# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Malcolm A. Halcrow' _publ_contact_author_email M.A.HALCROW@LEEDS.AC.UK _publ_section_title ; Thermal and Light-Induced Spin-Transitions in Iron(II) Complexes of 2,6-Bis(4-halopyrazolyl)pyridines - the Influence of Polymorphism on a Spin-Crossover Compound ; loop_ _publ_author_name 'Malcolm A. Halcrow' 'Saket Asthana' 'Simon A. Barrett' 'Chiara Carbonera' 'Colin A. Kilner' ; H.Lazar ; 'Jean-Francois Letard' 'Ruth Pritchard' # Attachment 'B907094J.cif' data_rpppcl _database_code_depnum_ccdc_archive 'CCDC 727065' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,6-bis(4-chloropyrazol-1-yl)pyridine ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H7 Cl2 N5' _chemical_formula_sum 'C11 H7 Cl2 N5' _chemical_formula_weight 280.12 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' Cl Cl 0.1484 0.1585 '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 16.329(3) _cell_length_b 3.8130(7) _cell_length_c 20.215(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.231(9) _cell_angle_gamma 90.00 _cell_volume 1220.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2650 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 23.90 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 0.520 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.728 _exptl_absorpt_correction_T_max 0.967 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 4 kW. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14836 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 29.35 _reflns_number_total 3276 _reflns_number_gt 1899 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2007' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2007' _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. No disorder is present in the model, and no restraints were applied. All non-H atoms were refined anisotropically, while H atoms were placed in calculated positions and refined with 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^)+(0.0594P)^2^+2.0231P] 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 3276 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1199 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1631 _refine_ls_wR_factor_gt 0.1420 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 Cl1 Cl 0.60886(6) 0.5763(3) 0.84967(5) 0.0410(3) Uani 1 1 d . . . N1 N 0.42290(18) 0.1955(9) 0.92158(13) 0.0318(7) Uani 1 1 d . . . C1 C 0.4354(2) 0.4652(9) 0.82324(17) 0.0269(8) Uani 1 1 d . . . H1 H 0.4211 0.5667 0.7790 0.032 Uiso 1 1 calc R . . Cl2 Cl 0.16001(6) 0.9030(3) 0.50510(4) 0.0366(3) Uani 1 1 d . . . N2 N 0.38107(17) 0.3181(8) 0.85780(13) 0.0264(7) Uani 1 1 d . . . C2 C 0.5149(2) 0.4342(10) 0.86645(17) 0.0296(8) Uani 1 1 d . . . N3 N 0.25935(17) 0.4013(8) 0.77103(13) 0.0238(6) Uani 1 1 d . . . C3 C 0.5036(2) 0.2677(11) 0.92617(17) 0.0338(9) Uani 1 1 d . . . H3 H 0.5483 0.2142 0.9648 0.041 Uiso 1 1 calc R . . N4 N 0.14409(17) 0.5137(8) 0.67929(13) 0.0256(7) Uani 1 1 d . . . C4 C 0.2914(2) 0.2824(9) 0.83463(16) 0.0244(7) Uani 1 1 d . . . N5 N 0.05906(18) 0.5432(10) 0.65101(15) 0.0389(8) Uani 1 1 d . . . C5 C 0.2432(2) 0.1380(9) 0.87647(16) 0.0274(8) Uani 1 1 d . . . H5 H 0.2687 0.0599 0.9215 0.033 Uiso 1 1 calc R . . C6 C 0.1561(2) 0.1143(10) 0.84892(17) 0.0306(8) Uani 1 1 d . . . H6 H 0.1211 0.0151 0.8753 0.037 Uiso 1 1 calc R . . C7 C 0.1199(2) 0.2349(10) 0.78306(17) 0.0297(8) Uani 1 1 d . . . H7 H 0.0608 0.2203 0.7636 0.036 Uiso 1 1 calc R . . C8 C 0.1748(2) 0.3781(9) 0.74718(15) 0.0241(7) Uani 1 1 d . . . C9 C 0.0544(2) 0.6783(12) 0.58919(18) 0.0403(10) Uani 1 1 d . . . H9 H 0.0029 0.7293 0.5567 0.048 Uiso 1 1 calc R . . C10 C 0.1353(2) 0.7355(10) 0.57819(16) 0.0296(8) Uani 1 1 d . . . C11 C 0.1922(2) 0.6274(9) 0.63676(16) 0.0257(7) Uani 1 1 d . . . H11 H 0.2521 0.6309 0.6458 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0313(5) 0.0343(6) 0.0557(6) 0.0023(5) 0.0075(4) 0.0015(4) N1 0.0392(17) 0.0349(19) 0.0187(14) 0.0054(13) 0.0024(12) 0.0074(14) C1 0.0333(18) 0.0238(19) 0.0227(16) 0.0030(14) 0.0054(14) 0.0027(15) Cl2 0.0548(6) 0.0333(5) 0.0209(4) 0.0045(4) 0.0080(4) 0.0025(4) N2 0.0366(16) 0.0250(17) 0.0169(13) 0.0032(12) 0.0053(11) 0.0033(13) C2 0.0314(18) 0.0236(19) 0.0324(18) -0.0041(16) 0.0052(15) 0.0039(16) N3 0.0326(15) 0.0219(15) 0.0174(12) 0.0010(12) 0.0067(11) 0.0012(13) C3 0.041(2) 0.033(2) 0.0221(17) -0.0025(16) -0.0035(15) 0.0101(18) N4 0.0293(15) 0.0260(17) 0.0212(13) 0.0018(12) 0.0055(11) 0.0003(12) C4 0.0324(18) 0.0178(17) 0.0238(16) -0.0001(14) 0.0087(13) 0.0034(14) N5 0.0291(16) 0.053(2) 0.0308(16) 0.0089(16) 0.0010(13) 0.0034(15) C5 0.0406(19) 0.025(2) 0.0194(15) 0.0045(14) 0.0125(14) 0.0044(16) C6 0.042(2) 0.027(2) 0.0278(17) 0.0016(16) 0.0162(15) -0.0020(16) C7 0.0329(18) 0.027(2) 0.0295(18) 0.0017(16) 0.0075(14) -0.0018(16) C8 0.0327(18) 0.0217(18) 0.0186(15) -0.0008(14) 0.0075(13) -0.0004(15) C9 0.036(2) 0.056(3) 0.0263(18) 0.0086(19) 0.0025(15) 0.0058(19) C10 0.042(2) 0.026(2) 0.0202(16) 0.0000(15) 0.0069(15) -0.0007(17) C11 0.0296(17) 0.0241(19) 0.0238(16) 0.0031(15) 0.0071(13) 0.0004(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C2 1.738(4) . ? N1 C3 1.327(5) . ? N1 N2 1.384(4) . ? C1 N2 1.376(4) . ? C1 C2 1.380(5) . ? C1 H1 0.9500 . ? Cl2 C10 1.746(3) . ? N2 C4 1.430(4) . ? C2 C3 1.416(5) . ? N3 C4 1.342(4) . ? N3 C8 1.348(4) . ? C3 H3 0.9500 . ? N4 C11 1.370(4) . ? N4 N5 1.370(4) . ? N4 C8 1.437(4) . ? C4 C5 1.401(5) . ? N5 C9 1.336(5) . ? C5 C6 1.398(5) . ? C5 H5 0.9500 . ? C6 C7 1.395(5) . ? C6 H6 0.9500 . ? C7 C8 1.396(5) . ? C7 H7 0.9500 . ? C9 C10 1.410(5) . ? C9 H9 0.9500 . ? C10 C11 1.377(5) . ? C11 H11 0.9500 . ? 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 C3 N1 N2 104.4(3) . . ? N2 C1 C2 105.5(3) . . ? N2 C1 H1 127.3 . . ? C2 C1 H1 127.3 . . ? C1 N2 N1 112.3(3) . . ? C1 N2 C4 127.5(3) . . ? N1 N2 C4 120.3(3) . . ? C1 C2 C3 106.2(3) . . ? C1 C2 Cl1 126.0(3) . . ? C3 C2 Cl1 127.8(3) . . ? C4 N3 C8 116.3(3) . . ? N1 C3 C2 111.6(3) . . ? N1 C3 H3 124.2 . . ? C2 C3 H3 124.2 . . ? C11 N4 N5 113.0(3) . . ? C11 N4 C8 126.4(3) . . ? N5 N4 C8 120.5(3) . . ? N3 C4 C5 124.5(3) . . ? N3 C4 N2 114.1(3) . . ? C5 C4 N2 121.4(3) . . ? C9 N5 N4 104.0(3) . . ? C6 C5 C4 116.9(3) . . ? C6 C5 H5 121.6 . . ? C4 C5 H5 121.6 . . ? C7 C6 C5 120.6(3) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 116.7(3) . . ? C6 C7 H7 121.6 . . ? C8 C7 H7 121.6 . . ? N3 C8 C7 124.9(3) . . ? N3 C8 N4 113.8(3) . . ? C7 C8 N4 121.3(3) . . ? N5 C9 C10 111.5(3) . . ? N5 C9 H9 124.2 . . ? C10 C9 H9 124.2 . . ? C11 C10 C9 106.2(3) . . ? C11 C10 Cl2 126.1(3) . . ? C9 C10 Cl2 127.7(3) . . ? N4 C11 C10 105.3(3) . . ? N4 C11 H11 127.3 . . ? C10 C11 H11 127.3 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 29.35 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.254 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.083 #=END data_rpppbr _database_code_depnum_ccdc_archive 'CCDC 727066' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,6-bis(4-bromopyrazol-1-yl)pyridine ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H7 Br2 N5' _chemical_formula_sum 'C11 H7 Br2 N5' _chemical_formula_weight 369.04 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' Br Br -0.2901 2.4595 '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 16.1867(15) _cell_length_b 3.8789(3) _cell_length_c 20.1485(17) _cell_angle_alpha 90.00 _cell_angle_beta 103.757(3) _cell_angle_gamma 90.00 _cell_volume 1228.76(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2553 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 27.95 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.995 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 6.585 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.754 _exptl_absorpt_correction_T_max 0.954 _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 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13364 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_sigmaI/netI 0.0626 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 2 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 28.21 _reflns_number_total 3023 _reflns_number_gt 2260 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2007' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2007' _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. No disorder is present in the model, and no restraints were applied. All non-H atoms were refined anisotropically, while H atoms were placed in calculated positions and refined with 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^)+(0.0000P)^2^+0.6769P] 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 3023 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0726 _refine_ls_wR_factor_gt 0.0659 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Br1 Br 0.61094(2) 0.60765(8) 0.85142(2) 0.03274(12) Uani 1 1 d . . . N1 N 0.41799(19) 0.1927(7) 0.92223(13) 0.0243(7) Uani 1 1 d . . . C1 C 0.4310(2) 0.4728(8) 0.82694(17) 0.0210(7) Uani 1 1 d . . . H1 H 0.4168 0.5790 0.7832 0.025 Uiso 1 1 calc R . . Br2 Br 0.16278(2) 0.92947(8) 0.506328(17) 0.02484(11) Uani 1 1 d . . . N2 N 0.37676(18) 0.3197(6) 0.85985(13) 0.0198(6) Uani 1 1 d . . . C2 C 0.5095(2) 0.4441(8) 0.86879(17) 0.0219(7) Uani 1 1 d . . . N3 N 0.25612(17) 