . . N28 N 0.14075(14) 0.5093(3) 0.63264(16) 0.0421(6) Uani 1 1 d . C . N29 N 0.20895(14) 0.5450(2) 0.64157(17) 0.0393(6) Uani 1 1 d . C . C30 C 0.22491(19) 0.6459(3) 0.6978(2) 0.0488(8) Uani 1 1 d D . . C31 C 0.1671(2) 0.6745(4) 0.7262(2) 0.0589(10) Uani 1 1 d . C . H31 H 0.1652 0.7411 0.7668 0.071 Uiso 1 1 calc R . . C32 C 0.1156(2) 0.5887(4) 0.6841(2) 0.0544(9) Uani 1 1 d . . . H32 H 0.0698 0.5839 0.6891 0.065 Uiso 1 1 calc R C . C33A C 0.2955(3) 0.7197(5) 0.7129(4) 0.0532(12) Uani 0.75 1 d PD C 1 H33A H 0.3313 0.6543 0.7081 0.064 Uiso 0.75 1 calc PR C 1 H33B H 0.2893 0.7885 0.6675 0.064 Uiso 0.75 1 calc PR C 1 O34A O 0.3201(2) 0.7818(4) 0.7934(2) 0.0645(10) Uani 0.75 1 d PD C 1 H34A H 0.3397 0.7243 0.8311 0.097 Uiso 0.75 1 calc PR C 1 C33B C 0.2923(9) 0.7004(19) 0.7452(12) 0.053(5) Uiso 0.25 1 d PD C 2 H33C H 0.2897 0.7998 0.7472 0.063 Uiso 0.25 1 calc PR C 2 H33D H 0.3081 0.6658 0.8050 0.063 Uiso 0.25 1 calc PR C 2 O34B O 0.3402(5) 0.6604(11) 0.7026(7) 0.054(2) Uiso 0.25 1 d PD C 2 H34B H 0.3294 0.6985 0.6545 0.081 Uiso 0.25 1 calc PR C 2 N35 N 0.16719(12) 0.2530(2) 0.41580(16) 0.0362(5) Uani 1 1 d . D . N36 N 0.22813(12) 0.3267(2) 0.43339(16) 0.0358(5) Uani 1 1 d . D . C37 C 0.26056(15) 0.2775(3) 0.38115(18) 0.0365(6) Uani 1 1 d D . . C38 C 0.22094(17) 0.1721(3) 0.3306(2) 0.0417(6) Uani 1 1 d . D . H38 H 0.2328 0.1201 0.2889 0.050 Uiso 1 1 calc R . . C39 C 0.16193(17) 0.1600(3) 0.3539(2) 0.0419(7) Uani 1 1 d . . . H39 H 0.1243 0.0981 0.3310 0.050 Uiso 1 1 calc R D . C40A C 0.3288(7) 0.3375(16) 0.3789(11) 0.038(3) Uani 0.75 1 d PD D 1 H40A H 0.3680 0.3036 0.4288 0.046 Uiso 0.75 1 calc PR D 1 H40B H 0.3374 0.3074 0.3259 0.046 Uiso 0.75 1 calc PR D 1 O41A O 0.32864(17) 0.4777(3) 0.3811(2) 0.0489(8) Uani 0.75 1 d PD D 1 H41A H 0.3005 0.5073 0.3346 0.073 Uiso 0.75 1 calc PR D 1 C40B C 0.333(3) 0.328(6) 0.389(3) 0.045(11) Uiso 0.25 1 d PD D 2 H40C H 0.3430 0.3012 0.3361 0.054 Uiso 0.25 1 calc PR D 2 H40D H 0.3319 0.4274 0.3903 0.054 Uiso 0.25 1 calc PR D 2 O41B O 0.3875(8) 0.2824(18) 0.4600(11) 0.100(5) Uiso 0.25 1 d PD D 2 H41B H 0.3810 0.2010 0.4688 0.149 Uiso 0.25 1 calc PR D 2 B42A B 0.4261(6) 0.4713(11) 0.8606(8) 0.069(4) Uiso 0.60 1 d PD E 1 F43A F 0.3693(2) 