Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author 'Dr. Malcolm A. Halcrow' _publ_contact_address ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; _publ_contact_author_phone '+44 (0)113 233 6506' _publ_contact_author_fax '+44 (0)113 233 6565' _publ_contact_author_email malcolmh@chem.leeds.ac.uk _publ_requested_journal 'Chemical Communications' _publ_contact_letter ; The following data is for a compound included in a manuscript we have just submitted to the Chemical Communications office. This corresponds to a revised version of submission B007526O. ; #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_requested_journal 'Chemical Communications' _publ_section_title ; An Unusual Abrupt Thermal Spin-State Transition in [FeL~2~][BF~4~]~2~ (L = 2,6-di{pyrazol-1-yl}pyridine). ; loop_ _publ_author_name _publ_author_address 'Joanne M. Holland' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Judith A. McAllister' ; Department of Chemistry, University of Cambridge, Lensfield Road, Cambridge CB2 1EW, UK AND Interdisciplinary Research Centre in Superconductivity, University of Cambridge, Madingley Road, Cambridge CB3 0HE, UK ; 'Zhibao Lu' ; Centre for Self-Organising Molecular Systems, School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Colin A. Kilner' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Mark Thornton-Pett' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Malcolm A. Halcrow' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; #================================================================= data_mh37ht _database_code_CSD 158392 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-[2,6-dipyrazol-1-ylpyridine]iron(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[C22 H18 Fe N10] 2[B F4]' _chemical_formula_sum 'C22 H18 B2 F8 Fe N10' _chemical_formula_weight 651.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.5301(3) _cell_length_b 8.5518(4) _cell_length_c 19.1757(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.9043(24) _cell_angle_gamma 90.00 _cell_volume 1393.70(9) _cell_formula_units_Z 2 _cell_measurement_temperature 375(2) _cell_measurement_reflns_used 15873 _cell_measurement_theta_min 5.42 _cell_measurement_theta_max 27.48 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.628 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8438 _exptl_absorpt_correction_T_max 0.9457 ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 375(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 ; 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_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15873 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 5.42 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6039 _reflns_number_gt 4814 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The F atoms of both anions are disordered over three orientations. For the anion centred on B34: F35-F38, occupancy 0.5 F39-F42, occupancy 0.25 F43-F46, occupancy 0.25 For the anion centred on B47: F48-F51, occupancy 0.5 F52-F55, occupancy 0.25 F56-F59, occupancy 0.25 All B-F distances were restrained to 1.37(2)\%A, and all non-bonded distances within each disorder orientation to 2.24(2)\%A. Attempts to model disorder in the B atoms were unsuccessful. All non-H atoms with occupancy >=0.5 were modeled anisotropically. ; _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^)+(0.0576P)^2^+0.1294P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.163(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.001(17) _refine_ls_number_reflns 6039 _refine_ls_number_parameters 454 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1198 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 0.73853(4) 0.84281(8) 0.748045(19) 0.08062(19) Uani 1 1 d . . . N2 N 0.7226(2) 0.8398(4) 0.63669(11) 0.0736(5) Uani 1 1 d . . . C3 C 0.5961(3) 0.8935(3) 0.59975(15) 0.0773(7) Uani 1 1 d . . . C4 C 0.5834(5) 0.8995(5) 0.52720(19) 0.1008(10) Uani 1 1 d . . . H4 H 0.4933 0.9377 0.5021 0.121 Uiso 1 1 calc R . . C5 C 0.7089(5) 0.8469(7) 0.49414(18) 0.1075(10) Uani 1 1 d . . . H5 H 0.7041 0.8496 0.4455 0.129 Uiso 1 1 calc R . . C6 C 0.8417(5) 0.7902(4) 0.5309(2) 0.0988(11) Uani 1 1 d . . . H6 H 0.9273 0.7548 0.5084 0.119 Uiso 1 1 calc R . . C7 C 0.8424(4) 0.7882(3) 0.60300(17) 0.0790(7) Uani 1 1 d . . . N8 N 0.4782(3) 0.9442(3) 0.64113(14) 0.0809(6) Uani 1 1 d . . . N9 N 0.5043(3) 0.9345(3) 0.71199(14) 0.0824(6) Uani 1 1 d . . . C10 C 0.3742(4) 0.9879(5) 0.7359(2) 0.0974(10) Uani 1 1 d . . . H10 H 0.3563 0.9938 0.7830 0.117 Uiso 1 1 calc R . . C11 C 0.2674(5) 1.0344(5) 0.6809(3) 0.1157(14) Uani 1 1 d . . . H11 H 0.1685 1.0778 0.6846 0.139 Uiso 1 1 calc R . . C12 C 0.3337(4) 1.0049(5) 0.6220(3) 0.1021(11) Uani 1 1 d . . . H12 H 0.2898 1.0224 0.5766 0.123 Uiso 1 1 calc R . . N13 N 0.9686(3) 0.7336(3) 0.64778(16) 0.0868(7) Uani 1 1 d . . . N14 N 0.9595(3) 0.7461(4) 0.71798(16) 0.0909(7) Uani 1 1 d . . . C15 C 1.0901(4) 0.6797(5) 0.7465(3) 0.1097(12) Uani 1 1 d . . . H15 H 1.1182 0.6719 0.7943 0.132 Uiso 1 1 calc R . . C16 C 1.1789(5) 0.6231(6) 0.6941(4) 0.1312(17) Uani 1 1 d . . . H16 H 1.2751 0.5717 0.7007 0.157 Uiso 1 1 calc R . . C17 C 1.1004(4) 0.6564(5) 0.6332(3) 0.1114(13) Uani 1 1 d . . . H17 H 1.1302 0.6315 0.5890 0.134 Uiso 1 1 calc R . . N18 N 0.7370(2) 0.8260(4) 0.85882(12) 0.0723(5) Uani 1 1 d . . . C19 C 0.7896(3) 0.9432(4) 0.89951(15) 0.0777(7) Uani 1 1 d . . . C20 C 0.7883(4) 0.9384(5) 0.97221(18) 0.0947(9) Uani 1 1 d . . . H20 H 0.8245 1.0219 1.0002 0.114 Uiso 1 1 calc R . . C21 C 0.7316(5) 0.8059(6) 1.0003(2) 0.1054(14) Uani 1 1 d . . . H21 H 0.7281 0.7993 1.0486 0.126 Uiso 1 1 calc R . . C22 C 0.6794(4) 0.6817(5) 0.9592(2) 0.0987(10) Uani 1 1 d . . . H22 H 0.6425 0.5905 0.9785 0.118 Uiso 1 1 calc R . . C23 C 0.6844(3) 0.6984(4) 0.88841(17) 0.0816(8) Uani 1 1 d . . . N24 N 0.8445(3) 1.0706(3) 0.86236(13) 0.0791(6) Uani 1 1 d . . . N25 N 0.8382(3) 1.0615(3) 0.79173(14) 0.0837(6) Uani 1 1 d . . . C26 C 0.9045(4) 1.1930(5) 0.7724(2) 0.1003(10) Uani 1 1 d . . . H26 H 0.9161 1.2210 0.7262 0.120 Uiso 1 1 calc R . . C27 C 0.9546(5) 1.2839(5) 0.8306(3) 0.1114(12) Uani 1 1 d . . . H27 H 1.0055 1.3801 0.8307 0.134 Uiso 1 1 calc R . . C28 C 0.9142(4) 1.2037(5) 0.8858(2) 0.1009(10) Uani 1 1 d . . . H28 H 0.9312 1.2344 0.9324 0.121 Uiso 1 1 calc R . . N29 N 0.6324(3) 0.5824(3) 0.83943(18) 0.0918(8) Uani 1 1 d . . . N30 N 0.6480(3) 0.6101(3) 0.77046(16) 0.0908(7) Uani 1 1 d . . . C31 C 0.5944(5) 0.4815(5) 0.7382(3) 0.1118(13) Uani 1 1 d . . . H31 H 0.5924 0.4654 0.6901 0.134 Uiso 1 1 calc R . . C32 C 0.5426(5) 0.3761(6) 0.7840(4) 0.1373(18) Uani 1 1 d . . . H32 H 0.4986 0.2785 0.7735 0.165 Uiso 1 1 calc R . . C33 C 0.5684(5) 0.4426(5) 0.8487(3) 0.1222(15) Uani 1 1 d . . . H33 H 0.5456 0.3988 0.8910 0.147 Uiso 1 1 calc R . . B34 B 0.7957(6) 0.2931(6) 0.5771(2) 0.1034(12) Uani 1 1 d D . . F35 F 0.6743(12) 0.2342(11) 0.6141(5) 0.115(2) Uani 0.50 1 d PD A 1 F36 F 0.7601(11) 0.2145(11) 0.5093(4) 0.150(4) Uani 0.50 1 d PD A 1 F37 F 0.7920(12) 0.4419(6) 0.5670(5) 