0.4007(6) 0.77350(13) 0.0176(6) Uani 1 1 d . . . C3 C 0.4990(2) 0.2694(8) 0.92721(16) 0.0243(8) Uani 1 1 d . . . H3 H 0.5441 0.2135 0.9653 0.029 Uiso 1 1 calc R . . N4 N 0.14255(17) 0.5104(6) 0.68267(13) 0.0177(6) Uani 1 1 d . . . C4 C 0.2879(2) 0.2802(7) 0.83636(16) 0.0180(7) Uani 1 1 d . . . N5 N 0.05769(18) 0.5215(7) 0.65318(15) 0.0272(7) Uani 1 1 d . . . C5 C 0.2393(2) 0.1243(8) 0.87624(17) 0.0217(7) Uani 1 1 d . . . H5 H 0.2645 0.0404 0.9207 0.026 Uiso 1 1 calc R . . C6 C 0.1530(2) 0.0960(7) 0.84879(17) 0.0212(7) Uani 1 1 d . . . H6 H 0.1177 -0.0093 0.8745 0.025 Uiso 1 1 calc R . . C7 C 0.1177(2) 0.2211(8) 0.78361(16) 0.0203(7) Uani 1 1 d . . . H7 H 0.0585 0.2036 0.7636 0.024 Uiso 1 1 calc R . . C8 C 0.1723(2) 0.3712(7) 0.74935(15) 0.0174(7) Uani 1 1 d . . . C9 C 0.0540(2) 0.6623(9) 0.59276(17) 0.0271(8) Uani 1 1 d . . . H9 H 0.0026 0.7060 0.5597 0.033 Uiso 1 1 calc R . . C10 C 0.1346(2) 0.7390(8) 0.58341(15) 0.0180(7) Uani 1 1 d . . . C11 C 0.1904(2) 0.6397(7) 0.64181(16) 0.0187(7) Uani 1 1 d . . . H11 H 0.2507 0.6573 0.6519 0.022 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0195(2) 0.02579(17) 0.0532(3) 0.00426(16) 0.00914(18) -0.00013(15) N1 0.0253(17) 0.0326(15) 0.0127(14) 0.0044(12) -0.0003(13) 0.0051(13) C1 0.0209(19) 0.0214(14) 0.0213(18) 0.0032(13) 0.0063(15) 0.0025(13) Br2 0.0337(2) 0.02347(15) 0.01772(18) 0.00280(13) 0.00681(15) 0.00297(15) N2 0.0199(16) 0.0227(13) 0.0163(14) 0.0021(11) 0.0033(13) 0.0036(12) C2 0.0185(18) 0.0202(14) 0.0265(19) 0.0001(14) 0.0047(15) 0.0021(14) N3 0.0193(15) 0.0168(11) 0.0172(14) -0.0010(10) 0.0055(12) -0.0001(11) C3 0.024(2) 0.0291(16) 0.0167(18) -0.0021(14) -0.0024(16) 0.0042(15) N4 0.0121(14) 0.0216(12) 0.0190(14) 0.0006(11) 0.0030(12) -0.0020(11) C4 0.0181(18) 0.0183(13) 0.0170(17) -0.0038(13) 0.0030(14) 0.0036(13) N5 0.0171(17) 0.0384(16) 0.0244(16) 0.0017(13) 0.0017(14) -0.0006(13) C5 0.029(2) 0.0224(14) 0.0156(17) 0.0016(13) 0.0095(16) 0.0016(15) C6 0.025(2) 0.0206(14) 0.0219(18) 0.0025(14) 0.0126(15) 0.0005(14) C7 0.0174(18) 0.0205(14) 0.0244(18) -0.0007(14) 0.0075(15) -0.0013(14) C8 0.0215(18) 0.0167(13) 0.0144(17) -0.0012(12) 0.0052(14) 0.0031(13) C9 0.020(2) 0.0397(19) 0.0186(18) 0.0033(15) -0.0011(16) 0.0028(16) C10 0.0195(18) 0.0195(14) 0.0149(16) -0.0012(13) 0.0041(14) 0.0009(14) C11 0.0167(17) 0.0217(14) 0.0193(17) -0.0009(13) 0.0073(15) 0.0010(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C2 1.870(3) . ? N1 C3 1.326(4) . ? N1 N2 1.367(3) . ? C1 C2 1.351(4) . ? C1 N2 1.357(4) . ? C1 H1 0.9500 . ? Br2 C10 1.872(3) . ? N2 C4 1.412(4) . ? C2 C3 1.403(5) . ? N3 C8 1.333(4) . ? N3 C4 1.333(4) . ? C3 H3 0.9500 . ? N4 C11 1.354(4) . ? N4 N5 1.361(4) . ? N4 C8 1.422(4) . ? C4 C5 1.390(4) . ? N5 C9 1.323(4) . ? C5 C6 1.378(5) . ? C5 H5 0.9500 . ? C6 C7 1.389(4) . ? C6 H6 0.9500 . ? C7 C8 1.374(4) . ? C7 H7 0.9500 . ? C9 C10 1.394(5) . ? C9 H9 0.9500 . ? C10 C11 1.358(4) . ? C11 H11 0.9500 . ? 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 C3 N1 N2 104.3(3) . . ? C2 C1 N2 106.3(3) . . ? C2 C1 H1 126.9 . . ? N2 C1 H1 126.9 . . ? C1 N2 N1 112.1(3) . . ? C1 N2 C4 127.6(3) . . ? N1 N2 C4 120.3(3) . . ? C1 C2 C3 106.3(3) . . ? C1 C2 Br1 126.3(3) . . ? C3 C2 Br1 127.4(3) . . ? C8 N3 C4 116.5(3) . . ? N1 C3 C2 111.1(3) . . ? N1 C3 H3 124.5 . . ? C2 C3 H3 124.5 . . ? C11 N4 N5 112.8(3) . . ? C11 N4 C8 126.9(3) . . ? N5 N4 C8 120.3(3) . . ? N3 C4 C5 124.0(3) . . ? N3 C4 N2 114.4(3) . . ? C5 C4 N2 121.7(3) . . ? C9 N5 N4 103.6(3) . . ? C6 C5 C4 117.5(3) . . ? C6 C5 H5 121.3 . . ? C4 C5 H5 121.3 . . ? C5 C6 C7 120.1(3) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C8 C7 C6 117.0(3) . . ? C8 C7 H7 121.5 . . ? C6 C7 H7 121.5 . . ? N3 C8 C7 125.0(3) . . ? N3 C8 N4 113.5(3) . . ? C7 C8 N4 121.5(3) . . ? N5 C9 C10 112.0(3) . . ? N5 C9 H9 124.0 . . ? C10 C9 H9 124.0 . . ? C11 C10 C9 105.9(3) . . ? C11 C10 Br2 126.0(3) . . ? C9 C10 Br2 128.1(2) . . ? N4 C11 C10 105.8(3) . . ? N4 C11 H11 127.1 . . ? C10 C11 H11 127.1 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.21 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.535 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.108 #=END data_rpfe25a _database_code_depnum_ccdc_archive 'CCDC 727067' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-di(4-chloropyrazol-1-yl)pyridine]iron(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H14 Cl4 Fe N10, 2[B F4]' _chemical_formula_sum 'C22 H14 B2 Cl4 F8 Fe N10' _chemical_formula_weight 789.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n n a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.1919(12) _cell_length_b 41.318(3) _cell_length_c 13.4331(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9541.9(12) _cell_formula_units_Z 12 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 107451 _cell_measurement_theta_min 0.99 _cell_measurement_theta_max 27.85 _exptl_crystal_description 'Square prism' _exptl_crystal_colour Brown _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4704 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.891 _exptl_absorpt_correction_T_max 0.993 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 2 kW. Although the data have a low mosaicity, the Fourier map has a high background noise. There are also several reflections which should be systematically absent (h0l with h+l odd and 0kl with k+l odd) that are weakly observed. XPREP and PLATON are both happy with our choice of space group, however. Therefore, the crystals appear to suffer from pseudosymmetry or mild twinning. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 107451 _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_av_sigmaI/netI 0.0184 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -52 _diffrn_reflns_limit_k_max 53 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 27.85 _reflns_number_total 11208 _reflns_number_gt 8913 _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 'XSEED (Barbour, 2003)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains: - One complex cation (Fe1--Cl37) and two anions (B59--F63 and B64--F68) lying on general positions. - An additional half-cation (Fe38--Cl58) spanning the C~2~ axis [x, 0.25, 0.25], with Fe38, N39, C42, N49 and C52 lying on this axis. - Two extra half-anions lying on the C~2~ axes [-0.25, 0, z] (B69--F73) and [0.25, 0, z] (B74--F78). The pyrazole groups of both half-ligands about Fe38, N43--Cl48 and N53--Cl58, are disordered about two sites labelled 'A' and 'B'. The Fe---N distances to these groups imply that they correspond to resolved high- and low-spin fractions of the complex at this site. The following restraints were applied to these moieties: C---C = 1.42(2), C=C = 1.36(2), C---N = 1.36(2), C=N = 1.32(2), N---N = 1.38(2), C---Cl = 1.74(2) and C{pyridine}--- N{pyrazole} = 1.41(2)\%A. The occupancies of the 'A' (high-spin) and 'B' (low-spin) sites of the ligand refined to 0.62 and 0.38. All four anion environments are also badly disordered. - B59---F63 is modelled over three equally occupied environments labelled 'A', 'B' and 'C'. - B64--F68 is disordered over three sites, also labelled 'A' (occupancy 0.50), 'B' (0.30) and 'C' (0.20). While the thermal parameters on some of the F atoms are high, attempts to refine a fourth partial site for this anion did not improve matters. - Half-anion B69--F73 was modelled as B69A--F71A (occupancy 0.17) with B69A lying on the C~2~ site, plus two other orientations on general sites about this special position, B69B--F73B and C69C--F73C (both with occupancy 0.17). - Half-anion B74--F78 was modelled as B74A--F78A (occupancy 0.25) with B74A lying on the C~2~ site, plus one other orientation on a general site about this special position, B74B--F78B (occupancy 0.25). All B---F bonds wre restrained to 1.40(2)\%A, and F...F distances within a given disorder site to 2.29(2)\%A. All wholly occupied non-H atoms, plus the major sites of the disordered Cl atoms, were refined anistropically, while all H atoms were placed in calculated positions and refined using a riding model. There are three residual Fourier peaks of 3.1-4.5 e.\%A^-3^, each lying 1.5-1.8\%A from a different pyridyl C atom. There is no chemically sensible way of incorporating these into the model. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1610P)^2^+70.9598P] 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 11208 _refine_ls_number_parameters 712 _refine_ls_number_restraints 137 _refine_ls_R_factor_all 0.1318 _refine_ls_R_factor_gt 0.1135 _refine_ls_wR_factor_ref 0.3368 _refine_ls_wR_factor_gt 0.3199 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.00046(5) 0.084089(17) 0.75248(6) 0.0279(2) Uani 1 1 d . . . N2 N -0.1086(3) 0.08214(12) 0.7254(4) 0.0385(12) Uani 1 1 d . . . C3 C -0.1586(4) 0.09442(16) 0.7921(6) 0.0456(16) Uani 1 1 d . . . C4 C -0.2412(5) 0.0936(2) 0.7780(10) 0.076(3) Uani 1 1 d . . . H4 H -0.2767 0.1026 0.8246 0.091 Uiso 1 1 calc R . . C5 C -0.2650(6) 0.0787(3) 0.6909(11) 0.090(4) Uani 1 1 d . . . H5 H -0.3193 0.0763 0.6802 0.108 Uiso 1 1 calc R . . C6 C -0.2141(6) 0.0667(2) 0.6167(8) 0.074(3) Uani 1 1 d . . . H6 H -0.2324 0.0576 0.5562 0.088 Uiso 1 1 calc R . . C7 C -0.1341(4) 0.06942(16) 0.6392(5) 0.0447(16) Uani 1 1 d . . . N8 N -0.0701(4) 0.05896(13) 0.5803(4) 0.0456(14) Uani 1 1 d . . . N9 N 0.0028(4) 0.06239(12) 0.6218(4) 0.0383(12) Uani 1 1 d . . . C10 C 0.0528(5) 0.05099(14) 0.5553(5) 0.0463(17) Uani 1 1 d . . . H10 H 0.1077 0.0500 0.5632 0.056 Uiso 1 1 calc R . . C11 C 0.0101(6) 0.04045(15) 0.4692(5) 0.057(2) Uani 1 1 d . . . C12 C -0.0673(6) 0.04511(16) 0.4869(5) 0.057(2) Uani 1 1 d . . . H12 H -0.1097 0.0400 0.4444 0.069 Uiso 1 1 calc R . . Cl13 Cl 0.0533(2) 0.02464(5) 0.36302(15) 0.0852(10) Uani 1 1 d . . . N14 N -0.1199(3) 0.10653(13) 0.8758(4) 0.0398(12) Uani 1 1 d . . . N15 N -0.0395(3) 0.10496(11) 0.8742(4) 0.0332(10) Uani 1 1 d . . . C16 C -0.0158(4) 0.11817(13) 0.9602(5) 0.0365(13) Uani 1 1 d . . . H16 H 0.0369 0.1204 0.9803 0.044 Uiso 1 1 calc R . . C17 C -0.0806(5) 0.12815(14) 1.0162(5) 0.0434(15) Uani 1 1 d . . . C18 C -0.1460(5) 0.12065(16) 0.9627(6) 0.0498(17) Uani 1 1 d . . . H18 H -0.1985 0.1244 0.9816 0.060 Uiso 1 1 calc R . . Cl19 Cl -0.07719(14) 0.14605(5) 1.13287(15) 0.0603(6) Uani 1 1 d . . . N20 N 0.1092(3) 0.08645(11) 0.7806(4) 0.0318(10) Uani 1 1 d . . . C21 C 0.1438(4) 0.06231(16) 0.8312(5) 0.0384(13) Uani 1 1 d . . . C22 C 0.2234(5) 0.0631(2) 0.8550(7) 0.067(2) Uani 1 1 d . . . H22 H 0.2468 0.0469 0.8953 0.080 Uiso 1 1 calc R . . C23 C 0.2666(5) 0.0891(2) 0.8164(8) 0.070(3) Uani 1 1 d . . . H23 H 0.3213 0.0895 0.8263 0.084 Uiso 1 1 calc R . . C24 C 0.2316(5) 0.1141(2) 0.7643(6) 0.057(2) Uani 1 1 d . . . H24 H 0.2609 0.1319 0.7397 0.068 Uiso 1 1 calc R . . C25 C 0.1512(4) 0.11202(15) 0.7495(5) 0.0394(14) Uani 1 1 d . . . N26 N 0.0910(3) 0.03751(12) 0.8531(4) 0.0372(11) Uani 1 1 d . . . N27 N 0.0149(3) 0.04213(11) 0.8216(4) 0.0313(10) Uani 1 1 d . . . C28 C -0.0218(4) 0.01456(13) 0.8414(4) 0.0356(13) Uani 1 1 d . . . H28 H -0.0753 0.0104 0.8290 0.043 Uiso 1 1 calc R . . C29 C 0.0322(5) -0.00805(14) 0.8847(5) 0.0431(16) Uani 1 1 d . . . C30 C 0.1016(4) 0.00719(16) 0.8918(5) 0.0428(15) Uani 1 1 d . . . H30 H 0.1484 -0.0014 0.9184 0.051 Uiso 1 1 calc R . . Cl31 Cl 0.01165(15) -0.04797(4) 0.91676(15) 0.0625(6) Uani 1 1 d . . . N32 N 0.1032(3) 0.13475(12) 0.7003(4) 0.0392(12) Uani 1 1 d . . . N33 N 0.0252(3) 0.12659(11) 0.6916(4) 0.0340(10) Uani 1 1 d . . . C34 C -0.0080(5) 0.15188(14) 0.6469(5) 0.0409(15) Uani 1 1 d . . . H34 H -0.0616 0.1535 0.6302 0.049 Uiso 1 1 calc R . . C35 C 0.0488(5) 0.17592(15) 0.6282(5) 0.0482(17) Uani 1 1 d . . . C36 C 0.1176(5) 0.16475(16) 0.6616(5) 0.0476(16) Uani 1 1 d . . . H36 H 0.1663 0.1755 0.6587 0.057 Uiso 1 1 calc R . . Cl37 Cl 0.03254(18) 0.21355(4) 0.57273(16) 0.0718(7) Uani 1 1 d . . . Fe38 Fe -0.01859(7) 0.2500 0.2500 0.0286(3) Uani 1 2 d S . . N39 N -0.1395(5) 0.2500 0.2500 0.0363(15) Uani 1 2 d S . . C40 C -0.1788(4) 0.24082(15) 0.1686(5) 0.0400(14) Uani 1 1 d D . . C41 C -0.2603(5) 0.2405(2) 0.1647(6) 0.059(2) Uani 1 1 d . A . H41 H -0.2870 0.2340 0.1061 0.070 Uiso 1 1 calc R . . C42 C -0.3010(7) 0.2500 0.2500 0.065(3) Uani 1 2 d S . . H42 H -0.3563 0.2500 0.2500 0.079 Uiso 1 2 calc SR A . N43A N -0.1334(6) 0.2321(3) 0.0867(7) 0.032(3) Uiso 0.62 1 d PD A 1 N44A N -0.0546(6) 0.2312(3) 0.1047(8) 0.031(3) Uiso 0.62 1 d PD A 1 C45A C -0.0245(6) 0.2200(2) 0.0197(7) 0.027(2) Uiso 0.62 1 d PD A 1 H45A H 0.0295 0.2171 0.0080 0.033 Uiso 0.62 1 calc PR A 1 C46A C -0.0818(6) 0.2132(2) -0.0489(7) 0.031(2) Uiso 0.62 1 d PD A 1 C47A C -0.1528(7) 0.2211(3) -0.0055(7) 0.032(2) Uiso 0.62 1 d PD A 1 H47A H -0.2033 0.2191 -0.0338 0.038 Uiso 0.62 1 calc PR A 1 Cl4A Cl -0.0681(3) 0.19716(15) -0.1680(5) 0.0516(12) Uani 0.62 1 d PD A 1 N43B N -0.1201(10) 0.2301(6) 0.0971(13) 0.045(7) Uiso 0.38 1 d PD A 2 N44B N -0.0392(10) 0.2321(5) 0.1158(13) 0.034(5) Uiso 0.38 1 d PD A 2 C45B C -0.0015(11) 0.2217(4) 0.0350(12) 0.032(4) Uiso 0.38 1 d PD A 2 H45B H 0.0535 0.2202 0.0291 0.038 Uiso 0.38 1 calc PR A 2 C46B C -0.0530(12) 0.2135(5) -0.0378(13) 0.052(5) Uiso 0.38 1 d PD A 2 C47B C -0.1291(13) 0.2192(6) -0.0005(14) 0.048(6) Uiso 0.38 1 d PD A 2 H47B H -0.1767 0.2163 -0.0352 0.058 Uiso 0.38 1 calc PR A 2 Cl4B Cl -0.0395(9) 0.2013(4) -0.1626(10) 0.097(5) Uani 0.38 1 d PD A 2 N49 N 0.1013(5) 0.2500 0.2500 0.0369(16) Uani 1 2 d S . . C50 C 0.1413(4) 0.22389(14) 0.2807(5) 0.0426(15) Uani 1 1 d D . . C51 C 0.2222(5) 0.22250(19) 0.2823(7) 0.058(2) Uani 1 1 d . A . H51 H 0.2487 0.2036 0.3044 0.070 Uiso 1 1 calc R . . C52 C 0.2635(8) 0.2500 0.2500 0.065(3) Uani 1 2 d S . . H52 H 0.3187 0.2500 0.2500 0.078 Uiso 1 2 calc SR A . N53A N 0.0982(6) 0.1980(2) 0.3106(9) 0.033(3) Uiso 0.62 1 d PD A 1 N54A N 0.0201(6) 0.2028(2) 0.3089(7) 0.030(2) Uiso 0.62 1 d PD A 1 C55A C -0.0130(6) 0.1758(2) 0.3418(7) 0.0253(19) Uiso 0.62 1 d PD A 1 H55A H -0.0673 0.1724 0.3493 0.02(2) Uiso 0.62 1 calc PR A 1 C56A C 0.0448(6) 0.15323(19) 0.3635(7) 0.0272(18) Uiso 0.62 1 d PD A 1 C57A C 0.1163(6) 0.1680(2) 0.3440(8) 0.029(2) Uiso 0.62 1 d PD A 1 H57A H 0.1667 0.1590 0.3523 0.07(4) Uiso 0.62 1 calc PR A 1 Cl5A Cl 0.0324(3) 0.11408(11) 0.4078(4) 0.0500(11) Uani 0.62 1 d PD A 1 N53B N 0.0807(9) 0.1994(4) 0.3098(14) 0.033(5) Uiso 0.38 1 d PD A 2 N54B N 0.0000(9) 0.2056(3) 0.3056(11) 0.027(4) Uiso 0.38 1 d PD A 2 C55B C -0.0389(12) 0.1796(4) 0.3350(15) 0.043(5) Uiso 0.38 1 d PD A 2 H55B H -0.0939 0.1779 0.3396 0.052 Uiso 0.38 1 calc PR A 2 C56B C 0.0131(12) 0.1555(4) 0.3575(17) 0.053(5) Uiso 0.38 1 d PD A 2 C57B C 0.0890(13) 0.1682(4) 0.3454(17) 0.051(6) Uiso 0.38 1 d PD A 2 H57B H 0.1365 0.1574 0.3591 0.061 Uiso 0.38 1 calc PR A 2 Cl5B Cl -0.0021(11) 0.1156(3) 0.3943(11) 0.131(6) Uani 0.38 1 d PD A 2 B59A B 0.1729(10) 0.1669(4) 0.9809(13) 0.049(6) Uiso 0.33 1 d PD B 1 F60A F 0.1689(12) 0.1908(5) 1.0572(14) 0.101(7) Uiso 0.33 1 d PD B 1 F61A F 0.1675(9) 0.1363(3) 1.0261(12) 0.061(4) Uiso 0.33 1 d PD B 1 F62A F 0.1088(8) 0.1714(4) 0.9198(11) 0.057(4) Uiso 0.33 1 d PD B 1 F63A F 0.2409(7) 0.1708(3) 0.9274(11) 0.054(3) Uiso 0.33 1 d PD B 1 B59B B 0.1600(13) 0.1760(5) 0.9936(16) 0.070(9) Uiso 0.33 1 d PD C 2 F60B F 0.1639(8) 0.2063(3) 1.0414(10) 0.050(3) Uiso 0.33 1 d PD C 2 F61B F 0.1235(18) 0.1542(6) 1.058(2) 0.200(16) Uiso 0.33 1 d PD C 2 F62B F 0.1194(14) 0.1797(6) 0.9054(15) 0.110(10) Uiso 0.33 1 d PD C 2 F63B F 0.2360(11) 0.1669(5) 0.9758(19) 0.119(9) Uiso 0.33 1 d PD C 2 B59C B 0.1717(11) 0.1673(5) 1.0557(15) 0.068(8) Uiso 0.33 1 d PD D 3 F60C F 0.2340(8) 0.1669(4) 1.1204(11) 0.071(4) Uiso 0.33 1 d PD D 3 F61C F 0.1022(8) 0.1649(4) 1.1096(13) 0.077(4) Uiso 0.33 1 d PD D 3 F62C F 0.1734(12) 0.1415(5) 0.9875(15) 0.100(7) Uiso 0.33 1 d PD D 3 F63C F 0.1688(15) 0.1966(5) 1.0024(19) 0.150(12) Uiso 0.33 1 d PD D 3 B64A B 0.2924(9) 0.1487(4) 0.5074(12) 0.069(5) Uiso 0.50 1 d PDU E 1 F65A F 0.2915(15) 0.1758(5) 0.5696(16) 0.214(15) Uiso 0.50 1 d PD E 1 F66A F 0.2222(6) 0.1319(3) 0.5139(8) 0.068(3) Uiso 0.50 1 d PD E 1 F67A F 0.3554(7) 0.1285(4) 0.5231(11) 0.101(5) Uiso 0.50 1 d PD E 1 F68A F 0.2996(7) 0.1602(3) 0.4077(8) 0.079(4) Uiso 0.50 1 d PD E 1 B64B B 0.2943(13) 0.1795(5) 0.5013(16) 0.079(10) Uiso 0.30 1 d PDU F 2 F65B F 0.2994(9) 0.1627(4) 0.5910(12) 0.056(4) Uiso 0.30 1 d PD F 2 F66B F 0.3595(11) 0.1990(6) 0.4887(19) 0.117(8) Uiso 0.30 1 d PD F 2 F67B F 0.2268(9) 0.1978(4) 0.4978(14) 0.076(5) Uiso 0.30 1 d PD F 2 F68B F 0.292(2) 0.1564(7) 0.423(2) 0.28(4) Uiso 0.30 1 d PD F 2 B64C B 0.3017(19) 0.1643(8) 0.509(2) 0.13(2) Uiso 0.20 1 d PDU G 3 F65C F 0.2974(13) 0.1756(6) 0.6070(16) 0.046(5) Uiso 0.20 1 d PD G 3 F66C F 0.2314(18) 0.1490(10) 0.485(3) 0.114(12) Uiso 0.20 1 d PD G 3 F67C F 0.3629(19) 0.1423(11) 0.500(3) 0.135(18) Uiso 0.20 1 d PD G 3 F68C F 0.314(4) 0.1903(11) 0.445(3) 0.40(8) Uiso 0.20 1 d PD G 3 B69A B -0.2500 0.0000 0.361(2) 0.060(14) Uiso 0.33 2 d SPDU . 1 F70A F -0.1834(6) 0.0042(5) 0.3039(15) 0.095(7) Uiso 0.33 1 d PD H 1 F71A F -0.2603(11) 0.0273(2) 0.4198(14) 0.083(6) Uiso 0.33 1 d PD I 1 B69B B -0.2488(17) 0.0046(7) 0.331(2) 0.060(13) Uiso 0.17 1 d PDU . 2 F70B F -0.1836(15) -0.0115(7) 0.3686(18) 0.054(6) Uiso 0.17 1 d PD . 2 F71B F -0.2500 0.0000 0.2269(16) 0.086(8) Uiso 0.33 2 d SPD . 2 F72B F -0.3165(18) -0.0091(14) 0.370(3) 0.14(3) Uiso 0.17 1 d PD . 2 F73B F -0.246(4) 0.0374(7) 0.353(3) 0.18(3) Uiso 0.17 1 d PD . 2 B69C B -0.2439(15) -0.0057(6) 0.353(2) 0.042(13) Uiso 0.17 1 d PDU . 3 F70C F -0.1669(13) 0.0051(7) 0.340(2) 0.052(7) Uiso 0.17 1 d PD . 3 F71C F -0.2816(18) -0.0031(8) 0.261(2) 0.083(10) Uiso 0.17 1 d PD . 3 F72C F -0.2435(13) -0.0377(5) 0.3850(19) 0.035(5) Uiso 0.17 1 d PD . 3 F73C F -0.280(2) 0.0140(8) 0.424(3) 0.132(19) Uiso 0.17 1 d PD . 3 B74A B 0.2500 0.0000 1.1196(18) 0.072(8) Uiso 0.50 2 d SPDU . 1 F75A F 0.2186(8) -0.0254(2) 1.0619(10) 0.107(5) Uiso 0.50 1 d PD J 1 F76A F 0.1907(6) 0.0132(3) 1.1772(10) 0.097(4) Uiso 0.50 1 d PD K 1 B74B B 0.2332(15) 0.0066(6) 1.1264(18) 0.14(3) Uiso 0.25 1 d PDU . 2 F75B F 0.3030(15) 0.0216(7) 1.150(2) 0.142(14) Uiso 0.25 1 d PD . 2 F76B F 0.2402(11) -0.0113(4) 1.0375(13) 0.059(5) Uiso 0.25 1 d PD . 2 F77B F 0.1748(15) 0.0302(5) 1.120(2) 0.107(9) Uiso 0.25 1 d PD L 2 F78B F 0.2096(15) -0.0137(6) 1.2045(16) 0.098(8) Uiso 0.25 1 d PD . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0377(4) 0.0210(4) 0.0250(4) -0.0007(3) -0.0060(3) 0.0016(3) N2 0.042(3) 0.029(2) 0.044(3) 0.001(2) -0.015(2) -0.001(2) C3 0.042(3) 0.038(3) 0.057(4) -0.003(3) -0.008(3) 0.006(3) C4 0.039(4) 0.066(5) 0.123(9) 0.001(6) -0.018(5) 0.008(4) C5 0.047(5) 0.098(8) 0.124(10) -0.002(7) -0.037(6) -0.002(5) C6 0.076(6) 0.067(5) 0.078(6) 0.001(5) -0.042(5) -0.008(5) C7 0.056(4) 0.035(3) 0.043(4) 0.003(3) -0.016(3) -0.005(3) N8 0.073(4) 0.029(2) 0.035(3) -0.003(2) -0.017(3) -0.008(3) N9 0.064(3) 0.023(2) 0.028(3) 0.0016(19) -0.004(2) -0.003(2) C10 0.083(5) 0.024(3) 0.032(3) 0.003(2) 0.008(3) -0.002(3) C11 0.129(8) 0.022(3) 0.020(3) -0.001(2) 0.003(4) -0.017(4) C12 0.108(7) 0.032(3) 0.032(3) 0.001(3) -0.017(4) -0.018(4) Cl13 0.184(3) 0.0386(9) 0.0333(9) -0.0108(7) 0.0277(13) -0.0234(13) N14 0.038(3) 0.034(3) 0.047(3) -0.003(2) -0.001(2) 0.007(2) N15 0.040(3) 0.025(2) 0.035(3) 0.0008(19) -0.003(2) 0.0016(19) C16 0.054(4) 0.025(3) 0.031(3) -0.004(2) 0.002(3) -0.005(2) C17 0.066(4) 0.025(3) 0.039(4) -0.003(2) 0.006(3) -0.004(3) C18 0.057(4) 0.035(3) 0.057(4) -0.010(3) 0.009(3) 0.010(3) Cl19 0.0907(15) 0.0438(9) 0.0464(10) -0.0167(8) 0.0139(9) -0.0109(9) N20 0.041(3) 0.030(2) 0.025(2) -0.0018(18) -0.0024(19) 0.0025(19) C21 0.042(3) 0.043(3) 0.030(3) 0.007(3) -0.005(2) 0.001(3) C22 0.050(4) 0.077(6) 0.073(6) 0.032(5) -0.018(4) 0.001(4) C23 0.041(4) 0.090(7) 0.079(6) 0.025(5) -0.014(4) -0.013(4) C24 0.052(4) 0.064(5) 0.056(5) 0.006(4) -0.002(3) -0.018(4) C25 0.049(3) 0.034(3) 0.036(3) 0.004(2) -0.001(3) -0.008(3) N26 0.043(3) 0.032(2) 0.036(3) 0.004(2) -0.002(2) 0.007(2) N27 0.043(3) 0.028(2) 0.023(2) -0.0008(18) -0.0009(19) 0.0032(19) C28 0.056(4) 0.024(3) 0.027(3) -0.001(2) 0.001(3) 0.000(2) C29 0.079(5) 0.025(3) 0.025(3) 0.004(2) 0.010(3) 0.010(3) C30 0.056(4) 0.038(3) 0.034(3) 0.011(3) 0.003(3) 0.012(3) Cl31 0.1151(18) 0.0259(7) 0.0465(10) 0.0078(7) 0.0138(10) 0.0030(9) N32 0.053(3) 0.032(2) 0.033(3) 0.002(2) 0.003(2) -0.007(2) N33 0.049(3) 0.027(2) 0.026(2) -0.0033(19) -0.002(2) 0.004(2) C34 0.068(4) 0.028(3) 0.027(3) -0.001(2) -0.005(3) 0.010(3) C35 0.087(5) 0.028(3) 0.029(3) 0.001(2) 0.001(3) 0.001(3) C36 0.069(5) 0.035(3) 0.039(4) 0.006(3) 0.008(3) -0.007(3) Cl37 0.138(2) 0.0315(8) 0.0463(10) 0.0123(7) -0.0035(12) 0.0102(11) Fe38 0.0327(6) 0.0207(5) 0.0323(6) 0.0013(4) 0.000 0.000 N39 0.045(4) 0.032(3) 0.032(4) -0.005(3) 0.000 0.000 C40 0.047(3) 0.038(3) 0.035(3) -0.011(3) 0.001(3) -0.002(3) C41 0.050(4) 0.077(5) 0.048(4) -0.021(4) -0.006(3) -0.004(4) C42 0.041(5) 0.100(10) 0.055(7) -0.029(7) 0.000 0.000 Cl4A 0.069(2) 0.048(3) 0.0376(18) -0.0145(18) 0.0080(18) 0.011(2) Cl4B 0.178(14) 0.065(5) 0.048(5) -0.027(3) 0.040(8) -0.029(8) N49 0.049(4) 0.026(3) 0.036(4) 0.000(3) 0.000 0.000 C50 0.062(4) 0.023(3) 0.043(4) 0.002(2) -0.004(3) 0.003(3) C51 0.053(4) 0.042(4) 0.080(6) 0.002(4) -0.011(4) 0.006(3) C52 0.056(7) 0.054(7) 0.084(9) 0.011(6) 0.000 0.000 Cl5A 0.073(2) 0.0205(13) 0.056(3) 0.0137(14) 0.0180(19) -0.0021(13) Cl5B 0.265(19) 0.040(4) 0.088(6) 0.030(4) -0.044(10) -0.041(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N20 1.909(5) . ? Fe1 N2 1.911(5) . ? Fe1 N9 1.971(5) . ? Fe1 N15 1.972(5) . ? Fe1 N27 1.982(5) . ? Fe1 N33 1.983(5) . ? N2 C3 1.342(10) . ? N2 C7 1.345(9) . ? C3 N14 1.398(9) . ? C3 C4 1.433(10) . ? C4 C5 1.385(16) . ? C5 C6 1.414(17) . ? C6 C7 1.412(12) . ? C7 N8 1.423(10) . ? N8 C12 1.380(9) . ? N8 N9 1.381(8) . ? N9 C10 1.327(9) . ? C10 C11 1.437(11) . ? C11 C12 1.365(14) . ? C11 Cl13 1.736(8) . ? N14 C18 1.381(9) . ? N14 N15 1.384(7) . ? N15 C16 1.341(8) . ? C16 C17 1.406(10) . ? C17 C18 1.370(11) . ? C17 Cl19 1.734(7) . ? N20 C21 1.346(8) . ? N20 C25 1.346(8) . ? C21 N26 1.400(8) . ? C21 C22 1.406(10) . ? C22 C23 1.404(12) . ? C23 C24 1.388(12) . ? C24 C25 1.399(10) . ? C25 N32 1.415(9) . ? N26 C30 1.368(8) . ? N26 N27 1.388(7) . ? N27 C28 1.329(8) . ? C28 C29 1.440(9) . ? C29 C30 1.352(11) . ? C29 Cl31 1.741(6) . ? N32 C36 1.367(8) . ? N32 N33 1.388(8) . ? N33 C34 1.334(8) . ? C34 C35 1.415(11) . ? C35 C36 1.347(11) . ? C35 Cl37 1.747(7) . ? Fe38 N44B 1.981(17) . ? Fe38 N54B 2.005(14) . ? Fe38 N49 2.061(8) . ? Fe38 N39 2.078(8) . ? Fe38 N44A 2.189(11) . ? Fe38 N54A 2.207(10) . ? N39 C40 1.340(7) . ? C40 N43A 1.395(10) . ? C40 C41 1.403(10) . ? C40 N43B 1.462(15) . ? C41 C42 1.399(10) . ? N43A C47A 1.362(12) . ? N43A N44A 1.377(13) . ? N44A C45A 1.338(11) . ? C45A C46A 1.378(12) . ? C46A C47A 1.391(12) . ? C46A Cl4A 1.749(10) . ? N43B C47B 1.394(17) . ? N43B N44B 1.415(16) . ? N44B C45B 1.335(16) . ? C45B C46B 1.362(17) . ? C46B C47B 1.420(17) . ? C46B Cl4B 1.766(16) . ? N49 C50 1.344(7) . ? C50 N53A 1.362(11) . ? C50 C51 1.393(11) . ? C50 N53B 1.503(14) . ? C51 C52 1.408(10) . ? N53A C57A 1.353(11) . ? N53A N54A 1.357(12) . ? N54A C55A 1.329(11) . ? C55A C56A 1.392(11) . ? C56A C57A 1.399(11) . ? C56A Cl5A 1.737(9) . ? N53B C57B 1.381(16) . ? N53B N54B 1.413(15) . ? N54B C55B 1.327(16) . ? C55B C56B 1.370(17) . ? C56B C57B 1.415(17) . ? C56B Cl5B 1.742(15) . ? B59A F63A 1.382(16) . ? B59A F62A 1.387(16) . ? B59A F61A 1.407(16) . ? B59A F60A 1.424(17) . ? B59B F63B 1.381(18) . ? B59B F62B 1.383(17) . ? B59B F61B 1.403(17) . ? B59B F60B 1.409(18) . ? B59C F60C 1.379(17) . ? B59C F61C 1.401(17) . ? B59C F62C 1.406(17) . ? B59C F63C 1.407(17) . ? B64A F67A 1.383(16) . ? B64A F66A 1.394(15) . ? B64A F65A 1.398(16) . ? B64A F68A 1.426(16) . ? B64B F67B 1.387(18) . ? B64B F66B 1.390(18) . ? B64B F65B 1.395(18) . ? B64B F68B 1.420(18) . ? B64C F67C 1.396(19) . ? B64C F68C 1.397(19) . ? B64C F66C 1.401(19) . ? B64C F65C 1.401(19) . ? B69A F70A 1.389(15) . ? B69A F71A 1.390(15) . ? B69B F73B 1.388(18) . ? B69B F70B 1.398(19) . ? B69B F72B 1.400(19) . ? B69B F71B 1.409(18) . ? B69C F72C 1.390(18) . ? B69C F71C 1.396(18) . ? B69C F73C 1.399(18) . ? B69C F70C 1.407(18) . ? B74A F76A 1.391(13) . ? B74A F75A 1.412(13) . ? B74B F75B 1.390(19) . ? B74B F78B 1.402(19) . ? B74B F77B 1.403(19) . ? B74B F76B 1.409(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 N20 Fe1 N2 179.3(2) . . ? N20 Fe1 N9 100.3(2) . . ? N2 Fe1 N9 80.3(3) . . ? N20 Fe1 N15 98.9(2) . . ? N2 Fe1 N15 80.4(2) . . ? N9 Fe1 N15 160.8(2) . . ? N20 Fe1 N27 80.2(2) . . ? N2 Fe1 N27 100.1(2) . . ? N9 Fe1 N27 90.9(2) . . ? N15 Fe1 N27 92.2(2) . . ? N20 Fe1 N33 80.0(2) . . ? N2 Fe1 N33 99.7(2) . . ? N9 Fe1 N33 91.8(2) . . ? N15 Fe1 N33 91.7(2) . . ? N27 Fe1 N33 160.2(2) . . ? C3 N2 C7 120.9(6) . . ? C3 N2 Fe1 119.1(5) . . ? C7 N2 Fe1 120.0(5) . . ? N2 C3 N14 111.5(6) . . ? N2 C3 C4 122.5(8) . . ? N14 C3 C4 125.9(8) . . ? C5 C4 C3 114.5(10) . . ? C4 C5 C6 124.6(8) . . ? C7 C6 C5 115.1(8) . . ? N2 C7 C6 122.2(8) . . ? N2 C7 N8 110.2(6) . . ? C6 C7 N8 127.6(7) . . ? C12 N8 N9 112.2(7) . . ? C12 N8 C7 131.3(7) . . ? N9 N8 C7 116.5(5) . . ? C10 N9 N8 106.2(6) . . ? C10 N9 Fe1 140.8(5) . . ? N8 N9 Fe1 112.8(4) . . ? N9 C10 C11 108.6(8) . . ? C12 C11 C10 108.4(7) . . ? C12 C11 Cl13 127.8(6) . . ? C10 C11 Cl13 123.8(8) . . ? C11 C12 N8 104.5(7) . . ? C18 N14 N15 110.9(6) . . ? C18 N14 C3 132.6(6) . . ? N15 N14 C3 116.5(5) . . ? C16 N15 N14 105.8(5) . . ? C16 N15 Fe1 141.8(5) . . ? N14 N15 Fe1 112.4(4) . . ? N15 C16 C17 109.8(6) . . ? C18 C17 C16 107.7(6) . . ? C18 C17 Cl19 126.7(6) . . ? C16 C17 Cl19 125.6(6) . . ? C17 C18 N14 105.8(6) . . ? C21 N20 C25 120.0(6) . . ? C21 N20 Fe1 119.7(4) . . ? C25 N20 Fe1 120.3(4) . . ? N20 C21 N26 111.2(5) . . ? N20 C21 C22 121.9(6) . . ? N26 C21 C22 126.9(6) . . ? C23 C22 C21 116.7(7) . . ? C24 C23 C22 121.8(7) . . ? C23 C24 C25 117.0(7) . . ? N20 C25 C24 122.4(6) . . ? N20 C25 N32 110.7(6) . . ? C24 C25 N32 127.0(6) . . ? C30 N26 N27 111.5(5) . . ? C30 N26 C21 131.6(6) . . ? N27 N26 C21 116.5(5) . . ? C28 N27 N26 105.6(5) . . ? C28 N27 Fe1 141.6(4) . . ? N26 N27 Fe1 112.4(4) . . ? N27 C28 C29 109.3(6) . . ? C30 C29 C28 107.2(5) . . ? C30 C29 Cl31 127.1(5) . . ? C28 C29 Cl31 125.7(6) . . ? C29 C30 N26 106.4(6) . . ? C36 N32 N33 111.3(6) . . ? C36 N32 C25 132.4(6) . . ? N33 N32 C25 116.2(5) . . ? C34 N33 N32 105.1(5) . . ? C34 N33 Fe1 142.0(5) . . ? N32 N33 Fe1 112.8(4) . . ? N33 C34 C35 109.5(7) . . ? C36 C35 C34 107.9(6) . . ? C36 C35 Cl37 126.0(6) . . ? C34 C35 Cl37 126.2(6) . . ? C35 C36 N32 106.2(7) . . ? N44B Fe38 N44B 159.4(9) 3 . ? N44B Fe38 N54B 91.8(7) . 3 ? N44B Fe38 N54B 91.5(7) . . ? N54B Fe38 N54B 161.6(8) 3 . ? N44B Fe38 N49 100.3(5) . . ? N54B Fe38 N49 80.8(4) . . ? N44B Fe38 N39 79.7(5) . . ? N54B Fe38 N39 99.2(4) . . ? N49 Fe38 N39 180.0 . . ? N49 Fe38 N44A 106.4(3) . . ? N39 Fe38 N44A 73.6(3) . . ? N44A Fe38 N44A 147.1(5) . 3 ? N44A Fe38 N54A 94.5(4) . 3 ? N49 Fe38 N54A 72.5(3) . . ? N39 Fe38 N54A 107.5(3) . . ? N44A Fe38 N54A 95.3(4) . . ? N54A Fe38 N54A 144.9(5) 3 . ? C40 N39 C40 119.5(8) . 