0.4336(4) 0.7903(3) 0.0605(9) Uiso 0.60 1 d PD E 1 F44A F 0.4348(3) 0.6090(5) 0.8648(4) 0.0717(13) Uiso 0.60 1 d PD E 1 F45A F 0.4872(3) 0.4065(6) 0.8594(5) 0.0828(15) Uiso 0.60 1 d PD E 1 F46A F 0.4120(3) 0.4301(5) 0.9374(3) 0.0821(13) Uiso 0.60 1 d PD E 1 B42B B 0.4345(8) 0.4702(14) 0.8783(11) 0.048(5) Uiso 0.30 1 d PD F 2 F43B F 0.3606(6) 0.4576(13) 0.8294(9) 0.111(4) Uiso 0.30 1 d PD F 2 F44B F 0.4467(5) 0.6045(8) 0.8989(7) 0.065(2) Uiso 0.30 1 d PD F 2 F45B F 0.4698(9) 0.4244(18) 0.8214(11) 0.151(8) Uiso 0.30 1 d PD F 2 F46B F 0.4517(7) 0.3898(13) 0.9474(8) 0.117(4) Uiso 0.30 1 d PD F 2 B42C B 0.4280(10) 0.471(2) 0.8375(14) 0.024(6) Uiso 0.10 1 d PD G 3 F43C F 0.3923(17) 0.371(3) 0.7814(18) 0.140(16) Uiso 0.10 1 d PD G 3 F44C F 0.4923(9) 0.4158(19) 0.8947(13) 0.045(5) Uiso 0.10 1 d PD G 3 F45C F 0.4414(9) 0.5730(16) 0.7880(10) 0.044(4) Uiso 0.10 1 d PD G 3 F46C F 0.3871(13) 0.508(3) 0.8873(16) 0.082(7) Uiso 0.10 1 d PD G 3 B47A B 0.0449(7) 0.0459(14) 0.7227(10) 0.051(6) Uiso 0.33 1 d PD H 1 F48A F -0.0268(4) 0.0457(8) 0.6804(6) 0.046(2) Uiso 0.33 1 d PD H 1 F49A F 0.0650(6) 0.1762(9) 0.7248(6) 0.071(3) Uiso 0.33 1 d PD H 1 F50A F 0.0635(10) -0.0027(18) 0.8079(9) 0.171(8) Uiso 0.33 1 d PD H 1 F51A F 0.0756(4) -0.0418(8) 0.6780(6) 0.0585(18) Uiso 0.33 1 d PD H 1 B47B B 0.0527(7) 0.0200(15) 0.7332(9) 0.046(5) Uiso 0.33 1 d PD I 2 F48B F 0.0006(4) -0.0592(7) 0.7425(5) 0.0689(18) Uiso 0.33 1 d PD I 2 F49B F 0.0298(5) 0.1573(8) 0.7380(6) 0.086(2) Uiso 0.33 1 d PD I 2 F50B F 0.1159(3) -0.0002(7) 0.7992(4) 0.0573(15) Uiso 0.33 1 d PD I 2 F51B F 0.0633(4) 0.0074(9) 0.6539(5) 0.0613(18) Uiso 0.33 1 d PD I 2 B47C B 0.0466(7) 0.0395(14) 0.7389(9) 0.034(4) Uiso 0.33 1 d PD J 3 F48C F -0.0238(5) 0.0274(11) 0.6977(7) 0.071(4) Uiso 0.33 1 d PD J 3 F49C F 0.0794(4) -0.0728(8) 0.7154(6) 0.069(2) Uiso 0.33 1 d PD J 3 F50C F 0.0829(5) 0.1469(9) 0.7247(6) 0.070(3) Uiso 0.33 1 d PD J 3 F51C F 0.0514(4) 0.0258(8) 0.8232(4) 0.0563(16) Uiso 0.33 1 d PD J 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 0.0278(3) 0.0405(3) 0.0467(3) -0.00508(17) 0.01677(19) -0.00304(15) N2 0.0313(12) 0.0369(12) 0.0473(13) -0.0007(10) 0.0180(10) -0.0011(9) C3 0.0399(16) 0.0411(15) 0.0550(18) -0.0022(13) 