0.158(3) Uani 0.50 1 d PD A 1 F38 F 0.9334(10) 0.2239(16) 0.6013(4) 0.151(3) Uani 0.50 1 d PD A 1 F39 F 0.714(3) 0.194(3) 0.6166(12) 0.214(15) Uiso 0.25 1 d PD A 2 F40 F 0.9433(15) 0.3129(18) 0.6118(7) 0.129(5) Uiso 0.25 1 d PD A 2 F41 F 0.7804(17) 0.265(2) 0.5096(6) 0.102(4) Uiso 0.25 1 d PD A 2 F42 F 0.723(3) 0.443(2) 0.5871(13) 0.206(12) Uiso 0.25 1 d PD A 2 F43 F 0.6544(16) 0.278(2) 0.6020(10) 0.129(7) Uiso 0.25 1 d PD A 3 F44 F 0.892(2) 0.1709(17) 0.5807(10) 0.151(7) Uiso 0.25 1 d PD A 3 F45 F 0.8008(16) 0.371(2) 0.5161(7) 0.150(4) Uiso 0.25 1 d PD A 3 F46 F 0.8665(17) 0.4092(16) 0.6264(7) 0.153(4) Uiso 0.25 1 d PD A 3 B47 B 0.7426(7) 0.3174(7) 1.0751(3) 0.1216(16) Uani 1 1 d D . . F48 F 0.6509(8) 0.3008(10) 1.0054(3) 0.130(3) Uani 0.50 1 d PD B 4 F49 F 0.6756(8) 0.1996(13) 1.1113(4) 0.132(3) Uani 0.50 1 d PD B 4 F50 F 0.8870(7) 0.3116(16) 1.0683(5) 0.203(5) Uani 0.50 1 d PD B 4 F51 F 0.6813(19) 0.4560(11) 1.1013(4) 0.200(5) Uani 0.50 1 d PD B 4 F52 F 0.8603(15) 0.3960(17) 1.1249(7) 0.148(4) Uiso 0.25 1 d PD B 5 F53 F 0.793(3) 0.338(2) 1.0140(7) 0.189(6) Uiso 0.25 1 d PD B 5 F54 F 0.7353(16) 0.1763(13) 1.1021(7) 0.121(5) Uiso 0.25 1 d PD B 5 F55 F 0.6142(15) 0.4143(16) 1.0837(9) 0.139(5) Uiso 0.25 1 d PD B 5 F56 F 0.646(2) 0.270(2) 1.1211(10) 0.173(10) Uiso 0.25 1 d PD B 6 F57 F 0.8033(19) 0.4606(14) 1.1001(8) 0.134(4) Uiso 0.25 1 d PD B 6 F58 F 0.8858(14) 0.2215(14) 1.0837(7) 0.119(4) Uiso 0.25 1 d PD B 6 F59 F 0.7032(16) 0.3195(15) 1.0067(5) 0.089(3) Uiso 0.25 1 d PD B 6 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 0.0806(3) 0.0910(3) 0.0697(2) -0.0055(2) 0.00335(16) 0.0033(2) N2 0.0734(10) 0.0738(12) 0.0734(11) -0.0007(15) 0.0057(9) -0.0032(14) C3 0.0778(15) 0.0759(17) 0.0774(16) -0.0001(12) 0.0016(13) -0.0091(12) C4 0.114(2) 0.103(2) 0.0822(19) 0.0071(17) -0.0132(18) -0.0108(19) C5 0.140(3) 0.110(2) 0.0732(17) -0.005(2) 0.0127(18) -0.013(3) C6 0.112(3) 0.096(2) 0.093(2) -0.0211(17) 0.036(2) -0.0162(18) C7 0.0772(16) 0.0715(16) 0.0895(19) -0.0100(13) 0.0138(14) -0.0076(12) N8 0.0716(12) 0.0808(15) 0.0893(16) 0.0028(12) 0.0009(11) 0.0010(11) N9 0.0722(12) 0.0836(15) 0.0921(17) -0.0036(13) 0.0122(11) 0.0007(11) C10 0.089(2) 0.089(2) 0.118(3) -0.0051(19) 0.0326(19) -0.0017(17) C11 0.0763(19) 0.094(2) 0.176(5) -0.010(3) 0.007(2) 0.0110(18) C12 0.0798(19) 0.096(3) 0.128(3) 0.010(2) -0.003(2) 0.0101(17) N13 0.0711(13) 0.0830(16) 0.107(2) -0.0172(13) 0.0106(13) -0.0009(11) N14 0.0754(14) 0.0939(18) 0.101(2) -0.0065(14) -0.0060(13) 0.0024(12) C15 0.082(2) 0.102(3) 0.141(3) 0.002(2) -0.016(2) -0.0018(19) C16 0.078(2) 0.114(3) 0.199(5) 0.000(3) 0.000(3) 0.017(2) C17 0.080(2) 0.095(3) 0.162(4) -0.015(2) 0.029(2) 0.0084(17) N18 0.0652(10) 0.0758(15) 0.0757(12) -0.0022(14) 0.0047(9) 0.0036(12) C19 0.0662(13) 0.090(2) 0.0765(16) 0.0002(15) 0.0025(12) 0.0092(14) C20 0.093(2) 0.113(3) 0.0765(19) -0.0057(18) -0.0014(15) 0.0038(19) C21 0.101(2) 0.138(4) 0.0786(19) 0.014(2) 0.0109(17) 0.021(2) C22 0.095(2) 0.107(3) 0.096(2) 0.027(2) 0.0184(17) 0.0067(19) C23 0.0672(14) 0.087(2) 0.091(2) 0.0061(16) 0.0092(13) 0.0101(14) N24 0.0722(12) 0.0864(16) 0.0779(15) -0.0052(12) 0.0014(10) 0.0012(11) N25 0.0808(13) 0.0851(16) 0.0848(16) 0.0077(12) 0.0053(11) 0.0044(12) C26 0.091(2) 0.098(3) 0.113(3) 0.017(2) 0.0143(18) 0.0032(19) C27 0.104(2) 0.089(2) 0.140(3) -0.005(2) 0.004(2) -0.0156(18) C28 0.090(2) 0.103(3) 0.108(3) -0.021(2) 0.0006(18) -0.0177(19) N29 0.0731(14) 0.0798(17) 0.124(2) 0.0032(15) 0.0151(14) 0.0014(12) N30 0.0843(15) 0.0876(17) 0.100(2) -0.0151(14) 0.0060(14) 0.0054(13) C31 0.093(2) 0.089(3) 0.151(4) -0.028(3) -0.008(2) 0.0057(19) C32 0.102(3) 0.091(3) 0.216(6) -0.027(3) -0.003(3) -0.013(2) C33 0.103(2) 0.082(2) 0.184(5) 0.008(3) 0.025(3) -0.008(2) B34 0.109(3) 0.109(3) 0.093(3) 0.005(2) 0.016(2) 0.002(2) F35 0.134(5) 0.090(4) 0.129(5) -0.009(4) 0.065(4) -0.022(4) F36 0.197(8) 0.143(7) 0.118(4) -0.033(4) 0.062(4) -0.048(6) F37 0.198(7) 0.069(3) 0.201(8) 0.006(3) -0.016(6) -0.047(3) F38 0.139(5) 0.203(9) 0.108(4) 0.004(6) 0.001(4) 0.066(6) B47 0.143(4) 0.129(4) 0.095(3) 0.003(3) 0.024(3) -0.026(4) F48 0.106(4) 0.165(7) 0.118(4) 0.028(3) -0.001(3) -0.029(4) F49 0.078(3) 0.172(8) 0.144(5) 0.065(5) 0.001(3) -0.030(4) F50 0.091(3) 0.337(15) 0.184(7) -0.011(9) 0.025(4) -0.087(6) F51 0.299(15) 0.183(8) 0.119(5) -0.048(5) 0.031(7) 0.013(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 N2 2.128(2) . ? Fe1 N18 2.130(2) . ? Fe1 N14 2.181(3) . ? Fe1 N30 2.190(3) . ? Fe1 N25 2.191(3) . ? Fe1 N9 2.202(3) . ? N2 C3 1.322(4) . ? N2 C7 1.330(4) . ? C3 C4 1.387(5) . ? C3 N8 1.402(4) . ? C4 C5 1.366(6) . ? C5 C6 1.371(6) . ? C6 C7 1.382(5) . ? C7 N13 1.398(4) . ? N8 C12 1.358(4) . ? N8 N9 1.361(4) . ? N9 C10 1.318(4) . ? C10 C11 1.392(6) . ? C11 C12 1.330(7) . ? N13 C17 1.354(4) . ? N13 N14 1.359(4) . ? N14 C15 1.326(4) . ? C15 C16 1.395(7) . ? C16 C17 1.326(7) . ? N18 C19 1.325(4) . ? N18 C23 1.326(5) . ? C19 C20 1.396(5) . ? C19 N24 1.404(4) . ? C20 C21 1.361(6) . ? C21 C22 1.374(6) . ? C22 C23 1.369(5) . ? C23 N29 1.411(5) . ? N24 C28 1.343(5) . ? N24 N25 1.353(4) . ? N25 C26 1.326(5) . ? C26 C27 1.396(6) . ? C27 C28 1.332(6) . ? N29 C33 1.333(5) . ? N29 N30 1.361(5) . ? N30 C31 1.324(5) . ? C31 C32 1.359(8) . ? C32 C33 1.365(8) . ? B34 F37 1.287(7) . ? B34 F41 1.312(12) . ? B34 F44 1.327(12) . ? B34 F43 1.341(12) . ? B34 F45 1.348(11) . ? B34 F38 1.361(7) . ? B34 F39 1.363(14) . ? B34 F40 1.383(11) . ? B34 F35 1.398(7) . ? B34 F42 1.441(14) . ? B34 F46 1.465(11) . ? B34 F36 1.472(8) . ? B47 F50 1.250(8) . ? B47 F53 1.294(12) . ? B47 F54 1.317(12) . ? B47 F56 1.322(13) . ? B47 F59 1.326(10) . ? B47 F49 1.375(8) . ? B47 F55 1.395(12) . ? B47 F57 1.398(12) . ? B47 F51 1.406(9) . ? B47 F58 1.468(11) . ? B47 F52 1.486(11) . ? B47 F48 1.496(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N18 173.95(12) . . ? N2 Fe1 N14 73.29(10) . . ? N18 Fe1 N14 108.50(10) . . ? N2 Fe1 N30 101.12(12) . . ? N18 Fe1 N30 73.18(12) . . ? N14 Fe1 N30 91.99(11) . . ? N2 Fe1 N25 112.53(11) . . ? N18 Fe1 N25 73.24(11) . . ? N14 Fe1 N25 96.24(11) . . ? N30 Fe1 N25 146.33(11) . . ? N2 Fe1 N9 73.20(10) . . ? N18 Fe1 N9 104.73(9) . . ? N14 Fe1 N9 146.48(11) . . ? N30 Fe1 N9 93.39(10) . . ? N25 Fe1 N9 97.37(10) . . ? C3 N2 C7 118.8(2) . . ? C3 N2 Fe1 120.8(2) . . ? C7 N2 Fe1 120.4(2) . . ? N2 C3 C4 122.7(3) . . ? N2 C3 N8 113.4(2) . . ? C4 C3 N8 123.9(3) . . ? C5 C4 C3 117.1(3) . . ? C4 C5 C6 121.6(3) . . ? C5 C6 C7 116.8(3) . . ? N2 C7 C6 123.0(3) . . ? N2 C7 N13 113.3(3) . . ? C6 C7 N13 123.7(3) . . ? C12 N8 N9 111.1(3) . . ? C12 N8 C3 130.0(3) . . ? N9 N8 C3 118.8(2) . . ? C10 N9 N8 104.8(3) . . ? C10 N9 Fe1 141.5(3) . . ? N8 N9 Fe1 113.71(17) . . ? N9 C10 C11 110.5(4) . . ? C12 C11 C10 106.9(3) . . ? C11 C12 N8 106.6(4) . . ? C17 N13 N14 111.2(3) . . ? C17 N13 C7 130.2(4) . . ? N14 N13 C7 118.4(2) . . ? C15 N14 N13 104.9(3) . . ? C15 N14 Fe1 140.2(3) . . ? N13 N14 Fe1 114.54(19) . . ? N14 C15 C16 109.9(4) . . ? C17 C16 C15 107.2(4) . . ? C16 C17 N13 106.8(4) . . ? C19 N18 C23 118.7(3) . . ? C19 N18 Fe1 