Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global #==================================================================== # 1. SUBMISSION DETAILS _journal_coden_Cambridge 222 _publ_contact_author_name 'Malcolm A. Halcrow' _publ_contact_author_address ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; _publ_contact_author_phone '+44 (0)113 3436506' _publ_contact_author_fax '+44 (0)113 3436565' _publ_contact_author_email m.a.halcrow@@leeds.ac.uk _publ_requested_journal 'Dalton Transactions' _publ_contact_letter ; The following set of data is for seven structures included in a manuscript we have just submitted to the Dalton Transactions office. ; #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Anion Doping as a Probe of Cooperativity in the Molecular Spin-Crossover Compound [FeL2][BF4]2 (L = 2,6-di{pyrazol-1-yl}pyridine) ; loop_ _publ_author_name _publ_author_address 'Chiara Carbonera' ; Institut de Chimie de la Matiere Condensee de Bordeaux, UPR CNRS 9048 - Universite de Bordeaux 1, Groupe des Sciences Moleculaires, 87 Av. Doc. A. Schweitzer, F-33608 Pessac, France. ; 'Colin A. Kilner' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Jean-Francois Letard' ; Institut de Chimie de la Matiere Condensee de Bordeaux, UPR CNRS 9048 - Universite de Bordeaux 1, Groupe des Sciences Moleculaires, 87 Av. Doc. A. Schweitzer, F-33608 Pessac, France. ; 'Malcolm A. Halcrow' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; #================================================================= data_c:\datasets\leeds\mh37on~1\mh37on~1\mh37300 _database_code_depnum_ccdc_archive 'CCDC 631320' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-di(pyrazol-1-yl)pyridine]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 8.5468(8) _cell_length_b 8.5592(7) _cell_length_c 19.1536(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.640(5) _cell_angle_gamma 90.00 _cell_volume 1394.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 44405 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 30.05 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _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 0.795 _exptl_absorpt_correction_T_max 0.939 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 2.5 kW. ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44405 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 30.05 _reflns_number_total 7324 _reflns_number_gt 6596 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The F atoms of both anions are disordered over three orientations. For the anion centred on B34: F35A-F38A, occupancy 0.5 F35B-F38B, occupancy 0.25 F35C-F38C, occupancy 0.25 For the anion centred on B39: F40A-F43A, occupancy 0.5 F40B-F43B, occupancy 0.25 F40C-F43C, occupancy 0.25 All B---F distances were restrained to 1.38(2)\%A, and non-bonded F...F contacts within each disorder orientation to 2.25(2)\%A. Attempts to model disorder in the B atoms were unsuccessful, and two wholly occupied B sites were used in the final refinement. This probably accounts for distortions away from an ideal tetrahedral geometry in the partial anions. All non-H atoms with occupancy >=0.5 were modeled anisotropically, and all H atoms were placed in calculated positions and refined using a riding model. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+0.1690P] 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 0.0100(12) _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 0.017(12) _refine_ls_number_reflns 7324 _refine_ls_number_parameters 454 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0954 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.056 _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 0.73852(3) 0.80773(4) 0.747502(12) 0.04979(9) Uani 1 1 d . . . N2 N 0.72287(15) 0.8034(2) 0.63538(7) 0.0439(3) Uani 1 1 d . . . C3 C 0.5939(2) 0.8577(2) 0.59758(10) 0.0473(4) Uani 1 1 d . . . C4 C 0.5798(3) 0.8635(3) 0.52463(11) 0.0636(5) Uani 1 1 d . . . H4 H 0.4892 0.9007 0.4992 0.076 Uiso 1 1 calc R . . C5 C 0.7076(3) 0.8110(4) 0.49158(10) 0.0696(6) Uani 1 1 d . . . H5 H 0.7028 0.8136 0.4429 0.084 Uiso 1 1 calc R . . C6 C 0.8420(3) 0.7547(3) 0.52971(12) 0.0630(6) Uani 1 1 d . . . H6 H 0.9279 0.7200 0.5078 0.076 Uiso 1 1 calc R . . C7 C 0.8423(2) 0.7527(2) 0.60197(10) 0.0481(4) Uani 1 1 d . . . N8 N 0.47505(18) 0.9066(2) 0.63873(9) 0.0495(3) Uani 1 1 d . . . N9 N 0.50248(19) 0.8965(2) 0.71056(9) 0.0508(4) Uani 1 1 d . . . C10 C 0.3711(3) 0.9498(3) 0.73456(14) 0.0617(5) Uani 1 1 d . . . H10 H 0.3549 0.9561 0.7818 0.074 Uiso 1 1 calc R . . C11 C 0.2607(3) 0.9951(3) 0.67928(17) 0.0735(7) Uani 1 1 d . . . H11 H 0.1612 1.0365 0.6829 0.088 Uiso 1 1 calc R . . C12 C 0.3289(3) 0.9661(3) 0.61917(15) 0.0661(6) Uani 1 1 d . . . H12 H 0.2845 0.9835 0.5735 0.079 Uiso 1 1 calc R . . N13 N 0.96912(19) 0.6967(2) 0.64796(10) 0.0537(4) Uani 1 1 d . . . N14 N 0.9602(2) 0.7111(2) 0.71884(10) 0.0580(4) Uani 1 1 d . . . C15 C 1.0897(3) 0.6417(3) 0.74841(16) 0.0733(7) Uani 1 1 d . . . H15 H 1.1166 0.6343 0.7965 0.088 Uiso 1 1 calc R . . C16 C 1.1798(3) 0.5814(4) 0.6977(2) 0.0883(9) Uani 1 1 d . . . H16 H 1.2747 0.5280 0.7055 0.106 Uiso 1 1 calc R . . C17 C 1.1001(3) 0.6169(3) 0.63418(18) 0.0751(7) Uani 1 1 d . . . H17 H 1.1297 0.5913 0.5902 0.090 Uiso 1 1 calc R . . N18 N 0.73570(16) 0.7876(2) 0.85875(7) 0.0434(3) Uani 1 1 d . . . C19 C 0.7872(2) 0.9053(2) 0.90075(10) 0.0461(4) Uani 1 1 d . . . C20 C 0.7864(3) 0.9000(3) 0.97329(11) 0.0594(5) Uani 1 1 d . . . H20 H 0.8223 0.9833 1.0017 0.071 Uiso 1 1 calc R . . C21 C 0.7293(3) 0.7645(3) 1.00113(12) 0.0669(7) Uani 1 1 d . . . H21 H 0.7261 0.7568 1.0494 0.080 Uiso 1 1 calc R . . C22 C 0.6769(3) 0.6403(3) 0.95893(12) 0.0627(5) Uani 1 1 d . . . H22 H 0.6399 0.5487 0.9777 0.075 Uiso 1 1 calc R . . C23 C 0.6823(2) 0.6591(3) 0.88750(11) 0.0503(4) Uani 1 1 d . . . N24 N 0.84466(18) 1.0334(2) 0.86443(8) 0.0489(3) Uani 1 1 d . . . N25 N 0.8395(2) 1.0257(2) 0.79263(9) 0.0520(4) Uani 1 1 d . . . C26 C 0.9080(3) 1.1578(3) 0.77423(13) 0.0635(5) Uani 1 1 d . . . H26 H 0.9211 1.1859 0.7283 0.076 Uiso 1 1 calc R . . C27 C 0.9576(3) 1.2486(3) 0.83330(15) 0.0741(6) Uani 1 1 d . . . H27 H 1.0086 1.3446 0.8341 0.089 Uiso 1 1 calc R . . C28 C 0.9151(3) 1.1664(3) 0.88922(14) 0.0667(6) Uani 1 1 d . . . H28 H 0.9314 1.1964 0.9360 0.080 Uiso 1 1 calc R . . N29 N 0.6319(2) 0.5436(2) 0.83707(11) 0.0559(4) Uani 1 1 d . . . N30 N 0.6498(2) 0.5723(2) 0.76823(10) 0.0573(4) Uani 1 1 d . . . C31 C 0.5982(3) 0.4440(3) 0.73383(16) 0.0727(7) Uani 1 1 d . . . H31 H 0.5977 0.4300 0.6857 0.087 Uiso 1 1 calc R . . C32 C 0.5449(3) 0.3338(3) 0.77949(18) 0.0860(8) Uani 1 1 d . . . H32 H 0.5025 0.2360 0.7681 0.103 Uiso 1 1 calc R . . C33 C 0.5684(3) 0.4009(3) 0.84560(19) 0.0772(7) Uani 1 1 d . . . H33 H 0.5450 0.3564 0.8876 0.093 Uiso 1 1 calc R . . B34 B 0.7975(4) 0.2504(4) 0.57765(15) 0.0667(7) Uani 1 1 d D . . F35A F 0.6769(12) 0.1905(9) 0.6144(5) 0.081(2) Uani 0.50 1 d PD A 1 F36A F 0.7572(6) 0.1982(6) 0.50512(18) 0.0713(10) Uani 0.50 1 d PD A 1 F37A F 0.7904(11) 0.4051(6) 0.5705(5) 0.133(4) Uani 0.50 1 d PD A 1 F38A F 0.9399(6) 0.1940(10) 0.6024(3) 0.1019(19) Uani 0.50 1 d PD A 1 F35B F 0.699(2) 0.191(2) 0.6216(10) 0.119(7) Uiso 0.25 1 d PD A 2 F36B F 0.9491(12) 0.2611(12) 0.6151(6) 0.087(3) Uiso 0.25 1 d PD A 2 F37B F 0.7960(13) 0.1671(12) 0.5180(5) 0.085(4) Uiso 0.25 1 d PD A 2 F38B F 0.7677(19) 0.4134(13) 0.5717(8) 0.087(4) Uiso 0.25 1 d PD A 2 F35C F 0.6593(14) 0.2260(16) 0.6048(8) 0.085(4) Uiso 0.25 1 d PD A 3 F36C F 0.9042(13) 0.1278(12) 0.5912(6) 0.097(4) Uiso 0.25 1 d PD A 3 F37C F 0.7929(13) 0.2831(16) 0.5119(5) 0.122(4) Uiso 0.25 1 d PD A 3 F38C F 0.8679(17) 0.3735(16) 0.6211(7) 0.163(5) Uiso 0.25 1 d PD A 3 B39 B 0.7379(4) 0.2748(4) 1.07435(17) 0.0820(9) Uani 1 1 d D . . F40A F 0.6601(9) 0.2649(10) 1.0018(3) 0.076(3) Uani 0.50 1 d PD B 1 F41A F 0.6743(6) 0.1552(9) 1.1097(3) 0.0802(17) Uani 0.50 1 d PD B 1 F42A F 0.8895(5) 0.2611(9) 1.0674(3) 0.114(2) Uani 0.50 1 d PD B 1 F43A F 0.6974(14) 0.4190(7) 1.0997(3) 0.163(4) Uani 0.50 1 d PD B 1 F40B F 0.8815(14) 0.3320(19) 1.1059(7) 0.165(5) Uiso 0.25 1 d PD B 2 F41B F 0.7328(12) 0.2830(14) 1.0064(4) 0.100(3) Uiso 0.25 1 d PD B 2 F42B F 0.7208(12) 0.1285(12) 1.1023(6) 0.087(4) Uiso 0.25 1 d PD B 2 F43B F 0.6265(12) 0.3792(12) 1.0993(6) 0.100(3) Uiso 0.25 1 d PD B 2 F40C F 0.6569(14) 0.2192(12) 1.1260(6) 0.098(5) Uiso 0.25 1 d PD B 3 F41C F 0.7946(13) 0.4237(13) 1.0973(7) 0.115(4) Uiso 0.25 1 d PD B 3 F42C F 0.8903(11) 0.1882(11) 1.0792(5) 0.086(3) Uiso 0.25 1 d PD B 3 F43C F 0.666(2) 0.262(3) 1.0100(7) 0.098(8) Uiso 0.25 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 0.05118(14) 0.05769(15) 0.03987(12) -0.00466(12) 0.00134(9) 0.00313(14) N2 0.0427(6) 0.0452(7) 0.0436(6) 0.0003(8) 0.0033(5) -0.0021(8) C3 0.0483(9) 0.0455(8) 0.0476(9) 0.0013(7) 0.0023(7) -0.0060(7) C4 0.0729(13) 0.0663(12) 0.0486(10) 0.0043(9) -0.0098(9) -0.0063(10) C5 0.0957(16) 0.0713(13) 0.0424(8) -0.0058(13) 0.0096(9) -0.0098(17) C6 0.0723(14) 0.0646(12) 0.0560(11) -0.0125(10) 0.0251(10) -0.0102(10) C7 0.0491(9) 0.0434(8) 0.0528(10) -0.0076(8) 0.0101(8) -0.0054(7) N8 0.0446(8) 0.0480(8) 0.0551(9) 0.0029(7) 0.0008(6) 0.0013(6) N9 0.0477(8) 0.0514(9) 0.0540(9) -0.0012(7) 0.0084(7) -0.0004(6) C10 0.0585(12) 0.0528(11) 0.0769(14) -0.0054(10) 0.0231(10) -0.0003(9) C11 0.0478(11) 0.0602(13) 0.113(2) -0.0042(13) 0.0092(12) 0.0082(10) C12 0.0524(11) 0.0563(12) 0.0870(17) 0.0086(12) -0.0051(11) 0.0075(9) N13 0.0443(8) 0.0511(9) 0.0663(10) -0.0085(8) 0.0088(7) -0.0005(7) N14 0.0481(9) 0.0601(10) 0.0639(10) -0.0049(8) -0.0039(7) 0.0017(7) C15 0.0549(12) 0.0692(15) 0.0913(18) 0.0058(14) -0.0153(12) 0.0007(11) C16 0.0506(13) 0.0723(16) 0.140(3) 0.0030(18) 0.0008(15) 0.0153(12) C17 0.0554(12) 0.0667(14) 0.106(2) -0.0111(14) 0.0230(13) 0.0082(10) N18 0.0382(6) 0.0483(9) 0.0436(6) -0.0015(7) 0.0031(5) 0.0032(6) C19 0.0386(8) 0.0530(10) 0.0462(9) -0.0011(8) 0.0013(7) 0.0055(7) C20 0.0594(11) 0.0718(14) 0.0460(10) -0.0055(10) 0.0001(8) 0.0042(10) C21 0.0670(13) 0.0879(19) 0.0462(10) 0.0093(11) 0.0075(9) 0.0102(11) C22 0.0595(12) 0.0691(13) 0.0605(12) 0.0177(11) 0.0114(9) 0.0056(10) C23 0.0409(9) 0.0537(10) 0.0567(10) 0.0034(9) 0.0064(7) 0.0064(8) N24 0.0452(8) 0.0533(9) 0.0473(8) -0.0029(7) 0.0002(6) 0.0000(6) N25 0.0541(9) 0.0537(9) 0.0479(8) 0.0038(7) 0.0033(7) 0.0037(7) C26 0.0624(12) 0.0588(12) 0.0699(14) 0.0137(11) 0.0095(10) 0.0017(10) C27 0.0699(14) 0.0625(13) 0.0895(17) -0.0003(13) 0.0065(13) -0.0145(11) C28 0.0597(12) 0.0699(14) 0.0696(14) -0.0163(12) 0.0012(10) -0.0126(11) N29 0.0458(8) 0.0470(8) 0.0753(11) -0.0010(8) 0.0082(8) 0.0011(7) N30 0.0532(9) 0.0544(9) 0.0640(11) -0.0113(8) 0.0034(8) 0.0044(7) C31 0.0578(12) 0.0639(14) 0.0937(18) -0.0255(13) -0.0058(12) 0.0092(10) C32 0.0671(14) 0.0562(16) 0.133(3) -0.0171(15) -0.0019(15) -0.0056(11) C33 0.0651(14) 0.0512(12) 0.116(2) 0.0064(14) 0.0117(14) -0.0069(10) B34 0.0752(17) 0.0684(15) 0.0577(14) 0.0052(12) 0.0130(12) -0.0022(13) F35A 0.106(4) 0.062(3) 0.085(4) -0.013(2) 0.056(3) -0.027(3) F36A 0.090(3) 0.079(3) 0.0451(15) 0.0029(16) 0.0116(16) 0.014(2) F37A 0.158(7) 0.048(2) 0.180(7) 0.024(3) -0.049(5) -0.039(3) F38A 0.091(3) 0.139(6) 0.075(3) 0.003(4) 0.000(2) 0.044(4) B39 0.095(2) 0.087(2) 0.0657(16) 0.0030(15) 0.0167(15) -0.0169(18) F40A 0.081(4) 0.092(4) 0.0539(19) 0.022(2) 0.0044(16) -0.0058(18) F41A 0.050(2) 0.112(4) 0.078(3) 0.047(3) 0.0003(18) -0.018(2) F42A 0.0657(19) 0.177(6) 0.102(3) -0.015(4) 0.0189(18) -0.059(3) F43A 0.312(13) 0.104(4) 0.089(3) -0.024(3) 0.099(6) -0.012(6) _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 2.1390(14) . ? Fe1 N18 2.1402(15) . ? Fe1 N14 2.1865(19) . ? Fe1 N25 2.1964(19) . ? Fe1 N30 2.203(2) . ? Fe1 N9 2.2063(17) . ? N2 C7 1.329(2) . ? N2 C3 1.341(2) . ? C3 C4 1.391(3) . ? C3 N8 1.409(3) . ? C4 C5 1.390(4) . ? C5 C6 1.385(4) . ? C6 C7 1.384(3) . ? C7 N13 1.412(3) . ? N8 C12 1.367(3) . ? N8 N9 1.375(2) . ? N9 C10 1.335(3) . ? C10 C11 1.402(4) . ? C11 C12 1.363(4) . ? N13 C17 1.359(3) . ? N13 N14 1.373(3) . ? N14 C15 1.333(3) . ? C15 C16 1.396(5) . ? C16 C17 1.370(5) . ? N18 C23 1.331(3) . ? N18 C19 1.336(3) . ? C19 C20 1.391(3) . ? C19 N24 1.412(3) . ? C20 