0.0245(14) -0.0039(12) C4 0.0454(19) 0.0481(19) 0.086(3) -0.0033(18) 0.0349(19) -0.0106(15) C5 0.0323(16) 0.064(2) 0.096(3) -0.002(2) 0.0273(18) -0.0077(16) C6 0.0327(16) 0.053(2) 0.090(3) 0.0023(19) 0.0214(17) 0.0023(14) C7 0.0324(14) 0.0399(15) 0.0537(17) -0.0026(13) 0.0165(13) -0.0011(12) N8 0.0480(15) 0.0393(13) 0.0513(14) 0.0023(11) 0.0278(12) -0.0003(11) N9 0.0422(14) 0.0418(13) 0.0461(14) 0.0017(11) 0.0228(11) 0.0052(11) C10 0.064(2) 0.0491(18) 0.0400(15) 0.0059(13) 0.0249(15) 0.0130(16) C11 0.084(3) 0.0448(18) 0.059(2) 0.0170(16) 0.033(2) 0.0102(18) C12 0.076(3) 0.0436(18) 0.064(2) 0.0082(15) 0.041(2) -0.0052(17) C13A 0.052(3) 0.044(3) 0.059(4) -0.001(3) 0.015(3) 0.006(3) O14A 0.0467(18) 0.062(2) 0.064(2) 0.0046(16) 0.0173(16) -0.0015(16) N15 0.0302(12) 0.0390(13) 0.0533(14) 0.0019(11) 0.0170(11) 0.0032(10) N16 0.0308(12) 0.0366(12) 0.0420(12) -0.0022(10) 0.0140(10) -0.0003(9) C17 0.0401(15) 0.0368(14) 0.0483(16) 0.0027(12) 0.0191(13) 0.0006(12) C18 0.049(2) 0.0415(17) 0.086(3) 0.0146(17) 0.0300(19) 0.0098(14) C19 0.0430(17) 0.0459(18) 0.076(2) 0.0098(16) 0.0251(17) 0.0107(14) C20A 0.036(3) 0.038(3) 0.052(4) 0.011(3) 0.015(3) -0.0036(19) O21A 0.0364(15) 0.0389(15) 0.072(2) 0.0190(14) 0.0240(15) 0.0018(12) N22 0.0268(11) 0.0408(13) 0.0414(12) 0.0061(10) 0.0138(9) 0.0022(9) C23 0.0316(14) 0.0512(17) 0.0466(16) 0.0101(13) 0.0178(12) 0.0055(12) C24 0.0337(16) 0.074(2) 0.065(2) 0.0067(18) 0.0260(15) 0.0015(15) C25 0.0310(16) 0.082(3) 0.072(2) 0.004(2) 0.0216(16) -0.0090(16) C26 0.0334(15) 0.066(2) 0.0575(19) -0.0020(16) 0.0134(14) -0.0103(15) C27 0.0287(13) 0.0430(15) 0.0422(15) 0.0053(12) 0.0104(11) -0.0013(11) N28 0.0392(13) 0.0514(15) 0.0411(13) 0.0075(11) 0.0207(11) 0.0105(11) N29 0.0375(13) 0.0403(13) 0.0429(13) 0.0024(10) 0.0168(11) 0.0038(10) C30 0.0560(19) 0.0425(16) 0.0467(17) -0.0005(13) 0.0153(15) 0.0111(14) C31 0.076(3) 0.059(2) 0.0473(18) -0.0024(16) 0.0270(18) 0.0191(19) C32 0.057(2) 0.067(2) 0.0496(18) 0.0084(16) 0.0317(17) 0.0223(18) C33A 0.067(3) 0.039(2) 0.050(3) -0.006(2) 0.014(3) -0.008(2) O34A 0.082(3) 0.059(2) 0.0475(18) -0.0100(16) 0.0148(18) -0.0036(19) N35 0.0294(11) 0.0373(12) 0.0414(12) 0.0010(10) 0.0108(10) -0.0045(9) N36 0.0311(11) 0.0371(12) 