120.4(2) . . ? C23 N18 Fe1 120.9(2) . . ? N18 C19 C20 122.3(3) . . ? N18 C19 N24 113.5(3) . . ? C20 C19 N24 124.2(3) . . ? C21 C20 C19 117.0(4) . . ? C20 C21 C22 121.6(3) . . ? C23 C22 C21 116.9(4) . . ? N18 C23 C22 123.4(3) . . ? N18 C23 N29 113.1(3) . . ? C22 C23 N29 123.5(3) . . ? C28 N24 N25 111.2(3) . . ? C28 N24 C19 130.2(3) . . ? N25 N24 C19 118.5(2) . . ? C26 N25 N24 104.5(3) . . ? C26 N25 Fe1 141.1(3) . . ? N24 N25 Fe1 114.37(19) . . ? N25 C26 C27 110.9(4) . . ? C28 C27 C26 105.5(4) . . ? C27 C28 N24 107.9(4) . . ? C33 N29 N30 111.1(4) . . ? C33 N29 C23 130.6(4) . . ? N30 N29 C23 118.2(3) . . ? C31 N30 N29 104.6(4) . . ? C31 N30 Fe1 140.9(3) . . ? N29 N30 Fe1 114.5(2) . . ? N30 C31 C32 111.5(5) . . ? C31 C32 C33 106.0(4) . . ? N29 C33 C32 106.8(5) . . ? F44 B34 F43 118.3(11) . . ? F44 B34 F45 111.5(10) . . ? F43 B34 F45 117.0(9) . . ? F37 B34 F38 119.4(8) . . ? F41 B34 F39 114.9(12) . . ? F41 B34 F40 120.5(9) . . ? F39 B34 F40 107.1(11) . . ? F37 B34 F35 115.0(8) . . ? F38 B34 F35 109.0(8) . . ? F41 B34 F42 106.7(11) . . ? F39 B34 F42 103.4(12) . . ? F40 B34 F42 102.1(10) . . ? F44 B34 F46 106.3(9) . . ? F43 B34 F46 99.9(10) . . ? F45 B34 F46 100.6(10) . . ? F37 B34 F36 108.5(7) . . ? F38 B34 F36 102.1(7) . . ? F35 B34 F36 100.2(5) . . ? F53 B47 F54 121.0(11) . . ? F56 B47 F59 123.0(11) . . ? F50 B47 F49 118.6(8) . . ? F53 B47 F55 110.6(11) . . ? F54 B47 F55 115.7(9) . . ? F56 B47 F57 105.9(10) . . ? F59 B47 F57 112.5(9) . . ? F50 B47 F51 118.0(9) . . ? F49 B47 F51 104.7(8) . . ? F56 B47 F58 108.2(10) . . ? F59 B47 F58 104.9(8) . . ? F57 B47 F58 99.8(8) . . ? F53 B47 F52 105.1(11) . . ? F54 B47 F52 102.3(9) . . ? F55 B47 F52 98.6(8) . . ? F50 B47 F48 110.3(6) . . ? F49 B47 F48 100.0(5) . . ? F51 B47 F48 102.5(7) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.143 _refine_diff_density_min -0.148 _refine_diff_density_rms 0.027 #=END data_mh37rt _database_code_CSD 158393 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-[2,6-dipyrazol-1-ylpyridine]iron(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[C22 H18 Fe N10] 2[B F4]' _chemical_formula_sum 'C22 H18 B2 F8 Fe N10' _chemical_formula_weight 651.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.4947(2) _cell_length_b 8.5070(2) _cell_length_c 19.0535(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.7050(18) _cell_angle_gamma 90.00 _cell_volume 1370.07(6) _cell_formula_units_Z 2 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used 15406 _cell_measurement_theta_min 3.40 _cell_measurement_theta_max 27.42 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.639 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8414 _exptl_absorpt_correction_T_max 0.9448 _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 ; ? ; _diffrn_ambient_temperature 290(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 ; 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_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15406 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 27.42 _reflns_number_total 5442 _reflns_number_gt 5099 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The F atoms of both anions are disordered over three orientations. For the anion centred on B34: F35-F38, occupancy 0.5 F39-F42, occupancy 0.25 F43-F46, occupancy 0.25 For the anion centred on B47: F48-F51, occupancy 0.5 F52-F55, occupancy 0.25 F56-F59, occupancy 0.25 All B-F distances were restrained to 1.37(2)\%A, and all non-bonded distances within each disorder orientation to 2.24\%A. Attempts to model disorder in the B atoms were unsuccessful. All non-H atoms with occupancy >=0.5 were modeled anisotropically. ; _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^)+(0.0615P)^2^+0.1825P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.179(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.022(15) _refine_ls_number_reflns 5442 _refine_ls_number_parameters 454 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.73833(4) 0.84482(6) 0.747392(16) 0.05782(16) Uani 1 1 d . . . N2 N 0.7219(2) 0.8415(3) 0.63540(10) 0.0531(4) Uani 1 1 d . . . C3 C 0.5939(3) 0.8950(3) 0.59721(13) 0.0554(5) Uani 1 1 d . . . C4 C 0.5797(4) 0.9009(4) 0.52431(15) 0.0701(7) Uani 1 1 d . . . H4 H 0.4881 0.9378 0.4987 0.084 Uiso 1 1 calc R . . C5 C 0.7079(4) 0.8495(5) 0.49125(14) 0.0753(7) Uani 1 1 d . . . H5 H 0.7036 0.8539 0.4423 0.090 Uiso 1 1 calc R . . C6 C 0.8419(4) 0.7920(4) 0.52924(16) 0.0721(8) Uani 1 1 d . . . H6 H 0.9281 0.7565 0.5072 0.087 Uiso 1 1 calc R . . C7 C 0.8421(3) 0.7895(3) 0.60204(14) 0.0578(6) Uani 1 1 d . . . N8 N 0.4742(3) 0.9434(3) 0.63880(12) 0.0577(5) Uani 1 1 d . . . N9 N 0.5021(3) 0.9333(3) 0.71044(12) 0.0593(5) Uani 1 1 d . . . C10 C 0.3706(4) 0.9859(4) 0.73441(18) 0.0698(7) Uani 1 1 d . . . H10 H 0.3538 0.9912 0.7818 0.084 Uiso 1 1 calc R . . C11 C 0.2606(4) 1.0322(4) 0.6788(2) 0.0803(9) Uani 1 1 d . . . H11 H 0.1609 1.0748 0.6823 0.096 Uiso 1 1 calc R . . C12 C 0.3279(4) 1.0029(4) 0.6191(2) 0.0730(8) Uani 1 1 d . . . H12 H 0.2829 1.0200 0.5733 0.088 Uiso 1 1 calc R . . N13 N 0.9693(3) 0.7342(3) 0.64808(14) 0.0616(5) Uani 1 1 d . . . N14 N 0.9604(3) 0.7477(3) 0.71916(14) 0.0653(6) Uani 1 1 d . . . C15 C 1.0904(4) 0.6790(4) 0.7488(2) 0.0806(9) Uani 1 1 d . . . H15 H 1.1185 0.6723 0.7972 0.097 Uiso 1 1 calc R . . C16 C 1.1790(4) 0.6185(5) 0.6976(3) 0.0956(12) Uani 1 1 d . . . H16 H 1.2740 0.5638 0.7053 0.115 Uiso 1 1 calc R . . C17 C 1.1012(4) 0.6539(4) 0.6348(2) 0.0814(9) Uani 1 1 d . . . H17 H 1.1318 0.6283 0.5907 0.098 Uiso 1 1 calc R . . N18 N 0.7355(2) 0.8253(3) 0.85854(10) 0.0529(5) Uani 1 1 d . . . C19 C 0.7871(3) 0.9419(3) 0.90095(13) 0.0551(5) Uani 1 1 d . . . C20 C 0.7860(4) 0.9360(4) 0.97362(15) 0.0676(7) Uani 1 1 d . . . H20 H 0.8227 1.0193 1.0023 0.081 Uiso 1 1 calc R . . C21 C 0.7279(4) 0.8005(4) 1.00134(16) 0.0741(9) Uani 1 1 d . . . H21 H 0.7238 0.7927 1.0498 0.089 Uiso 1 1 calc R . . C22 C 0.6759(4) 0.6766(4) 0.95869(16) 0.0699(7) Uani 1 1 d . . . H22 H 0.6382 0.5845 0.9773 0.084 Uiso 1 1 calc R . . C23 C 0.6822(3) 0.6953(3) 0.88720(15) 0.0586(6) Uani 1 1 d . . . N24 N 0.8445(3) 1.0708(3) 0.86434(11) 0.0579(5) Uani 1 1 d . . . N25 N 0.8394(3) 1.0626(3) 0.79277(12) 0.0609(5) Uani 1 1 d . . . C26 C 0.9079(4) 1.1942(4) 0.77456(18) 0.0711(7) Uani 1 1 d . . . H26 H 0.9217 1.2222 0.7284 0.085 Uiso 1 1 calc R . . C27 C 0.9564(4) 1.2850(4) 0.8333(2) 0.0812(9) Uani 1 1 d . . . H27 H 1.0068 1.3822 0.8340 0.097 Uiso 1 1 calc R . . C28 C 0.9153(4) 1.2029(4) 0.88947(18) 0.0737(8) Uani 1 1 d . . . H28 H 0.9328 1.2325 0.9366 0.088 Uiso 1 1 calc R . . N29 N 0.6318(3) 0.5798(3) 0.83678(14) 0.0634(5) Uani 1 1 d . . . N30 N 0.6496(3) 0.6098(3) 0.76781(13) 0.0651(6) Uani 1 1 d . . . C31 C 0.5966(4) 0.4795(4) 0.7337(2) 0.0792(9) Uani 1 1 d . . . H31 H 0.5956 0.4648 0.6853 0.095 Uiso 1 1 calc R . . C32 C 0.5440(4) 0.3708(4) 0.7790(3) 0.0934(11) Uani 1 1 d . . . H32 H 0.5011 0.2724 0.7676 0.112 Uiso 1 1 calc R . . C33 C 0.5681(4) 0.4375(4) 0.8449(3) 0.0856(10) Uani 1 1 d . . . H33 H 0.5446 0.3925 0.8871 0.103 Uiso 1 