3 ? C40 N39 Fe38 120.3(4) . . ? N39 C40 N43A 115.8(7) . . ? N39 C40 C41 122.5(6) . . ? N43A C40 C41 121.8(7) . . ? N39 C40 N43B 105.9(9) . . ? C41 C40 N43B 131.5(9) . . ? C42 C41 C40 117.8(7) . . ? C41 C42 C41 120.0(10) 3 . ? C47A N43A N44A 113.1(9) . . ? C47A N43A C40 131.8(10) . . ? N44A N43A C40 114.7(9) . . ? C45A N44A N43A 103.9(10) . . ? C45A N44A Fe38 140.8(9) . . ? N43A N44A Fe38 115.2(7) . . ? N44A C45A C46A 111.4(9) . . ? C45A C46A C47A 107.5(8) . . ? C45A C46A Cl4A 126.3(8) . . ? C47A C46A Cl4A 126.2(8) . . ? N43A C47A C46A 104.1(9) . . ? C47B N43B N44B 107.2(15) . . ? C47B N43B C40 129.6(16) . . ? N44B N43B C40 123.0(14) . . ? C45B N44B N43B 108.3(16) . . ? C45B N44B Fe38 140.6(14) . . ? N43B N44B Fe38 111.0(11) . . ? N44B C45B C46B 110.3(16) . . ? C45B C46B C47B 107.8(15) . . ? C45B C46B Cl4B 131.8(15) . . ? C47B C46B Cl4B 120.3(15) . . ? N43B C47B C46B 106.4(16) . . ? C50 N49 C50 118.5(8) 3 . ? C50 N49 Fe38 120.8(4) 3 . ? C50 N49 Fe38 120.8(4) . . ? N49 C50 N53A 116.3(7) . . ? N49 C50 C51 123.3(6) . . ? N53A C50 C51 120.4(7) . . ? N49 C50 N53B 105.4(8) . . ? C51 C50 N53B 131.3(9) . . ? C50 C51 C52 117.8(8) . . ? C51 C52 C51 119.5(11) 3 . ? C57A N53A N54A 111.6(9) . . ? C57A N53A C50 133.7(10) . . ? N54A N53A C50 114.7(8) . . ? C55A N54A N53A 107.1(9) . . ? C55A N54A Fe38 137.1(8) . . ? N53A N54A Fe38 115.7(6) . . ? N54A C55A C56A 109.1(9) . . ? C55A C56A C57A 107.2(7) . . ? C55A C56A Cl5A 127.4(7) . . ? C57A C56A Cl5A 125.4(7) . . ? N53A C57A C56A 105.0(9) . . ? C57B N53B N54B 106.5(14) . . ? C57B N53B C50 130.3(15) . . ? N54B N53B C50 123.1(12) . . ? C55B N54B N53B 109.6(15) . . ? C55B N54B Fe38 140.5(14) . . ? N53B N54B Fe38 109.8(9) . . ? N54B C55B C56B 109.0(17) . . ? C55B C56B C57B 107.9(15) . . ? C55B C56B Cl5B 130.7(16) . . ? C57B C56B Cl5B 121.5(15) . . ? N53B C57B C56B 106.9(16) . . ? F63A B59A F62A 110.5(13) . . ? F63A B59A F61A 112.6(14) . . ? F62A B59A F61A 108.8(13) . . ? F63A B59A F60A 109.6(14) . . ? F62A B59A F60A 107.2(14) . . ? F61A B59A F60A 108.0(14) . . ? F63B B59B F62B 111.1(16) . . ? F63B B59B F61B 110.7(16) . . ? F62B B59B F61B 112.1(16) . . ? F63B B59B F60B 106.1(15) . . ? F62B B59B F60B 108.6(15) . . ? F61B B59B F60B 108.1(16) . . ? F60C B59C F61C 109.7(14) . . ? F60C B59C F62C 112.7(15) . . ? F61C B59C F62C 107.5(14) . . ? F60C B59C F63C 111.0(15) . . ? F61C B59C F63C 107.1(15) . . ? F62C B59C F63C 108.7(15) . . ? F67A B64A F66A 111.7(13) . . ? F67A B64A F65A 113.6(15) . . ? F66A B64A F65A 110.6(14) . . ? F67A B64A F68A 106.0(12) . . ? F66A B64A F68A 107.5(12) . . ? F65A B64A F68A 107.1(14) . . ? F67B B64B F66B 110.9(16) . . ? F67B B64B F65B 110.7(15) . . ? F66B B64B F65B 110.1(15) . . ? F67B B64B F68B 108.8(17) . . ? F66B B64B F68B 108.5(17) . . ? F65B B64B F68B 107.8(17) . . ? F67C B64C F68C 109.5(18) . . ? F67C B64C F66C 109.8(17) . . ? F68C B64C F66C 109.7(18) . . ? F67C B64C F65C 109.6(17) . . ? F68C B64C F65C 109.4(18) . . ? F66C B64C F65C 108.8(17) . . ? F70A B69A F70A 113(2) 2_455 . ? F70A B69A F71A 108.5(9) . . ? F70A B69A F71A 108.1(9) . 2_455 ? F71A B69A F71A 111(2) . 2_455 ? F73B B69B F70B 110.9(17) . . ? F73B B69B F72B 110.0(17) . . ? F70B B69B F72B 109.7(17) . . ? F73B B69B F71B 110.5(18) . . ? F70B B69B F71B 107.9(16) . . ? F72B B69B F71B 107.9(17) . . ? F72C B69C F71C 110.4(17) . . ? F72C B69C F73C 110.0(17) . . ? F71C B69C F73C 110.8(17) . . ? F72C B69C F70C 109.5(16) . . ? F71C B69C F70C 107.9(16) . . ? F73C B69C F70C 108.2(17) . . ? F76A B74A F76A 112.4(18) 2 . ? F76A B74A F75A 108.5(7) . . ? F76A B74A F75A 107.1(7) . 2 ? F75A B74A F75A 113.4(18) . 2 ? F75B B74B F78B 110.2(18) . . ? F75B B74B F77B 108.7(17) . . ? F78B B74B F77B 104.8(16) . . ? F75B B74B F76B 110.9(17) . . ? F78B B74B F76B 110.3(17) . . ? F77B B74B F76B 111.9(17) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 4.459 _refine_diff_density_min -0.776 _refine_diff_density_rms 0.154 #=END data_rpfe21 _database_code_depnum_ccdc_archive 'CCDC 727068' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-bis{4-iodopyrazol-1-yl}pyridine]iron(II) ditetrafluoroborate bis-acetone solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H14 Fe I4 N10, 2[B F4], 2[C3 H6 O]' _chemical_formula_sum 'C28 H26 B2 F8 Fe I4 N10 O2' _chemical_formula_weight 1271.66 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' I I -0.4742 1.8119 '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' Fe Fe 0.3463 0.8444 '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 11.4909(1) _cell_length_b 10.0039(1) _cell_length_c 35.3093(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.6172(4) _cell_angle_gamma 90.00 _cell_volume 4058.70(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 50105 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.50 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour Orange-brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.081 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 3.492 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.519 _exptl_absorpt_correction_T_max 0.912 _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 50105 _diffrn_reflns_av_R_equivalents 0.1075 _diffrn_reflns_av_sigmaI/netI 0.0672 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9257 _reflns_number_gt 6425 _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. One of the BF~4~^-^ ions and one acetone molecule are disordered. The anion B43--F47 is disordered over two discrete sites, labelled 'A' and 'B' with a refined occupancy ratio of 0.64:0.36. The restraints B---F = 1.38(2) and F...F = 2.26(2)\%A were applied to these two partial anion sites. The methyl groups only of the solvent molecule C52--O55 were also disordered over two sites, labelled 'A' and 'B'. The occupancy ratio of these two sites refined to 0.53:0.47, so they were treated as equally occupied in the final least squares cycles. The disordered C---C bonds were restrained to 1.50(2)\%A, and the 1,3-C...C distances between each pair of disordered methyl groups to 2.60(2)\%A. All non-H atoms with occupancy >0.5 were refined anisotropically, and all H atoms were placed in calculated positions and refined using a riding model. The fully occupied methyl group torsions were allowed to refine freely, while those of the partial methyl group environments were fixed. The deepest residual Fourier hole of -1.7 e.\%A^-3^ is 0.8\%A from I31. ; _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^)+(0.0579P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9257 _refine_ls_number_parameters 518 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1124 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.32804(6) -0.04261(6) 0.125421(17) 0.02194(15) Uani 1 1 d . . . N2 N 0.2167(3) -0.0691(3) 0.08597(10) 0.0230(8) Uani 1 1 d . . . C3 C 0.2507(4) -0.1147(4) 0.05224(12) 0.0249(10) Uani 1 1 d . . . C4 C 0.1745(4) -0.1426(5) 0.02329(13) 0.0307(11) Uani 1 1 d . . . H4 H 0.2005 -0.1764 -0.0003 0.037 Uiso 1 1 calc R . . C5 C 0.0568(5) -0.1191(5) 0.02997(14) 0.0363(12) Uani 1 1 d . . . H5 H 0.0011 -0.1370 0.0105 0.044 Uiso 1 1 calc R . . C6 C 0.0196(5) -0.0699(5) 0.06462(14) 0.0349(12) Uani 1 1 d . . . H6 H -0.0603 -0.0537 0.0694 0.042 Uiso 1 1 calc R . . C7 C 0.1043(4) -0.0460(4) 0.09153(13) 0.0251(10) Uani 1 1 d . . . N8 N 0.3717(4) -0.1307(4) 0.05157(10) 0.0255(9) Uani 1 1 d . . . N9 N 0.4317(3) -0.1027(4) 0.08492(10) 0.0248(8) Uani 1 1 d . . . C10 C 0.5419(4) -0.1221(4) 0.07729(13) 0.0267(10) Uani 1 1 d . . . H10 H 0.6040 -0.1100 0.0949 0.032 Uiso 1 1 calc R . . C11 C 0.5561(4) -0.1631(5) 0.03944(13) 0.0291(11) Uani 1 1 d . . . C12 C 0.4476(4) -0.1663(4) 0.02358(13) 0.0274(10) Uani 1 1 d . . . H12 H 0.4283 -0.1887 -0.0019 0.033 Uiso 1 1 calc R . . I13 I 0.71110(3) -0.21189(3) 0.013399(9) 0.03700(11) Uani 1 1 d . . . N14 N 0.0872(3) 0.0042(4) 0.12817(10) 0.0262(8) Uani 1 1 d . . . N15 N 0.1848(3) 0.0125(4) 0.15150(10) 0.0249(8) Uani 1 1 d . . . C16 C 0.1481(4) 0.0671(4) 0.18383(13) 0.0257(10) Uani 1 1 d . . . H16 H 0.1958 0.0837 0.2055 0.031 Uiso 1 1 calc R . . C17 C 0.0273(4) 0.0969(5) 0.18117(14) 0.0300(11) Uani 1 1 d . . . C18 C -0.0077(4) 0.0560(5) 0.14562(13) 0.0304(11) Uani 1 1 d . . . H18 H -0.0840 0.0627 0.1352 0.036 Uiso 1 1 calc R . . I19 I -0.07450(3) 0.19870(4) 0.219185(10) 0.04017(11) Uani 1 1 d . . . N20 N 0.4476(3) -0.0228(3) 0.16229(10) 0.0209(8) Uani 1 1 d . . . C21 C 0.4815(4) -0.1289(4) 0.18329(12) 0.0234(10) Uani 1 1 d . . . C22 C 0.5761(4) -0.1246(5) 0.20765(13) 0.0298(11) Uani 1 1 d . . . H22 H 0.6000 -0.2004 0.2220 0.036 Uiso 1 1 calc R . . C23 C 0.6349(4) -0.0026(5) 0.21004(13) 0.0327(11) Uani 1 1 d . . . H23 H 0.6994 0.0048 0.2270 0.039 Uiso 1 1 calc R . . C24 C 0.6027(4) 0.1086(5) 0.18864(13) 0.0307(11) Uani 1 1 d . . . H24 H 0.6434 0.1911 0.1903 0.037 Uiso 1 1 calc R . . C25 C 0.5085(4) 0.0913(4) 0.16500(12) 0.0240(10) Uani 1 1 d . . . N26 N 0.4093(3) -0.2390(4) 0.17595(10) 0.0228(8) Uani 1 1 d . . . N27 N 0.3218(3) -0.2198(3) 0.14949(10) 0.0218(8) Uani 1 1 d . . . C28 C 0.2578(4) -0.3300(4) 0.15053(13) 0.0280(11) Uani 1 1 d . . . H28 H 0.1912 -0.3467 0.1351 0.034 Uiso 1 1 calc R . . C29 C 0.3030(4) -0.4187(4) 0.17791(13) 0.0262(10) Uani 1 1 d . . . C30 C 0.3991(4) -0.3592(4) 0.19356(13) 0.0268(10) Uani 1 1 d . . . H30 H 0.4486 -0.3946 0.2128 0.032 Uiso 1 1 calc R . . I31 I 0.23668(3) -0.60448(3) 0.191413(9) 0.03875(11) Uani 1 1 d . . . N32 N 0.4637(4) 0.1854(3) 0.13900(10) 0.0256(9) Uani 1 1 d . . . N33 N 0.3728(3) 0.1439(4) 0.11612(10) 0.0236(8) Uani 1 1 d . . . C34 C 0.3518(4) 0.2455(5) 0.09266(12) 0.0277(11) Uani 1 1 d . . . H34 H 0.2931 0.2466 0.0735 0.033 Uiso 1 1 calc R . . C35 C 0.4300(5) 0.3517(4) 0.10054(13) 0.0302(11) Uani 1 1 d . . . C36 C 0.4983(5) 0.3122(4) 0.12990(14) 0.0301(11) Uani 1 1 d . . . H36 H 0.5583 0.3626 0.1418 0.036 Uiso 1 1 calc R . . I37 I 0.44517(4) 0.52608(3) 0.069889(10) 0.04757(12) Uani 1 1 d . . . B38 B 0.7404(6) 0.1656(6) 0.08648(17) 0.0404(15) Uani 1 1 d . . . F39 F 