C21 1.386(4) . ? C21 C22 1.383(4) . ? C22 C23 1.383(3) . ? C23 N29 1.419(3) . ? N24 C28 1.352(3) . ? N24 N25 1.373(2) . ? N25 C26 1.337(3) . ? C26 C27 1.403(4) . ? C27 C28 1.360(4) . ? N29 C33 1.354(3) . ? N29 N30 1.365(3) . ? N30 C31 1.333(3) . ? C31 C32 1.393(5) . ? C32 C33 1.387(4) . ? B34 F37C 1.287(9) . ? B34 F37A 1.332(6) . ? B34 F37B 1.346(9) . ? B34 F35B 1.350(12) . ? B34 F38A 1.352(5) . ? B34 F35C 1.352(11) . ? B34 F36C 1.398(10) . ? B34 F35A 1.401(5) . ? B34 F38B 1.421(11) . ? B34 F36B 1.421(10) . ? B34 F38C 1.437(11) . ? B34 F36A 1.468(5) . ? B39 F41B 1.301(9) . ? B39 F42A 1.321(6) . ? B39 F43C 1.327(11) . ? B39 F40C 1.349(10) . ? B39 F41A 1.369(5) . ? B39 F42B 1.375(10) . ? B39 F43A 1.382(6) . ? B39 F40B 1.401(11) . ? B39 F41C 1.417(11) . ? B39 F43B 1.423(10) . ? B39 F40A 1.482(7) . ? B39 F42C 1.494(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N18 172.98(7) . . ? N2 Fe1 N14 73.23(6) . . ? N18 Fe1 N14 108.32(6) . . ? N2 Fe1 N25 113.16(7) . . ? N18 Fe1 N25 73.68(7) . . ? N14 Fe1 N25 95.93(7) . . ? N2 Fe1 N30 100.15(7) . . ? N18 Fe1 N30 73.10(7) . . ? N14 Fe1 N30 91.23(7) . . ? N25 Fe1 N30 146.60(7) . . ? N2 Fe1 N9 73.68(6) . . ? N18 Fe1 N9 104.33(6) . . ? N14 Fe1 N9 146.88(7) . . ? N25 Fe1 N9 98.35(7) . . ? N30 Fe1 N9 93.03(7) . . ? C7 N2 C3 118.84(16) . . ? C7 N2 Fe1 120.91(12) . . ? C3 N2 Fe1 120.19(12) . . ? N2 C3 C4 122.65(19) . . ? N2 C3 N8 113.61(16) . . ? C4 C3 N8 123.74(19) . . ? C5 C4 C3 116.9(2) . . ? C6 C5 C4 121.33(18) . . ? C7 C6 C5 116.8(2) . . ? N2 C7 C6 123.5(2) . . ? N2 C7 N13 112.90(16) . . ? C6 C7 N13 123.64(19) . . ? C12 N8 N9 111.03(19) . . ? C12 N8 C3 130.31(19) . . ? N9 N8 C3 118.66(15) . . ? C10 N9 N8 104.87(18) . . ? C10 N9 Fe1 141.35(16) . . ? N8 N9 Fe1 113.76(12) . . ? N9 C10 C11 111.2(2) . . ? C12 C11 C10 106.0(2) . . ? C11 C12 N8 106.9(2) . . ? C17 N13 N14 111.3(2) . . ? C17 N13 C7 130.2(2) . . ? N14 N13 C7 118.22(16) . . ? C15 N14 N13 104.8(2) . . ? C15 N14 Fe1 140.0(2) . . ? N13 N14 Fe1 114.57(13) . . ? N14 C15 C16 111.2(3) . . ? C17 C16 C15 106.0(2) . . ? N13 C17 C16 106.6(3) . . ? C23 N18 C19 118.68(16) . . ? C23 N18 Fe1 121.09(14) . . ? C19 N18 Fe1 120.23(13) . . ? N18 C19 C20 122.91(19) . . ? N18 C19 N24 113.49(16) . . ? C20 C19 N24 123.59(19) . . ? C21 C20 C19 116.6(2) . . ? C22 C21 C20 121.7(2) . . ? C23 C22 C21 116.6(2) . . ? N18 C23 C22 123.5(2) . . ? N18 C23 N29 112.80(17) . . ? C22 C23 N29 123.7(2) . . ? C28 N24 N25 111.20(19) . . ? C28 N24 C19 130.19(19) . . ? N25 N24 C19 118.51(16) . . ? C26 N25 N24 104.56(18) . . ? C26 N25 Fe1 141.28(16) . . ? N24 N25 Fe1 114.06(12) . . ? N25 C26 C27 111.2(2) . . ? C28 C27 C26 105.4(2) . . ? N24 C28 C27 107.6(2) . . ? C33 N29 N30 111.3(2) . . ? C33 N29 C23 130.2(2) . . ? N30 N29 C23 118.50(17) . . ? C31 N30 N29 105.4(2) . . ? C31 N30 Fe1 140.1(2) . . ? N29 N30 Fe1 114.33(13) . . ? N30 C31 C32 111.1(3) . . ? C33 C32 C31 105.4(2) . . ? N29 C33 C32 106.7(3) . . ? F37C B34 F37A 71.7(8) . . ? F37C B34 F37B 44.6(7) . . ? F37A B34 F37B 116.3(7) . . ? F37C B34 F35B 137.1(11) . . ? F37A B34 F35B 114.4(11) . . ? F37B B34 F35B 112.1(10) . . ? F37C B34 F38A 111.1(6) . . ? F37A B34 F38A 114.9(6) . . ? F37B B34 F38A 92.4(5) . . ? F35B B34 F38A 104.2(11) . . ? F37C B34 F35C 117.8(8) . . ? F37A B34 F35C 99.3(7) . . ? F37B B34 F35C 108.0(9) . . ? F35B B34 F35C 22.8(12) . . ? F38A B34 F35C 126.9(7) . . ? F37C B34 F36C 107.5(7) . . ? F37A B34 F36C 141.9(7) . . ? F37B B34 F36C 73.3(7) . . ? F35B B34 F36C 92.2(11) . . ? F38A B34 F36C 28.1(5) . . ? F35C B34 F36C 113.0(7) . . ? F37C B34 F35A 128.2(8) . . ? F37A B34 F35A 112.8(6) . . ? F37B B34 F35A 106.6(7) . . ? F35B B34 F35A 8.9(13) . . ? F38A B34 F35A 112.0(6) . . ? F35C B34 F35A 15.7(8) . . ? F36C B34 F35A 97.5(7) . . ? F37C B34 F38B 73.7(9) . . ? F37A B34 F38B 8.0(10) . . ? F37B B34 F38B 117.7(8) . . ? F35B B34 F38B 107.5(10) . . ? F38A B34 F38B 121.8(8) . . ? F35C B34 F38B 91.5(9) . . ? F36C B34 F38B 149.4(9) . . ? F35A B34 F38B 105.4(8) . . ? F37C B34 F36B 114.7(7) . . ? F37A B34 F36B 91.0(6) . . ? F37B B34 F36B 113.2(6) . . ? F35B B34 F36B 107.8(10) . . ? F38A B34 F36B 25.9(4) . . ? F35C B34 F36B 127.1(8) . . ? F36C B34 F36B 53.7(6) . . ? F35A B34 F36B 116.7(8) . . ? F38B B34 F36B 97.2(8) . . ? F37C B34 F38C 112.2(8) . . ? F37A B34 F38C 48.9(7) . . ? F37B B34 F38C 148.0(8) . . ? F35B B34 F38C 99.6(11) . . ? F38A B34 F38C 75.4(6) . . ? F35C B34 F38C 102.9(8) . . ? F36C B34 F38C 102.3(7) . . ? F35A B34 F38C 105.3(7) . . ? F38B B34 F38C 52.3(9) . . ? F36B B34 F38C 49.6(6) . . ? F37C B34 F36A 32.7(6) . . ? F37A B34 F36A 101.6(5) . . ? F37B B34 F36A 18.8(4) . . ? F35B B34 F36A 111.9(9) . . ? F38A B34 F36A 110.0(4) . . ? F35C B34 F36A 100.6(7) . . ? F36C B34 F36A 92.0(6) . . ? F35A B34 F36A 104.4(5) . . ? F38B B34 F36A 101.5(7) . . ? F36B B34 F36A 127.9(5) . . ? F38C B34 F36A 144.8(6) . . ? F41B B39 F42A 80.9(5) . . ? F41B B39 F43C 26.8(10) . . ? F42A B39 F43C 105.6(10) . . ? F41B B39 F40C 141.6(8) . . ? F42A B39 F40C 128.4(6) . . ? F43C B39 F40C 115.3(10) . . ? F41B B39 F41A 124.0(6) . . ? F42A B39 F41A 115.1(5) . . ? F43C B39 F41A 103.1(10) . . ? F40C B39 F41A 27.8(5) . . ? F41B B39 F42B 116.3(7) . . ? F42A B39 F42B 95.8(6) . . ? F43C B39 F42B 103.1(11) . . ? F40C B39 F42B 46.5(7) . . ? F41A B39 F42B 20.6(5) . . ? F41B B39 F43A 108.6(6) . . ? F42A B39 F43A 113.4(6) . . ? F43C B39 F43A 107.0(11) . . ? F40C B39 F43A 83.9(5) . . ? F41A B39 F43A 111.6(5) . . ? F42B B39 F43A 129.5(6) . . ? F41B B39 F40B 110.8(7) . . ? F42A B39 F40B 41.3(6) . . ? F43C B39 F40B 137.4(11) . . ? F40C B39 F40B 107.3(8) . . ? F41A B39 F40B 114.9(7) . . ? F42B B39 F40B 105.8(8) . . ? F43A B39 F40B 77.1(8) . . ? F41B B39 F41C 103.8(8) . . ? F42A B39 F41C 78.6(6) . . ? F43C B39 F41C 118.5(11) . . ? F40C B39 F41C 105.9(7) . . ? F41A B39 F41C 131.2(7) . . ? F42B B39 F41C 138.1(8) . . ? F43A B39 F41C 34.8(6) . . ? F40B B39 F41C 45.1(8) . . ? F41B B39 F43B 110.2(7) . . ? F42A B39 F43B 141.8(6) . . ? F43C B39 F43B 95.8(11) . . ? F40C B39 F43B 64.3(6) . . ? F41A B39 F43B 89.5(6) . . ? F42B B39 F43B 109.9(6) . . ? F43A B39 F43B 28.6(6) . . ? F40B B39 F43B 102.8(8) . . ? F41C B39 F43B 63.3(7) . . ? F41B B39 F40A 25.4(5) . . ? F42A B39 F40A 104.8(4) . . ? F43C B39 F40A 1.9(12) . . ? F40C B39 F40A 116.9(7) . . ? F41A B39 F40A 104.9(5) . . ? F42B B39 F40A 104.9(6) . . ? F43A B39 F40A 106.0(6) . . ? F40B B39 F40A 135.8(7) . . ? F41C B39 F40A 116.8(7) . . ? F43B B39 F40A 95.6(6) . . ? F41B B39 F42C 91.9(7) . . ? F42A B39 F42C 26.4(4) . . ? F43C B39 F42C 109.7(10) . . ? F40C B39 F42C 106.6(6) . . ? F41A B39 F42C 89.1(5) . . ? F42B B39 F42C 69.5(6) . . ? F43A B39 F42C 131.9(7) . . ? F40B B39 F42C 54.9(8) . . ? F41C B39 F42C 99.1(6) . . ? F43B B39 F42C 154.1(7) . . ? F40A B39 F42C 109.8(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.294 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.040 #=END data_c:\datasets\leeds\mh37on~1\mh37on~2\mh37150 _database_code_depnum_ccdc_archive 'CCDC 631321' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-di(pyrazol-1-yl)pyridine]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 8.4966(7) _cell_length_b 8.5537(6) _cell_length_c 18.4300(15) _cell_angle_alpha 90.00 _cell_angle_beta 98.353(4) _cell_angle_gamma 90.00 _cell_volume 1325.23(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 41538 _cell_measurement_theta_min 1.12 _cell_measurement_theta_max 30.04 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour Brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.660 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.774 _exptl_absorpt_correction_T_max 0.937 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 2.5 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 41538 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 30.04 _reflns_number_total 6945 _reflns_number_gt 6883 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. No disorder was detected during refinement, and no restraints were applied. All non-H atoms were refined anisotropically, while all H atoms were placed in calculated positions and refined using a riding model. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0162P)^2^+1.0341P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.037(10) _refine_ls_number_reflns 6945 _refine_ls_number_parameters 388 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0753 _refine_ls_wR_factor_gt 0.0748 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.155 _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 0.71393(3) 0.84221(3) 0.746480(13) 0.01519(6) Uani 1 1 d . . . N2 N 0.70916(18) 0.8622(2) 0.64324(8) 0.0167(3) Uani 1 1 d . . . C3 C 0.5809(2) 0.9218(2) 0.60134(10) 0.0183(3) Uani 1 1 d . . . C4 C 0.5700(3) 0.9364(3) 0.52588(11) 0.0230(4) Uani 1 1 d . . . H4 H 0.4786 0.9795 0.4970 0.028 Uiso 1 1 calc R . . C5 C 0.7012(3) 0.8841(3) 0.49458(11) 0.0252(4) Uani 1 1 d . . . H5 H 0.6986 0.8925 0.4430 0.030 Uiso 1 1 calc R . . C6 C 0.8351(2) 0.8202(3) 0.53640(10) 0.0228(4) Uani 1 1 d . . . H6 H 0.9236 0.7850 0.5148 0.027 Uiso 1 1 calc R . . C7 C 0.8328(2) 0.8107(2) 0.61149(10) 0.0175(4) Uani 1 1 d . . . N8 N 0.4646(2) 0.9647(2) 0.64487(9) 0.0193(3) Uani 1 1 d . . . N9 N 0.4995(2) 0.9372(2) 0.71925(9) 0.0181(3) Uani 1 1 d . . . C10 C 0.3710(2) 0.9849(3) 0.74745(12) 0.0220(4) Uani 1 1 d . . . H10 H 0.3602 0.9801 0.7980 0.026 Uiso 1 1 calc R . . C11 C 0.2538(3) 1.0433(3) 0.69178(13) 0.0255(4) Uani 1 1 d . . . H11 H 0.1527 1.0845 0.6978 0.031 Uiso 1 1 calc R . . C12 C 0.3156(2) 1.0284(3) 0.62725(12) 0.0237(4) Uani 1 1 d . . . H12 H 0.2650 1.0568 0.5797 0.028 Uiso 1 1 calc R . . N13 N 0.9517(2) 0.7467(2) 0.66437(9) 0.0195(3) Uani 1 1 d . . . N14 N 0.9244(2) 0.7536(2) 0.73658(9) 0.0184(3) Uani 1 1 d . . . C15 C 1.0496(2) 0.6850(3) 0.77512(12) 0.0222(4) Uani 1 1 d . . . H15 H 1.0645 0.6726 0.8269 0.027 Uiso 1 1 calc R . . C16 C 1.1581(3) 0.6326(3) 0.72880(13) 0.0278(4) Uani 1 1 d . . . H16 H 1.2564 0.5805 0.7432 0.033 Uiso 1 1 calc R . . C17 C 1.0923(2) 0.6724(3) 0.65900(12) 0.0241(4) Uani 1 1 d . . . H17 H 1.1359 0.6524 0.6153 0.029 Uiso 1 1 calc R . . N18 N 0.71880(19) 0.81503(19) 0.84963(8) 0.0173(3) Uani 1 1 d . . . C19 C 0.7781(2) 0.9272(2) 0.89648(10) 0.0177(4) Uani 1 1 d . . . C20 C 0.7866(2) 0.9120(3) 0.97195(11) 0.0225(4) Uani 1 1 d . . . H20 H 0.8284 0.9927 1.0046 0.027 Uiso 1 1 calc R . . C21 C 0.7303(2) 0.7715(3) 0.99755(11) 0.0234(4) Uani 1 1 d . . . H21 H 0.7335 0.7568 1.0488 0.028 Uiso 1 1 calc R . . C22 C 0.6696(2) 0.6528(3) 0.94984(11) 0.0226(4) Uani 1 1 d . . . H22 H 0.6322 0.5574 0.9674 0.027 Uiso 1 1 calc R . . C23 C 0.6664(2) 0.6804(2) 0.87562(10) 0.0183(4) Uani 1 1 d . . . N24 N 0.8305(2) 1.0552(2) 0.85864(9) 0.0194(3) Uani 1 1 d . . . N25 N 0.8122(2) 1.0442(2) 0.78267(9) 0.0184(3) Uani 1 1 d . . . C26 C 0.8777(2) 1.1735(3) 0.76034(12) 0.0230(4) Uani 1 1 d . . . H26 H 0.8823 1.1990 0.7105 0.028 Uiso 1 1 calc R . . C27 C 0.9398(3) 1.2683(3) 0.82107(12) 0.0268(4) Uani 1 1 d . . . H27 H 0.9926 1.3659 0.8197 0.032 Uiso 1 1 calc R . . C28 C 0.9078(3) 1.1895(3) 0.88229(12) 0.0255(4) Uani 1 1 d . . . H28 H 0.9345 1.2224 0.9318 0.031 Uiso 1 1 calc R . . N29 N 0.6112(2) 0.5781(2) 0.81764(9) 0.0195(3) Uani 1 1 d . . . N30 N 0.62398(19) 0.6293(2) 0.74757(9) 0.0177(3) Uani 1 1 d . . . C31 C 0.5758(3) 0.5097(3) 0.70385(12) 0.0235(4) Uani 1 1 d . . . H31 H 0.5725 0.5104 0.6521 0.028 Uiso 1 1 calc R . . C32 C 0.5303(3) 0.3815(3) 0.74429(13) 0.0267(4) Uani 1 1 d . . . H32 H 0.4912 0.2832 0.7256 0.032 Uiso 1 1 calc R . . C33 C 0.5544(2) 0.4287(3) 0.81647(12) 0.0239(4) Uani 1 1 d . . . H33 H 0.5351 0.3687 0.8576 0.029 Uiso 1 1 calc R . . B34 B 0.8007(3) 0.3036(3) 0.56024(13) 0.0269(5) Uani 1 1 d . . . F35 F 0.67987(18) 0.25580(18) 0.59926(7) 0.0320(3) Uani 1 1 d . . . F36 F 0.7685(2) 0.2516(2) 0.48760(8) 0.0398(4) Uani 1 1 d . . . F37 F 0.8059(2) 0.46689(19) 0.55982(9) 0.0434(4) Uani 1 1 d . . . F38 F 0.9458(2) 0.2431(3) 0.59299(9) 0.0564(5) Uani 1 1 d . . . B39 B 0.7164(3) 0.2805(4) 1.05415(14) 0.0290(5) Uani 1 1 d . . . F40 F 0.63904(17) 0.26675(19) 0.98207(7) 0.0331(3) Uani 1 1 d . . . F41 F 0.68305(17) 0.1500(2) 1.09549(8) 0.0370(4) Uani 1 1 d . . . F42 F 0.88085(18) 0.2829(3) 1.05290(8) 0.0493(5) Uani 1 1 