1 calc R . . B34 B 0.7968(5) 0.2867(5) 0.5771(2) 0.0726(9) Uani 1 1 d D . . F35 F 0.6829(15) 0.2294(13) 0.6176(5) 0.084(3) Uani 0.50 1 d PD A 1 F36 F 0.7637(13) 0.2134(10) 0.5096(4) 0.118(4) Uani 0.50 1 d PD A 1 F37 F 0.7820(15) 0.4425(8) 0.5676(7) 0.146(5) Uani 0.50 1 d PD A 1 F38 F 0.9445(8) 0.2505(17) 0.6056(4) 0.131(6) Uani 0.50 1 d PD A 1 F39 F 0.690(3) 0.223(3) 0.6153(12) 0.134(13) Uiso 0.25 1 d PD A 2 F40 F 0.948(2) 0.253(3) 0.6035(13) 0.186(17) Uiso 0.25 1 d PD A 2 F41 F 0.7716(14) 0.243(2) 0.5059(6) 0.059(2) Uiso 0.25 1 d PD A 2 F42 F 0.780(2) 0.4498(14) 0.5755(10) 0.086(4) Uiso 0.25 1 d PD A 2 F43 F 0.6532(15) 0.254(2) 0.6015(9) 0.087(6) Uiso 0.25 1 d PD A 3 F44 F 0.9023(15) 0.1679(13) 0.5957(7) 0.106(5) Uiso 0.25 1 d PD A 3 F45 F 0.7912(15) 0.3146(19) 0.5104(5) 0.120(5) Uiso 0.25 1 d PD A 3 F46 F 0.858(2) 0.4167(17) 0.6166(9) 0.167(6) Uiso 0.25 1 d PD A 3 B47 B 0.7368(6) 0.3110(5) 1.0739(2) 0.0863(12) Uani 1 1 d D . . F48 F 0.6583(9) 0.2983(9) 1.0018(3) 0.076(2) Uani 0.50 1 d PD B 4 F49 F 0.6743(8) 0.1903(11) 1.1096(4) 0.085(2) Uani 0.50 1 d PD B 4 F50 F 0.8905(6) 0.2952(12) 1.0677(4) 0.124(3) Uani 0.50 1 d PD B 4 F51 F 0.6932(19) 0.4530(9) 1.0993(4) 0.160(5) Uani 0.50 1 d PD B 4 F52 F 0.8813(17) 0.374(2) 1.1020(9) 0.169(7) Uiso 0.25 1 d PD B 5 F53 F 0.7223(17) 0.3180(16) 1.0051(5) 0.090(4) Uiso 0.25 1 d PD B 5 F54 F 0.7198(16) 0.1651(14) 1.1012(8) 0.093(5) Uiso 0.25 1 d PD B 5 F55 F 0.6265(17) 0.4121(16) 1.1000(8) 0.113(5) Uiso 0.25 1 d PD B 5 F56 F 0.6564(18) 0.2514(16) 1.1258(7) 0.104(6) Uiso 0.25 1 d PD B 6 F57 F 0.7880(18) 0.4602(15) 1.0963(9) 0.120(5) Uiso 0.25 1 d PD B 6 F58 F 0.8873(15) 0.2251(15) 1.0789(8) 0.099(4) Uiso 0.25 1 d PD B 6 F59 F 0.663(3) 0.306(3) 1.0101(8) 0.133(13) Uiso 0.25 1 d PD B 6 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 0.0592(2) 0.0662(2) 0.04744(19) -0.00397(16) 0.00212(12) 0.00314(19) N2 0.0521(9) 0.0535(10) 0.0535(9) -0.0021(12) 0.0049(7) -0.0009(12) C3 0.0542(13) 0.0561(13) 0.0551(13) 0.0006(10) 0.0017(10) -0.0061(10) C4 0.0774(18) 0.0717(17) 0.0583(14) 0.0038(12) -0.0078(13) -0.0080(14) C5 0.100(2) 0.0754(17) 0.0515(12) -0.0043(16) 0.0107(12) -0.010(2) C6 0.0805(19) 0.0748(18) 0.0647(16) -0.0138(13) 0.0252(14) -0.0127(14) C7 0.0591(14) 0.0536(12) 0.0617(14) -0.0081(10) 0.0115(11) -0.0064(10) N8 0.0516(11) 0.0568(12) 0.0639(12) 0.0041(9) 0.0011(9) 0.0013(9) N9 0.0548(11) 0.0599(12) 0.0636(12) -0.0015(10) 0.0089(9) -0.0010(9) C10 0.0661(17) 0.0630(16) 0.0834(19) -0.0056(14) 0.0230(14) 0.0008(13) C11 0.0547(16) 0.0692(18) 0.117(3) -0.0059(18) 0.0081(16) 0.0069(14) C12 0.0603(16) 0.0622(17) 0.094(2) 0.0082(15) -0.0041(15) 0.0067(13) N13 0.0515(11) 0.0600(12) 0.0738(14) -0.0066(10) 0.0092(9) 0.0004(9) N14 0.0548(12) 0.0686(14) 0.0705(14) -0.0047(11) -0.0027(10) 0.0022(10) C15 0.0614(17) 0.074(2) 0.102(2) 0.0077(18) -0.0126(16) -0.0022(15) C16 0.0563(18) 0.087(2) 0.142(4) 0.000(2) 0.001(2) 0.0145(17) C17 0.0636(18) 0.0681(18) 0.116(3) -0.0102(17) 0.0246(18) 0.0058(14) N18 0.0476(9) 0.0587(13) 0.0524(9) 0.0002(10) 0.0045(7) 0.0029(10) C19 0.0506(12) 0.0599(14) 0.0542(12) -0.0006(11) 0.0025(9) 0.0053(10) C20 0.0674(16) 0.0774(19) 0.0567(14) -0.0057(13) -0.0001(12) 0.0035(14) C21 0.0740(18) 0.095(3) 0.0530(14) 0.0073(14) 0.0069(12) 0.0105(15) C22 0.0681(17) 0.0753(18) 0.0673(17) 0.0129(14) 0.0110(12) 0.0016(14) C23 0.0486(13) 0.0622(14) 0.0646(14) 0.0035(12) 0.0046(10) 0.0048(11) N24 0.0534(11) 0.0628(13) 0.0567(12) -0.0034(9) 0.0019(8) -0.0001(9) N25 0.0591(12) 0.0670(13) 0.0562(12) 0.0032(10) 0.0043(9) 0.0051(10) C26 0.0703(18) 0.0665(17) 0.0774(18) 0.0123(14) 0.0107(13) 0.0019(14) C27 0.0724(19) 0.0729(18) 0.098(2) -0.0022(17) 0.0064(16) -0.0123(15) C28 0.0657(17) 0.0776(19) 0.0770(18) -0.0133(15) 0.0024(13) -0.0130(15) N29 0.0543(12) 0.0580(13) 0.0785(15) 0.0000(11) 0.0095(10) 0.0025(10) N30 0.0598(13) 0.0647(13) 0.0704(15) -0.0101(11) 0.0038(10) 0.0046(11) C31 0.0668(18) 0.0697(19) 0.098(2) -0.0203(17) -0.0055(16) 0.0063(15) C32 0.076(2) 0.062(2) 0.140(3) -0.020(2) -0.0014(19) -0.0086(16) C33 0.0710(19) 0.0566(17) 0.130(3) 0.0066(18) 0.0139(19) -0.0048(14) B34 0.078(2) 0.073(2) 0.0677(19) 0.0044(15) 0.0129(16) -0.0034(16) F35 0.103(5) 0.079(4) 0.075(4) -0.011(3) 0.044(4) -0.024(4) F36 0.180(8) 0.099(6) 0.084(4) -0.019(3) 0.056(4) -0.035(4) F37 0.195(9) 0.057(3) 0.169(9) 0.022(3) -0.065(6) -0.049(4) F38 0.070(3) 0.239(15) 0.085(4) 0.061(6) 0.009(2) 0.047(5) B47 0.097(3) 0.092(3) 0.072(2) 0.0063(19) 0.0175(19) -0.014(2) F48 0.073(4) 0.095(4) 0.060(2) 0.0187(19) 0.0060(17) -0.009(2) F49 0.055(3) 0.118(6) 0.082(4) 0.041(4) 0.002(2) -0.018(3) F50 0.070(3) 0.198(8) 0.105(4) -0.025(5) 0.020(2) -0.063(4) F51 0.296(16) 0.105(5) 0.093(4) -0.019(3) 0.087(8) 0.000(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.1248(19) . ? Fe1 N18 2.127(2) . ? Fe1 N14 2.175(3) . ? Fe1 N25 2.184(3) . ? Fe1 N30 2.185(3) . ? Fe1 N9 2.193(2) . ? N2 C3 1.327(3) . ? N2 C7 1.331(3) . ? C3 C4 1.383(4) . ? C3 N8 1.412(4) . ? C4 C5 1.382(5) . ? C5 C6 1.377(5) . ? C6 C7 1.387(4) . ? C7 N13 1.403(4) . ? N8 C12 1.360(4) . ? N8 N9 1.365(3) . ? N9 C10 1.326(4) . ? C10 C11 1.398(5) . ? C11 C12 1.345(5) . ? N13 C17 1.357(4) . ? N13 N14 1.369(4) . ? N14 C15 1.326(4) . ? C15 C16 1.390(6) . ? C16 C17 1.341(6) . ? N18 C19 1.327(4) . ? N18 C23 1.332(4) . ? C19 C20 1.387(4) . ? C19 N24 1.412(4) . ? C20 C21 1.379(5) . ? C21 C22 1.376(5) . ? C22 C23 1.378(4) . ? C23 N29 1.410(4) . ? N24 C28 1.340(4) . ? N24 N25 1.362(3) . ? N25 C26 1.324(4) . ? C26 C27 1.389(5) . ? C27 C28 1.352(5) . ? N29 C33 1.341(4) . ? N29 N30 1.362(4) . ? N30 C31 1.340(4) . ? C31 C32 1.370(6) . ? C32 C33 1.375(6) . ? B34 F45 1.289(10) . ? B34 F39 1.333(14) . ? B34 F37 1.342(8) . ? B34 F38 1.353(7) . ? B34 F40 1.365(14) . ? B34 F44 1.374(11) . ? B34 F43 1.376(12) . ? B34 F35 1.385(7) . ? B34 F42 1.395(12) . ? B34 F41 1.401(11) . ? B34 F46 1.408(12) . ? B34 F36 1.431(8) . ? B47 F53 1.305(10) . ? B47 F59 1.312(13) . ? B47 F50 1.329(7) . ? B47 F56 1.356(12) . ? B47 F54 1.359(11) . ? B47 F51 1.366(8) . ? B47 F49 1.368(6) . ? B47 F57 1.395(12) . ? B47 F52 1.396(12) . ? B47 F55 1.399(12) . ? B47 F58 1.467(12) . ? B47 F48 1.470(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N18 173.15(10) . . ? N2 Fe1 N14 73.65(9) . . ? N18 Fe1 N14 108.21(9) . . ? N2 Fe1 N25 113.14(9) . . ? N18 Fe1 N25 73.44(9) . . ? N14 Fe1 N25 95.95(9) . . ? N2 Fe1 N30 100.21(10) . . ? N18 Fe1 N30 73.31(10) . . ? N14 Fe1 N30 91.12(10) . . ? N25 Fe1 N30 146.58(9) . . ? N2 Fe1 N9 73.47(8) . . ? N18 Fe1 N9 104.24(8) . . ? N14 Fe1 N9 147.08(9) . . ? N25 Fe1 N9 98.46(9) . . ? N30 Fe1 N9 92.88(9) . . ? C3 N2 C7 118.5(2) . . ? C3 N2 Fe1 120.97(17) . . ? C7 N2 Fe1 120.47(17) . . ? N2 C3 C4 123.3(3) . . ? N2 C3 N8 112.9(2) . . ? C4 C3 N8 123.8(2) . . ? C5 C4 C3 116.9(3) . . ? C6 C5 C4 121.4(3) . . ? C5 C6 C7 116.7(3) . . ? N2 C7 C6 123.2(3) . . ? N2 C7 N13 113.1(2) . . ? C6 C7 N13 123.7(3) . . ? C12 N8 N9 111.2(2) . . ? C12 N8 C3 130.1(3) . . ? N9 N8 C3 118.7(2) . . ? C10 N9 N8 104.8(2) . . ? C10 N9 Fe1 141.3(2) . . ? N8 N9 Fe1 