0.8426(3) 0.1612(3) 0.06577(8) 0.0442(7) Uani 1 1 d . . . F40 F 0.6447(3) 0.1674(3) 0.06281(9) 0.0530(9) Uani 1 1 d . . . F41 F 0.7374(3) 0.0516(4) 0.10911(10) 0.0696(12) Uani 1 1 d . . . F42 F 0.7443(3) 0.2763(4) 0.10950(11) 0.0705(12) Uani 1 1 d . . . B43A B 0.3140(11) 0.9744(12) 0.2673(3) 0.032(3) Uani 0.64 1 d PD A 1 F44A F 0.3073(9) 0.8553(8) 0.2464(2) 0.051(2) Uani 0.64 1 d PD A 1 F45A F 0.2055(5) 1.0193(6) 0.27453(16) 0.0626(15) Uani 0.64 1 d PD A 1 F46A F 0.3746(6) 0.9476(6) 0.30079(16) 0.0681(19) Uani 0.64 1 d PD A 1 F47A F 0.3777(7) 1.0682(6) 0.2463(2) 0.0345(15) Uani 0.64 1 d PD A 1 B43B B 0.3343(16) 0.9545(19) 0.2706(5) 0.035(8) Uiso 0.36 1 d PD B 2 F44B F 0.2747(13) 0.8729(17) 0.2455(5) 0.042(5) Uiso 0.36 1 d PD B 2 F45B F 0.2744(13) 0.9674(14) 0.3035(4) 0.104(5) Uiso 0.36 1 d PD B 2 F46B F 0.4429(9) 0.8966(10) 0.2785(3) 0.061(3) Uiso 0.36 1 d PD B 2 F47B F 0.3520(14) 1.0799(14) 0.2548(4) 0.050(5) Uiso 0.36 1 d PD B 2 C48 C 0.0226(5) 0.3615(6) 0.05783(16) 0.0469(15) Uani 1 1 d . . . C49 C 0.0395(6) 0.3679(6) 0.10008(16) 0.0529(16) Uani 1 1 d . . . H49A H 0.0991 0.3031 0.1079 0.079 Uiso 1 1 calc R . . H49B H -0.0340 0.3467 0.1125 0.079 Uiso 1 1 calc R . . H49C H 0.0645 0.4581 0.1073 0.079 Uiso 1 1 calc R . . C50 C -0.0740(6) 0.4455(6) 0.04185(19) 0.0607(18) Uani 1 1 d . . . H50A H -0.0812 0.4295 0.0145 0.091 Uiso 1 1 calc R . . H50B H -0.0569 0.5401 0.0464 0.091 Uiso 1 1 calc R . . H50C H -0.1472 0.4218 0.0542 0.091 Uiso 1 1 calc R . . O51 O 0.0861(4) 0.2915(5) 0.03864(13) 0.0617(12) Uani 1 1 d . . . C52 C 0.0939(6) 0.1968(6) 0.35827(17) 0.0541(17) Uani 1 1 d D . . C53A C 0.2174(11) 0.1890(17) 0.3671(4) 0.063(4) Uiso 0.50 1 d PD C 1 H53A H 0.2284 0.1785 0.3945 0.094 Uiso 0.50 1 calc PR C 1 H53B H 0.2558 0.2711 0.3587 0.094 Uiso 0.50 1 calc PR C 1 H53C H 0.2513 0.1121 0.3540 0.094 Uiso 0.50 1 calc PR C 1 C54A C 0.0507(15) 0.2201(16) 0.3177(4) 0.061(4) Uiso 0.50 1 d PD C 1 H54A H -0.0345 0.2251 0.3174 0.092 Uiso 0.50 1 calc PR C 1 H54B H 0.0759 0.1461 0.3016 0.092 Uiso 0.50 1 calc PR C 1 H54C H 0.0829 0.3042 0.3082 0.092 Uiso 0.50 1 calc PR C 1 C53B C 0.2133(12) 0.1363(16) 0.3710(4) 0.061(4) Uiso 0.50 1 d PD C 2 H53D H 0.2069 0.1010 0.3968 0.092 Uiso 0.50 1 calc PR C 2 H53E H 0.2731 0.2061 0.3705 0.092 Uiso 0.50 1 calc PR C 2 H53F H 0.2348 0.0639 0.3538 0.092 Uiso 0.50 1 calc PR C 2 C54B C 0.0929(17) 0.249(2) 0.3177(4) 0.085(6) Uiso 0.50 1 d PD C 2 H54D H 0.0160 0.2861 0.3116 0.127 Uiso 0.50 1 calc PR C 2 H54E H 0.1101 0.1755 0.3003 0.127 Uiso 0.50 1 calc PR C 2 H54F H 0.1520 0.3190 0.3151 0.127 Uiso 0.50 1 calc PR C 2 O55 O 0.0166(4) 0.1955(4) 0.38123(13) 0.0556(11) Uani 1 1 d . C . 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 0.0242(4) 0.0192(3) 0.0224(3) 0.0001(2) -0.0011(3) -0.0018(3) N2 0.031(2) 0.0151(18) 0.0227(18) 0.0018(15) -0.0008(16) -0.0020(16) C3 0.028(3) 0.022(2) 0.025(2) 0.0028(18) -0.0020(19) -0.0008(19) C4 0.037(3) 0.028(3) 0.027(2) -0.002(2) -0.007(2) -0.001(2) C5 0.039(3) 0.037(3) 0.033(3) -0.003(2) -0.011(2) -0.004(2) C6 0.033(3) 0.036(3) 0.035(3) -0.004(2) -0.006(2) -0.002(2) C7 0.025(3) 0.022(2) 0.029(2) 0.0037(19) -0.006(2) 0.0012(19) N8 0.032(2) 0.025(2) 0.0194(18) 0.0021(15) -0.0034(16) -0.0025(17) N9 0.028(2) 0.0225(19) 0.0236(18) 0.0016(15) -0.0050(16) -0.0060(16) C10 0.025(3) 0.027(2) 0.028(2) 0.003(2) -0.001(2) -0.001(2) C11 0.036(3) 0.026(2) 0.025(2) 0.0047(19) 0.007(2) -0.005(2) C12 0.036(3) 0.024(2) 0.022(2) 0.0011(19) 0.001(2) -0.004(2) I13 0.0341(2) 0.0477(2) 0.02941(18) -0.00286(14) 0.00782(14) -0.00297(15) N14 0.026(2) 0.027(2) 0.0251(19) 0.0008(16) 0.0004(17) -0.0008(17) N15 0.021(2) 0.027(2) 0.026(2) 0.0035(16) -0.0047(16) -0.0013(16) C16 0.023(3) 0.023(2) 0.031(2) -0.0003(19) 0.001(2) -0.0057(19) C17 0.027(3) 0.025(2) 0.038(3) 0.002(2) 0.001(2) -0.005(2) C18 0.026(3) 0.033(3) 0.032(3) -0.002(2) 0.000(2) 0.001(2) I19 0.0295(2) 0.0474(2) 0.0437(2) -0.01407(16) 0.00610(15) -0.00270(15) N20 0.025(2) 0.0163(18) 0.0212(18) -0.0018(15) 0.0017(15) -0.0011(15) C21 0.023(2) 0.022(2) 0.025(2) -0.0040(18) 0.0039(19) -0.0025(19) C22 0.029(3) 0.027(3) 0.033(2) 0.003(2) -0.004(2) 0.001(2) C23 0.029(3) 0.041(3) 0.027(2) -0.001(2) -0.009(2) -0.007(2) C24 0.034(3) 0.026(3) 0.031(2) 0.002(2) -0.006(2) -0.008(2) C25 0.026(3) 0.023(2) 0.023(2) -0.0019(18) 0.0042(19) -0.0001(19) N26 0.024(2) 0.0215(19) 0.0228(18) 0.0016(15) -0.0017(16) 0.0006(16) N27 0.020(2) 0.0226(19) 0.0231(18) 0.0007(15) -0.0031(15) 0.0002(15) C28 0.031(3) 0.024(2) 0.029(2) -0.0018(19) 0.002(2) -0.003(2) C29 0.033(3) 0.018(2) 0.028(2) 0.0025(18) 0.005(2) -0.0017(19) C30 0.032(3) 0.022(2) 0.027(2) 0.0030(19) 0.001(2) -0.001(2) I31 0.0555(3) 0.02574(18) 0.03499(19) 0.00321(13) -0.00098(16) -0.01482(15) N32 0.030(2) 0.022(2) 0.0248(19) -0.0044(16) 0.0011(17) -0.0078(16) N33 0.024(2) 0.0244(19) 0.0222(18) -0.0018(16) 0.0022(16) -0.0009(16) C34 0.036(3) 0.025(2) 0.023(2) 0.0025(19) 0.001(2) 0.004(2) C35 0.041(3) 0.016(2) 0.033(3) 0.003(2) 0.007(2) 0.002(2) C36 0.037(3) 0.020(2) 0.033(3) -0.003(2) 0.011(2) -0.005(2) I37 0.0736(3) 0.02363(19) 0.0457(2) 0.01009(15) 0.00972(19) -0.00254(17) B38 0.044(4) 0.043(4) 0.034(3) -0.007(3) -0.005(3) 0.003(3) F39 0.044(2) 0.0470(18) 0.0415(17) -0.0016(14) 0.0127(15) 0.0055(15) F40 0.048(2) 0.064(2) 0.0467(18) -0.0068(16) -0.0131(16) 0.0098(17) F41 0.055(2) 0.092(3) 0.061(2) 0.032(2) -0.0262(18) -0.038(2) F42 0.044(2) 0.098(3) 0.070(2) -0.047(2) 0.0124(19) -0.010(2) B43A 0.036(7) 0.034(6) 0.026(6) 0.008(4) -0.001(5) -0.005(5) F44A 0.064(6) 0.038(4) 0.052(4) -0.014(3) 0.026(4) -0.013(4) F45A 0.045(3) 0.070(4) 0.073(4) -0.004(3) 0.017(3) 0.015(3) F46A 0.090(5) 0.060(4) 0.053(3) 0.023(3) -0.040(3) -0.018(3) F47A 0.045(4) 0.027(3) 0.031(3) 0.003(2) 0.005(3) -0.007(2) C48 0.042(4) 0.050(4) 0.049(3) -0.005(3) 0.010(3) -0.017(3) C49 0.051(4) 0.055(4) 0.052(4) -0.013(3) -0.002(3) 0.002(3) C50 0.067(5) 0.056(4) 0.059(4) 0.015(3) 0.001(3) -0.003(3) O51 0.041(3) 0.082(3) 0.063(3) -0.028(2) 0.018(2) -0.010(2) C52 0.069(5) 0.048(4) 0.045(3) -0.011(3) -0.002(3) 0.003(3) O55 0.051(3) 0.054(3) 0.061(3) -0.007(2) 0.003(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N20 1.893(4) . ? Fe1 N2 1.900(4) . ? Fe1 N33 1.964(4) . ? Fe1 N9 1.965(4) . ? Fe1 N27 1.967(3) . ? Fe1 N15 1.974(4) . ? N2 C7 1.329(6) . ? N2 C3 1.337(6) . ? C3 C4 1.368(6) . ? C3 N8 1.399(6) . ? C4 C5 1.396(7) . ? C5 C6 1.390(7) . ? C6 C7 1.373(6) . ? C7 N14 1.404(6) . ? N8 C12 1.372(6) . ? N8 N9 1.387(5) . ? N9 C10 1.312(6) . ? C10 C11 1.409(6) . ? C11 C12 1.361(7) . ? C11 I13 2.072(5) . ? N14 C18 1.361(6) . ? N14 N15 1.386(5) . ? N15 C16 1.338(6) . ? C16 C17 1.421(7) . ? C17 C18 1.376(7) . ? C17 I19 2.060(5) . ? N20 C25 1.341(5) . ? N20 C21 1.349(6) . ? C21 C22 1.380(6) . ? C21 N26 1.401(6) . ? C22 C23 1.397(7) . ? C23 C24 1.392(7) . ? C24 C25 1.371(7) . ? C25 N32 1.409(6) . ? N26 C30 1.359(6) . ? N26 N27 1.378(5) . ? N27 C28 1.327(6) . ? C28 C29 1.407(6) . ? C29 C30 1.366(7) . ? C29 I31 2.066(4) . ? N32 C36 1.368(5) . ? N32 N33 1.378(5) . ? N33 C34 1.331(6) . ? C34 C35 1.418(7) . ? C35 C36 1.352(7) . ? C35 I37 2.062(4) . ? B38 F40 1.374(7) . ? B38 F42 1.374(7) . ? B38 F39 1.390(8) . ? B38 F41 1.393(7) . ? B43A F45A 1.352(13) . ? B43A F46A 1.393(12) . ? B43A F44A 1.402(11) . ? B43A F47A 1.405(10) . ? B43B F45B 1.363(17) . ? B43B F44B 1.381(17) . ? B43B F47B 1.389(17) . ? B43B F46B 1.400(17) . ? C48 O51 1.222(7) . ? C48 C50 1.498(9) . ? C48 C49 1.504(8) . ? C52 O55 1.210(8) . ? C52 C53A 1.451(13) . ? C52 C54B 1.525(14) . ? C52 C54A 1.528(12) . ? C52 C53B 1.561(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N20 Fe1 N2 175.51(16) . . ? N20 Fe1 N33 79.98(15) . . ? N2 Fe1 N33 100.68(15) . . ? N20 Fe1 N9 95.23(15) . . ? N2 Fe1 N9 80.34(16) . . ? N33 Fe1 N9 90.40(15) . . ? N20 Fe1 N27 80.02(14) . . ? N2 Fe1 N27 99.43(15) . . ? N33 Fe1 N27 159.88(15) . . ? N9 Fe1 N27 93.67(15) . . ? N20 Fe1 N15 104.66(15) . . ? N2 Fe1 N15 79.78(16) . . ? N33 Fe1 N15 91.95(15) . . ? N9 Fe1 N15 160.08(15) . . ? N27 Fe1 N15 90.90(15) . . ? C7 N2 C3 119.0(4) . . ? C7 N2 Fe1 121.0(3) . . ? C3 N2 Fe1 120.0(3) . . ? N2 C3 C4 123.0(5) . . ? N2 C3 N8 110.7(4) . . ? C4 C3 N8 126.3(4) . . ? C3 C4 C5 116.9(5) . . ? C6 C5 C4 121.1(5) . . ? C7 C6 C5 116.6(5) . . ? N2 C7 C6 123.4(4) . . ? N2 C7 N14 110.1(4) . . ? C6 C7 N14 126.5(5) . . ? C12 N8 N9 110.4(4) . . ? C12 N8 C3 132.9(4) . . ? N9 N8 C3 116.6(4) . . ? C10 N9 N8 105.6(4) . . ? C10 N9 Fe1 142.1(3) . . ? N8 N9 Fe1 112.3(3) . . ? N9 C10 C11 111.1(4) . . ? C12 C11 C10 106.4(4) . . ? C12 C11 I13 126.9(3) . . ? C10 C11 I13 126.7(4) . . ? C11 C12 N8 106.5(4) . . ? C18 N14 N15 110.8(4) . . ? C18 N14 C7 132.4(4) . . ? N15 N14 C7 116.7(4) . . ? C16 N15 N14 105.7(4) . . ? C16 N15 Fe1 141.7(3) . . ? N14 N15 Fe1 112.3(3) . . ? N15 C16 C17 110.2(4) . . ? C18 C17 C16 105.9(4) . . ? C18 C17 I19 125.4(4) . . ? C16 C17 I19 128.4(4) . . ? N14 C18 C17 107.4(4) . . ? C25 N20 C21 118.9(4) . . ? C25 N20 Fe1 120.8(3) . . ? C21 N20 Fe1 119.9(3) . . ? N20 C21 C22 122.6(4) . . ? N20 C21 N26 110.5(4) . . ? C22 C21 N26 126.9(4) . . ? C21 C22 C23 116.2(4) . . ? C24 C23 C22 122.7(4) . . ? C25 C24 C23 115.6(4) . . ? N20 C25 C24 124.0(4) . . ? N20 C25 N32 109.6(4) . . ? C24 C25 N32 126.4(4) . . ? C30 N26 N27 111.6(4) . . ? C30 N26 C21 