d . . . F43 F 0.6647(3) 0.4138(2) 1.08554(10) 0.0630(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 0.01531(10) 0.01876(11) 0.01159(10) 0.00020(11) 0.00225(7) 0.00053(11) N2 0.0182(6) 0.0183(8) 0.0134(6) -0.0002(6) 0.0017(5) -0.0002(6) C3 0.0183(8) 0.0204(9) 0.0159(8) 0.0013(7) 0.0015(6) -0.0011(7) C4 0.0276(10) 0.0254(10) 0.0152(8) 0.0025(8) 0.0002(7) -0.0003(8) C5 0.0351(11) 0.0272(11) 0.0138(8) -0.0002(7) 0.0052(7) -0.0043(8) C6 0.0272(9) 0.0260(12) 0.0169(8) -0.0026(8) 0.0085(7) -0.0018(8) C7 0.0187(8) 0.0178(10) 0.0165(8) -0.0002(6) 0.0038(6) -0.0010(6) N8 0.0188(7) 0.0223(8) 0.0161(7) 0.0012(6) 0.0000(6) 0.0010(6) N9 0.0197(7) 0.0195(7) 0.0153(7) 0.0001(6) 0.0032(6) 0.0000(6) C10 0.0199(9) 0.0238(10) 0.0230(9) -0.0017(8) 0.0054(7) -0.0004(8) C11 0.0186(9) 0.0264(10) 0.0316(11) -0.0003(9) 0.0043(8) 0.0030(8) C12 0.0196(9) 0.0244(10) 0.0256(10) 0.0005(8) -0.0020(7) 0.0028(8) N13 0.0199(8) 0.0225(8) 0.0169(7) -0.0015(6) 0.0057(6) 0.0006(6) N14 0.0185(7) 0.0220(8) 0.0151(7) -0.0005(6) 0.0038(6) 0.0011(6) C15 0.0202(9) 0.0239(10) 0.0218(9) 0.0010(8) 0.0005(7) 0.0003(8) C16 0.0209(9) 0.0292(11) 0.0333(11) 0.0039(9) 0.0039(8) 0.0048(8) C17 0.0218(9) 0.0255(10) 0.0264(10) -0.0001(8) 0.0085(8) 0.0040(8) N18 0.0174(6) 0.0213(9) 0.0138(6) 0.0004(6) 0.0041(5) 0.0014(6) C19 0.0149(8) 0.0235(9) 0.0149(8) -0.0002(7) 0.0029(6) 0.0025(7) C20 0.0218(9) 0.0315(11) 0.0144(8) -0.0024(8) 0.0033(7) 0.0007(8) C21 0.0227(9) 0.0338(11) 0.0135(8) 0.0036(8) 0.0022(7) 0.0028(8) C22 0.0223(9) 0.0284(10) 0.0176(8) 0.0066(8) 0.0051(7) 0.0022(8) C23 0.0162(8) 0.0226(9) 0.0164(8) 0.0034(7) 0.0037(6) 0.0015(7) N24 0.0208(8) 0.0241(8) 0.0135(7) -0.0012(6) 0.0029(6) -0.0016(7) N25 0.0200(8) 0.0228(8) 0.0125(7) 0.0017(6) 0.0028(6) 0.0010(6) C26 0.0213(9) 0.0253(10) 0.0231(9) 0.0029(8) 0.0059(7) 0.0005(8) C27 0.0266(10) 0.0251(11) 0.0286(10) -0.0020(9) 0.0039(8) -0.0058(8) C28 0.0254(10) 0.0275(10) 0.0232(10) -0.0071(8) 0.0026(8) -0.0048(8) N29 0.0190(7) 0.0217(8) 0.0180(7) 0.0021(6) 0.0032(6) 0.0005(6) N30 0.0175(7) 0.0201(8) 0.0157(7) 0.0012(6) 0.0034(6) 0.0015(6) C31 0.0220(9) 0.0243(10) 0.0239(10) -0.0042(8) 0.0026(8) 0.0005(8) C32 0.0269(10) 0.0200(10) 0.0330(11) -0.0025(8) 0.0035(8) 0.0002(7) C33 0.0219(9) 0.0212(10) 0.0288(10) 0.0048(8) 0.0039(8) 0.0001(7) B34 0.0328(12) 0.0278(13) 0.0217(10) 0.0043(9) 0.0095(9) 0.0027(9) F35 0.0390(7) 0.0352(8) 0.0248(6) -0.0009(6) 0.0144(6) -0.0023(6) F36 0.0602(10) 0.0406(9) 0.0224(6) -0.0013(6) 0.0182(7) 0.0003(7) F37 0.0568(10) 0.0302(8) 0.0414(9) 0.0015(7) 0.0008(7) -0.0134(7) F38 0.0400(9) 0.0950(15) 0.0368(8) 0.0262(10) 0.0147(7) 0.0271(10) B39 0.0322(12) 0.0363(13) 0.0206(10) 0.0032(10) 0.0109(9) 0.0021(11) F40 0.0328(7) 0.0441(8) 0.0223(6) 0.0069(6) 0.0033(5) 0.0052(6) F41 0.0285(7) 0.0516(10) 0.0299(7) 0.0172(7) 0.0007(5) -0.0051(7) F42 0.0299(7) 0.0913(15) 0.0273(7) -0.0002(8) 0.0061(6) -0.0234(8) F43 0.1173(19) 0.0440(11) 0.0311(9) -0.0040(8) 0.0219(10) 0.0208(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 1.9049(15) . ? Fe1 N18 1.9097(16) . ? Fe1 N14 1.9751(17) . ? Fe1 N30 1.9760(18) . ? Fe1 N25 1.9912(18) . ? Fe1 N9 1.9913(17) . ? N2 C3 1.342(2) . ? N2 C7 1.349(2) . ? C3 C4 1.386(3) . ? C3 N8 1.409(2) . ? C4 C5 1.401(3) . ? C5 C6 1.390(3) . ? C6 C7 1.389(2) . ? C7 N13 1.408(2) . ? N8 C12 1.373(3) . ? N8 N9 1.380(2) . ? N9 C10 1.339(3) . ? C10 C11 1.413(3) . ? C11 C12 1.374(3) . ? N13 C17 1.370(3) . ? N13 N14 1.385(2) . ? N14 C15 1.327(3) . ? C15 C16 1.417(3) . ? C16 C17 1.369(3) . ? N18 C19 1.339(3) . ? N18 C23 1.348(3) . ? C19 C20 1.389(3) . ? C19 N24 1.405(3) . ? C20 C21 1.400(3) . ? C21 C22 1.392(3) . ? C22 C23 1.384(3) . ? C23 N29 1.408(3) . ? N24 C28 1.363(3) . ? N24 N25 1.389(2) . ? N25 C26 1.330(3) . ? C26 C27 1.420(3) . ? C27 C28 1.375(3) . ? N29 C33 1.365(3) . ? N29 N30 1.383(2) . ? N30 C31 1.330(3) . ? C31 C32 1.410(3) . ? C32 C33 1.377(3) . ? B34 F38 1.391(3) . ? B34 F35 1.398(3) . ? B34 F37 1.398(3) . ? B34 F36 1.399(3) . ? B39 F43 1.379(3) . ? B39 F40 1.399(3) . ? B39 F42 1.401(3) . ? B39 F41 1.403(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 178.15(8) . . ? N2 Fe1 N14 80.23(7) . . ? N18 Fe1 N14 98.99(7) . . ? N2 Fe1 N30 98.08(7) . . ? N18 Fe1 N30 80.22(7) . . ? N14 Fe1 N30 90.23(7) . . ? N2 Fe1 N25 101.77(7) . . ? N18 Fe1 N25 79.91(7) . . ? N14 Fe1 N25 91.30(7) . . ? N30 Fe1 N25 160.06(6) . . ? N2 Fe1 N9 79.97(7) . . ? N18 Fe1 N9 100.80(7) . . ? N14 Fe1 N9 160.19(7) . . ? N30 Fe1 N9 92.15(7) . . ? N25 Fe1 N9 93.10(7) . . ? C3 N2 C7 119.57(16) . . ? C3 N2 Fe1 120.43(13) . . ? C7 N2 Fe1 119.95(13) . . ? N2 C3 C4 122.81(18) . . ? N2 C3 N8 110.46(16) . . ? C4 C3 N8 126.73(18) . . ? C3 C4 C5 116.31(19) . . ? C6 C5 C4 122.24(18) . . ? C7 C6 C5 116.54(18) . . ? N2 C7 C6 122.51(17) . . ? N2 C7 N13 110.62(16) . . ? C6 C7 N13 126.86(17) . . ? C12 N8 N9 111.12(17) . . ? C12 N8 C3 131.86(18) . . ? N9 N8 C3 117.01(16) . . ? C10 N9 N8 105.30(17) . . ? C10 N9 Fe1 142.57(15) . . ? N8 N9 Fe1 112.13(12) . . ? N9 C10 C11 110.75(19) . . ? C12 C11 C10 106.16(19) . . ? N8 C12 C11 106.67(19) . . ? C17 N13 N14 111.03(17) . . ? C17 N13 C7 132.51(17) . . ? N14 N13 C7 116.44(16) . . ? C15 N14 N13 105.22(16) . . ? C15 N14 Fe1 141.86(14) . . ? N13 N14 Fe1 112.66(12) . . ? N14 C15 C16 111.00(19) . . ? C17 C16 C15 105.98(19) . . ? C16 C17 N13 106.77(19) . . ? C19 N18 C23 119.74(16) . . ? C19 N18 Fe1 120.41(13) . . ? C23 N18 Fe1 119.82(13) . . ? N18 C19 C20 122.56(19) . . ? N18 C19 N24 110.80(16) . . ? C20 C19 N24 126.63(19) . . ? C19 C20 C21 116.60(19) . . ? C22 C21 C20 121.75(18) . . ? C23 C22 C21 116.9(2) . . ? N18 C23 C22 122.46(19) . . ? N18 C23 N29 110.63(16) . . ? C22 C23 N29 126.91(19) . . ? C28 N24 N25 110.97(17) . . ? C28 N24 C19 132.12(18) . . ? N25 N24 C19 116.75(16) . . ? C26 N25 N24 105.35(17) . . ? C26 N25 Fe1 142.35(15) . . ? N24 N25 Fe1 112.13(12) . . ? N25 C26 C27 110.79(19) . . ? C28 C27 C26 105.8(2) . . ? N24 C28 C27 107.11(19) . . ? C33 N29 N30 110.95(17) . . ? C33 N29 C23 132.22(17) . . ? N30 N29 C23 116.68(17) . . ? C31 N30 N29 105.23(17) . . ? C31 N30 Fe1 142.05(15) . . ? N29 N30 Fe1 112.62(13) . . ? N30 C31 C32 111.21(19) . . ? C33 C32 C31 105.62(19) . . ? N29 C33 C32 106.99(19) . . ? F38 B34 F35 109.81(19) . . ? F38 B34 F37 110.3(2) . . ? F35 B34 F37 108.71(19) . . ? F38 B34 F36 109.6(2) . . ? F35 B34 F36 110.1(2) . . ? F37 B34 F36 108.31(19) . . ? F43 B39 F40 109.5(2) . . ? F43 B39 F42 111.9(2) . . ? F40 B39 F42 108.52(18) . . ? F43 B39 F41 109.17(19) . . ? F40 B39 F41 110.2(2) . . ? F42 B39 F41 107.5(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.554 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.057 #=END data_c:\datasets\leeds\mh140a~1\mh140a~1\mh140art _database_code_depnum_ccdc_archive 'CCDC 631322' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) 1.56:0.44 tetrafluoroborate: perchlorate salt ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H18 Fe N10, 1.56[B F4], 0.44[Cl O4]' _chemical_formula_sum 'C22 H18 B1.56 Cl0.44 F6.24 Fe N10 O1.76' _chemical_formula_weight 657.50 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.5441(6) _cell_length_b 8.5611(6) _cell_length_c 19.2084(13) _cell_angle_alpha 90.00 _cell_angle_beta 95.582(4) _cell_angle_gamma 90.00 _cell_volume 1398.37(17) _cell_formula_units_Z 2 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 42289 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 30.05 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 663 _exptl_absorpt_coefficient_mu 0.663 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.642 _exptl_absorpt_correction_T_max 0.764 _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 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42289 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 30.05 _reflns_number_total 7960 _reflns_number_gt 5169 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Extensive anion disorder in the model meant that distinct BF~4~^-^ and ClO~4~^-^ sites could not be distinguished. However, refinement of the same crystal at 150 K, when the rotational disorder in the two anions has frozen out, yielded relative occupancies of BF~4~^-^ and ClO~4~^-^ in the two sites of 0.77:0.23 for B34-F38:Cl34-O38 and 0.79:0.21 for B39-F43:Cl39-O43. This formulation was used for the density calculation at this temperature as well. For simplicity, however, the rotationally disordered anions were modelled using partial B and F atoms only. The F atoms of both anions are disordered over three orientations. For the anion centred on B34: F35A-F38A, occupancy 0.5 F35B-F38B, occupancy 0.25 F35C-F38C, occupancy 0.25 For the anion centred on B39: F40A-F43A, occupancy 0.5 F40B-F43B, occupancy 0.25 F40C-F43C, occupancy 0.25 All B---F distances were restrained to 1.37(2)\%A, and non-bonded F...F contacts within each disorder orientation to 2.24(2)\%A. Attempts to model disorder in the B atoms were unsuccessful, and two wholly occupied B sites were used in the final refinement. This probably accounts for distortions away from an ideal tetrahedral geometry in the partial anions. All non-H atoms with occupancy >=0.5 were modeled anisotropically, and all H atoms were placed in calculated positions and refined using a riding model. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+0.2241P] 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 0.0050(13) _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 0.047(17) _refine_ls_number_reflns 7960 _refine_ls_number_parameters 455 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1366 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.037 _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 0.26141(5) 0.16965(7) 0.25239(2) 0.05535(15) Uani 1 1 d . . . N2 N 0.2780(3) 0.1738(4) 0.36431(11) 0.0486(5) Uani 1 1 d . . . C3 C 0.4059(4) 0.1196(4) 0.40191(15) 0.0527(7) Uani 1 1 d . . . C4 C 0.4205(5) 0.1131(4) 0.47460(18) 0.0714(10) Uani 1 1 d . . . H4 H 0.5108 0.0751 0.4999 0.086 Uiso 1 1 calc R . . C5 C 0.2925(5) 0.1667(6) 0.50740(16) 0.0745(9) Uani 1 1 d . . . H5 H 0.2973 0.1643 0.5560 0.089 Uiso 1 1 calc R . . C6 C 0.1580(5) 0.2235(4) 0.46942(18) 0.0677(9) Uani 1 1 d . . . H6 H 0.0721 0.2587 0.4912 0.081 Uiso 1 1 calc R . . C7 C 0.1585(4) 0.2251(4) 0.39746(17) 0.0553(7) Uani 1 1 d . . . N8 N 0.5254(3) 0.0701(3) 0.36051(14) 0.0542(6) Uani 1 1 d . . . N9 N 0.4968(3) 0.0807(3) 0.28889(14) 0.0560(6) Uani 1 1 d . . . C10 C 0.6279(4) 0.0277(4) 0.2650(2) 0.0687(9) Uani 1 1 d . . . H10 H 0.6447 0.0228 0.2180 0.082 Uiso 1 1 calc R . . C11 C 0.7375(4) -0.0196(5) 0.3201(2) 0.0775(11) Uani 1 1 d . . . H11 H 0.8360 -0.0635 0.3166 0.093 Uiso 1 1 calc R . . C12 C 0.6697(4) 0.0120(4) 0.3796(2) 0.0729(10) Uani 1 1 d . . . H12 H 0.7147 -0.0036 0.4251 0.087 Uiso 1 1 calc R . . N13 N 0.0308(3) 0.2804(3) 0.35217(15) 0.0583(6) Uani 1 1 d . . . N14 N 0.0390(3) 0.2662(4) 0.28142(15) 0.0634(7) Uani 1 1 d . . . C15 C -0.0894(5) 0.3351(5) 0.2517(2) 0.0789(11) Uani 1 1 d . . . H15 H -0.1159 0.3428 0.2037 0.095 Uiso 1 1 calc R . . C16 C -0.1784(5) 0.3939(6) 0.3019(3) 0.0961(15) Uani 1 1 d . . . H16 H -0.2733 0.4471 0.2940 0.115 Uiso 1 1 calc R . . C17 C -0.0995(5) 0.3585(5) 0.3661(3) 0.0797(11) Uani 1 1 d . . . H17 H -0.1299 0.3834 0.4100 0.096 Uiso 1 1 calc R . . N18 N 0.2637(3) 0.1893(3) 0.14142(11) 0.0482(6) Uani 1 1 d . . . C19 C 0.2120(3) 0.0727(4) 0.09972(15) 0.0503(7) Uani 1 1 d . . . C20 C 0.2131(4) 0.0796(5) 0.02712(18) 0.0666(9) Uani 1 1 d . . . H20 H 0.1760 -0.0029 -0.0013 0.080 Uiso 1 1 calc R . . C21 C 0.2708(5) 0.2126(5) -0.00048(19) 0.0732(11) Uani 1 1 d . . . H21 H 0.2755 0.2193 -0.0486 0.088 Uiso 1 1 calc R . . C22 C 0.3223(4) 0.3375(5) 0.04147(18) 0.0676(9) Uani 1 1 d . . . H22 H 0.3587 0.4292 0.0226 0.081 Uiso 1 1 calc R . . C23 C 0.3170(3) 0.3192(4) 0.11320(17) 0.0553(7) Uani 1 1 d . . . N24 N 0.1544(3) -0.0565(3) 0.13581(13) 0.0539(6) Uani 1 1 d . . . N25 N 0.1602(3) -0.0477(3) 0.20756(13) 0.0562(6) Uani 1 1 d . . . C26 C 0.0921(4) -0.1803(5) 0.2254(2) 0.0700(9) Uani 1 1 d . . . H26 H 0.0790 -0.2084 0.2712 0.084 Uiso 1 1 calc R . . C27 C 0.0432(5) -0.2717(5) 0.1675(2) 0.0781(10) Uani 1 1 d . . . H27 H -0.0069 -0.3681 0.1670 0.094 Uiso 1 1 calc R . . C28 C 0.0850(4) -0.1885(5) 