113.89(16) . . ? N9 C10 C11 110.9(3) . . ? C12 C11 C10 106.3(3) . . ? C11 C12 N8 106.8(3) . . ? C17 N13 N14 110.8(3) . . ? C17 N13 C7 130.6(3) . . ? N14 N13 C7 118.4(2) . . ? C15 N14 N13 105.0(3) . . ? C15 N14 Fe1 140.2(3) . . ? N13 N14 Fe1 114.30(17) . . ? N14 C15 C16 110.5(4) . . ? C17 C16 C15 106.9(3) . . ? C16 C17 N13 106.8(4) . . ? C19 N18 C23 118.5(2) . . ? C19 N18 Fe1 120.81(19) . . ? C23 N18 Fe1 120.73(19) . . ? N18 C19 C20 123.1(3) . . ? N18 C19 N24 112.9(2) . . ? C20 C19 N24 124.0(3) . . ? C21 C20 C19 116.8(3) . . ? C22 C21 C20 121.3(3) . . ? C21 C22 C23 117.0(3) . . ? N18 C23 C22 123.3(3) . . ? N18 C23 N29 113.0(2) . . ? C22 C23 N29 123.7(3) . . ? C28 N24 N25 111.7(2) . . ? C28 N24 C19 129.7(2) . . ? N25 N24 C19 118.5(2) . . ? C26 N25 N24 104.3(2) . . ? C26 N25 Fe1 141.2(2) . . ? N24 N25 Fe1 114.35(17) . . ? N25 C26 C27 111.2(3) . . ? C28 C27 C26 105.7(3) . . ? N24 C28 C27 107.0(3) . . ? C33 N29 N30 111.4(3) . . ? C33 N29 C23 130.4(3) . . ? N30 N29 C23 118.1(2) . . ? C31 N30 N29 104.4(3) . . ? C31 N30 Fe1 140.9(3) . . ? N29 N30 Fe1 114.62(18) . . ? N30 C31 C32 111.6(3) . . ? C31 C32 C33 105.6(3) . . ? N29 C33 C32 107.0(4) . . ? F37 B34 F38 110.5(8) . . ? F39 B34 F40 112.3(13) . . ? F45 B34 F44 110.5(8) . . ? F45 B34 F43 115.0(9) . . ? F44 B34 F43 110.0(9) . . ? F37 B34 F35 111.1(8) . . ? F38 B34 F35 111.6(7) . . ? F39 B34 F42 110.1(12) . . ? F40 B34 F42 107.9(13) . . ? F39 B34 F41 112.0(12) . . ? F40 B34 F41 110.5(12) . . ? F42 B34 F41 103.6(9) . . ? F45 B34 F46 110.9(9) . . ? F44 B34 F46 104.1(9) . . ? F43 B34 F46 105.7(10) . . ? F37 B34 F36 107.6(7) . . ? F38 B34 F36 110.7(7) . . ? F35 B34 F36 105.2(6) . . ? F59 B47 F56 115.7(13) . . ? F53 B47 F54 115.1(9) . . ? F50 B47 F51 115.1(8) . . ? F50 B47 F49 113.7(6) . . ? F51 B47 F49 110.8(7) . . ? F59 B47 F57 114.9(13) . . ? F56 B47 F57 106.4(9) . . ? F53 B47 F52 111.0(9) . . ? F54 B47 F52 109.1(10) . . ? F53 B47 F55 109.2(9) . . ? F54 B47 F55 108.9(8) . . ? F52 B47 F55 102.8(10) . . ? F59 B47 F58 112.2(12) . . ? F56 B47 F58 105.4(8) . . ? F57 B47 F58 100.9(8) . . ? F50 B47 F48 105.5(5) . . ? F51 B47 F48 106.4(6) . . ? F49 B47 F48 104.3(5) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.205 _refine_diff_density_min -0.197 _refine_diff_density_rms 0.035 #=END data_mh37240 _database_code_CSD 158394 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-[2,6-dipyrazol-1-ylpyridine]iron(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[C22 H18 Fe N10] 2[B F4]' _chemical_formula_sum 'C22 H18 B2 F8 Fe N10' _chemical_formula_weight 651.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.4977(3) _cell_length_b 8.5665(3) _cell_length_c 18.4299(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.0931(12) _cell_angle_gamma 90.00 _cell_volume 1328.25(9) _cell_formula_units_Z 2 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 10234 _cell_measurement_theta_min 1.12 _cell_measurement_theta_max 27.53 _exptl_crystal_description Plate _exptl_crystal_colour 'Dark brown' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.659 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7427 _exptl_absorpt_correction_T_max 0.9678 _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 ; ? ; _diffrn_ambient_temperature 240(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 ; 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_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10234 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 27.53 _reflns_number_total 5538 _reflns_number_gt 4656 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The F atoms of both anions are disordered over three orientations. The anion centred on B34 is disordered by rotation about the B34-F35 bond: F36-F38, occupancy 0.5 F39-F41, occupancy 0.25 F42-F44, occupancy 0.25 The anion centred on B45 is disordered by rotation about the B45-F46 bond: F46-F48, occupancy 0.4 F49-F51, occupancy 0.3 F52-F55, occupancy 0.3 All B-F distances were restrained to 1.39(2)\%A, and all non-bonded distances within each disorder orientation to 2.27\%A. All non-H atoms with occupancy >0.5 were modeled anisotropically. ; _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^)+(0.0524P)^2^+0.5454P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.024(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(19) _refine_ls_number_reflns 5538 _refine_ls_number_parameters 408 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1240 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.005 _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 0.71469(6) 0.84152(6) 0.74661(3) 0.03450(16) Uani 1 1 d . . . N2 N 0.7092(4) 0.8607(5) 0.64394(16) 0.0359(7) Uani 1 1 d . . . C3 C 0.5816(5) 0.9209(5) 0.6024(2) 0.0405(9) Uani 1 1 d . . . C4 C 0.5717(6) 0.9346(6) 0.5279(2) 0.0476(10) Uani 1 1 d . . . H4 H 0.4813 0.9774 0.4996 0.057 Uiso 1 1 calc R . . C5 C 0.6995(6) 0.8834(5) 0.4960(2) 0.0509(12) Uani 1 1 d . . . H5 H 0.6962 0.8921 0.4449 0.061 Uiso 1 1 calc R . . C6 C 0.8320(5) 0.8197(6) 0.5370(2) 0.0467(10) Uani 1 1 d . . . H6 H 0.9190 0.7846 0.5151 0.056 Uiso 1 1 calc R . . C7 C 0.8312(5) 0.8097(4) 0.6117(2) 0.0372(9) Uani 1 1 d . . . N8 N 0.4662(4) 0.9649(4) 0.64601(18) 0.0398(7) Uani 1 1 d . . . N9 N 0.5017(4) 0.9360(4) 0.72070(18) 0.0379(7) Uani 1 1 d . . . C10 C 0.3742(5) 0.9841(6) 0.7484(3) 0.0467(10) Uani 1 1 d . . . H10 H 0.3625 0.9792 0.7983 0.056 Uiso 1 1 calc R . . C11 C 0.2596(6) 1.0429(6) 0.6934(3) 0.0521(11) Uani 1 1 d . . . H11 H 0.1599 1.0843 0.6996 0.062 Uiso 1 1 calc R . . C12 C 0.3194(5) 1.0288(5) 0.6296(3) 0.0478(11) Uani 1 1 d . . . H12 H 0.2690 1.0578 0.5829 0.057 Uiso 1 1 calc R . . N13 N 0.9503(4) 0.7464(4) 0.66381(18) 0.0385(7) Uani 1 1 d . . . N14 N 0.9236(4) 0.7526(4) 0.73568(17) 0.0381(7) Uani 1 1 d . . . C15 C 1.0487(5) 0.6848(5) 0.7732(2) 0.0442(10) Uani 1 1 d . . . H15 H 1.0641 0.6725 0.8244 0.053 Uiso 1 1 calc R . . C16 C 1.1543(6) 0.6341(6) 0.7277(3) 0.0557(12) Uani 1 1 d . . . H16 H 1.2512 0.5821 0.7417 0.067 Uiso 1 1 calc R . . C17 C 1.0898(5) 0.6743(6) 0.6589(3) 0.0498(11) Uani 1 1 d . . . H17 H 1.1339 0.6557 0.6157 0.060 Uiso 1 1 calc R . . N18 N 0.7203(4) 0.8154(4) 0.84961(17) 0.0371(8) Uani 1 1 d . . . C19 C 0.7786(5) 0.9269(5) 0.8963(2) 0.0368(8) Uani 1 1 d . . . C20 C 0.7866(5) 0.9137(6) 0.9703(2) 0.0449(10) Uani 1 1 d . . . H20 H 0.8277 0.9941 1.0022 0.054 Uiso 1 1 calc R . . C21 C 0.7308(6) 0.7747(6) 0.9961(2) 0.0475(11) Uani 1 1 d . . . H21 H 0.7342 0.7613 1.0470 0.057 Uiso 1 1 calc R . . C22 C 0.6702(5) 0.6546(6) 0.9496(2) 0.0477(10) Uani 1 1 d . . . H22 H 0.6336 0.5604 0.9673 0.057 Uiso 1 1 calc R . . C23 C 0.6671(5) 0.6824(5) 0.8757(2) 0.0377(9) Uani 1 1 d . . . N24 N 0.8322(4) 1.0544(4) 0.85819(18) 0.0398(8) Uani 1 1 d . . . N25 N 0.8125(4) 1.0424(4) 0.78199(18) 0.0376(7) Uani 1 1 d . . . C26 C 0.8776(5) 1.1716(5) 0.7601(2) 0.0452(10) Uani 1 1 d . . . H26 H 0.8827 1.1970 0.7109 0.054 Uiso 1 1 calc R . . C27 C 0.9384(6) 1.2659(6) 0.8203(3) 0.0517(11) Uani 1 1 d . . . H27 H 0.9894 1.3630 0.8191 0.062 Uiso 1 1 calc R . . C28 C 0.9075(6) 