0.0417(12) 0.0008(10) 0.0151(10) -0.0030(9) C37 0.0361(14) 0.0357(14) 0.0390(14) 0.0033(11) 0.0143(11) 0.0030(11) C38 0.0448(16) 0.0371(14) 0.0436(15) -0.0024(12) 0.0148(13) 0.0004(12) C39 0.0405(15) 0.0364(14) 0.0460(16) -0.0025(12) 0.0105(13) -0.0038(12) C40A 0.033(4) 0.039(5) 0.048(5) -0.001(3) 0.021(3) 0.002(2) O41A 0.0402(16) 0.0332(14) 0.084(2) -0.0063(14) 0.0356(16) -0.0063(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.128(2) . ? Fe1 N22 2.144(2) . ? Fe1 N9 2.174(3) . ? Fe1 N29 2.181(3) . ? Fe1 N36 2.191(2) . ? Fe1 N16 2.273(2) . ? N2 C7 1.331(4) . ? N2 C3 1.341(4) . ? C3 C4 1.384(5) . ? C3 N8 1.403(4) . ? C4 C5 1.374(6) . ? C5 C6 1.385(6) . ? C6 C7 1.380(4) . ? C7 N15 1.405(4) . ? N8 C12 1.356(4) . ? N8 N9 1.365(4) . ? N9 C10 1.336(4) . ? C10 C11 1.405(6) . ? C10 C13A 1.432(7) . ? C10 C13B 1.678(18) . ? C11 C12 1.355(6) . ? C13A O14A 1.413(7) . ? C13B O14B 1.411(16) . ? N15 C19 1.353(4) . ? N15 N16 1.368(3) . ? N16 C17 1.323(4) . ? C17 C18 1.408(5) . ? C17 C20B 1.49(3) . ? C17 C20A 1.509(8) . ? C18 C19 1.351(5) . ? C20A O21A 1.429(8) . ? C20B O21B 1.384(19) . ? N22 C27 1.328(4) . ? N22 C23 1.342(4) . ? C23 C24 1.385(4) . ? C23 N28 1.392(5) . ? C24 C25 1.371(6) . ? C25 C26 1.389(5) . ? C26 C27 1.387(4) . ? C27 N35 1.408(4) . ? N28 C32 1.369(4) . ? N28 N29 1.373(4) . ? N29 C30 1.329(4) . ? C30 C31 1.413(5) . ? C30 C33B 1.425(19) . ? C30 C33A 1.539(7) . ? C31 C32 1.343(6) . ? C33A O34A 1.395(6) . ? C33B O34B 1.420(15) . ? N35 C39 1.353(4) . ? N35 N36 1.370(3) . ? N36 C37 1.330(4) . ? C37 C38 1.409(4) . ? C37 C40B 1.49(6) . ? C37 C40A 1.503(16) . ? C38 C39 1.364(4) . ? C40A O41A 1.394(16) . ? C40B O41B 1.39(2) . ? B42A F44A 1.378(11) . ? B42A F43A 1.381(12) . ? B42A F45A 1.388(11) . ? B42A F46A 1.443(13) . ? B42B F46B 1.338(15) . ? B42B F44B 1.379(14) . ? B42B F45B 1.423(15) . ? B42B F43B 1.439(15) . ? B42C F45C 1.380(17) . ? B42C F46C 1.386(17) . ? B42C F43C 1.387(18) . ? B42C F44C 1.432(17) . ? B47A F49A 1.352(14) . ? B47A F48A 1.374(14) . ? B47A F51A 1.406(14) . ? B47A F50A 1.412(15) . ? B47B F48B 1.357(13) . ? B47B F50B 1.384(14) . ? B47B F51B 1.394(14) . ? B47B F49B 1.450(15) . ? B47C F48C 1.355(13) . ? B47C F50C 1.355(13) . ? B47C F51C 1.365(14) . ? B47C F49C 1.411(14) . ? 