0.1114(2) 0.0717(10) Uani 1 1 d . . . H28 H 0.0683 -0.2183 0.0647 0.086 Uiso 1 1 calc R . . N29 N 0.3672(3) 0.4346(3) 0.16286(16) 0.0613(7) Uani 1 1 d . . . N30 N 0.3499(3) 0.4050(3) 0.23167(15) 0.0623(7) Uani 1 1 d . . . C31 C 0.4033(5) 0.5307(5) 0.2663(2) 0.0771(11) Uani 1 1 d . . . H31 H 0.4058 0.5437 0.3145 0.093 Uiso 1 1 calc R . . C32 C 0.4554(5) 0.6416(5) 0.2201(3) 0.0943(14) Uani 1 1 d . . . H32 H 0.4984 0.7393 0.2313 0.113 Uiso 1 1 calc R . . C33 C 0.4289(5) 0.5742(5) 0.1537(3) 0.0823(12) Uani 1 1 d . . . H33 H 0.4504 0.6185 0.1115 0.099 Uiso 1 1 calc R . . B34 B 0.2033(4) 0.7247(3) 0.42288(15) 0.0406(6) Uani 1 1 d D . . F35A F 0.3225(13) 0.7849(10) 0.3850(5) 0.077(2) Uani 0.50 1 d PD A 1 F36A F 0.2409(11) 0.7796(11) 0.4945(3) 0.083(2) Uani 0.50 1 d PD A 1 F37A F 0.2034(14) 0.5717(8) 0.4268(7) 0.134(5) Uani 0.50 1 d PD A 1 F38A F 0.0652(11) 0.7936(19) 0.3994(4) 0.119(4) Uani 0.50 1 d PD A 1 F35B F 0.297(3) 0.790(3) 0.3792(13) 0.164(14) Uiso 0.25 1 d PD A 2 F36B F 0.0493(17) 0.7198(17) 0.3878(9) 0.097(6) Uiso 0.25 1 d PD A 2 F37B F 0.209(3) 0.803(2) 0.4822(8) 0.108(9) Uiso 0.25 1 d PD A 2 F38B F 0.239(2) 0.5693(16) 0.4296(10) 0.089(5) Uiso 0.25 1 d PD A 2 F35C F 0.3421(18) 0.750(2) 0.4000(10) 0.105(8) Uiso 0.25 1 d PD A 3 F36C F 0.103(3) 0.844(2) 0.4095(14) 0.186(16) Uiso 0.25 1 d PD A 3 F37C F 0.2048(19) 0.660(3) 0.4854(7) 0.151(5) Uiso 0.25 1 d PD A 3 F38C F 0.130(2) 0.604(2) 0.3779(9) 0.168(7) Uiso 0.25 1 d PD A 3 B39 B 0.2607(4) 0.7013(4) -0.07484(16) 0.0508(8) Uani 1 1 d D . . F40A F 0.3369(9) 0.7145(8) -0.0022(3) 0.073(2) Uani 0.50 1 d PD B 1 F41A F 0.3242(9) 0.8248(12) -0.1091(4) 0.085(2) Uani 0.50 1 d PD B 1 F42A F 0.1101(7) 0.7172(13) -0.0668(4) 0.127(3) Uani 0.50 1 d PD B 1 F43A F 0.302(2) 0.5613(10) -0.0984(5) 0.179(6) Uani 0.50 1 d PD B 1 F40B F 0.1181(17) 0.639(2) -0.1078(9) 0.166(7) Uiso 0.25 1 d PD B 2 F41B F 0.257(2) 0.683(3) -0.0081(6) 0.153(9) Uiso 0.25 1 d PD B 2 F42B F 0.275(2) 0.8439(16) -0.1004(10) 0.112(8) Uiso 0.25 1 d PD B 2 F43B F 0.3718(17) 0.5993(18) -0.1001(9) 0.110(5) Uiso 0.25 1 d PD B 2 F40C F 0.3425(18) 0.7580(16) -0.1264(7) 0.102(7) Uiso 0.25 1 d PD B 3 F41C F 0.2051(18) 0.5544(15) -0.0951(9) 0.116(5) Uiso 0.25 1 d PD B 3 F42C F 0.1128(15) 0.7893(15) -0.0797(8) 0.094(4) Uiso 0.25 1 d PD B 3 F43C F 0.337(3) 0.704(3) -0.0138(8) 0.154(15) Uiso 0.25 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 0.0560(2) 0.0624(3) 0.0470(2) -0.0043(2) 0.00208(16) 0.0033(2) N2 0.0489(11) 0.0466(11) 0.0504(11) 0.0007(14) 0.0057(9) -0.0007(14) C3 0.0537(16) 0.0505(16) 0.0535(16) 0.0006(12) 0.0041(13) -0.0064(12) C4 0.083(2) 0.071(2) 0.0569(18) 0.0056(16) -0.0079(17) -0.0117(18) C5 0.109(3) 0.071(2) 0.0450(14) -0.008(2) 0.0123(16) -0.010(3) C6 0.078(2) 0.065(2) 0.0636(19) -0.0134(16) 0.0274(18) -0.0127(17) C7 0.0554(17) 0.0486(15) 0.0633(17) -0.0112(13) 0.0140(14) -0.0106(13) N8 0.0486(13) 0.0515(14) 0.0620(15) 0.0017(12) 0.0028(11) 0.0001(11) N9 0.0503(13) 0.0541(14) 0.0640(15) 0.0004(12) 0.0078(11) 0.0005(11) C10 0.061(2) 0.058(2) 0.092(3) -0.0031(18) 0.0288(19) -0.0012(16) C11 0.0500(19) 0.064(2) 0.118(3) -0.002(2) 0.004(2) 0.0058(17) C12 0.060(2) 0.063(2) 0.092(3) 0.008(2) -0.007(2) 0.0084(17) N13 0.0484(14) 0.0550(15) 0.0722(17) -0.0083(12) 0.0091(12) 0.0005(12) N14 0.0518(15) 0.0653(17) 0.0719(18) -0.0047(13) -0.0005(13) 0.0042(13) C15 0.063(2) 0.070(2) 0.099(3) 0.005(2) -0.017(2) -0.0014(19) C16 0.054(2) 0.080(3) 0.154(5) 0.003(3) 0.009(3) 0.014(2) C17 0.060(2) 0.065(2) 0.117(3) -0.010(2) 0.024(2) 0.0075(17) N18 0.0445(11) 0.0527(15) 0.0473(11) -0.0010(12) 0.0037(9) 0.0063(12) C19 0.0455(15) 0.0537(17) 0.0514(15) -0.0027(13) 0.0026(12) 0.0064(13) C20 0.065(2) 0.079(2) 0.0546(18) -0.0080(17) 0.0001(15) -0.0002(18) C21 0.076(2) 0.091(3) 0.0529(17) 0.0069(18) 0.0083(16) 0.010(2) C22 0.064(2) 0.072(2) 0.068(2) 0.0166(18) 0.0098(16) 0.0027(17) C23 0.0447(15) 0.0570(18) 0.0639(18) 0.0011(15) 0.0040(13) 0.0036(14) N24 0.0499(14) 0.0565(15) 0.0545(14) -0.0036(12) 0.0000(11) -0.0018(11) N25 0.0566(14) 0.0586(15) 0.0531(14) 0.0030(12) 0.0033(11) 0.0037(12) C26 0.069(2) 0.067(2) 0.075(2) 0.0087(19) 0.0097(18) 0.0011(18) C27 0.077(2) 0.060(2) 0.097(3) 0.001(2) 0.006(2) -0.0135(17) C28 0.061(2) 0.073(2) 0.080(2) -0.020(2) 0.0036(17) -0.0125(18) N29 0.0518(15) 0.0526(15) 0.0802(19) 0.0014(13) 0.0109(13) 0.0024(12) N30 0.0554(16) 0.0594(16) 0.0721(18) -0.0115(13) 0.0061(13) 0.0033(13) C31 0.064(2) 0.062(2) 0.103(3) -0.025(2) -0.003(2) 0.0103(18) C32 0.071(2) 0.060(3) 0.151(4) -0.019(3) 0.002(2) -0.0078(19) C33 0.070(2) 0.057(2) 0.121(4) 0.010(2) 0.015(2) -0.0015(18) B34 0.0460(16) 0.0378(13) 0.0387(14) 0.0060(11) 0.0086(12) 0.0010(12) F35A 0.097(4) 0.064(4) 0.077(4) -0.014(3) 0.051(4) -0.030(3) F36A 0.100(5) 0.096(5) 0.055(3) 0.006(3) 0.022(3) 0.016(4) F37A 0.165(10) 0.057(3) 0.169(8) 0.013(4) -0.045(7) -0.047(4) F38A 0.095(5) 0.184(11) 0.079(4) 0.026(6) 0.013(4) 0.059(7) B39 0.067(2) 0.045(2) 0.0413(14) 0.0039(12) 0.0135(14) -0.0121(15) F40A 0.090(5) 0.077(3) 0.051(2) 0.014(2) 0.004(2) 0.001(2) F41A 0.060(4) 0.115(7) 0.080(4) 0.039(5) 0.000(3) -0.025(4) F42A 0.079(3) 0.191(9) 0.113(5) -0.024(6) 0.019(3) -0.071(5) F43A 0.32(2) 0.130(7) 0.104(6) -0.001(5) 0.098(10) 0.000(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N18 2.140(2) . ? Fe1 N2 2.141(2) . ? Fe1 N25 2.193(3) . ? Fe1 N14 2.193(3) . ? Fe1 N9 2.201(3) . ? Fe1 N30 2.202(3) . ? N2 C7 1.330(4) . ? N2 C3 1.333(4) . ? C3 C4 1.391(5) . ? C3 N8 1.419(4) . ? C4 C5 1.391(6) . ? C5 C6 1.388(6) . ? C6 C7 1.383(5) . ? C7 N13 1.409(4) . ? N8 C12 1.347(4) . ? N8 N9 1.377(4) . ? N9 C10 1.330(4) . ? C10 C11 1.403(6) . ? C11 C12 1.358(6) . ? N13 C17 1.347(5) . ? N13 N14 1.373(4) . ? N14 C15 1.325(5) . ? C15 C16 1.380(7) . ? C16 C17 1.381(7) . ? N18 C19 1.328(4) . ? N18 C23 1.337(5) . ? C19 C20 1.397(5) . ? C19 N24 1.419(4) . ? C20 C21 1.368(6) . ? C21 C22 1.385(6) . ? C22 C23 1.392(5) . ? C23 N29 1.410(4) . ? N24 C28 1.340(4) . ? N24 N25 1.376(4) . ? N25 C26 1.335(5) . ? C26 C27 1.391(5) . ? C27 C28 1.367(5) . ? N29 C33 1.325(5) . ? N29 N30 1.368(4) . ? N30 C31 1.323(5) . ? C31 C32 1.401(7) . ? C32 C33 1.399(7) . ? B34 F35A 1.405(6) . ? B34 F36A 1.459(7) . ? B34 F37A 1.312(7) . ? B34 F38A 1.357(7) . ? B34 F35B 1.340(14) . ? B34 F36B 1.420(13) . ? B34 F37B 1.320(13) . ? B34 F38B 1.368(13) . ? B34 F35C 1.321(13) . ? B34 F36C 1.343(14) . ? B34 F37C 1.322(12) . ? B34 F38C 1.450(13) . ? B39 F40A 1.486(6) . ? B39 F41A 1.384(6) . ? B39 F42A 1.318(7) . ? B39 F43A 1.342(8) . ? B39 F40B 1.420(13) . ? B39 F41B 1.296(12) . ? B39 F42B 1.326(12) . ? B39 F43B 1.410(12) . ? B39 F40C 1.356(12) . ? B39 F41C 1.387(12) . ? B39 F42C 1.467(11) . ? B39 F43C 1.285(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 N18 Fe1 N2 173.06(12) . . ? N18 Fe1 N25 73.56(10) . . ? N2 Fe1 N25 113.17(11) . . ? N18 Fe1 N14 108.40(10) . . ? N2 Fe1 N14 73.31(10) . . ? N25 Fe1 N14 95.83(11) . . ? N18 Fe1 N9 104.35(10) . . ? N2 Fe1 N9 73.54(10) . . ? N25 Fe1 N9 98.32(10) . . ? N14 Fe1 N9 146.82(11) . . ? N18 Fe1 N30 73.23(11) . . ? N2 Fe1 N30 100.14(11) . . ? N25 Fe1 N30 146.61(10) . . ? N14 Fe1 N30 91.26(11) . . ? N9 Fe1 N30 93.16(10) . . ? C7 N2 C3 118.9(3) . . ? C7 N2 Fe1 120.5(2) . . ? C3 N2 Fe1 120.58(19) . . ? N2 C3 C4 123.1(3) . . ? N2 C3 N8 113.4(2) . . ? C4 C3 N8 123.5(3) . . ? C3 C4 C5 116.3(3) . . ? C6 C5 C4 121.6(3) . . ? C7 C6 C5 116.5(3) . . ? N2 C7 C6 123.6(3) . . ? N2 C7 N13 113.6(3) . . ? C6 C7 N13 122.9(3) . . ? C12 N8 N9 111.4(3) . . ? C12 N8 C3 130.4(3) . . ? N9 N8 C3 118.2(2) . . ? C10 N9 N8 104.4(3) . . ? C10 N9 Fe1 141.5(3) . . ? N8 N9 Fe1 114.14(18) . . ? N9 C10 C11 111.2(3) . . ? C12 C11 C10 105.6(3) . . ? N8 C12 C11 107.4(4) . . ? C17 N13 N14 111.3(3) . . ? C17 N13 C7 130.4(3) . . ? N14 N13 C7 118.0(2) . . ? C15 N14 N13 105.5(3) . . ? C15 N14 Fe1 139.4(3) . . ? N13 N14 Fe1 114.46(19) . . ? N14 C15 C16 110.5(4) . . ? C15 C16 C17 106.9(4) . . ? N13 C17 C16 105.8(4) . . ? C19 N18 C23 119.2(3) . . ? C19 N18 Fe1 120.5(2) . . ? C23 N18 Fe1 120.4(2) . . ? N18 C19 C20 122.4(3) . . ? N18 C19 N24 113.7(2) . . ? C20 C19 N24 123.9(3) . . ? C21 C20 C19 117.4(3) . . ? C20 C21 C22 121.6(3) . . ? C21 C22 C23 116.7(3) . . ? N18 C23 C22 122.7(3) . . ? N18 C23 N29 113.7(3) . . ? C22 C23 N29 123.6(3) . . ? C28 N24 N25 111.6(3) . . ? C28 N24 C19 130.5(3) . . ? N25 N24 C19 117.8(2) . . ? C26 N25 N24 103.7(3) . . ? C26 N25 Fe1 141.8(2) . . ? N24 N25 Fe1 114.45(19) . . ? N25 C26 C27 112.2(3) . . ? C28 C27 C26 104.9(3) . . ? N24 C28 C27 107.7(3) . . ? C33 N29 N30 112.2(3) . . ? C33 N29 C23 129.8(4) . . ? N30 N29 C23 118.0(3) . . ? C31 N30 N29 105.7(3) . . ? C31 N30 Fe1 139.6(3) . . ? N29 N30 Fe1 114.5(2) . . ? N30 C31 C32 110.4(4) . . ? C33 C32 C31 105.4(4) . . ? N29 C33 C32 106.4(4) . . ? F37A B34 F38A 116.6(9) . . ? F37A B34 F35A 113.6(7) . . ? F38A B34 F35A 108.6(8) . . ? F37A B34 F36A 105.5(7) . . ? F38A B34 F36A 106.2(6) . . ? F35A B34 F36A 105.4(5) . . ? F37B B34 F35B 110.8(13) . . ? F37B B34 F38B 115.1(11) . . ? F35B B34 F38B 109.0(12) . . ? F37B B34 F36B 112.2(11) . . ? F35B B34 F36B 107.4(12) . . ? F38B B34 F36B 101.8(10) . . ? F35C B34 F37C 116.1(10) . . ? F35C B34 F36C 112.8(13) . . ? F37C B34 F36C 116.4(12) . . ? F35C B34 F38C 105.6(11) . . ? F37C B34 F38C 101.9(11) . . ? F36C B34 F38C 101.4(12) . . ? F42A B39 F43A 115.2(8) . . ? F42A B39 F41A 114.1(7) . . ? F43A B39 F41A 113.1(7) . . ? F42A B39 F40A 103.1(5) . . ? F43A B39 F40A 106.2(7) . . ? F41A B39 F40A 103.5(5) . . ? F41B B39 F42B 119.5(12) . . ? F41B B39 F43B 110.1(10) . . ? F42B B39 F43B 110.6(9) . . ? F41B B39 F40B 107.1(10) . . ? F42B B39 F40B 106.7(10) . . ? F43B B39 F40B 101.1(10) . . ? F43C B39 F40C 114.0(12) . . ? F43C B39 F41C 113.7(13) . . ? F40C B39 F41C 107.9(9) . . ? F43C B39 F42C 114.0(12) . . ? F40C B39 F42C 105.8(8) . . ? F41C B39 F42C 100.3(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.425 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.046 #=END data_c:\datasets\leeds\mh140a~1\mh140a~2\mh140alt _database_code_depnum_ccdc_archive 'CCDC 631323' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) 1.56:0.44 tetrafluoroborate: perchlorate salt ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H18 Fe N10, 1.56[B F4], 0.44[Cl O4]' _chemical_formula_sum 'C22 H18 B1.56 Cl0.44 F6.24 Fe N10 O1.76' _chemical_formula_weight 657.50 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.5049(3) _cell_length_b 8.5662(4) _cell_length_c 18.4963(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.411(2) _cell_angle_gamma 90.00 _cell_volume 1333.05(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 39976 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 30.05 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour Brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 663 _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_T_max 0.903 _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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39976 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 30.05 _reflns_number_total 7581 _reflns_number_gt 6386 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Although distinct BF~4~^-^ and ClO~4~^-^ sites in the model could not be satisfactorily refined, microanalysis of the sample confirmed the presence of ca. 15% perchlorate in the crystal in the sample. In addition, attempts to refine the two, crystallographically ordered, anion sites as 100% BF~4~^-^ afforded B atoms that were non-positive definite. This problem was solved by including a fraction of Cl in these sites. Both anion sites were modelled using partial BF~4~^-^ and ClO~4~^-^ molecules, with equivalent atoms in each partial ion constrained to have identical coordinates and thermal parameters (SHELXL EXYZ and EADP instructions). The relative occupancies of BF~4~^-^ and ClO~4~^-^ in each site were refined as 0.771(6):0.229(6) for B34-F38:Cl34-O38 and 0.786(5):0.214(5) for B39-F43:Cl39-O43. These fixed occupancies were used in the final refinement. All non-H atoms were refined anisotropically, and no restraints were applied. All H atoms were placed in caclulated positions and refined using a riding model. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+1.0444P] 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 0.0045(7) _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 0.041(15) _refine_ls_number_reflns 7581 _refine_ls_number_parameters 391 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.1004 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.28651(5) 0.15822(5) 0.25354(2) 0.01859(10) Uani 1 1 d . . . N2 N 0.2920(3) 0.1376(3) 0.35652(12) 0.0196(5) Uani 1 1 d . . . C3 C 0.4193(4) 0.0783(4) 0.39820(16) 0.0228(6) Uani 1 1 d . . . C4 C 0.4307(4) 0.0628(4) 0.47317(17) 0.0281(7) Uani 1 1 d . . . H4 H 0.5217 0.0190 0.5019 0.034 Uiso 1 1 calc R . . C5 C 0.2994(4) 0.1160(4) 0.50432(16) 0.0277(7) Uani 1 1 d . . . H5 H 0.3022 0.1081 0.5557 0.033 Uiso 1 1 calc R . . C6 C 0.1668(4) 0.1792(4) 0.46298(16) 0.0270(7) Uani 1 1 d . . . H6 H 0.0785 0.2139 0.4848 0.032 Uiso 1 1 calc R . . C7 C 0.1675(3) 0.1899(3) 0.38807(15) 0.0202(6) Uani 1 1 d . . . N8 N 0.5344(3) 0.0354(3) 0.35464(13) 0.0228(5) Uani 1 1 d . . . N9 N 0.5004(3) 0.0635(3) 0.28048(13) 0.0218(5) Uani 1 1 d . . . C10 C 0.6285(4) 0.0156(4) 0.25294(18) 0.0251(6) Uani 1 1 d . . . H10 H 0.6398 0.0204 0.2026 0.030 Uiso 1 1 calc R . . C11 C 0.7446(4) -0.0429(4) 0.30801(18) 0.0288(7) Uani 1 1 d . . . H11 H 0.8454 -0.0845 0.3020 0.035 Uiso 1 1 calc R . . C12 C 0.6837(4) -0.0280(4) 0.37222(18) 0.0277(7) Uani 1 1 d . . . H12 H 0.7346 -0.0560 0.4196 0.033 Uiso 1 1 calc R . . N13 N 0.0497(3) 0.2533(3) 0.33571(14) 0.0238(5) Uani 1 1 d . . . N14 N 0.0763(3) 0.2471(3) 0.26339(13) 0.0218(5) Uani 1 1 d . . . C15 C -0.0485(4) 0.3158(4) 0.22580(18) 0.0268(7) Uani 1 1 d . . . H15 H -0.0637 0.3285 0.1742 0.032 Uiso 1 1 calc R . . C16 C -0.1563(4) 0.3680(4) 0.27139(19) 0.0307(7) Uani 1 1 d . . . H16 H -0.2543 0.4204 0.2570 0.037 Uiso 1 1 calc R . . C17 C -0.0910(4) 0.3277(4) 0.34021(18) 0.0278(7) Uani 1 1 d . . . H17 H -0.1350 0.3475 0.3837 0.033 Uiso 1 1 calc R . . N18 N 0.2815(3) 0.1861(3) 0.15053(12) 0.0213(6) Uani 1 1 d . . . C19 C 0.2211(3) 0.0741(4) 0.10409(16) 0.0224(6) Uani 1 1 d . . . C20 C 0.2121(4) 0.0890(4) 0.02915(17) 0.0268(7) Uani 1 1 d . . . H20 H 0.1702 0.0084 -0.0033 0.032 Uiso 1 1 calc R . . C21 C 0.2685(4) 0.2300(4) 0.00369(17) 0.0281(7) Uani 1 1 d . . . H21 H 0.2645 0.2449 -0.0474 0.034 Uiso 1 1 calc R . . C22 C 0.3301(4) 0.3488(4) 0.05116(17) 0.0275(7) Uani 1 1 d . . . H22 H 0.3683 0.4439 0.0338 0.033 Uiso 1 1 calc R . . C23 C 0.3324(4) 0.3202(4) 0.12491(16) 0.0226(6) Uani 1 1 d . . . N24 N 0.1688(3) -0.0546(3) 0.14155(13) 0.0231(5) Uani 1 1 d . . . N25 N 0.1874(3) -0.0434(3) 0.21726(13) 0.0222(5) Uani 1 1 d . . . C26 C 0.1224(4) -0.1719(4) 0.23939(18) 0.0265(7) Uani 1 1 d . . . H26 H 0.1176 -0.1974 0.2890 0.032 Uiso 1 1 calc R . . C27 C 0.0608(4) -0.2662(4) 0.17892(18) 0.0308(7) Uani 1 1 d . . . H27 H 0.0088 -0.3641 0.1803 0.037 Uiso 1 1 calc R . . C28 C 0.0916(4) -0.1877(4) 0.11790(19) 0.0329(8) Uani 1 1 d . . . H28 H 0.0641 -0.2202 0.0686 0.039 Uiso 1 1 calc R . . N29 N 0.3886(3) 0.4220(3) 0.18271(14) 0.0240(5) Uani 1 1 d . . . N30 N 0.3759(3) 0.3713(3) 0.25217(13) 0.0205(5) Uani 1 1 d . . . C31 C 0.4249(4) 0.4902(4) 0.29551(18) 0.0273(7) Uani 1 1 d . . . H31 H 0.4288 0.4890 0.3471 0.033 Uiso 1 1 calc R . . C32 C 0.4701(4) 0.6173(4) 0.25598(19) 0.0313(7) Uani 1 1 d . . . H32 H 0.5097 0.7149 0.2750 0.038 Uiso 1 1 calc R . . C33 C 0.4453(4) 0.5719(4) 0.18400(18) 0.0277(7) Uani 1 1 d . . . H33 H 0.4639 0.6326 0.1431 0.033 Uiso 1 1 calc R . . B34 B 0.1987(3) 0.6968(3) 0.43992(12) 0.0404(6) Uani 0.77 1 d P A 1 F35 F 0.3190(3) 0.7437(3) 0.40070(11) 0.0358(5) Uani 0.77 1 d P A 1 F36 F 0.2289(3) 0.7494(3) 0.51251(11) 0.0441(6) Uani 0.77 1 d P A 1 F37 F 0.1932(3) 0.5319(3) 0.44043(13) 0.0487(6) Uani 0.77 1 d P A 1 F38 F 0.0526(3) 0.7564(4) 0.40671(13) 0.0598(8) Uani 0.77 1 d P A 1 Cl34 Cl 0.1987(3) 0.6968(3) 0.43992(12) 0.0404(6) Uani 0.23 1 d P B 2 O35 O 0.3190(3) 0.7437(3) 0.40070(11) 0.0358(5) Uani 0.23 1 d P B 2 O36 O 0.2289(3) 0.7494(3) 0.51251(11) 0.0441(6) Uani 0.23 1 d P B 2 O37 O 0.1932(3) 0.5319(3) 0.44043(13) 0.0487(6) Uani 0.23 1 d P B 2 O38 O 0.0526(3) 0.7564(4) 0.40671(13) 0.0598(8) Uani 0.23 1 d P B 2 B39 B 0.2834(3) 0.7204(3) -0.05453(13) 0.0417(6) Uani 0.79 1 d P C 1 F40 F 0.3616(3) 0.7340(3) 0.01791(10) 0.0382(5) Uani 0.79 1 d P C 1 F41 F 0.3170(3) 0.8505(3) -0.09575(12) 0.0418(6) Uani 0.79 1 d P C 1 F42 F 0.1191(3) 0.7191(4) -0.05273(12) 0.0545(8) Uani 0.79 1 d P C 1 F43 F 0.3355(4) 0.5870(3) -0.08550(14) 0.0728(10) Uani 0.79 1 d P C 1 Cl39 Cl 0.2834(3) 0.7204(3) -0.05453(13) 0.0417(6) Uani 0.21 1 d P D 2 O40 O 0.3616(3) 0.7340(3) 0.01791(10) 0.0382(5) Uani 0.21 1 d P D 2 O41 O 0.3170(3) 0.8505(3) -0.09575(12) 0.0418(6) Uani 0.21 1 d P D 2 O42 O 0.1191(3) 0.7191(4) -0.05273(12) 0.0545(8) Uani 0.21 1 d P D 2 O43 O 0.3355(4) 0.5870(3) -0.08550(14) 0.0728(10) Uani 0.21 1 d P D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01898(18) 0.02111(19) 0.01538(16) 0.00005(18) 0.00150(13) 0.0009(2) N2 0.0225(11) 0.0186(13) 0.0173(10) -0.0006(10) 0.0010(9) -0.0019(11) C3 0.0241(15) 0.0233(15) 0.0207(14) -0.0011(12) 0.0021(12) -0.0010(12) C4 0.0309(17) 0.0311(17) 0.0206(14) 0.0034(13) -0.0019(12) -0.0033(14) C5 0.0408(18) 0.0252(16) 0.0172(13) -0.0021(11) 0.0045(13) -0.0041(13) C6 0.0329(16) 0.0259(18) 0.0242(13) -0.0046(13) 0.0103(12) -0.0021(14) C7 0.0240(14) 0.0167(16) 0.0197(12) -0.0012(10) 0.0024(11) -0.0024(11) N8 0.0213(13) 0.0251(13) 0.0205(12) 0.0028(10) -0.0020(10) 0.0009(11) N9 0.0237(13) 0.0216(12) 0.0203(12) -0.0006(10) 0.0036(10) -0.0020(10) C10 0.0242(16) 0.0250(15) 0.0265(15) -0.0017(12) 0.0046(13) -0.0018(13) C11 0.0230(16) 0.0255(16) 0.0376(18) 0.0003(14) 0.0036(14) 0.0015(13) C12 0.0198(15) 0.0305(17) 0.0304(16) 0.0011(14) -0.0042(13) 0.0033(13) N13 0.0219(13) 0.0275(13) 0.0228(12) -0.0022(11) 0.0054(10) -0.0009(11) N14 0.0210(12) 0.0236(13) 0.0207(12) -0.0008(10) 0.0021(10) 0.0009(10) C15 0.0248(16) 0.0273(16) 0.0271(16) 0.0032(13) -0.0003(13) -0.0010(13) C16 0.0206(16) 0.0304(18) 0.0406(19) 0.0041(15) 0.0027(14) 0.0042(14) C17 0.0258(16) 0.0280(17) 0.0315(17) -0.0019(13) 0.0106(13) 0.0042(13) N18 0.0206(11) 0.0247(15) 0.0184(11) -0.0013(10) 0.0026(9) 0.0007(10) C19 0.0160(14) 0.0281(16) 0.0224(14) -0.0010(12) 0.0010(11) 0.0003(12) C20 0.0253(16) 0.0363(17) 0.0194(14) -0.0031(13) 0.0057(12) 0.0001(14) C21 0.0307(17) 0.0357(18) 0.0183(14) 0.0067(13) 0.0050(13) 0.0041(15) C22 0.0288(17) 0.0322(17) 0.0222(15) 0.0066(13) 0.0059(13) 0.0016(14) C23 0.0217(15) 0.0261(16) 0.0202(14) 0.0050(12) 0.0035(12) 0.0037(12) N24 0.0232(13) 0.0277(14) 0.0175(11) -0.0037(10) 0.0004(10) -0.0031(11) N25 0.0214(13) 0.0279(13) 0.0163(11) 0.0009(10) -0.0007(10) -0.0008(11) C26 0.0265(16) 0.0260(16) 0.0272(16) 0.0032(13) 0.0049(13) 0.0002(13) C27 0.0277(16) 0.0293(17) 0.0350(17) -0.0018(14) 0.0035(14) -0.0075(14) C28 0.0366(19) 0.0295(17) 0.0318(17) -0.0110(14) 0.0028(15) -0.0037(15) N29 0.0224(13) 0.0245(13) 0.0244(13) 0.0016(11) 0.0011(10) 0.0022(11) N30 0.0184(12) 0.0233(13) 0.0201(12) 0.0011(10) 0.0038(10) 0.0014(10) C31 0.0248(16) 0.0284(17) 0.0283(16) -0.0055(13) 0.0027(13) 0.0001(13) C32 0.0279(16) 0.0251(17) 0.0395(18) -0.0043(13) 0.0004(14) -0.0007(13) C33 0.0252(16) 0.0234(16) 0.0345(17) 0.0057(13) 0.0046(13) -0.0012(13) B34 0.0500(14) 0.0403(14) 0.0323(10) 0.0048(9) 0.0107(10) 0.0036(10) F35 0.0435(12) 0.0374(12) 0.0290(10) -0.0021(9) 0.0137(9) -0.0028(10) F36 0.0654(16) 0.0457(13) 0.0245(10) -0.0020(10) 0.0173(10) 0.0004(12) F37 0.0638(17) 0.0304(12) 0.0490(14) 0.0013(11) -0.0010(12) -0.0125(12) F38 0.0436(14) 0.100(2) 0.0380(12) 0.0264(14) 0.0144(11) 0.0281(15) Cl34 0.0500(14) 0.0403(14) 0.0323(10) 0.0048(9) 0.0107(10) 0.0036(10) O35 0.0435(12) 0.0374(12) 0.0290(10) -0.0021(9) 0.0137(9) -0.0028(10) O36 0.0654(16) 0.0457(13) 0.0245(10) -0.0020(10) 0.0173(10) 0.0004(12) O37 0.0638(17) 0.0304(12) 0.0490(14) 0.0013(11) -0.0010(12) -0.0125(12) O38 0.0436(14) 0.100(2) 0.0380(12) 0.0264(14) 0.0144(11) 0.0281(15) B39 0.0469(14) 0.0484(14) 0.0318(11) 0.0051(10) 0.0125(11) 0.0009(12) F40 0.0394(12) 0.0502(13) 0.0239(10) 0.0082(9) 0.0007(9) 0.0059(10) F41 0.0325(12) 0.0562(15) 0.0350(11) 0.0187(11) -0.0010(9) -0.0090(11) F42 0.0317(11) 0.101(2) 0.0317(11) -0.0034(12) 0.0064(9) -0.0240(13) F43 0.131(3) 0.0528(17) 0.0375(14) -0.0077(12) 0.0230(16) 0.0254(17) Cl39 0.0469(14) 0.0484(14) 0.0318(11) 0.0051(10) 0.0125(11) 0.0009(12) O40 0.0394(12) 0.0502(13) 0.0239(10) 0.0082(9) 0.0007(9) 0.0059(10) O41 0.0325(12) 0.0562(15) 0.0350(11) 0.0187(11) -0.0010(9) -0.0090(11) O42 0.0317(11) 0.101(2) 0.0317(11) -0.0034(12) 0.0064(9) -0.0240(13) O43 0.131(3) 0.0528(17) 0.0375(14) -0.0077(12) 0.0230(16) 0.0254(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.907(2) . ? Fe1 N18 1.914(2) . ? Fe1 N14 1.976(3) . ? Fe1 N30 1.979(3) . ? Fe1 N9 1.987(3) . ? Fe1 N25 1.994(3) . ? N2 C3 1.334(4) . ? N2 C7 1.358(4) . ? C3 C4 1.382(4) . ? C3 N8 1.404(4) . ? C4 C5 1.405(5) . ? C5 C6 1.377(5) . ? C6 C7 1.390(4) . ? C7 N13 1.397(4) . ? N8 C12 1.376(4) . ? N8 N9 1.381(3) . ? N9 C10 1.334(4) . ? C10 C11 1.403(5) . ? C11 C12 1.369(5) . ? N13 C17 1.369(4) . ? N13 N14 1.390(3) . ? N14 C15 1.320(4) . ? C15 C16 1.406(5) . ? C16 C17 1.357(5) . ? N18 C23 1.338(4) . ? N18 C19 1.339(4) . ? C19 C20 1.383(4) . ? C19 N24 1.408(4) . ? C20 C21 1.406(5) . ? C21 C22 1.395(5) . ? C22 C23 1.383(4) . ? C23 N29 1.408(4) . ? N24 C28 1.356(4) . ? N24 N25 1.389(3) . ? N25 C26 1.324(4) . ? C26 C27 1.416(5) . ? C27 C28 1.372(5) . ? N29 C33 1.371(4) . ? N29 N30 1.375(3) . ? N30 C31 1.325(4) . ? C31 C32 1.396(5) . ? C32 C33 1.373(5) . ? B34 F35 1.397(3) . ? B34 F38 1.399(3) . ? B34 F36 1.404(3) . ? B34 F37 1.413(3) . ? B39 F43 1.380(4) . ? B39 F42 1.403(3) . ? B39 F41 1.403(3) . ? B39 F40 1.411(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 178.14(12) . . ? N2 Fe1 N14 80.44(10) . . ? N18 Fe1 N14 98.92(10) . . ? N2 Fe1 N30 98.32(10) . . ? N18 Fe1 N30 79.92(11) . . ? N14 Fe1 N30 90.02(10) . . ? N2 Fe1 N9 79.86(10) . . ? N18 Fe1 N9 100.76(10) . . ? N14 Fe1 N9 160.29(10) . . ? N30 Fe1 N9 92.33(10) . . ? N2 Fe1 N25 101.74(11) . . ? N18 Fe1 N25 80.00(11) . . ? N14 Fe1 N25 91.21(11) . . ? N30 Fe1 N25 159.82(10) . . ? N9 Fe1 N25 93.25(11) . . ? C3 N2 C7 119.7(2) . . ? C3 N2 Fe1 120.77(19) . . ? C7 N2 Fe1 119.48(19) . . ? N2 C3 C4 123.2(3) . . ? N2 C3 N8 110.1(2) . . ? C4 C3 N8 126.7(3) . . ? C3 C4 C5 115.9(3) . . ? C6 C5 C4 122.4(3) . . ? C5 C6 C7 117.2(3) . . ? N2 C7 C6 121.6(3) . . ? N2 C7 N13 110.8(2) . . ? C6 C7 N13 127.6(3) . . ? C12 N8 N9 110.8(3) . . ? C12 N8 C3 131.6(3) . . ? N9 N8 C3 117.5(2) . . ? C10 N9 N8 105.2(2) . . ? C10 N9 Fe1 143.0(2) . . ? N8 N9 Fe1 111.80(18) . . ? N9 C10 C11 111.1(3) . . ? C12 C11 C10 106.3(3) . . ? C11 C12 N8 106.5(3) . . ? C17 N13 N14 110.1(2) . . ? C17 N13 C7 133.1(3) . . ? N14 N13 C7 116.8(2) . . ? C15 N14 N13 105.0(2) . . ? C15 N14 Fe1 142.4(2) . . ? N13 N14 Fe1 112.35(18) . . ? N14 C15 C16 111.8(3) . . ? C17 C16 C15 105.6(3) . . ? C16 C17 N13 107.6(3) . . ? C23 N18 C19 120.1(3) . . ? C23 N18 Fe1 119.9(2) . . ? C19 N18 Fe1 120.0(2) . . ? N18 C19 C20 122.5(3) . . ? N18 C19 N24 111.4(2) . . ? C20 C19 N24 126.2(3) . . ? C19 C20 C21 116.3(3) . . ? C22 C21 C20 122.1(3) . . ? C23 C22 C21 116.2(3) . . ? N18 C23 C22 122.9(3) . . ? N18 C23 N29 110.7(2) . . ? C22 C23 N29 126.4(3) . . ? C28 N24 N25 111.2(3) . . ? C28 N24 C19 132.3(3) . . ? N25 N24 C19 116.4(2) . . ? C26 N25 N24 105.2(2) . . ? C26 N25 Fe1 142.3(2) . . ? N24 N25 Fe1 112.29(19) . . ? N25 C26 C27 110.7(3) . . ? C28 C27 C26 106.1(3) . . ? N24 C28 C27 106.8(3) . . ? C33 N29 N30 110.8(3) . . ? C33 N29 C23 132.3(3) . . ? N30 N29 C23 116.7(2) . . ? C31 N30 N29 105.2(3) . . ? C31 N30 Fe1 142.0(2) . . ? N29 N30 Fe1 112.70(19) . . ? N30 C31 C32 111.6(3) . . ? C33 C32 C31 105.8(3) . . ? N29 C33 C32 106.6(3) . . ? F35 B34 F38 109.73(19) . . ? F35 B34 F36 111.0(2) . . ? F38 B34 F36 109.2(2) . . ? F35 B34 F37 108.6(2) . . ? F38 B34 F37 109.9(3) . . ? F36 B34 F37 108.4(2) . . ? F43 B39 F42 112.6(3) . . ? F43 B39 F41 109.2(2) . . ? F42 B39 F41 107.6(2) . . ? F43 B39 F40 109.1(2) . . ? F42 B39 F40 108.1(2) . . ? F41 B39 F40 110.2(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.399 _refine_diff_density_min -0.794 _refine_diff_density_rms 0.074 #=END data_c:\datasets\leeds\mh140b~1\mh140b~1\mh140brt _database_code_depnum_ccdc_archive 'CCDC 631324' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) 0.87:1.13 tetrafluoroborate: perchlorate salt ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H18 Fe N10, 0.87[B F4], 1.13[Cl O4]' _chemical_formula_sum 'C22 H18 B0.87 Cl1.13 F3.48 Fe N10 O4.52' _chemical_formula_weight 666.22 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.5693(3) _cell_length_b 8.5868(3) _cell_length_c 19.3352(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.597(2) _cell_angle_gamma 90.00 _cell_volume 1415.96(9) _cell_formula_units_Z 2 _cell_measurement_temperature 300(2) _diffrn_reflns_number 18134 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 30.05 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 674 _exptl_absorpt_coefficient_mu 0.713 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.792 _exptl_absorpt_correction_T_max 0.927 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 4 kW. ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? #_diffrn_reflns_number 18134 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 30.05 _reflns_number_total 7704 _reflns_number_gt 5063 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Extensive anion disorder in the model meant that distinct BF~4~^-^ and ClO~4~^-^ sites could not be distinguished. However, refinement of the same crystal at 150 K, when distinct partial BF~4~^-^ and ClO~4~^-^ sites were resolved, yielded relative occupancies of BF~4~^-^ and ClO~4~^-^ in the two sites of 0.42:0.58 for B34-F38:Cl34-O38 and 0.45:0.55 for B39-F43:Cl39-O43. This formulation was used for the density calculation at this temperature as well. The B/Cl sites for each anion (B34/Cl34 and B39/Cl39) were modelled using partial B and Cl atoms with the relative occupancies given above, constrained to have the same coordinates and anisotropic thermal parameters (SHELXL EXYZ and EADP instructions). All the other partial atoms in the rotationally disordered anions were modelled as F, since F and O atoms cannot be distinguished in a Fourier map under these conditions. The tabulated distances and angles involving to B34 and B39 in fact refer to the combined B34/Cl34 and B39/Cl39 sites. The F atoms of both anions are disordered over three orientations. For the anion centred on B34/Cl34: F35A-F38A, occupancy 0.5 F35B-F38B, occupancy 0.25 F35C-F38C, occupancy 0.25 For the anion centred on B39/Cl39: F40A-F43A, occupancy 0.4 F40B-F43B, occupancy 0.3 F40C-F43C, occupancy 0.3 All B/Cl---F bonds were restrained to 1.42(2)\%A, and all non-bonded distances within each disorder orientation to 2.32(2)\%A. Attempts to model disorder in theB/Cl sites were unsuccessful, and a single wholly occupied B/Cl site for each anions was used in the final refinement. This probably accounts for distortions away from an ideal tetrahedral geometry in the partial anions. All non-H atoms with occupancy >=0.5 were modeled anisotropically, and all H atoms were placed in calculated positions and refined using a riding model. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0904P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.024(19) _refine_ls_number_reflns 7704 _refine_ls_number_parameters 433 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0848 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1551 _refine_ls_wR_factor_gt 0.1343 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.73895(5) 0.83070(8) 0.74769(2) 0.05467(16) Uani 1 1 d . . . N2 N 0.7225(3) 0.8281(4) 0.63685(13) 0.0497(6) Uani 1 1 d . . . C3 C 0.5945(4) 0.8799(4) 0.59847(17) 0.0509(7) Uani 1 1 d . . . C4 C 0.5795(5) 0.8871(5) 0.5270(2) 0.0704(11) Uani 1 1 d . . . H4 H 0.4893 0.9254 0.5021 0.084 Uiso 1 1 calc R . . C5 C 0.7077(5) 0.8334(7) 0.4939(2) 0.0758(10) Uani 1 1 d . . . H5 H 0.7025 0.8352 0.4457 0.091 Uiso 1 1 calc R . . C6 C 0.8417(5) 0.7780(5) 0.5316(2) 0.0678(11) Uani 1 1 d . . . H6 H 0.9274 0.7436 0.5098 0.081 Uiso 1 1 calc R . . C7 C 0.8421(4) 0.7760(4) 0.60271(19) 0.0544(8) Uani 1 1 d . . . N8 N 0.4752(3) 0.9304(4) 0.64040(16) 0.0535(7) Uani 1 1 d . . . N9 N 0.5042(3) 0.9195(4) 0.71159(15) 0.0542(7) Uani 1 1 d . . . C10 C 0.3737(5) 0.9738(5) 0.7350(2) 0.0655(10) Uani 1 1 d . . . H10 H 0.3576 0.9797 0.7818 0.079 Uiso 1 1 calc R . . C11 C 0.2647(4) 1.0204(5) 0.6815(3) 0.0787(13) Uani 1 1 d . . . H11 H 0.1662 1.0628 0.6856 0.094 Uiso 1 1 calc R . . C12 C 0.3300(4) 0.9921(5) 0.6223(3) 0.0725(11) Uani 1 1 d . . . H12 H 0.2847 1.0109 0.5774 0.087 Uiso 1 1 calc R . . N13 N 0.9680(3) 0.7198(4) 0.64873(17) 0.0576(7) Uani 1 1 d . . . N14 N 0.9599(3) 0.7337(4) 0.71893(17) 0.0624(8) Uani 1 1 d . . . C15 C 1.0896(5) 0.6616(6) 0.7473(3) 0.0790(13) Uani 1 1 d . . . H15 H 1.1151 0.6500 0.7949 0.095 Uiso 1 1 calc R . . C16 C 1.1788(5) 0.6077(6) 0.6985(4) 0.0954(17) Uani 1 1 d . . . H16 H 1.2748 0.5569 0.7064 0.114 Uiso 1 1 calc R . . C17 C 1.0996(5) 0.6428(6) 0.6344(3) 0.0818(14) Uani 1 1 d . . . H17 H 1.1302 0.6187 0.5909 0.098 Uiso 1 1 calc R . . N18 N 0.7370(3) 0.8113(4) 0.85785(14) 0.0491(6) Uani 1 1 d . . . C19 C 0.7895(3) 0.9272(4) 0.90047(18) 0.0506(8) Uani 1 1 d . . . C20 C 0.7899(4) 0.9213(6) 0.9712(2) 0.0649(10) Uani 1 1 d . . . H20 H 0.8275 1.0036 0.9993 0.078 Uiso 1 1 calc R . . C21 C 0.7311(5) 0.7857(7) 0.9993(2) 0.0770(14) Uani 1 1 d . . . H21 H 0.7273 0.7782 1.0471 0.092 Uiso 1 1 calc R . . C22 C 0.6786(5) 0.6630(6) 0.9572(2) 0.0669(10) Uani 1 1 d . . . H22 H 0.6408 0.5719 0.9756 0.080 Uiso 1 1 calc R . . C23 C 0.6848(4) 0.6816(4) 0.8862(2) 0.0544(8) Uani 1 1 d . . . N24 N 0.8458(3) 1.0551(4) 0.86355(14) 0.0530(7) Uani 1 1 d . . . N25 N 0.8394(3) 1.0473(4) 0.79215(15) 0.0567(7) Uani 1 1 d . . . C26 C 0.9074(4) 1.1776(5) 0.7744(2) 0.0678(10) Uani 1 1 d . . . H26 H 0.9204 1.2059 0.7289 0.081 Uiso 1 1 calc R . . C27 C 0.9579(5) 1.2684(6) 0.8334(2) 0.0770(12) Uani 1 1 d . . . H27 H 1.0091 1.3640 0.8339 0.092 Uiso 1 1 calc R . . C28 C 0.9169(5) 1.1886(6) 0.8885(2) 0.0718(11) Uani 1 1 d . . . H28 H 0.9337 1.2186 0.9348 0.086 Uiso 1 1 calc R . . N29 N 0.6347(3) 0.5659(4) 0.83631(18) 0.0597(8) Uani 1 1 d . . . N30 N 0.6498(3) 0.5952(4) 0.76835(17) 0.0605(8) Uani 1 1 d . . . C31 C 0.5947(5) 0.4678(6) 0.7349(3) 0.0794(13) Uani 1 1 d . . . H31 H 0.5920 0.4540 0.6871 0.095 Uiso 1 1 calc R . . C32 C 0.5422(5) 0.3589(6) 0.7795(3) 0.0899(15) Uani 1 1 d . . . H32 H 0.4979 0.2622 0.7683 0.108 Uiso 1 1 calc R . . C33 C 0.5698(5) 0.4248(5) 0.8446(3) 0.0840(14) Uani 1 1 d . . . H33 H 0.5478 0.3803 0.8864 0.101 Uiso 1 1 calc R . . B34 B 0.7968(2) 0.2745(2) 0.57724(9) 0.0761(4) Uani 0.42 1 d PD . . Cl34 Cl 0.7968(2) 0.2745(2) 0.57724(9) 0.0761(4) Uani 0.58 1 d P . . F35A F 0.6922(10) 0.2075(9) 0.6205(4) 0.0747(17) Uani 0.50 1 d PD A 1 F36A F 0.7618(9) 0.2259(10) 0.5060(3) 0.0781(19) Uani 0.50 1 d PD A 1 F37A F 0.7696(10) 0.4376(6) 0.5739(4) 0.098(2) Uani 0.50 1 d PD A 1 F38A F 0.9503(7) 0.2443(13) 0.6047(4) 0.114(4) Uani 0.50 1 d PD A 1 F35B F 0.660(3) 0.268(4) 0.6086(16) 0.213(17) Uiso 0.25 1 d PD A 2 F36B F 0.934(3) 0.233(4) 0.6199(14) 0.30(3) Uiso 0.25 1 d PD A 2 F37B F 0.788(2) 0.176(2) 0.5164(8) 0.101(7) Uiso 0.25 1 d PD A 2 F38B F 0.823(3) 0.4273(18) 0.5496(12) 0.142(10) Uiso 0.25 1 d PD A 2 F35C F 0.6514(12) 0.2361(17) 0.6010(7) 0.056(3) Uiso 0.25 1 d PD A 3 F36C F 0.9059(15) 0.1530(15) 0.5919(7) 0.087(4) Uiso 0.25 1 d PD A 3 F37C F 0.7922(17) 0.324(2) 0.5098(6) 0.118(5) Uiso 0.25 1 d PD A 3 F38C F 0.859(2) 0.4060(18) 0.6203(9) 0.149(6) Uiso 0.25 1 d PD A 3 B39 B 0.7392(2) 0.2982(2) 1.07489(10) 0.0885(6) Uani 0.45 1 d PD . . Cl39 Cl 0.7392(2) 0.2982(2) 1.07489(10) 0.0885(6) Uani 0.55 1 d P . . F40A F 0.6586(10) 0.2722(12) 1.0001(4) 0.073(3) Uiso 0.40 1 d PD B 1 F41A F 0.6716(10) 0.1821(11) 1.1125(4) 0.073(2) Uiso 0.40 1 d PD B 1 F42A F 0.8849(8) 0.2933(12) 1.0629(4) 0.099(2) Uiso 0.40 1 d PD B 1 F43A F 0.6895(18) 0.4447(12) 1.0985(6) 0.137(4) Uiso 0.40 1 d PD B 1 F40B F 0.8795(15) 0.356(2) 1.1050(8) 0.161(6) Uiso 0.30 1 d PD B 2 F41B F 0.7366(16) 0.3042(18) 1.0037(5) 0.112(4) Uiso 0.30 1 d PD B 2 F42B F 0.7031(13) 0.1428(11) 1.0988(6) 0.084(3) Uiso 0.30 1 d PD B 2 F43B F 0.6172(14) 0.4080(14) 1.0941(6) 0.103(3) Uiso 0.30 1 d PD B 2 F40C F 0.6547(11) 0.2432(14) 1.1280(5) 0.087(3) Uiso 0.30 1 d PD B 3 F41C F 0.7920(13) 0.4509(11) 1.1008(5) 0.091(3) Uiso 0.30 1 d PD B 3 F42C F 0.8972(8) 0.2152(12) 1.0776(5) 0.074(2) Uiso 0.30 1 d PD B 3 F43C F 0.6616(16) 0.3077(19) 1.0092(6) 0.094(5) 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 0.0560(2) 0.0623(3) 0.0449(2) -0.0045(2) 0.00083(17) 0.0032(2) N2 0.0491(11) 0.0491(15) 0.0508(13) -0.0022(17) 0.0038(9) -0.0001(15) C3 0.0538(16) 0.0482(19) 0.0498(18) -0.0010(14) 0.0004(13) -0.0054(13) C4 0.082(2) 0.070(3) 0.055(2) 0.0032(19) -0.0108(18) -0.005(2) C5 0.106(3) 0.074(3) 0.0484(18) -0.004(3) 0.0109(18) -0.003(3) C6 0.074(2) 0.073(3) 0.060(2) -0.0126(19) 0.0232(18) -0.0072(19) C7 0.0534(16) 0.0498(18) 0.062(2) -0.0098(16) 0.0145(14) -0.0076(14) N8 0.0472(12) 0.0473(16) 0.0652(18) 0.0024(14) 0.0019(12) 0.0021(12) N9 0.0527(13) 0.0518(17) 0.0586(17) -0.0008(14) 0.0078(12) 0.0007(12) C10 0.065(2) 0.059(2) 0.076(3) -0.006(2) 0.0217(18) -0.0047(18) C11 0.0458(17) 0.060(3) 0.130(4) -0.004(3) 0.009(2) 0.0077(17) C12 0.059(2) 0.059(3) 0.096(3) 0.011(2) -0.010(2) 0.0060(18) N13 0.0483(14) 0.0500(17) 0.075(2) -0.0097(15) 0.0106(13) -0.0005(12) N14 0.0512(15) 0.063(2) 0.070(2) -0.0031(16) -0.0077(13) 0.0021(13) C15 0.059(2) 0.072(3) 0.102(3) 0.002(3) -0.013(2) -0.004(2) C16 0.052(2) 0.076(3) 0.157(5) -0.004(3) 0.003(3) 0.014(2) C17 0.058(2) 0.066(3) 0.124(4) -0.005(3) 0.026(2) 0.0069(19) N18 0.0439(11) 0.0503(18) 0.0531(14) 0.0003(15) 0.0048(10) 0.0059(13) C19 0.0421(14) 0.055(2) 0.0544(19) -0.0076(16) 0.0025(12) 0.0070(14) C20 0.067(2) 0.072(3) 0.055(2) -0.008(2) -0.0007(16) 0.0030(19) C21 0.073(2) 0.109(4) 0.049(2) 0.008(2) 0.0029(17) 0.016(2) C22 0.067(2) 0.070(3) 0.066(2) 0.015(2) 0.0136(18) 0.0058(19) C23 0.0473(15) 0.052(2) 0.064(2) 0.0025(17) 0.0054(14) 0.0054(14) N24 0.0512(14) 0.0562(18) 0.0508(16) -0.0036(14) 0.0016(11) 0.0017(12) N25 0.0590(15) 0.0598(19) 0.0506(16) 0.0002(14) 0.0016(12) 0.0075(13) C26 0.064(2) 0.063(3) 0.077(3) 0.015(2) 0.0107(18) 0.0027(19) C27 0.070(2) 0.065(3) 0.095(3) 0.002(2) 0.006(2) -0.0164(19) C28 0.063(2) 0.071(3) 0.080(3) -0.020(2) 0.0042(19) -0.013(2) N29 0.0487(14) 0.0513(18) 0.080(2) -0.0040(16) 0.0091(13) 0.0019(13) N30 0.0591(16) 0.0558(18) 0.066(2) -0.0145(15) 0.0023(13) 0.0049(14) C31 0.070(2) 0.066(3) 0.101(3) -0.024(3) -0.003(2) 0.012(2) C32 0.077(2) 0.051(3) 0.138(4) -0.017(3) -0.005(3) -0.005(2) C33 0.069(2) 0.050(2) 0.134(5) 0.014(3) 0.017(3) -0.001(2) B34 0.0803(9) 0.0730(10) 0.0762(10) 0.0083(8) 0.0142(8) -0.0023(7) Cl34 0.0803(9) 0.0730(10) 0.0762(10) 0.0083(8) 0.0142(8) -0.0023(7) F35A 0.090(4) 0.076(4) 0.061(4) -0.003(3) 0.022(3) -0.014(3) F36A 0.113(5) 0.067(4) 0.056(3) 0.009(3) 0.020(3) 0.012(4) F37A 0.136(6) 0.042(3) 0.113(5) 0.007(3) -0.005(5) -0.031(3) F38A 0.075(3) 0.182(10) 0.083(4) 0.048(5) 0.003(3) 0.030(5) B39 0.0982(11) 0.0902(15) 0.0801(11) 0.0098(10) 0.0238(9) -0.0185(10) Cl39 0.0982(11) 0.0902(15) 0.0801(11) 0.0098(10) 0.0238(9) -0.0185(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.134(3) . ? Fe1 N18 2.138(3) . ? Fe1 N14 2.189(3) . ? Fe1 N25 2.190(3) . ? Fe1 N9 2.201(3) . ? Fe1 N30 2.212(4) . ? N2 C3 1.339(4) . ? N2 C7 1.349(4) . ? C3 C4 1.376(5) . ? C3 N8 1.432(4) . ? C4 C5 1.402(6) . ? C5 C6 1.383(6) . ? C6 C7 1.374(5) . ? C7 N13 1.415(5) . ? N8 C12 1.366(5) . ? N8 N9 1.378(4) . ? N9 C10 1.331(5) . ? C10 C11 1.383(6) . ? C11 C12 1.343(7) . ? N13 C17 1.359(5) . ? N13 N14 1.371(4) . ? N14 C15 1.342(5) . ? C15 C16 1.352(7) . ? C16 C17 1.386(8) . ? N18 C23 1.338(5) . ? N18 C19 1.341(5) . ? C19 C20 1.368(5) . ? C19 N24 1.419(5) . ? C20 C21 1.399(7) . ? C21 C22 1.379(7) . ? C22 C23 1.389(5) . ? C23 N29 1.422(5) . ? N24 C28 1.364(5) . ? N24 N25 1.378(4) . ? N25 C26 1.322(5) . ? C26 C27 1.414(6) . ? C27 C28 1.342(6) . ? N29 C33 1.349(6) . ? N29 N30 1.356(5) . ? N30 C31 1.334(6) . ? C31 C32 1.377(8) . ? C32 C33 1.379(7) . ? B34 F38A 1.394(6) . ? B34 F35A 1.407(5) . ? B34 