1.1863(6) 0.8805(3) 0.0507(11) Uani 1 1 d . . . H28 H 0.9346 1.2186 0.9294 0.061 Uiso 1 1 calc R . . N29 N 0.6120(4) 0.5783(4) 0.81824(19) 0.0417(8) Uani 1 1 d . . . N30 N 0.6250(4) 0.6292(4) 0.74879(18) 0.0391(7) Uani 1 1 d . . . C31 C 0.5760(5) 0.5099(5) 0.7056(3) 0.0472(10) Uani 1 1 d . . . H31 H 0.5723 0.5098 0.6544 0.057 Uiso 1 1 calc R . . C32 C 0.5311(6) 0.3857(5) 0.7460(3) 0.0541(12) Uani 1 1 d . . . H32 H 0.4915 0.2888 0.7278 0.065 Uiso 1 1 calc R . . C33 C 0.5556(5) 0.4317(5) 0.8178(3) 0.0507(11) Uani 1 1 d . . . H33 H 0.5368 0.3726 0.8587 0.061 Uiso 1 1 calc R . . B34 B 0.8026(6) 0.3042(6) 0.5604(3) 0.0531(14) Uani 1 1 d D . . F35 F 0.6827(4) 0.2581(4) 0.59893(15) 0.0640(8) Uani 1 1 d D A . F36 F 0.7739(12) 0.2723(11) 0.4874(4) 0.061(3) Uiso 0.50 1 d PD A 1 F37 F 0.8000(13) 0.4705(8) 0.5673(6) 0.067(3) Uiso 0.50 1 d PD A 1 F38 F 0.9474(9) 0.2473(13) 0.5919(5) 0.061(3) Uiso 0.50 1 d PD A 1 F39 F 0.9571(13) 0.2903(17) 0.6031(8) 0.062(5) Uiso 0.25 1 d PD A 2 F40 F 0.8046(16) 0.2321(15) 0.4953(5) 0.046(3) Uiso 0.25 1 d PD A 2 F41 F 0.785(2) 0.4705(13) 0.5497(10) 0.057(5) Uiso 0.25 1 d PD A 2 F42 F 0.9225(12) 0.1958(14) 0.5847(6) 0.047(3) Uiso 0.25 1 d PD A 3 F43 F 0.7362(13) 0.2398(13) 0.4846(4) 0.031(3) Uiso 0.25 1 d PD A 3 F44 F 0.8470(16) 0.4482(12) 0.5521(8) 0.057(4) Uiso 0.25 1 d PD A 3 B45 B 0.7210(7) 0.2839(7) 1.0550(3) 0.0570(14) Uani 1 1 d D . . F46 F 0.6435(4) 0.2728(4) 0.98426(14) 0.0648(8) Uani 1 1 d D B . F47 F 0.6814(15) 0.1447(11) 1.0924(6) 0.040(3) Uiso 0.40 1 d PD B 1 F48 F 0.8828(9) 0.2805(16) 1.0518(5) 0.044(2) Uiso 0.40 1 d PD B 1 F49 F 0.6760(15) 0.4132(10) 1.0883(5) 0.058(3) Uiso 0.40 1 d PD B 1 F50 F 0.8916(11) 0.2323(15) 1.0556(6) 0.056(4) Uiso 0.30 1 d PD B 2 F51 F 0.7418(16) 0.4377(12) 1.0866(7) 0.081(4) Uiso 0.30 1 d PD B 2 F52 F 0.6715(11) 0.1933(12) 1.1061(5) 0.044(2) Uiso 0.30 1 d PD B 2 F53 F 0.8688(11) 0.3316(17) 1.0542(6) 0.066(4) Uiso 0.30 1 d PD B 3 F54 F 0.703(2) 0.1505(19) 1.0935(10) 0.071(9) Uiso 0.30 1 d PD B 3 F55 F 0.6264(14) 0.4079(12) 1.0811(6) 0.056(4) Uiso 0.30 1 d PD B 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 0.0350(3) 0.0390(3) 0.0293(2) -0.0001(2) 0.00373(18) 0.0010(3) N2 0.0367(16) 0.0375(19) 0.0331(15) 0.0012(15) 0.0030(12) 0.0001(16) C3 0.041(2) 0.040(2) 0.040(2) 0.0019(17) 0.0017(17) -0.0016(17) C4 0.052(3) 0.055(3) 0.034(2) 0.0053(19) -0.0003(18) 0.000(2) C5 0.065(3) 0.056(3) 0.032(2) -0.0001(17) 0.008(2) -0.005(2) C6 0.058(2) 0.048(3) 0.0360(19) -0.0044(19) 0.0144(18) -0.001(2) C7 0.041(2) 0.034(3) 0.0364(19) -0.0028(14) 0.0046(16) -0.0051(15) N8 0.0394(18) 0.0450(19) 0.0339(17) 0.0000(14) 0.0010(14) 0.0010(15) N9 0.0395(18) 0.0377(19) 0.0366(18) 0.0006(13) 0.0055(14) -0.0004(14) C10 0.041(2) 0.051(3) 0.049(3) -0.0021(19) 0.012(2) -0.0001(19) C11 0.043(2) 0.047(3) 0.066(3) 0.000(2) 0.007(2) 0.0038(19) C12 0.043(2) 0.041(2) 0.055(3) 0.0000(19) -0.004(2) 0.0058(18) N13 0.0392(18) 0.0385(18) 0.0380(18) -0.0023(14) 0.0063(14) -0.0029(14) N14 0.0382(17) 0.0420(19) 0.0331(17) -0.0013(14) 0.0020(14) 0.0008(14) C15 0.040(2) 0.045(2) 0.046(2) 0.0047(18) 0.0006(19) 0.0012(18) C16 0.042(2) 0.056(3) 0.069(3) 0.005(2) 0.007(2) 0.010(2) C17 0.045(2) 0.051(3) 0.056(3) -0.002(2) 0.016(2) 0.0052(19) N18 0.0337(15) 0.045(2) 0.0329(15) 0.0017(14) 0.0051(12) 0.0015(14) C19 0.033(2) 0.046(2) 0.032(2) 0.0015(16) 0.0039(15) -0.0011(16) C20 0.045(2) 0.057(3) 0.032(2) -0.0036(18) 0.0037(18) 0.0007(19) C21 0.051(3) 0.062(3) 0.029(2) 0.0059(19) 0.0048(18) 0.006(2) C22 0.047(2) 0.059(3) 0.038(2) 0.0100(19) 0.0070(18) 0.004(2) C23 0.034(2) 0.044(2) 0.036(2) 0.0046(16) 0.0045(16) 0.0041(16) N24 0.0401(19) 0.047(2) 0.0313(17) -0.0027(14) 0.0018(14) -0.0022(15) N25 0.0398(18) 0.0430(19) 0.0296(16) 0.0017(14) 0.0033(13) 0.0010(14) C26 0.044(2) 0.046(2) 0.047(2) 0.0067(19) 0.0104(19) 0.0004(18) C27 0.051(3) 0.049(3) 0.055(3) 0.002(2) 0.007(2) -0.007(2) C28 0.050(3) 0.056(3) 0.045(3) -0.012(2) 0.003(2) -0.009(2) N29 0.0423(19) 0.044(2) 0.0393(19) 0.0012(15) 0.0080(15) -0.0001(15) N30 0.0387(18) 0.0425(19) 0.0361(17) 0.0029(14) 0.0055(14) 0.0076(14) C31 0.044(2) 0.048(3) 0.049(3) -0.012(2) 0.005(2) -0.0038(18) C32 0.050(3) 0.046(3) 0.065(3) -0.010(2) 0.006(2) -0.0015(18) C33 0.046(2) 0.046(3) 0.061(3) 0.006(2) 0.010(2) -0.0038(19) B34 0.060(3) 0.063(4) 0.038(3) 0.005(2) 0.013(2) 0.002(2) F35 0.076(2) 0.0679(19) 0.0512(16) -0.0044(14) 0.0211(14) -0.0034(15) B45 0.062(3) 0.068(4) 0.044(3) 0.009(2) 0.019(3) 0.007(3) F46 0.0703(19) 0.079(2) 0.0442(15) 0.0093(13) 0.0045(13) 0.0078(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 Fe1 N2 1.893(3) . ? Fe1 N18 1.905(3) . ? Fe1 N14 1.968(3) . ? Fe1 N30 1.975(4) . ? Fe1 N9 1.979(3) . ? Fe1 N25 1.981(4) . ? N2 C7 1.339(5) . ? N2 C3 1.340(5) . ? C3 C4 1.369(6) . ? C3 N8 1.404(5) . ? C4 C5 1.377(7) . ? C5 C6 1.377(7) . ? C6 C7 1.380(5) . ? C7 N13 1.403(5) . ? N8 C12 1.357(6) . ? N8 N9 1.389(5) . ? N9 C10 1.326(6) . ? C10 C11 1.397(7) . ? C11 C12 1.350(7) . ? N13 C17 1.351(6) . ? N13 N14 1.376(5) . ? N14 C15 1.319(5) . ? C15 C16 1.382(7) . ? C16 C17 1.354(7) . ? N18 C19 1.333(5) . ? N18 C23 1.340(5) . ? C19 C20 1.361(6) . ? C19 N24 1.408(5) . ? C20 C21 1.390(7) . ? C21 C22 1.392(7) . ? C22 C23 1.379(6) . ? C23 N29 1.412(5) . ? N24 C28 1.335(6) . ? N24 N25 1.395(4) . ? N25 C26 1.325(6) . ? C26 C27 1.410(7) . ? C27 C28 1.359(7) . ? N29 C33 1.344(6) . ? N29 N30 1.371(5) . ? N30 C31 1.325(5) . ? C31 C32 1.383(7) . ? C32 C33 1.368(7) . ? B34 F44 1.305(10) . ? B34 F40 1.352(10) . ? B34 F36 1.360(8) . ? B34 F38 1.374(9) . ? B34 F35 1.378(6) . ? B34 F42 1.404(10) . ? B34 F37 1.431(9) . ? B34 F39 1.437(11) . ? B34 F41 1.443(12) . ? B34 F43 1.533(9) . ? B45 F53 1.323(10) . ? B45 F52 1.333(9) . ? B45 F49 1.347(9) . ? B45 F54 1.364(12) . ? B45 F46 1.380(6) . ? B45 F48 1.384(9) . ? B45 F51 1.441(11) . ? B45 F47 1.441(9) . ? B45 F55 1.454(10) . ? B45 F50 1.514(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N18 178.25(18) . . ? N2 Fe1 N14 80.05(14) . . ? N18 Fe1 N14 99.21(14) . . ? N2 Fe1 N30 98.34(15) . . ? N18 Fe1 N30 80.06(15) . . ? N14 Fe1 N30 90.11(15) . . ? N2 Fe1 N9 80.22(14) . . ? N18 Fe1 N9 100.50(14) . . ? N14 Fe1 N9 160.26(13) . . ? N30 Fe1 N9 92.24(14) . . ? N2 Fe1 N25 101.75(15) . . ? N18 Fe1 N25 79.83(15) . . ? N14 Fe1 N25 91.57(15) . . ? N30 Fe1 N25 159.82(13) . . ? N9 Fe1 N25 92.92(14) . . ? C7 N2 C3 119.1(3) . . ? C7 N2 Fe1 120.3(3) . . ? C3 N2 Fe1 120.6(3) . . ? N2 C3 C4 122.5(4) . . ? N2 C3 N8 110.5(3) . . ? C4 C3 N8 127.1(4) . . ? C3 C4 C5 117.4(4) . . ? C4 C5 C6 121.7(4) . . ? C5 C6 C7 116.9(4) . . ? N2 C7 C6 122.4(4) . . ? N2 C7 N13 110.5(3) . . ? C6 C7 N13 127.1(4) . . ? C12 N8 N9 110.9(4) . . ? C12 N8 C3 132.5(4) . . ? N9 N8 C3 116.6(3) . . ? C10 N9 N8 104.5(3) . . ? C10 N9 Fe1 143.4(3) . . ? N8 N9 Fe1 112.0(2) . . ? N9 C10 C11 110.9(4) . . ? C12 C11 C10 106.8(4) . . ? C11 C12 N8 106.8(4) . . ? C17 N13 N14 110.4(3) . . ? C17 N13 C7 133.3(4) . . ? N14 N13 C7 116.3(3) . . ? C15 N14 N13 104.9(3) . . ? C15 N14 Fe1 142.1(3) . . ? N13 N14 Fe1 112.8(2) . . ? N14 C15 C16 111.4(4) . . ? C17 