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 N22 164.68(10) . . ? N2 Fe1 N9 73.55(10) . . ? N22 Fe1 N9 121.11(10) . . ? N2 Fe1 N29 114.10(10) . . ? N22 Fe1 N29 73.07(10) . . ? N9 Fe1 N29 88.62(9) . . ? N2 Fe1 N36 99.95(9) . . ? N22 Fe1 N36 73.07(9) . . ? N9 Fe1 N36 104.78(9) . . ? N29 Fe1 N36 145.79(10) . . ? N2 Fe1 N16 72.69(9) . . ? N22 Fe1 N16 92.97(9) . . ? N9 Fe1 N16 145.84(9) . . ? N29 Fe1 N16 100.43(9) . . ? N36 Fe1 N16 86.05(9) . . ? C7 N2 C3 117.9(3) . . ? C7 N2 Fe1 121.7(2) . . ? C3 N2 Fe1 120.3(2) . . ? N2 C3 C4 123.4(3) . . ? N2 C3 N8 113.0(3) . . ? C4 C3 N8 123.6(3) . . ? C5 C4 C3 116.9(3) . . ? C4 C5 C6 121.3(3) . . ? C7 C6 C5 117.0(3) . . ? N2 C7 C6 123.5(3) . . ? N2 C7 N15 113.3(3) . . ? C6 C7 N15 123.2(3) . . ? C12 N8 N9 111.4(3) . . ? C12 N8 C3 130.2(3) . . ? N9 N8 C3 118.4(3) . . ? C10 N9 N8 104.9(3) . . ? C10 N9 Fe1 140.1(2) . . ? N8 N9 Fe1 114.72(19) . . ? N9 C10 C11 110.7(3) . . ? N9 C10 C13A 123.2(4) . . ? C11 C10 C13A 125.9(4) . . ? N9 C10 C13B 113.2(6) . . ? C11 C10 C13B 136.0(7) . . ? C12 C11 C10 105.9(3) . . ? C11 C12 N8 107.2(3) . . ? O14A C13A C10 110.0(4) . . ? O14B C13B C10 104.0(11) . . ? C19 N15 N16 111.4(3) . . ? C19 N15 C7 128.9(3) . . ? N16 N15 C7 119.6(2) . . ? C17 N16 N15 104.9(2) . . ? C17 N16 Fe1 142.4(2) . . ? N15 N16 Fe1 111.38(17) . . ? N16 C17 C18 110.7(3) . . ? N16 C17 C20B 125.5(13) . . ? C18 C17 C20B 122.7(13) . . ? N16 C17 C20A 120.4(4) . . ? C18 C17 C20A 128.9(4) . . ? C19 C18 C17 106.0(3) . . ? C18 C19 N15 106.9(3) . . ? O21A C20A C17 106.4(6) . . ? O21B C20B C17 109(2) . . ? C27 N22 C23 119.2(3) . . ? C27 N22 Fe1 120.35(19) . . ? C23 N22 Fe1 120.3(2) . . ? N22 C23 C24 122.2(3) . . ? N22 C23 N28 113.1(3) . . ? C24 C23 N28 124.7(3) . . ? C25 C24 C23 117.1(3) . . ? C24 C25 C26 122.2(3) . . ? C27 C26 C25 116.1(3) . . ? N22 C27 C26 123.1(3) . . ? N22 C27 N35 113.2(2) . . ? C26 C27 N35 123.7(3) . . ? C32 N28 N29 110.0(3) . . ? C32 N28 C23 131.3(3) . . ? N29 N28 C23 118.5(2) . . ? C30 N29 N28 105.8(3) . . ? C30 N29 Fe1 138.3(2) . . ? N28 N29 Fe1 114.85(19) . . ? N29 C30 C31 110.3(3) . . ? N29 C30 C33B 129.4(7) . . ? C31 C30 C33B 118.3(7) . . ? N29 C30 C33A 117.9(3) . . ? C31 C30 C33A 