F37A 1.420(6) . ? B34 F36A 1.443(6) . ? B34 F35B 1.374(15) . ? B34 F36B 1.415(15) . ? B34 F38B 1.444(14) . ? B34 F37B 1.446(13) . ? B34 F37C 1.369(11) . ? B34 F35C 1.409(10) . ? B34 F36C 1.411(10) . ? B34 F38C 1.473(12) . ? B39 F42A 1.293(7) . ? B39 F41A 1.393(7) . ? B39 F43A 1.417(10) . ? B39 F40A 1.556(8) . ? B39 F40B 1.375(11) . ? B39 F41B 1.376(10) . ? B39 F42B 1.456(9) . ? B39 F43B 1.482(9) . ? B39 F43C 1.378(10) . ? B39 F40C 1.395(8) . ? B39 F41C 1.460(9) . ? B39 F42C 1.527(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 173.43(13) . . ? N2 Fe1 N14 73.45(11) . . ? N18 Fe1 N14 108.32(11) . . ? N2 Fe1 N25 112.82(13) . . ? N18 Fe1 N25 73.49(12) . . ? N14 Fe1 N25 96.10(12) . . ? N2 Fe1 N9 73.51(10) . . ? N18 Fe1 N9 104.32(10) . . ? N14 Fe1 N9 146.91(12) . . ? N25 Fe1 N9 98.20(11) . . ? N2 Fe1 N30 100.48(13) . . ? N18 Fe1 N30 73.30(12) . . ? N14 Fe1 N30 91.18(12) . . ? N25 Fe1 N30 146.63(11) . . ? N9 Fe1 N30 93.02(11) . . ? C3 N2 C7 117.4(3) . . ? C3 N2 Fe1 121.6(2) . . ? C7 N2 Fe1 121.1(2) . . ? N2 C3 C4 124.2(3) . . ? N2 C3 N8 112.2(3) . . ? C4 C3 N8 123.6(3) . . ? C3 C4 C5 116.3(4) . . ? C6 C5 C4 121.3(3) . . ? C7 C6 C5 116.9(3) . . ? N2 C7 C6 123.9(4) . . ? N2 C7 N13 112.0(3) . . ? C6 C7 N13 124.1(3) . . ? C12 N8 N9 110.6(3) . . ? C12 N8 C3 130.9(3) . . ? N9 N8 C3 118.4(3) . . ? C10 N9 N8 103.9(3) . . ? C10 N9 Fe1 141.8(3) . . ? N8 N9 Fe1 114.23(19) . . ? N9 C10 C11 112.0(4) . . ? C12 C11 C10 106.1(3) . . ? C11 C12 N8 107.3(4) . . ? C17 N13 N14 111.5(4) . . ? C17 N13 C7 129.4(4) . . ? N14 N13 C7 118.9(3) . . ? C15 N14 N13 104.2(3) . . ? C15 N14 Fe1 140.7(3) . . ? N13 N14 Fe1 114.4(2) . . ? N14 C15 C16 112.0(5) . . ? C15 C16 C17 106.8(4) . . ? N13 C17 C16 105.5(5) . . ? C23 N18 C19 118.1(3) . . ? C23 N18 Fe1 120.5(3) . . ? C19 N18 Fe1 121.3(2) . . ? N18 C19 C20 123.7(4) . . ? N18 C19 N24 112.0(3) . . ? C20 C19 N24 124.3(3) . . ? C19 C20 C21 116.9(4) . . ? C22 C21 C20 121.1(4) . . ? C21 C22 C23 116.9(4) . . ? N18 C23 C22 123.2(4) . . ? N18 C23 N29 113.3(3) . . ? C22 C23 N29 123.5(4) . . ? C28 N24 N25 111.6(3) . . ? C28 N24 C19 129.4(3) . . ? N25 N24 C19 118.9(3) . . ? C26 N25 N24 104.1(3) . . ? C26 N25 Fe1 141.6(3) . . ? N24 N25 Fe1 114.2(2) . . ? N25 C26 C27 111.5(4) . . ? C28 C27 C26 105.9(4) . . ? C27 C28 N24 106.9(4) . . ? C33 N29 N30 111.2(4) . . ? C33 N29 C23 130.4(4) . . ? N30 N29 C23 118.5(3) . . ? C31 N30 N29 104.7(4) . . ? C31 N30 Fe1 140.8(3) . . ? N29 N30 Fe1 114.3(2) . . ? N30 C31 C32 112.0(5) . . ? C31 C32 C33 104.8(4) . . ? N29 C33 C32 107.2(5) . . ? F38A B34 F35A 109.3(5) . . ? F38A B34 F37A 110.2(6) . . ? F35A B34 F37A 108.6(5) . . ? F38A B34 F36A 114.2(5) . . ? F35A B34 F36A 111.4(4) . . ? F37A B34 F36A 102.9(5) . . ? F35B B34 F36B 115.4(14) . . ? F35B B34 F38B 111.9(13) . . ? F36B B34 F38B 107.1(14) . . ? F35B B34 F37B 110.9(13) . . ? F36B B34 F37B 107.6(13) . . ? F38B B34 F37B 103.2(10) . . ? F37C B34 F35C 116.1(8) . . ? F37C B34 F36C 112.3(8) . . ? F35C B34 F36C 110.6(8) . . ? F37C B34 F38C 105.9(10) . . ? F35C B34 F38C 106.2(8) . . ? F36C B34 F38C 104.9(9) . . ? F42A B39 F41A 121.9(6) . . ? F42A B39 F43A 114.4(7) . . ? F41A B39 F43A 108.3(7) . . ? F42A B39 F40A 100.2(5) . . ? F41A B39 F40A 102.3(5) . . ? F43A B39 F40A 107.8(6) . . ? F40B B39 F41B 109.8(8) . . ? F40B B39 F42B 113.5(8) . . ? F41B B39 F42B 111.7(7) . . ? F40B B39 F43B 106.0(8) . . ? F41B B39 F43B 106.5(7) . . ? F42B B39 F43B 109.0(6) . . ? F43C B39 F40C 117.4(8) . . ? F43C B39 F41C 111.7(8) . . ? F40C B39 F41C 102.5(6) . . ? F43C B39 F42C 113.9(7) . . ? F40C B39 F42C 109.8(6) . . ? F41C B39 F42C 99.4(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.351 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.056 #=END data_c:\datasets\leeds\mh140b~1\mh140b~2\mh140blt _database_code_depnum_ccdc_archive 'CCDC 631325' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) 0.87:1.13 tetrafluoroborate: perchlorate salt ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H18 Fe N10, 0.87[B F4], 1.13[Cl O4]' _chemical_formula_sum 'C22 H18 B0.87 Cl1.13 F3.48 Fe N10 O4.52' _chemical_formula_weight 666.22 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.5348(3) _cell_length_b 8.5892(3) _cell_length_c 18.6089(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.567(2) _cell_angle_gamma 90.00 _cell_volume 1348.94(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17339 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 30.05 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour Brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 674 _exptl_absorpt_coefficient_mu 0.748 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.767 _exptl_absorpt_correction_T_max 0.941 _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 17339 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 30.05 _reflns_number_total 7318 _reflns_number_gt 6678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Distinct ClO~4~^-^ and BF~4~^-^ environments were detected in the Fourier map for each anion site. These were modelled with the partial B and Cl atoms in each anion site constrained to have identical coordinates and thermal parameters (SHELXL EXYZ and EADP instructions). This was necessary, since the isotropic thermal parameters of both partial atoms became meaninglessly high when they were allowed to refine freely. The fact that separate partial B and Cl atoms could not be resolved probably accounts for deviations from tetrahedrality observed in the bond lengths and angles of these ions. The following refined restraints were also applied: B---F = 1.42(2)\%A, F...F = 2.32(2)\%A, Cl---O = 1.44(2)\%A, O...O = 2.35(2)\%A. The relative occupancies of BF~4~^-^ and ClO~4~^-^ in each site were refined as 0.420(4):0.580(6) for B34-F38:Cl34-O38 and 0.450(4):0.550(4) for B39-F43:Cl39-O43. These fixed occupancies were used in the final refinement, and are close to the predicted BF~4~^-^:ClO~4~^-^ ratio of 1:1 obtained from microanalysis of the bulk sample. All non-H atoms except for the partial F atoms (which have occupancy <0.5) were refined anisotropically. All H atoms were placed in calculated positions and refined using a riding model. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+0.4939P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.023(13) _refine_ls_number_reflns 7318 _refine_ls_number_parameters 422 _refine_ls_number_restraints 41 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.081 _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 0.71237(4) 0.84146(4) 0.746513(17) 0.01767(8) Uani 1 1 d . . . N2 N 0.7065(2) 0.8623(3) 0.64390(11) 0.0189(4) Uani 1 1 d . . . C3 C 0.5796(3) 0.9224(3) 0.60286(14) 0.0220(5) Uani 1 1 d . . . C4 C 0.5686(3) 0.9388(4) 0.52810(15) 0.0268(5) Uani 1 1 d . . . H4 H 0.4780 0.9834 0.4997 0.032 Uiso 1 1 calc R . . C5 C 0.6995(4) 0.8856(3) 0.49649(15) 0.0281(6) Uani 1 1 d . . . H5 H 0.6965 0.8941 0.4454 0.034 Uiso 1 1 calc R . . C6 C 0.8322(3) 0.8213(4) 0.53809(14) 0.0268(6) Uani 1 1 d . . . H6 H 0.9201 0.7860 0.5167 0.032 Uiso 1 1 calc R . . C7 C 0.8303(3) 0.8111(3) 0.61212(13) 0.0206(5) Uani 1 1 d . . . N8 N 0.4640(3) 0.9652(3) 0.64603(12) 0.0231(4) Uani 1 1 d . . . N9 N 0.4995(2) 0.9372(3) 0.71961(12) 0.0205(4) Uani 1 1 d . . . C10 C 0.3714(3) 0.9843(3) 0.74720(16) 0.0252(5) Uani 1 1 d . . . H10 H 0.3603 0.9786 0.7972 0.030 Uiso 1 1 calc R . . C11 C 0.2549(3) 1.0438(4) 0.69218(17) 0.0284(6) Uani 1 1 d . . . H11 H 0.1545 1.0855 0.6982 0.034 Uiso 1 1 calc R . . C12 C 0.3158(3) 1.0294(3) 0.62850(17) 0.0267(6) Uani 1 1 d . . . H12 H 0.2654 1.0581 0.5814 0.032 Uiso 1 1 calc R . . N13 N 0.9479(2) 0.7465(3) 0.66495(12) 0.0226(4) Uani 1 1 d . . . N14 N 0.9210(2) 0.7522(3) 0.73639(12) 0.0212(4) Uani 1 1 d . . . C15 C 1.0453(3) 0.6832(3) 0.77457(16) 0.0263(6) Uani 1 1 d . . . H15 H 1.0601 0.6703 0.8258 0.032 Uiso 1 1 calc R . . C16 C 1.1534(3) 0.6310(4) 0.72870(17) 0.0310(6) Uani 1 1 d . . . H16 H 1.2508 0.5782 0.7430 0.037 Uiso 1 1 calc R . . C17 C 1.0884(3) 0.6725(3) 0.65966(17) 0.0282(6) Uani 1 1 d . . . H17 H 1.1321 0.6538 0.6164 0.034 Uiso 1 1 calc R . . N18 N 0.7181(2) 0.8127(3) 0.84889(11) 0.0197(5) Uani 1 1 d . . . C19 C 0.7788(3) 0.9240(3) 0.89549(14) 0.0213(5) Uani 1 1 d . . . C20 C 0.7889(3) 0.9078(4) 0.97018(15) 0.0267(6) Uani 1 1 d . . . H20 H 0.8313 0.9878 1.0026 0.032 Uiso 1 1 calc R . . C21 C 0.7334(3) 0.7679(4) 0.99528(15) 0.0275(6) Uani 1 1 d . . . H21 H 0.7380 0.7527 1.0461 0.033 Uiso 1 1 calc R . . C22 C 0.6710(3) 0.6490(4) 0.94741(15) 0.0264(6) Uani 1 1 d . . . H22 H 0.6335 0.5537 0.9644 0.032 Uiso 1 1 calc R . . C23 C 0.6675(3) 0.6790(3) 0.87441(15) 0.0220(5) Uani 1 1 d . . . N24 N 0.8308(3) 1.0529(3) 0.85826(12) 0.0229(5) Uani 1 1 d . . . N25 N 0.8115(2) 1.0423(3) 0.78314(12) 0.0211(4) Uani 1 1 d . . . C26 C 0.8772(3) 1.1709(4) 0.76097(16) 0.0265(6) Uani 1 1 d . . . H26 H 0.8819 1.1962 0.7116 0.032 Uiso 1 1 calc R . . C27 C 0.9394(3) 1.2652(4) 0.82148(16) 0.0310(6) Uani 1 1 d . . . H27 H 0.9917 1.3626 0.8204 0.037 Uiso 1 1 calc R . . C28 C 0.9076(3) 1.1850(4) 0.88224(16) 0.0284(6) Uani 1 1 d . . . H28 H 0.9345 1.2168 0.9314 0.034 Uiso 1 1 calc R . . N29 N 0.6104(3) 0.5779(3) 0.81633(12) 0.0226(4) Uani 1 1 d . . . N30 N 0.6219(2) 0.6294(3) 0.74736(12) 0.0206(4) Uani 1 1 d . . . C31 C 0.5727(3) 0.5111(3) 0.70380(16) 0.0265(6) Uani 1 1 d . . . H31 H 0.5683 0.5127 0.6525 0.032 Uiso 1 1 calc R . . C32 C 0.5281(3) 0.3834(3) 0.74332(17) 0.0302(6) Uani 1 1 d . . . H32 H 0.4888 0.2859 0.7244 0.036 Uiso 1 1 calc R . . C33 C 0.5529(3) 0.4286(3) 0.81483(17) 0.0274(6) Uani 1 1 d . . . H33 H 0.5340 0.3682 0.8554 0.033 Uiso 1 1 calc R . . B34 B 0.80366(13) 0.30544(13) 0.56023(6) 0.0340(3) Uani 0.42 1 d PD A 1 F35 F 0.6796(14) 0.2701(15) 0.5996(7) 0.034(3) Uiso 0.42 1 d PD A 1 F36 F 0.7542(8) 0.2501(10) 0.4848(4) 0.0263(17) Uiso 0.42 1 d PD A 1 F37 F 0.8305(9) 0.4645(9) 0.5559(5) 0.040(2) Uiso 0.42 1 d PD A 1 F38 F 0.9384(8) 0.2194(7) 0.5896(4) 0.0374(18) Uiso 0.42 1 d PD A 1 Cl34 Cl 0.80366(13) 0.30544(13) 0.56023(6) 0.0340(3) Uani 0.58 1 d PD B 2 O35 O 0.6856(12) 0.2484(13) 0.6003(5) 0.030(2) Uani 0.58 1 d PD B 2 O36 O 0.7929(8) 0.2527(9) 0.4899(3) 0.0384(15) Uani 0.58 1 d PD B 2 O37 O 0.7924(7) 0.4765(6) 0.5610(3) 0.0300(11) Uani 0.58 1 d PD B 2 O38 O 0.9623(5) 0.2694(7) 0.5979(2) 0.0326(10) Uani 0.58 1 d PD B 2 B39 B 0.71509(14) 0.27743(16) 1.05427(6) 0.0358(3) Uani 0.45 1 d PD C 1 F40 F 0.6428(11) 0.2775(10) 0.9837(5) 0.029(2) Uiso 0.45 1 d PD C 1 F41 F 0.6765(7) 0.1653(7) 1.1021(3) 0.0299(16) Uiso 0.45 1 d PD C 1 F42 F 0.8901(6) 0.2541(6) 1.0538(3) 0.0294(14) Uiso 0.45 1 d PD C 1 F43 F 0.6952(7) 0.4239(8) 1.0885(4) 0.054(2) Uiso 0.45 1 d PD C 1 Cl39 Cl 0.71509(14) 0.27743(16) 1.05427(6) 0.0358(3) Uani 0.55 1 d PD D 2 O40 O 0.6316(10) 0.2476(11) 0.9794(4) 0.0290(15) Uani 0.55 1 d PD D 2 O41 O 0.6890(6) 0.1305(6) 1.0911(3) 0.0219(10) Uani 0.55 1 d PD D 2 O42 O 0.8730(5) 0.3069(6) 1.0515(3) 0.0270(10) Uani 0.55 1 d PD D 2 O43 O 0.6387(6) 0.4036(5) 1.0830(2) 0.0305(9) Uani 0.55 1 d PD D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01828(14) 0.02051(16) 0.01411(15) 0.00029(15) 0.00206(10) 0.00065(14) N2 0.0221(8) 0.0193(12) 0.0147(9) -0.0005(8) 0.0005(7) -0.0010(8) C3 0.0236(11) 0.0232(13) 0.0190(12) 0.0012(10) 0.0030(9) -0.0016(10) C4 0.0330(13) 0.0306(15) 0.0154(12) 0.0024(11) -0.0009(10) -0.0010(11) C5 0.0391(14) 0.0275(14) 0.0181(12) -0.0006(10) 0.0053(10) -0.0036(11) C6 0.0327(12) 0.0287(16) 0.0206(12) -0.0028(11) 0.0089(9) -0.0013(12) C7 0.0238(10) 0.0190(14) 0.0193(11) 0.0012(9) 0.0042(8) -0.0017(9) N8 0.0231(10) 0.0272(12) 0.0173(10) 0.0013(9) -0.0024(8) 0.0010(9) N9 0.0227(9) 0.0215(11) 0.0172(10) 0.0010(8) 0.0031(8) 0.0007(8) C10 0.0239(12) 0.0268(14) 0.0253(14) -0.0016(11) 0.0051(10) -0.0004(10) C11 0.0228(12) 0.0256(14) 0.0362(16) 0.0001(12) 0.0029(11) 0.0032(10) C12 0.0199(11) 0.0275(14) 0.0306(15) 0.0009(12) -0.0028(10) 0.0016(10) N13 0.0221(9) 0.0269(12) 0.0191(10) -0.0011(9) 0.0041(8) 0.0006(8) N14 0.0216(9) 0.0237(12) 0.0181(10) -0.0010(9) 0.0022(8) -0.0006(8) C15 0.0237(12) 0.0278(14) 0.0263(14) 0.0057(11) 0.0004(10) 0.0008(10) C16 0.0228(12) 0.0307(16) 0.0393(17) 0.0028(13) 0.0041(11) 0.0058(11) C17 0.0248(12) 0.0288(15) 