C16 C15 106.1(4) . . ? N13 C17 C16 107.2(4) . . ? C19 N18 C23 119.4(3) . . ? C19 N18 Fe1 120.9(3) . . ? C23 N18 Fe1 119.6(3) . . ? N18 C19 C20 123.3(4) . . ? N18 C19 N24 110.5(3) . . ? C20 C19 N24 126.2(4) . . ? C19 C20 C21 116.3(4) . . ? C20 C21 C22 122.4(4) . . ? C23 C22 C21 115.8(4) . . ? N18 C23 C22 122.7(4) . . ? N18 C23 N29 111.2(3) . . ? C22 C23 N29 126.1(4) . . ? C28 N24 N25 110.9(3) . . ? C28 N24 C19 132.7(4) . . ? N25 N24 C19 116.4(3) . . ? C26 N25 N24 104.4(3) . . ? C26 N25 Fe1 143.0(3) . . ? N24 N25 Fe1 112.4(2) . . ? N25 C26 C27 111.2(4) . . ? C28 C27 C26 105.3(4) . . ? N24 C28 C27 108.2(4) . . ? C33 N29 N30 111.5(4) . . ? C33 N29 C23 132.4(4) . . ? N30 N29 C23 115.9(3) . . ? C31 N30 N29 104.8(4) . . ? C31 N30 Fe1 142.0(3) . . ? N29 N30 Fe1 113.2(3) . . ? N30 C31 C32 111.0(4) . . ? C33 C32 C31 106.4(4) . . ? N29 C33 C32 106.3(4) . . ? F36 B34 F38 111.8(7) . . ? F44 B34 F35 125.3(7) . . ? F40 B34 F35 115.4(7) . . ? F36 B34 F35 114.1(6) . . ? F38 B34 F35 111.3(5) . . ? F44 B34 F42 116.9(9) . . ? F35 B34 F42 101.7(6) . . ? F36 B34 F37 106.5(6) . . ? F38 B34 F37 109.8(7) . . ? F35 B34 F37 102.6(5) . . ? F40 B34 F39 108.9(8) . . ? F35 B34 F39 112.3(7) . . ? F40 B34 F41 110.1(9) . . ? F35 B34 F41 106.4(8) . . ? F39 B34 F41 103.0(9) . . ? F44 B34 F43 108.0(8) . . ? F35 B34 F43 99.3(5) . . ? F42 B34 F43 102.1(7) . . ? F53 B45 F54 116.0(10) . . ? F53 B45 F46 109.8(6) . . ? F52 B45 F46 118.1(6) . . ? F49 B45 F46 111.0(6) . . ? F54 B45 F46 111.1(10) . . ? F49 B45 F48 112.6(9) . . ? F46 B45 F48 107.6(5) . . ? F52 B45 F51 106.3(8) . . ? F46 B45 F51 117.4(6) . . ? F49 B45 F47 111.3(7) . . ? F46 B45 F47 106.4(6) . . ? F48 B45 F47 107.7(8) . . ? F53 B45 F55 110.4(8) . . ? F54 B45 F55 109.6(10) . . ? F46 B45 F55 98.6(6) . . ? F52 B45 F50 102.8(7) . . ? F46 B45 F50 108.4(6) . . ? F51 B45 F50 101.6(8) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.531 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.173 #=END data_mh37lt _database_code_CSD 158395 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-[2,6-dipyrazol-1-ylpyridine]iron(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[C22 H18 Fe N10] 2[B F4]' _chemical_formula_sum 'C22 H18 B2 F8 Fe N10' _chemical_formula_weight 651.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.4575(2) _cell_length_b 8.5233(2) _cell_length_c 18.3756(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.2896(13) _cell_angle_gamma 90.00 _cell_volume 1310.78(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19914 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 27.47 _exptl_crystal_description Prism _exptl_crystal_colour Brown _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.668 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8351 _exptl_absorpt_correction_T_max 0.9424 _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 ; ? ; _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 ; 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_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19914 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5715 _reflns_number_gt 5556 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _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. There is no disorder in this structure. All non-H atoms were refined anisotropically. ; _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^)+(0.0403P)^2^+0.3045P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.055(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.009(10) _refine_ls_number_reflns 5715 _refine_ls_number_parameters 389 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0793 _refine_ls_wR_factor_gt 0.0775 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.064 _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 0.71441(3) 0.84219(3) 0.746416(13) 0.02402(9) Uani 1 1 d . . . N2 N 0.70929(19) 0.8616(2) 0.64309(9) 0.0263(3) Uani 1 1 d . . . C3 C 0.5818(2) 0.9217(3) 0.60140(11) 0.0282(4) Uani 1 1 d . . . C4 C 0.5713(3) 0.9361(3) 0.52592(12) 0.0325(4) Uani 1 1 d . . . H4 H 0.4797 0.9798 0.4970 0.039 Uiso 1 1 calc R . . C5 C 0.7009(3) 0.8837(3) 0.49446(12) 0.0340(5) Uani 1 1 d . . . H5 H 0.6977 0.8917 0.4427 0.041 Uiso 1 1 calc R . . C6 C 0.8355(3) 0.8196(3) 0.53642(11) 0.0323(5) Uani 1 1 d . . . H6 H 0.9245 0.7842 0.5147 0.039 Uiso 1 1 calc R . . C7 C 0.8329(2) 0.8102(2) 0.61136(11) 0.0259(4) Uani 1 1 d . . . N8 N 0.4649(2) 0.9647(2) 0.64470(10) 0.0280(4) Uani 1 1 d . . . N9 N 0.4995(2) 0.9370(2) 0.71918(10) 0.0277(4) Uani 1 1 d . . . C10 C 0.3714(3) 0.9847(3) 0.74721(13) 0.0311(4) Uani 1 1 d . . . H10 H 0.3604 0.9799 0.7979 0.037 Uiso 1 1 calc R . . C11 C 0.2541(3) 1.0434(3) 0.69176(13) 0.0348(5) Uani 1 1 d . . . H11 H 0.1526 1.0849 0.6978 0.042 Uiso 1 1 calc R . . C12 C 0.3163(3) 1.0286(3) 0.62705(13) 0.0319(4) Uani 1 1 d . . . H12 H 0.2658 1.0573 0.5793 0.038 Uiso 1 1 calc R . . N13 N 0.9522(2) 0.7463(2) 0.66421(9) 0.0281(4) Uani 1 1 d . . . N14 N 0.9250(2) 0.7535(2) 0.73625(9) 0.0278(4) Uani 1 1 d . . . C15 C 1.0497(3) 0.6855(3) 0.77452(12) 0.0319(5) Uani 1 1 d . . . H15 H 1.0648 0.6740 0.8265 0.038 Uiso 1 1 calc R . . C16 C 1.1583(3) 0.6321(3) 0.72841(13) 0.0374(5) Uani 1 1 d . . . H16 H 1.2566 0.5789 0.7427 0.045 Uiso 1 1 calc R . . C17 C 1.0920(3) 0.6728(3) 0.65928(13) 0.0337(5) Uani 1 1 d . . . H17 H 1.1358 0.6533 0.6154 0.040 Uiso 1 1 calc R . . N18 N 0.7190(2) 0.8151(2) 0.84949(9) 0.0262(4) Uani 1 1 d . . . C19 C 0.7783(2) 0.9270(3) 0.89613(11) 0.0268(4) Uani 1 1 d . . . C20 C 0.7866(3) 0.9119(3) 0.97189(12) 0.0319(4) Uani 1 1 d . . . H20 H 0.8287 0.9929 1.0046 0.038 Uiso 1 1 calc R . . C21 C 0.7303(3) 0.7725(3) 0.99714(12) 0.0327(5) Uani 1 1 d . . . H21 H 0.7333 0.7582 1.0486 0.039 Uiso 1 1 calc R . . C22 C 0.6692(3) 0.6524(3) 0.94966(12) 0.0325(5) Uani 1 1 d . . . H22 H 0.6315 0.5566 0.9672 0.039 Uiso 1 1 calc R . . C23 C 0.6669(2) 0.6812(3) 0.87576(12) 0.0279(4) Uani 1 1 d . . . N24 N 0.8310(2) 1.0555(2) 0.85869(9) 0.0283(4) Uani 1 1 d . . . N25 N 0.8128(2) 1.0446(2) 0.78260(9) 0.0273(4) Uani 1 1 d . . . C26 C 0.8782(3) 1.1733(3) 0.76068(12) 0.0319(5) Uani 1 1 d . . . H26 H 0.8830 1.1989 0.7107 0.038 Uiso 1 1 calc R . . C27 C 0.9400(3) 1.2680(3) 0.82096(13) 0.0364(5) Uani 1 1 d . . . H27 H 0.9928 1.3660 0.8194 0.044 Uiso 1 1 calc R . . C28 C 0.9081(3) 1.1893(3) 0.88216(13) 0.0348(5) Uani 1 1 d . . . H28 H 0.9350 1.2225 0.9318 0.042 Uiso 1 1 calc R . . N29 N 0.6115(2) 0.5782(2) 0.81765(10) 0.0291(4) Uani 1 1 d . . . N30 N 0.6245(2) 0.6291(2) 0.74764(9) 0.0275(3) Uani 1 1 d . . . C31 C 0.5762(3) 0.5091(3) 0.70413(13) 0.0324(5) Uani 1 1 d . . . H31 H 0.5732 0.5095 0.6522 0.039 Uiso 1 1 calc R . . C32 C 0.5303(3) 0.3819(3) 0.74436(13) 0.0361(5) Uani 1 1 d . . . H32 H 0.4906 0.2835 0.7255 0.043 Uiso 1 1 calc R . . C33 C 0.5543(3) 0.4284(3) 0.81670(13) 0.0338(5) Uani 1 1 d . . . H33 H 0.5348 0.3681 0.8580 0.041 Uiso 1 1 calc R . . B34 B 0.8009(3) 0.3037(3) 0.56048(14) 0.0361(6) Uani 1 1 d . . . F35 F 0.68005(17) 0.25586(18) 0.59948(7) 0.0415(3) Uani 1 1 d . . . F36 F 0.7684(2) 0.2517(2) 