131.7(4) . . ? N27 N26 C21 116.2(3) . . ? C28 N27 N26 105.4(3) . . ? C28 N27 Fe1 141.6(3) . . ? N26 N27 Fe1 112.9(3) . . ? N27 C28 C29 110.0(4) . . ? C30 C29 C28 107.1(4) . . ? C30 C29 I31 126.6(3) . . ? C28 C29 I31 126.3(3) . . ? N26 C30 C29 105.9(4) . . ? C36 N32 N33 111.2(4) . . ? C36 N32 C25 131.9(4) . . ? N33 N32 C25 116.7(3) . . ? C34 N33 N32 105.4(4) . . ? C34 N33 Fe1 141.5(3) . . ? N32 N33 Fe1 112.7(3) . . ? N33 C34 C35 109.8(4) . . ? C36 C35 C34 107.0(4) . . ? C36 C35 I37 126.7(4) . . ? C34 C35 I37 126.0(3) . . ? C35 C36 N32 106.5(4) . . ? F40 B38 F42 111.7(5) . . ? F40 B38 F39 110.8(5) . . ? F42 B38 F39 108.4(5) . . ? F40 B38 F41 109.6(5) . . ? F42 B38 F41 108.8(5) . . ? F39 B38 F41 107.6(5) . . ? F45A B43A F46A 110.8(8) . . ? F45A B43A F44A 109.6(9) . . ? F46A B43A F44A 107.8(10) . . ? F45A B43A F47A 111.4(10) . . ? F46A B43A F47A 108.6(8) . . ? F44A B43A F47A 108.5(8) . . ? F45B B43B F44B 110.6(15) . . ? F45B B43B F47B 109.5(14) . . ? F44B B43B F47B 110.4(14) . . ? F45B B43B F46B 109.1(14) . . ? F44B B43B F46B 108.5(13) . . ? F47B B43B F46B 108.6(14) . . ? O51 C48 C50 123.9(6) . . ? O51 C48 C49 120.2(6) . . ? C50 C48 C49 115.9(6) . . ? O55 C52 C53A 125.4(8) . . ? O55 C52 C54A 113.3(9) . . ? C53A C52 C54A 121.1(10) . . ? O55 C52 C54B 129.4(9) . . ? O55 C52 C53B 116.9(8) . . ? C54B C52 C53B 113.7(10) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.916 _refine_diff_density_min -1.766 _refine_diff_density_rms 0.212 #=END data_rpfe21y _database_code_depnum_ccdc_archive 'CCDC 727069' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-bis{4-iodopyrazol-1-yl}pyridine]iron(II) ditetrafluoroborate mono-acetone solvate ; _chemical_name_common ; Bis(2,6-bis(4-iodopyrazol-1-yl)pyridine)iron(ii) ditetrafluoroborate mono-acetone solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C22 H14 Fe I4 N10, 2[B F4], C3 H6 O' _chemical_formula_sum 'C25 H20 B2 F8 Fe I4 N10 O' _chemical_formula_weight 1213.58 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 15.6789(2) _cell_length_b 16.5181(2) _cell_length_c 15.9708(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.3400(10) _cell_angle_gamma 90.00 _cell_volume 4110.91(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 79452 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 27.48 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.961 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 3.441 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.297 _exptl_absorpt_correction_T_max 0.530 _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 296(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 79452 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9332 _reflns_number_gt 6939 _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. Anion B38-F42 is modelled over two equally occupied sites labelled 'A' and 'B'. The F atoms of anion B43-F47 are refined over three equally occupied orientations, ('A', 'B' and 'C'), which share a common wholly occupied B atom B43. Attempts to refine separate partial sites for this B atom were unsatisfactory. All B---F bonds were restrained to the refined value of 1.38(2)\%A, and F...F contacts within each partial anion to 2.25(2)\%A. The acetone molecule C48-O51 is also disordered, over three sites labelled 'A' (occupancy 0.25), 'B' (0.50) and 'C' (0.25). The following fixed restraints were applied to this residue: C---C = 1.54(2), C=O = 1.22(2), 1,3-C...C = 2.67(2) and 1,3-C...O = 2.37(2)\%A. All wholly occupied non-H atoms were refined anisotropically, while H atoms were placed in calculated positions and refined using a riding model. The torsions of the partial methyl group environments were fixed. The highest residual Fourier peak of +2.1 e.\%A^-3^ and hole of -1.9 e.\%A^-3^ both lie 0.9-1.0\%A from I31. Although no other residues were apparent in the final Fourier map, the unit cell contains two solvent-accessible void areas of 202 \%A^3^ each. Hence, the crystal may contain undetected, highly disordered additional solvent. ; _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^)+(0.1326P)^2^+11.7433P] 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 9332 _refine_ls_number_parameters 481 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_gt 0.0725 _refine_ls_wR_factor_ref 0.2439 _refine_ls_wR_factor_gt 0.2162 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.73629(6) 0.29083(6) 0.47279(6) 0.0622(3) Uani 1 1 d . . . N2 N 0.6786(4) 0.1756(4) 0.4867(3) 0.0621(12) Uani 1 1 d . . . C3 C 0.6282(4) 0.1427(4) 0.4227(4) 0.0615(14) Uani 1 1 d . . . C4 C 0.5913(6) 0.0676(5) 0.4273(5) 0.081(2) Uani 1 1 d . . . H4 H 0.5556 0.0461 0.3825 0.097 Uiso 1 1 calc R . . C5 C 0.6101(7) 0.0251(6) 0.5024(6) 0.090(3) Uani 1 1 d . . . H5 H 0.5878 -0.0267 0.5071 0.108 Uiso 1 1 calc R . . C6 C 0.6608(7) 0.0579(5) 0.5701(5) 0.088(3) Uani 1 1 d . . . H6 H 0.6730 0.0299 0.6205 0.105 Uiso 1 1 calc R . . C7 C 0.6926(5) 0.1351(5) 0.5586(4) 0.0706(18) Uani 1 1 d . . . N8 N 0.6181(4) 0.1928(3) 0.3513(3) 0.0600(12) Uani 1 1 d . . . N9 N 0.6585(4) 0.2660(4) 0.3548(4) 0.0662(14) Uani 1 1 d . . . C10 C 0.6403(5) 0.2987(5) 0.2797(5) 0.0695(17) Uani 1 1 d . . . H10 H 0.6598 0.3488 0.2633 0.083 Uiso 1 1 calc R . . C11 C 0.5864(5) 0.2457(5) 0.2278(5) 0.0664(16) Uani 1 1 d . . . C12 C 0.5738(5) 0.1800(4) 0.2748(4) 0.0642(15) Uani 1 1 d . . . H12 H 0.5411 0.1347 0.2580 0.077 Uiso 1 1 calc R . . I13 I 0.53700(4) 0.26825(4) 0.10443(4) 0.0895(2) Uani 1 1 d . . . N14 N 0.7452(4) 0.1760(4) 0.6217(3) 0.0725(16) Uani 1 1 d . . . N15 N 0.7795(4) 0.2492(4) 0.6000(4) 0.0704(15) Uani 1 1 d . . . C16 C 0.8217(5) 0.2756(5) 0.6711(5) 0.0732(19) Uani 1 1 d . . . H16 H 0.8519 0.3241 0.6762 0.088 Uiso 1 1 calc R . . C17 C 0.8153(5) 0.2221(5) 0.7372(5) 0.076(2) Uani 1 1 d . . . C18 C 0.7660(6) 0.1602(6) 0.7038(5) 0.085(2) Uani 1 1 d . . . H18 H 0.7496 0.1149 0.7326 0.103 Uiso 1 1 calc R . . I19 I 0.86550(4) 0.23827(4) 0.86147(3) 0.0870(2) Uani 1 1 d . . . N20 N 0.7870(4) 0.4104(4) 0.4769(3) 0.0649(13) Uani 1 1 d . . . C21 C 0.8596(4) 0.4267(5) 0.4430(4) 0.0669(16) Uani 1 1 d . . . C22 C 0.8918(6) 0.5045(6) 0.4380(5) 0.081(2) Uani 1 1 d . . . H22 H 0.9420 0.5149 0.4139 0.097 Uiso 1 1 calc R . . C23 C 0.8455(7) 0.5657(6) 0.4707(7) 0.101(3) Uani 1 1 d . . . H23 H 0.8660 0.6185 0.4697 0.121 Uiso 1 1 calc R . . C24 C 0.7715(7) 0.5515(6) 0.5042(7) 0.091(2) Uani 1 1 d . . . H24 H 0.7398 0.5931 0.5249 0.109 Uiso 1 1 calc R . . C25 C 0.7456(5) 0.4716(5) 0.5058(5) 0.0685(16) Uani 1 1 d . . . N26 N 0.8994(4) 0.3568(4) 0.4154(4) 0.0679(14) Uani 1 1 d . . . N27 N 0.8595(4) 0.2835(4) 0.4200(4) 0.0711(15) Uani 1 1 d . . . C28 C 0.9113(6) 0.2299(6) 0.3931(6) 0.079(2) Uani 1 1 d . . . H28 H 0.9005 0.1746 0.3881 0.095 Uiso 1 1 calc R . . C29 C 0.9867(6) 0.2693(7) 0.3728(6) 0.088(2) Uani 1 1 d . . . C30 C 0.9764(5) 0.3494(6) 0.3866(5) 0.078(2) Uani 1 1 d . . . H30 H 1.0146 0.3908 0.3778 0.093 Uiso 1 1 calc R . . I31 I 1.09314(6) 0.21500(7) 0.32870(8) 0.1391(4) Uani 1 1 d . . . N32 N 0.6691(4) 0.4463(4) 0.5374(4) 0.0724(15) Uani 1 1 d . . . N33 N 0.6435(4) 0.3694(4) 0.5255(4) 0.0751(16) Uani 1 1 d . . . C34 C 0.5693(5) 0.3636(7) 0.5607(6) 0.088(2) Uani 1 1 d . . . H34 H 0.5361 0.3170 0.5614 0.105 Uiso 1 1 calc R . . C35 C 0.5504(5) 0.4361(7) 0.5950(6) 0.087(2) Uani 1 1 d . . . C36 C 0.6127(6) 0.4883(7) 0.5808(6) 0.089(2) Uani 1 1 d . . . H36 H 0.6169 0.5424 0.5971 0.107 Uiso 1 1 calc R . . I37 I 0.44325(5) 0.46250(6) 0.65648(5) 0.1198(3) Uani 1 1 d . . . B38A B 0.8857(11) 0.4911(10) 0.7185(11) 0.07(2) Uiso 0.50 1 d PD A 1 F39A F 0.9201(10) 0.4677(9) 0.6462(8) 0.096(5) Uiso 0.50 1 d PD A 1 F40A F 0.7973(7) 0.4925(9) 0.7021(8) 0.099(4) Uiso 0.50 1 d PD A 1 F41A F 0.9112(8) 0.5702(6) 0.7395(8) 0.101(3) Uiso 0.50 1 d PD A 1 F42A F 0.9085(7) 0.4403(7) 0.7857(6) 0.086(3) Uiso 0.50 1 d PD A 1 B38B B 0.8837(10) 0.4898(9) 0.7139(11) 0.062(17) Uiso 0.50 1 d PD B 2 F39B F 0.9169(8) 0.4485(8) 0.6504(7) 0.079(4) Uiso 0.50 1 d PD B 2 F40B F 0.7999(7) 0.4663(8) 0.7183(9) 0.101(4) Uiso 0.50 1 d PD B 2 F41B F 0.8820(8) 0.5732(6) 0.7025(8) 0.100(3) Uiso 0.50 1 d PD B 2 F42B F 0.9338(9) 0.4713(8) 0.7885(8) 0.111(4) Uiso 0.50 1 d PD B 2 B43 B 0.7440(7) 0.0207(8) 0.2703(7) 0.146(7) Uani 1 1 d D . . F44A F 0.7753(12) 0.0887(10) 0.3017(15) 0.120(6) Uiso 0.33 1 d PD C 1 F45A F 0.6552(8) 0.0199(12) 0.2504(14) 0.092(7) Uiso 0.33 1 d PD C 1 F46A F 0.7586(15) -0.0412(12) 0.3348(12) 0.143(8) Uiso 0.33 1 d PD C 1 F47A F 0.7817(13) -0.0094(13) 0.2027(11) 0.104(7) Uiso 0.33 1 d PD C 1 F44B F 0.734(2) 0.0849(17) 0.2097(19) 0.22(2) Uiso 0.33 1 d PD C 2 F45B F 0.6674(15) -0.017(2) 0.271(3) 0.27(3) Uiso 0.33 1 d PD C 2 F46B F 0.8088(14) -0.0263(13) 0.2554(16) 0.138(8) Uiso 0.33 1 d PD C 2 F47B F 0.7665(17) 0.0618(17) 0.3475(14) 0.152(9) Uiso 0.33 1 d PD C 2 F44C F 0.7607(18) 0.0989(10) 0.241(2) 0.147(9) Uiso 0.33 1 d PD C 3 F45C F 0.6591(10) 0.0117(17) 0.2713(17) 0.107(9) Uiso 0.33 1 d PD C 3 F46C F 0.791(2) 0.005(3) 0.3442(15) 0.37(4) Uiso 0.33 1 d PD C 3 F47C F 0.7695(14) -0.0337(12) 0.2078(12) 0.099(6) Uiso 0.33 1 d PD C 3 C48A C 0.7829(19) 0.332(5) 1.052(3) 0.15(2) Uiso 0.25 1 d PD D 1 H48A H 0.7694 0.3163 0.9945 0.226 Uiso 0.25 1 calc PR D 1 H48B H 0.7798 0.3900 1.0566 0.226 Uiso 0.25 1 calc PR D 1 H48C H 