131.4(4) . . ? C32 C31 C30 106.1(3) . . ? C31 C32 N28 107.8(3) . . ? O34A C33A C30 112.4(5) . . ? O34B C33B C30 107.3(13) . . ? C39 N35 N36 111.5(2) . . ? C39 N35 C27 130.4(3) . . ? N36 N35 C27 118.2(2) . . ? C37 N36 N35 105.0(2) . . ? C37 N36 Fe1 139.5(2) . . ? N35 N36 Fe1 113.95(17) . . ? N36 C37 C38 110.7(3) . . ? N36 C37 C40B 119(3) . . ? C38 C37 C40B 130(3) . . ? N36 C37 C40A 120.9(7) . . ? C38 C37 C40A 128.3(7) . . ? C39 C38 C37 105.7(3) . . ? N35 C39 C38 107.0(3) . . ? O41A C40A C37 112.7(10) . . ? O41B C40B C37 116(4) . . ? F44A B42A F43A 111.5(9) . . ? F44A B42A F45A 111.3(8) . . ? F43A B42A F45A 110.5(9) . . ? F44A B42A F46A 107.2(8) . . ? F43A B42A F46A 108.1(8) . . ? F45A B42A F46A 108.0(9) . . ? F46B B42B F44B 113.2(13) . . ? F46B B42B F45B 109.0(13) . . ? F44B B42B F45B 112.6(12) . . ? F46B B42B F43B 110.6(12) . . ? F44B B42B F43B 106.8(11) . . ? F45B B42B F43B 104.4(13) . . ? F45C B42C F46C 115.1(16) . . ? F45C B42C F43C 107.0(16) . . ? F46C B42C F43C 108.0(16) . . ? F45C B42C F44C 111.1(14) . . ? F46C B42C F44C 107.0(15) . . ? F43C B42C F44C 108.4(16) . . ? F49A B47A F48A 105.5(11) . . ? F49A B47A F51A 115.3(12) . . ? F48A B47A F51A 107.4(10) . . ? F49A B47A F50A 108.8(12) . . ? F48A B47A F50A 113.1(13) . . ? F51A B47A F50A 106.8(12) . . ? F48B B47B F50B 111.5(10) . . ? F48B B47B F51B 114.5(11) . . ? F50B B47B F51B 109.9(10) . . ? F48B B47B F49B 105.6(10) . . ? F50B B47B F49B 108.6(10) . . ? F51B B47B F49B 106.5(10) . . ? F48C B47C F50C 120.9(12) . . ? F48C B47C F51C 102.2(10) . . ? F50C B47C F51C 113.1(10) . . ? F48C B47C F49C 107.2(10) . . ? F50C B47C F49C 104.5(10) . . ? F51C B47C F49C 108.5(11) . . ? 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 O14A H14A F50A 0.84 1.94 2.718(14) 154.0 4_565 O14B H14B O21B 0.84 2.00 2.79(2) 156.1 1_565 O21A H21A F51A 0.84 1.94 2.766(8) 166.0 . O34A H34A F44A 0.84 2.13 2.798(7) 135.8 . O34B H34B N8 0.84 2.22 2.944(10) 143.8 . O34B H34B N9 0.84 2.37 3.058(11) 139.9 . O41A H41A O21A 0.84 2.25 3.040(5) 155.9 4_565 O41A H41A O34A 0.84 2.28 2.766(5) 117.6 4_575 O41B H41B F46B 0.84 1.81 2.19(2) 105.6 4_565 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.971 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.143