0.48788(8) 0.0490(4) Uani 1 1 d . . . F37 F 0.8051(2) 0.4666(2) 0.56006(9) 0.0537(4) Uani 1 1 d . . . F38 F 0.9448(2) 0.2428(3) 0.59309(9) 0.0655(5) Uani 1 1 d . . . B39 B 0.7171(3) 0.2807(4) 1.05459(15) 0.0376(6) Uani 1 1 d . . . F40 F 0.63926(18) 0.2679(2) 0.98256(7) 0.0428(3) Uani 1 1 d . . . F41 F 0.68298(17) 0.1507(2) 1.09559(8) 0.0459(4) Uani 1 1 d . . . F42 F 0.88097(19) 0.2826(3) 1.05317(8) 0.0599(5) Uani 1 1 d . . . F43 F 0.6658(3) 0.4139(2) 1.08579(10) 0.0744(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02456(13) 0.02726(15) 0.02016(13) 0.00016(11) 0.00291(9) 0.00056(11) N2 0.0261(7) 0.0278(9) 0.0246(7) 0.0006(7) 0.0026(6) -0.0008(7) C3 0.0300(10) 0.0259(10) 0.0287(10) -0.0008(8) 0.0042(8) -0.0005(8) C4 0.0377(11) 0.0345(12) 0.0242(10) 0.0019(8) 0.0006(8) -0.0009(9) C5 0.0461(12) 0.0331(12) 0.0234(9) 0.0000(8) 0.0068(9) -0.0041(8) C6 0.0363(10) 0.0347(13) 0.0274(9) -0.0028(9) 0.0094(8) -0.0023(9) C7 0.0272(9) 0.0249(11) 0.0257(9) -0.0006(7) 0.0044(7) -0.0012(7) N8 0.0276(8) 0.0305(9) 0.0249(8) 0.0008(7) 0.0006(7) 0.0009(7) N9 0.0291(8) 0.0291(9) 0.0251(8) -0.0003(7) 0.0042(6) -0.0013(7) C10 0.0289(10) 0.0304(11) 0.0347(11) -0.0020(8) 0.0064(8) -0.0009(8) C11 0.0277(10) 0.0336(12) 0.0430(12) -0.0017(9) 0.0044(9) 0.0015(9) C12 0.0278(10) 0.0319(11) 0.0343(11) -0.0004(9) -0.0011(8) 0.0041(8) N13 0.0283(8) 0.0307(9) 0.0256(8) -0.0019(7) 0.0044(7) -0.0011(7) N14 0.0291(8) 0.0301(9) 0.0240(8) -0.0009(7) 0.0031(7) 0.0000(7) C15 0.0294(10) 0.0328(11) 0.0324(11) 0.0024(9) 0.0005(8) 0.0006(8) C16 0.0281(10) 0.0377(12) 0.0463(13) 0.0032(10) 0.0047(10) 0.0050(9) C17 0.0305(10) 0.0336(11) 0.0383(12) -0.0013(9) 0.0097(9) 0.0036(8) N18 0.0256(7) 0.0286(10) 0.0246(7) -0.0004(7) 0.0039(6) 0.0010(6) C19 0.0234(9) 0.0313(11) 0.0256(10) -0.0011(8) 0.0034(7) 0.0008(8) C20 0.0306(10) 0.0417(12) 0.0233(10) -0.0028(9) 0.0038(8) 0.0015(9) C21 0.0310(10) 0.0438(12) 0.0232(10) 0.0037(9) 0.0037(8) 0.0028(9) C22 0.0311(10) 0.0396(12) 0.0274(10) 0.0066(9) 0.0061(8) 0.0025(9) C23 0.0256(9) 0.0312(11) 0.0273(10) 0.0013(8) 0.0044(8) 0.0010(8) N24 0.0295(8) 0.0322(9) 0.0228(8) -0.0004(7) 0.0032(7) -0.0007(7) N25 0.0281(8) 0.0331(9) 0.0205(8) 0.0010(7) 0.0030(7) 0.0027(7) C26 0.0303(10) 0.0338(11) 0.0323(11) 0.0040(9) 0.0069(9) -0.0001(8) C27 0.0346(11) 0.0355(12) 0.0396(12) -0.0015(9) 0.0073(9) -0.0058(9) C28 0.0345(11) 0.0364(12) 0.0328(11) -0.0074(9) 0.0026(9) -0.0048(9) N29 0.0293(8) 0.0302(10) 0.0280(9) 0.0019(7) 0.0046(7) -0.0001(7) N30 0.0263(8) 0.0322(9) 0.0237(8) 0.0020(7) 0.0030(6) 0.0023(7) C31 0.0314(10) 0.0317(12) 0.0337(11) -0.0064(9) 0.0037(9) -0.0001(8) C32 0.0369(11) 0.0279(12) 0.0424(12) -0.0034(8) 0.0021(10) 0.0002(8) C33 0.0304(10) 0.0291(11) 0.0418(12) 0.0047(9) 0.0054(9) 0.0001(8) B34 0.0437(14) 0.0384(15) 0.0276(11) 0.0041(10) 0.0101(10) 0.0021(10) F35 0.0481(8) 0.0451(8) 0.0342(7) -0.0021(6) 0.0155(6) -0.0022(6) F36 0.0695(10) 0.0494(9) 0.0314(7) -0.0016(6) 0.0180(7) 0.0008(8) F37 0.0662(11) 0.0408(9) 0.0521(9) 0.0007(7) 0.0015(8) -0.0136(8) F38 0.0491(9) 0.1031(15) 0.0467(9) 0.0266(10) 0.0157(8) 0.0290(10) B39 0.0419(14) 0.0425(14) 0.0303(12) 0.0045(10) 0.0120(11) 0.0018(11) F40 0.0434(8) 0.0547(9) 0.0298(7) 0.0065(6) 0.0035(6) 0.0049(6) F41 0.0375(7) 0.0605(10) 0.0383(8) 0.0162(7) 0.0010(6) -0.0070(7) F42 0.0386(8) 0.1055(15) 0.0358(7) 0.0003(8) 0.0059(6) -0.0247(8) F43 0.1307(19) 0.0561(11) 0.0396(9) -0.0037(8) 0.0234(10) 0.0240(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.9001(16) . ? Fe1 N18 1.9029(17) . ? Fe1 N14 1.9682(18) . ? Fe1 N30 1.9701(19) . ? Fe1 N9 1.9860(18) . ? Fe1 N25 1.9880(19) . ? N2 C3 1.332(3) . ? N2 C7 1.342(3) . ? C3 C4 1.383(3) . ? C3 N8 1.404(3) . ? C4 C5 1.385(3) . ? C5 C6 1.391(3) . ? C6 C7 1.383(3) . ? C7 N13 1.405(3) . ? N8 C12 1.365(3) . ? N8 N9 1.378(2) . ? N9 C10 1.329(3) . ? C10 C11 1.407(3) . ? C11 C12 1.374(3) . ? N13 C17 1.353(3) . ? N13 N14 1.377(2) . ? N14 C15 1.315(3) . ? C15 C16 1.412(3) . ? C16 C17 1.358(3) . ? N18 C19 1.331(3) . ? N18 C23 1.338(3) . ? C19 C20 1.390(3) . ? C19 N24 1.400(3) . ? C20 C21 1.385(3) . ? C21 C22 1.395(3) . ? C22 C23 1.377(3) . ? C23 N29 1.409(3) . ? N24 C28 1.354(3) . ? N24 N25 1.387(2) . ? N25 C26 1.317(3) . ? C26 C27 1.409(3) . ? C27 C28 1.369(3) . ? N29 C33 1.364(3) . ? N29 N30 1.377(2) . ? N30 C31 1.326(3) . ? C31 C32 1.398(3) . ? C32 C33 1.374(3) . ? B34 F38 1.378(3) . ? B34 F37 1.390(3) . ? B34 F35 1.391(3) . ? B34 F36 1.395(3) . ? B39 F43 1.371(3) . ? B39 F42 1.390(3) . ? B39 F41 1.393(3) . ? B39 F40 1.395(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N18 178.00(9) . . ? N2 Fe1 N14 80.16(7) . . ? N18 Fe1 N14 99.16(7) . . ? N2 Fe1 N30 97.94(7) . . ? N18 Fe1 N30 80.16(7) . . ? N14 Fe1 N30 90.15(7) . . ? N2 Fe1 N9 79.90(7) . . ? N18 Fe1 N9 100.76(7) . . ? N14 Fe1 N9 160.06(7) . . ? N30 Fe1 N9 92.14(7) . . ? N2 Fe1 N25 101.94(8) . . ? N18 Fe1 N25 79.93(7) . . ? N14 Fe1 N25 91.41(8) . . ? N30 Fe1 N25 160.03(7) . . ? N9 Fe1 N25 93.13(7) . . ? C3 N2 C7 119.52(17) . . ? C3 N2 Fe1 120.52(14) . . ? C7 N2 Fe1 119.93(14) . . ? N2 C3 C4 122.70(19) . . ? N2 C3 N8 110.63(18) . . ? C4 C3 N8 126.7(2) . . ? C3 C4 C5 116.8(2) . . ? C4 C5 C6 121.9(2) . . ? C7 C6 C5 116.45(19) . . ? N2 C7 C6 122.61(19) . . ? N2 C7 N13 110.65(17) . . ? C6 C7 N13 126.73(19) . . ? C12 N8 N9 111.16(18) . . ? C12 N8 C3 131.96(19) . . ? N9 N8 C3 116.87(17) . . ? C10 N9 N8 105.31(18) . . ? C10 N9 Fe1 142.62(16) . . ? N8 N9 Fe1 112.07(13) . . ? N9 C10 C11 110.9(2) . . ? C12 C11 C10 106.1(2) . . ? N8 C12 C11 106.57(19) . . ? C17 N13 N14 110.72(18) . . ? C17 N13 C7 132.87(18) . . ? N14 N13 C7 116.39(17) . . ? C15 N14 N13 105.20(18) . . ? C15 N14 Fe1 141.77(15) . . ? N13 N14 Fe1 112.77(13) . . ? N14 C15 C16 111.2(2) . . ? C17 C16 C15 105.2(2) . . ? N13 C17 C16 107.6(2) . . ? C19 N18 C23 119.47(18) . . ? C19 N18 Fe1 120.35(14) . . ? C23 N18 Fe1 120.15(14) . . ? N18 C19 C20 122.6(2) . . ? N18 C19 N24 111.18(17) . . ? C20 C19 N24 126.2(2) . . ? C21 C20 C19 116.4(2) . . ? C20 C21 C22 122.3(2) . . ? C23 C22 C21 115.9(2) . . ? N18 C23 C22 123.3(2) . . ? N18 C23 N29 110.39(18) . . ? C22 C23 N29 126.3(2) . . ? C28 N24 N25 110.84(18) . . ? C28 N24 C19 132.51(18) . . ? N25 N24 C19 116.50(17) . . ? C26 N25 N24 105.20(18) . . ? C26 N25 Fe1 142.59(16) . . ? N24 N25 Fe1 112.03(13) . . ? N25 C26 C27 111.2(2) . . ? C28 C27 C26 105.7(2) . . ? N24 C28 C27 107.1(2) . . ? C33 N29 N30 111.03(18) . . ? C33 N29 C23 132.14(19) . . ? N30 N29 C23 116.68(17) . . ? C31 N30 N29 105.13(18) . . ? C31 N30 Fe1 142.19(15) . . ? N29 N30 Fe1 112.59(13) . . ? N30 C31 C32 111.4(2) . . ? C33 C32 C31 105.9(2) . . ? N29 C33 C32 106.5(2) . . ? F38 B34 F37 110.9(2) . . ? F38 B34 F35 109.52(19) . . ? F37 B34 F35 108.5(2) . . ? F38 B34 F36 109.6(2) . . ? F37 B34 F36 108.3(2) . . ? F35 B34 F36 110.0(2) . . ? F43 B39 F42 112.0(3) . . ? F43 B39 F41 109.3(2) . . ? F42 B39 F41 107.7(2) . . ? F43 B39 F40 109.1(2) . . ? F42 B39 F40 108.6(2) . . ? F41 B39 F40 110.2(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.501 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.164