0.7426 0.3079 1.0858 0.226 Uiso 0.25 1 calc PR D 1 C49A C 0.907(2) 0.314(3) 1.1791(16) 0.090(10) Uiso 0.25 1 d PD D 1 H49A H 0.9678 0.3220 1.1857 0.136 Uiso 0.25 1 calc PR D 1 H49B H 0.8927 0.2670 1.2096 0.136 Uiso 0.25 1 calc PR D 1 H49C H 0.8795 0.3608 1.2007 0.136 Uiso 0.25 1 calc PR D 1 C50A C 0.875(2) 0.303(5) 1.0844(19) 0.23(6) Uiso 0.25 1 d PD D 1 O51A O 0.9284(16) 0.309(2) 1.0350(15) 0.082(8) Uiso 0.25 1 d PD D 1 C48B C 0.7893(12) 0.2757(18) 1.089(2) 0.132(9) Uiso 0.50 1 d PD E 2 H48D H 0.7752 0.2424 1.0403 0.199 Uiso 0.50 1 calc PR E 2 H48E H 0.7515 0.3215 1.0867 0.199 Uiso 0.50 1 calc PR E 2 H48F H 0.7829 0.2447 1.1390 0.199 Uiso 0.50 1 calc PR E 2 C49B C 0.926(2) 0.355(2) 1.1655(19) 0.151(12) Uiso 0.50 1 d PD E 2 H49D H 0.9765 0.3804 1.1492 0.227 Uiso 0.50 1 calc PR E 2 H49E H 0.9416 0.3195 1.2125 0.227 Uiso 0.50 1 calc PR E 2 H49F H 0.8867 0.3951 1.1811 0.227 Uiso 0.50 1 calc PR E 2 C50B C 0.8832(12) 0.3053(15) 1.0917(13) 0.084(7) Uiso 0.50 1 d PD E 2 O51B O 0.9245(10) 0.2782(12) 1.0402(10) 0.091(5) Uiso 0.50 1 d PD E 2 C48C C 0.808(3) 0.255(3) 1.155(3) 0.131(17) Uiso 0.25 1 d PD F 3 H48G H 0.7652 0.2246 1.1204 0.196 Uiso 0.25 1 calc PR F 3 H48H H 0.7819 0.3025 1.1759 0.196 Uiso 0.25 1 calc PR F 3 H48I H 0.8323 0.2225 1.2008 0.196 Uiso 0.25 1 calc PR F 3 C49C C 0.947(4) 0.344(4) 1.136(5) 0.17(3) Uiso 0.25 1 d PD F 3 H49G H 0.9881 0.3510 1.0968 0.260 Uiso 0.25 1 calc PR F 3 H49H H 0.9753 0.3250 1.1890 0.260 Uiso 0.25 1 calc PR F 3 H49I H 0.9193 0.3947 1.1448 0.260 Uiso 0.25 1 calc PR F 3 C50C C 0.8785(16) 0.2810(18) 1.1014(17) 0.057(7) Uiso 0.25 1 d PD F 3 O51C O 0.901(2) 0.2327(18) 1.0496(18) 0.106(9) Uiso 0.25 1 d PD F 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 0.0645(5) 0.0660(5) 0.0563(5) 0.0009(4) 0.0079(4) -0.0161(4) N2 0.067(3) 0.070(3) 0.050(3) 0.000(2) 0.007(2) -0.014(3) C3 0.061(3) 0.068(4) 0.056(3) -0.003(3) 0.010(3) -0.016(3) C4 0.083(5) 0.083(5) 0.075(5) 0.000(4) 0.001(4) -0.032(4) C5 0.118(7) 0.076(5) 0.077(5) 0.001(4) 0.012(5) -0.039(5) C6 0.107(6) 0.087(5) 0.068(4) 0.012(4) 0.008(4) -0.040(5) C7 0.083(4) 0.079(4) 0.051(3) 0.005(3) 0.010(3) -0.027(4) N8 0.062(3) 0.060(3) 0.058(3) -0.002(2) 0.006(2) -0.008(2) N9 0.070(3) 0.063(3) 0.066(3) -0.001(2) 0.008(3) -0.013(3) C10 0.074(4) 0.070(4) 0.064(4) 0.004(3) 0.003(3) -0.013(3) C11 0.064(4) 0.076(4) 0.058(4) 0.001(3) 0.004(3) 0.004(3) C12 0.063(4) 0.068(4) 0.060(3) 0.000(3) -0.001(3) -0.005(3) I13 0.0928(4) 0.1017(5) 0.0692(3) 0.0111(3) -0.0123(3) 0.0015(3) N14 0.086(4) 0.081(4) 0.050(3) 0.008(3) 0.004(3) -0.029(3) N15 0.078(4) 0.071(4) 0.063(3) 0.002(3) 0.010(3) -0.021(3) C16 0.082(5) 0.079(5) 0.058(4) 0.000(3) 0.004(3) -0.021(4) C17 0.077(5) 0.095(5) 0.055(4) 0.004(3) 0.004(3) -0.023(4) C18 0.100(6) 0.103(6) 0.052(4) 0.007(4) 0.002(4) -0.038(5) I19 0.0965(4) 0.1067(5) 0.0559(3) 0.0019(2) -0.0007(2) -0.0282(3) N20 0.066(3) 0.075(4) 0.053(3) 0.004(2) 0.002(2) -0.016(3) C21 0.062(4) 0.080(4) 0.059(3) 0.001(3) 0.006(3) -0.019(3) C22 0.080(5) 0.089(5) 0.073(5) 0.008(4) 0.009(4) -0.026(4) C23 0.114(7) 0.069(5) 0.120(8) 0.001(5) 0.013(6) -0.027(5) C24 0.102(6) 0.077(5) 0.097(6) -0.006(4) 0.019(5) -0.013(5) C25 0.071(4) 0.069(4) 0.066(4) 0.001(3) 0.007(3) -0.010(3) N26 0.059(3) 0.084(4) 0.061(3) 0.001(3) 0.007(2) -0.019(3) N27 0.069(3) 0.076(4) 0.069(3) -0.002(3) 0.010(3) -0.008(3) C28 0.078(5) 0.084(5) 0.076(5) 0.003(4) 0.013(4) -0.005(4) C29 0.061(4) 0.124(8) 0.078(5) 0.005(5) 0.012(4) 0.000(4) C30 0.067(4) 0.090(5) 0.078(5) -0.003(4) 0.017(3) -0.013(4) I31 0.0987(6) 0.1397(8) 0.1881(10) 0.0005(6) 0.0575(6) 0.0201(5) N32 0.074(4) 0.075(4) 0.069(4) -0.002(3) 0.013(3) 0.002(3) N33 0.069(3) 0.086(4) 0.071(4) -0.001(3) 0.010(3) -0.011(3) C34 0.067(4) 0.114(7) 0.085(5) 0.002(5) 0.018(4) -0.014(4) C35 0.068(4) 0.121(7) 0.073(5) 0.007(5) 0.016(4) 0.014(5) C36 0.081(5) 0.106(7) 0.079(5) -0.005(5) 0.007(4) 0.010(5) I37 0.0943(5) 0.1749(8) 0.0951(5) 0.0160(5) 0.0324(4) 0.0375(5) B43 0.135(14) 0.21(2) 0.092(9) 0.001(11) 0.028(9) -0.013(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N20 2.128(6) . ? Fe1 N2 2.129(6) . ? Fe1 N9 2.168(6) . ? Fe1 N15 2.181(7) . ? Fe1 N33 2.187(7) . ? Fe1 N27 2.194(7) . ? N2 C7 1.326(9) . ? N2 C3 1.337(8) . ? C3 C4 1.374(10) . ? C3 N8 1.404(9) . ? C4 C5 1.392(13) . ? C5 C6 1.380(12) . ? C6 C7 1.389(10) . ? C7 N14 1.402(9) . ? N8 C12 1.353(9) . ? N8 N9 1.364(8) . ? N9 C10 1.316(10) . ? C10 C11 1.419(11) . ? C11 C12 1.347(11) . ? C11 I13 2.069(7) . ? N14 C18 1.341(9) . ? N14 N15 1.383(8) . ? N15 C16 1.323(10) . ? C16 C17 1.390(11) . ? C17 C18 1.354(11) . ? C17 I19 2.070(8) . ? N20 C25 1.312(10) . ? N20 C21 1.340(9) . ? C21 C22 1.387(11) . ? C21 N26 1.406(10) . ? C22 C23 1.381(15) . ? C23 C24 1.350(15) . ? C24 C25 1.381(12) . ? C25 N32 1.416(10) . ? N26 C30 1.344(10) . ? N26 N27 1.369(9) . ? N27 C28 1.306(11) . ? C28 C29 1.418(13) . ? C29 C30 1.354(14) . ? C29 I31 2.085(9) . ? N32 N33 1.339(9) . ? N32 C36 1.370(11) . ? N33 C34 1.349(10) . ? C34 C35 1.364(14) . ? C35 C36 1.342(14) . ? C35 I37 2.083(8) . ? B38A F42A 1.377(16) . ? B38A F40A 1.382(16) . ? B38A F39A 1.382(16) . ? B38A F41A 1.397(16) . ? B38B F39B 1.372(16) . ? B38B F40B 1.379(15) . ? B38B F42B 1.387(16) . ? B38B F41B 1.390(15) . ? B43 F44A 1.305(15) . ? B43 F47A 1.380(15) . ? B43 F45A 1.393(15) . ? B43 F46A 1.452(15) . ? B43 F46B 1.321(15) . ? B43 F45B 1.350(16) . ? B43 F47B 1.417(16) . ? B43 F44B 1.433(17) . ? B43 F45C 1.341(15) . ? B43 F46C 1.347(16) . ? B43 F44C 1.406(16) . ? B43 F47C 1.432(15) . ? C48A C50A 1.55(2) . ? C49A C50A 1.55(2) . ? C50A O51A 1.22(2) . ? C48B C50B 1.548(16) . ? C49B C50B 1.526(16) . ? C50B O51B 1.188(15) . ? C48C C50C 1.528(18) . ? C49C C50C 1.551(18) . ? C50C O51C 1.225(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N20 Fe1 N2 171.1(2) . . ? N20 Fe1 N9 112.0(2) . . ? N2 Fe1 N9 73.6(2) . . ? N20 Fe1 N15 100.8(2) . . ? N2 Fe1 N15 73.3(2) . . ? N9 Fe1 N15 146.9(2) . . ? N20 Fe1 N33 72.5(2) . . ? N2 Fe1 N33 100.5(2) . . ? N9 Fe1 N33 96.4(2) . . ? N15 Fe1 N33 88.8(3) . . ? N20 Fe1 N27 73.8(2) . . ? N2 Fe1 N27 113.1(2) . . ? N9 Fe1 N27 95.2(2) . . ? N15 Fe1 N27 98.3(3) . . ? N33 Fe1 N27 146.3(2) . . ? C7 N2 C3 119.0(6) . . ? C7 N2 Fe1 120.6(4) . . ? C3 N2 Fe1 120.4(4) . . ? N2 C3 C4 122.9(7) . . ? N2 C3 N8 112.7(6) . . ? C4 C3 N8 124.4(6) . . ? C3 C4 C5 116.8(7) . . ? C6 C5 C4 121.7(7) . . ? C5 C6 C7 116.2(8) . . ? N2 C7 C6 123.3(7) . . ? N2 C7 N14 114.0(6) . . ? C6 C7 N14 122.6(7) . . ? C12 N8 N9 111.4(6) . . ? C12 N8 C3 130.0(6) . . ? N9 N8 C3 118.7(5) . . ? C10 N9 N8 105.9(6) . . ? C10 N9 Fe1 139.3(5) . . ? N8 N9 Fe1 114.6(4) . . ? N9 C10 C11 109.6(7) . . ? C12 C11 C10 106.5(6) . . ? C12 C11 I13 127.9(6) . . ? C10 C11 I13 125.6(6) . . ? C11 C12 N8 106.7(6) . . ? C18 N14 N15 110.8(6) . . ? C18 N14 C7 132.0(6) . . ? N15 N14 C7 117.1(6) . . ? C16 N15 N14 104.2(6) . . ? C16 N15 Fe1 140.3(5) . . ? N14 N15 Fe1 114.8(4) . . ? N15 C16 C17 111.8(7) . . ? C18 C17 C16 105.4(7) . . ? C18 C17 I19 128.0(6) . . ? C16 C17 I19 126.5(6) . . ? N14 C18 C17 107.8(7) . . ? C25 N20 C21 117.5(6) . . ? C25 N20 Fe1 122.0(5) . . ? C21 N20 Fe1 120.3(5) . . ? N20 C21 C22 122.7(8) . . ? N20 C21 N26 112.9(6) . . ? C22 C21 N26 124.4(7) . . ? C23 C22 C21 116.5(8) . . ? C24 C23 C22 122.2(9) . . ? C23 C24 C25 116.1(9) . . ? N20 C25 C24 124.9(8) . . ? N20 C25 N32 111.6(6) . . ? C24 C25 N32 123.5(8) . . ? C30 N26 N27 111.7(7) . . ? C30 N26 C21 129.0(7) . . ? N27 N26 C21 119.2(6) . . ? C28 N27 N26 106.1(6) . . ? C28 N27 Fe1 140.3(6) . . ? N26 N27 Fe1 113.5(5) . . ? N27 C28 C29 109.2(8) . . ? C30 C29 C28 107.1(8) . . ? C30 C29 I31 126.2(7) . . ? C28 C29 I31 126.7(8) . . ? N26 C30 C29 105.8(7) . . ? N33 N32 C36 110.6(7) . . ? N33 N32 C25 118.9(6) . . ? C36 N32 C25 130.5(8) . . ? N32 N33 C34 105.5(7) . . ? N32 N33 Fe1 114.6(5) . . ? C34 N33 Fe1 139.3(7) . . ? N33 C34 C35 109.9(8) . . ? C36 C35 C34 107.5(8) . . ? C36 C35 I37 125.9(8) . . ? C34 C35 I37 126.6(7) . . ? C35 C36 N32 106.4(9) . . ? F42A B38A F40A 109.1(13) . . ? F42A B38A F39A 112.9(13) . . ? F40A B38A F39A 108.7(14) . . ? F42A B38A F41A 109.9(14) . . ? F40A B38A F41A 106.5(13) . . ? F39A B38A F41A 109.5(13) . . ? F39B B38B F40B 109.8(13) . . ? F39B B38B F42B 107.5(12) . . ? F40B B38B F42B 110.3(13) . . ? F39B B38B F41B 113.5(13) . . ? F40B B38B F41B 106.4(12) . . ? F42B B38B F41B 109.4(14) . . ? F44A B43 F47A 115.8(13) . . ? F44A B43 F45A 114.8(13) . . ? F47A B43 F45A 108.8(13) . . ? F44A B43 F46A 108.1(13) . . ? F47A B43 F46A 104.7(13) . . ? F45A B43 F46A 103.3(12) . . ? F46B B43 F45B 115.8(16) . . ? F46B B43 F47B 108.4(13) . . ? F45B B43 F47B 110.6(15) . . ? F46B B43 F44B 109.9(15) . . ? F45B B43 F44B 108.2(15) . . ? F47B B43 F44B 103.3(14) . . ? F45C B43 F46C 114.8(16) . . ? F45C B43 F44C 109.1(15) . . ? F46C B43 F44C 111.0(16) . . ? F45C B43 F47C 107.0(13) . . ? F46C B43 F47C 108.8(16) . . ? F44C B43 F47C 105.6(13) . . ? O51A C50A C48A 116(2) . . ? O51A C50A C49A 117(2) . . ? C48A C50A C49A 118(2) . . ? O51B C50B C49B 120.6(16) . . ? O51B C50B C48B 116.9(15) . . ? C49B C50B C48B 121.6(14) . . ? O51C C50C C48C 117.9(19) . . ? O51C C50C C49C 116.4(18) . . ? C48C C50C C49C 120.0(18) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.082 _refine_diff_density_min -1.926 _refine_diff_density_rms 0.138