0.0329(15) -0.0015(12) 0.0110(11) 0.0030(11) N18 0.0201(8) 0.0230(13) 0.0163(9) -0.0008(8) 0.0033(7) 0.0012(8) C19 0.0179(10) 0.0265(14) 0.0198(12) -0.0008(10) 0.0036(9) 0.0020(9) C20 0.0254(12) 0.0364(15) 0.0187(12) -0.0014(11) 0.0044(10) 0.0028(11) C21 0.0273(12) 0.0367(16) 0.0185(13) 0.0041(12) 0.0036(10) 0.0047(12) C22 0.0259(12) 0.0320(15) 0.0218(13) 0.0074(11) 0.0049(10) 0.0024(11) C23 0.0195(10) 0.0264(14) 0.0203(12) 0.0021(10) 0.0034(9) 0.0023(9) N24 0.0229(10) 0.0280(12) 0.0170(10) -0.0009(9) 0.0007(8) -0.0018(9) N25 0.0222(9) 0.0259(12) 0.0148(10) 0.0015(9) 0.0018(8) 0.0010(8) C26 0.0258(12) 0.0288(15) 0.0257(14) 0.0026(11) 0.0063(10) -0.0006(10) C27 0.0321(13) 0.0297(16) 0.0316(15) -0.0031(12) 0.0055(11) -0.0102(12) C28 0.0304(13) 0.0313(15) 0.0227(14) -0.0096(11) 0.0015(11) -0.0043(11) N29 0.0235(9) 0.0236(11) 0.0207(11) 0.0017(9) 0.0031(8) 0.0008(9) N30 0.0214(9) 0.0214(11) 0.0196(10) 0.0005(8) 0.0046(8) 0.0028(8) C31 0.0269(12) 0.0256(14) 0.0272(14) -0.0056(11) 0.0048(11) 0.0000(10) C32 0.0302(13) 0.0226(14) 0.0372(16) -0.0030(11) 0.0030(11) -0.0013(10) C33 0.0264(12) 0.0204(13) 0.0363(16) 0.0046(12) 0.0074(11) -0.0010(10) B34 0.0402(5) 0.0359(7) 0.0274(5) 0.0046(4) 0.0097(4) 0.0035(4) Cl34 0.0402(5) 0.0359(7) 0.0274(5) 0.0046(4) 0.0097(4) 0.0035(4) O35 0.051(4) 0.023(3) 0.021(3) -0.001(2) 0.019(2) 0.000(2) O36 0.037(3) 0.060(4) 0.021(2) -0.0050(19) 0.013(2) -0.001(3) O37 0.028(2) 0.018(2) 0.046(3) -0.0002(16) 0.008(2) -0.0042(18) O38 0.031(2) 0.044(3) 0.023(2) 0.008(2) 0.0046(16) 0.003(2) B39 0.0404(6) 0.0423(6) 0.0263(5) 0.0040(5) 0.0104(4) 0.0001(5) Cl39 0.0404(6) 0.0423(6) 0.0263(5) 0.0040(5) 0.0104(4) 0.0001(5) O40 0.042(3) 0.029(4) 0.014(2) 0.001(2) -0.0007(16) -0.004(3) O41 0.029(2) 0.020(2) 0.018(2) -0.0024(17) 0.0077(15) 0.0060(17) O42 0.0239(18) 0.027(3) 0.031(2) 0.0057(19) 0.0059(14) -0.0006(18) O43 0.035(2) 0.034(2) 0.024(2) -0.0129(16) 0.0087(18) -0.0064(19) _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 1.911(2) . ? Fe1 N18 1.914(2) . ? Fe1 N14 1.973(2) . ? Fe1 N30 1.979(2) . ? Fe1 N9 1.989(2) . ? Fe1 N25 1.996(2) . ? N2 C3 1.333(3) . ? N2 C7 1.358(3) . ? C3 C4 1.387(4) . ? C3 N8 1.410(3) . ? C4 C5 1.414(4) . ? C5 C6 1.388(4) . ? C6 C7 1.383(3) . ? C7 N13 1.410(3) . ? N8 C12 1.374(3) . ? N8 N9 1.379(3) . ? N9 C10 1.338(3) . ? C10 C11 1.412(4) . ? C11 C12 1.369(4) . ? N13 C17 1.373(3) . ? N13 N14 1.383(3) . ? N14 C15 1.326(4) . ? C15 C16 1.420(4) . ? C16 C17 1.369(4) . ? N18 C23 1.339(3) . ? N18 C19 1.342(3) . ? C19 C20 1.387(4) . ? C19 N24 1.412(3) . ? C20 C21 1.397(4) . ? C21 C22 1.407(4) . ? C22 C23 1.378(4) . ? C23 N29 1.415(4) . ? N24 C28 1.352(4) . ? N24 N25 1.386(3) . ? N25 C26 1.332(4) . ? C26 C27 1.424(4) . ? C27 C28 1.385(4) . ? N29 C33 1.372(4) . ? N29 N30 1.375(3) . ? N30 C31 1.328(4) . ? C31 C32 1.404(4) . ? C32 C33 1.372(4) . ? B34 F37 1.389(8) . ? B34 F35 1.407(10) . ? B34 F38 1.407(7) . ? B34 F36 1.482(8) . ? Cl34 O36 1.375(6) . ? Cl34 O35 1.427(10) . ? Cl34 O38 1.462(4) . ? Cl34 O37 1.473(5) . ? B39 F40 1.365(8) . ? B39 F41 1.384(6) . ? B39 F43 1.432(7) . ? B39 F42 1.508(5) . ? Cl39 O42 1.380(5) . ? Cl39 O43 1.410(5) . ? Cl39 O41 1.469(5) . ? Cl39 O40 1.490(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 177.95(11) . . ? N2 Fe1 N14 80.24(9) . . ? N18 Fe1 N14 98.92(9) . . ? N2 Fe1 N30 98.15(9) . . ? N18 Fe1 N30 79.96(9) . . ? N14 Fe1 N30 90.10(9) . . ? N2 Fe1 N9 79.80(9) . . ? N18 Fe1 N9 101.01(8) . . ? N14 Fe1 N9 160.04(9) . . ? N30 Fe1 N9 92.28(9) . . ? N2 Fe1 N25 101.95(9) . . ? N18 Fe1 N25 79.92(9) . . ? N14 Fe1 N25 91.48(9) . . ? N30 Fe1 N25 159.81(9) . . ? N9 Fe1 N25 93.06(9) . . ? C3 N2 C7 119.6(2) . . ? C3 N2 Fe1 120.44(16) . . ? C7 N2 Fe1 119.91(17) . . ? N2 C3 C4 122.8(2) . . ? N2 C3 N8 110.6(2) . . ? C4 C3 N8 126.6(2) . . ? C3 C4 C5 116.4(3) . . ? C6 C5 C4 121.8(3) . . ? C7 C6 C5 116.8(2) . . ? N2 C7 C6 122.6(2) . . ? N2 C7 N13 110.1(2) . . ? C6 C7 N13 127.3(2) . . ? C12 N8 N9 111.3(2) . . ? C12 N8 C3 131.8(2) . . ? N9 N8 C3 116.8(2) . . ? C10 N9 N8 104.9(2) . . ? C10 N9 Fe1 142.8(2) . . ? N8 N9 Fe1 112.29(15) . . ? N9 C10 C11 111.0(2) . . ? C12 C11 C10 106.1(2) . . ? C11 C12 N8 106.6(3) . . ? C17 N13 N14 110.9(2) . . ? C17 N13 C7 132.1(2) . . ? N14 N13 C7 116.9(2) . . ? C15 N14 N13 105.4(2) . . ? C15 N14 Fe1 141.64(19) . . ? N13 N14 Fe1 112.77(16) . . ? N14 C15 C16 111.0(3) . . ? C17 C16 C15 105.9(2) . . ? C16 C17 N13 106.8(2) . . ? C23 N18 C19 119.7(2) . . ? C23 N18 Fe1 120.13(18) . . ? C19 N18 Fe1 120.10(18) . . ? N18 C19 C20 122.5(3) . . ? N18 C19 N24 111.1(2) . . ? C20 C19 N24 126.4(3) . . ? C19 C20 C21 116.6(3) . . ? C20 C21 C22 121.9(3) . . ? C23 C22 C21 116.0(3) . . ? N18 C23 C22 123.3(3) . . ? N18 C23 N29 110.4(2) . . ? C22 C23 N29 126.3(3) . . ? C28 N24 N25 111.5(2) . . ? C28 N24 C19 131.9(2) . . ? N25 N24 C19 116.4(2) . . ? C26 N25 N24 105.4(2) . . ? C26 N25 Fe1 142.0(2) . . ? N24 N25 Fe1 112.45(17) . . ? N25 C26 C27 110.6(2) . . ? C28 C27 C26 105.5(3) . . ? N24 C28 C27 107.0(2) . . ? C33 N29 N30 110.9(2) . . ? C33 N29 C23 132.1(2) . . ? N30 N29 C23 116.8(2) . . ? C31 N30 N29 105.3(2) . . ? C31 N30 Fe1 141.93(19) . . ? N29 N30 Fe1 112.68(17) . . ? N30 C31 C32 111.3(3) . . ? C33 C32 C31 105.8(3) . . ? N29 C33 C32 106.7(3) . . ? F37 B34 F35 112.7(6) . . ? F37 B34 F38 114.0(4) . . ? F35 B34 F38 108.6(6) . . ? F37 B34 F36 106.7(5) . . ? F35 B34 F36 107.0(6) . . ? F38 B34 F36 107.5(4) . . ? O37 Cl34 O35 106.6(5) . . ? O37 Cl34 O38 105.3(3) . . ? O35 Cl34 O38 110.6(4) . . ? O37 Cl34 O36 110.0(4) . . ? O35 Cl34 O36 115.6(5) . . ? O38 Cl34 O36 108.2(3) . . ? F40 B39 F41 120.1(5) . . ? F40 B39 F43 111.2(5) . . ? F41 B39 F43 105.7(3) . . ? F40 B39 F42 107.4(5) . . ? F41 B39 F42 104.0(3) . . ? F43 B39 F42 107.6(3) . . ? O40 Cl39 O41 101.8(4) . . ? O40 Cl39 O43 107.6(4) . . ? O41 Cl39 O43 111.9(3) . . ? O40 Cl39 O42 109.3(4) . . ? O41 Cl39 O42 113.1(3) . . ? O43 Cl39 O42 112.5(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.493 _refine_diff_density_min -0.571 _refine_diff_density_rms 0.068 #=END data_c:\datasets\leeds\mh140c\mh140c _database_code_depnum_ccdc_archive 'CCDC 631326' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) 0.32:1.68 tetrafluoroborate: perchlorate salt ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H18 Fe N10, 0.32[B F4], 1.68[Cl O4]' _chemical_formula_sum 'C22 H18 B0.32 Cl1.68 F1.28 Fe N10 O6.72' _chemical_formula_weight 673.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.4602(17) _cell_length_b 9.3419(11) _cell_length_c 20.202(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.320(6) _cell_angle_gamma 90.00 _cell_volume 2693.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5419 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 26.02 _exptl_crystal_description 'Square prism' _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1370 _exptl_absorpt_coefficient_mu 0.809 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.888 _exptl_absorpt_correction_T_max 1.040 _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 5419 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 26.02 _reflns_number_total 2365 _reflns_number_gt 2150 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains half a complex dication, with Fe(1) lying on the crystallographic C~2~ axis [0, y, 0.25]; and, one anion site occupying a general position. Distinct BF~4~^-^ and ClO~4~^-^ sites in the model could not be satisfactorily refined, although microanalysis of the sample implied that ca. 15% of the anion content of the crystal should be tetrafluoroborate. The anion site was modelled using partial BF~4~^-^ and ClO~4~^-^ molecules, with equivalent atoms in each partial ion constrained to have identical coordinated and thermal parameters (SHELXL EXYZ and EADP instructions). The relative occupancies of BF~4~^-^ and ClO~4~^-^ in the anion site were refined as 0.157(7):0.843(7) for B18-F22:Cl18-O22. These fixed occupancies were used in the final refinement. All non-H atoms were refined anisotropically, and no restraints were applied. All H atoms were placed in calculated positions and refined using a riding model. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+7.0562P] 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 2365 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0752 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.0000 0.69648(5) 0.2500 0.01778(13) Uani 1 2 d S . . N2 N 0.01422(12) 0.7456(2) 0.35670(8) 0.0187(4) Uani 1 1 d . . . C3 C -0.03026(14) 0.6664(2) 0.39696(10) 0.0191(4) Uani 1 1 d . . . C4 C -0.02808(16) 0.6960(3) 0.46495(10) 0.0246(5) Uani 1 1 d . . . H4 H -0.0625 0.6406 0.4920 0.029 Uiso 1 1 calc R . . C5 C 0.02712(17) 0.8111(3) 0.49086(10) 0.0275(5) Uani 1 1 d . . . H5 H 0.0303 0.8353 0.5368 0.033 Uiso 1 1 calc R . . C6 C 0.07813(16) 0.8921(3) 0.45112(10) 0.0261(5) Uani 1 1 d . . . H6 H 0.1178 0.9684 0.4692 0.031 Uiso 1 1 calc R . . C7 C 0.06762(15) 0.8548(2) 0.38353(10) 0.0210(5) Uani 1 1 d . . . N8 N -0.07734(12) 0.5470(2) 0.36382(8) 0.0194(4) Uani 1 1 d . . . N9 N -0.06791(12) 0.5235(2) 0.29788(8) 0.0208(4) Uani 1 1 d . . . C10 C -0.10464(15) 0.3939(2) 0.28356(10) 0.0240(5) Uani 1 1 d . . . H10 H -0.1082 0.3484 0.2412 0.029 Uiso 1 1 calc R . . C11 C -0.13771(16) 0.3327(3) 0.33958(11) 0.0265(5) Uani 1 1 d . . . H11 H -0.1667 0.2420 0.3419 0.032 Uiso 1 1 calc R . . C12 C -0.11884(15) 0.4326(3) 0.38964(10) 0.0246(5) Uani 1 1 d . . . H12 H -0.1321 0.4240 0.4340 0.029 Uiso 1 1 calc R . . N13 N 0.11352(12) 0.9267(2) 0.33618(9) 0.0220(4) Uani 1 1 d . . . N14 N 0.10717(13) 0.8687(2) 0.27277(8) 0.0223(4) Uani 1 1 d . . . C15 C 0.15588(15) 0.9582(3) 0.23998(11) 0.0258(5) Uani 1 1 d . . . H15 H 0.1643 0.9461 0.1946 0.031 Uiso 1 1 calc R . . C16 C 0.19332(16) 1.0732(3) 0.28130(12) 0.0292(5) Uani 1 1 d . . . H16 H 0.2303 1.1503 0.2695 0.035 Uiso 1 1 calc R . . C17 C 0.16510(16) 1.0505(2) 0.34195(12) 0.0277(5) Uani 1 1 d . . . H17 H 0.1787 1.1093 0.3807 0.033 Uiso 1 1 calc R . . Cl18 Cl 0.29708(4) 0.95932(8) 0.08960(3) 0.02998(18) Uani 0.84 1 d P A 1 O19 O 0.21857(16) 0.8692(3) 0.09230(12) 0.0818(9) Uani 0.84 1 d P A 1 O20 O 0.38171(14) 0.8784(2) 0.10646(9) 0.0486(5) Uani 0.84 1 d P A 1 O21 O 0.29769(15) 1.0733(2) 0.13786(12) 0.0586(6) Uani 0.84 1 d P A 1 O22 O 0.29502(17) 1.0156(4) 0.02400(11) 0.0913(10) Uani 0.84 1 d P A 1 B18 B 0.29708(4) 0.95932(8) 0.08960(3) 0.02998(18) Uani 0.16 1 d P B 2 F20 F 0.38171(14) 0.8784(2) 0.10646(9) 0.0486(5) Uani 0.16 1 d P B 2 F22 F 0.29502(17) 1.0156(4) 0.02400(11) 0.0913(10) Uani 0.16 1 d P B 2 F21 F 0.29769(15) 1.0733(2) 0.13786(12) 0.0586(6) Uani 0.16 1 d P B 2 F19 F 0.21857(16) 0.8692(3) 0.09230(12) 0.0818(9) Uani 0.16 1 d P B 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 0.0228(2) 0.0180(2) 0.0131(2) 0.000 0.00462(16) 0.000 N2 0.0198(8) 0.0197(9) 0.0165(8) 0.0000(7) 0.0029(7) 0.0012(8) C3 0.0185(10) 0.0213(12) 0.0173(9) 0.0018(8) 0.0025(8) 0.0047(9) C4 0.0293(12) 0.0286(13) 0.0162(10) 0.0024(9) 0.0047(9) 0.0065(11) C5 0.0367(13) 0.0295(13) 0.0153(9) -0.0025(9) 0.0010(9) 0.0111(11) C6 0.0303(12) 0.0244(13) 0.0213(10) -0.0051(9) -0.0027(9) 0.0038(10) C7 0.0210(10) 0.0202(12) 0.0214(10) -0.0005(9) 0.0026(8) 0.0051(9) N8 0.0215(9) 0.0228(10) 0.0145(8) 0.0021(7) 0.0045(7) 0.0010(8) N9 0.0244(9) 0.0235(11) 0.0149(8) 0.0008(7) 0.0048(7) -0.0014(8) C10 0.0270(11) 0.0232(12) 0.0208(10) -0.0007(9) 0.0012(9) -0.0016(10) C11 0.0277(12) 0.0238(13) 0.0276(11) 0.0061(9) 0.0029(9) -0.0036(10) C12 0.0248(11) 0.0285(13) 0.0209(10) 0.0084(9) 0.0052(9) 0.0005(10) N13 0.0236(9) 0.0197(10) 0.0224(9) -0.0033(7) 0.0032(7) -0.0010(8) N14 0.0231(9) 0.0246(10) 0.0193(8) -0.0006(7) 0.0044(7) 0.0001(8) C15 0.0237(11) 0.0265(13) 0.0279(11) 0.0070(9) 0.0057(9) 0.0010(10) C16 0.0243(12) 0.0213(13) 0.0412(13) 0.0077(10) 0.0032(10) -0.0015(10) C17 0.0270(12) 0.0182(12) 0.0360(12) -0.0022(9) -0.0005(10) -0.0008(10) Cl18 0.0277(3) 0.0408(4) 0.0231(3) 0.0052(3) 0.0090(3) 0.0004(3) O19 0.0575(14) 0.121(2) 0.0744(15) -0.0497(16) 0.0342(12) -0.0530(15) O20 0.0506(11) 0.0542(13) 0.0402(10) 0.0024(9) 0.0048(9) 0.0165(10) O21 0.0636(13) 0.0390(12) 0.0830(15) -0.0147(11) 0.0414(12) -0.0054(11) O22 0.0759(16) 0.160(3) 0.0463(12) 0.0570(15) 0.0332(11) 0.0606(18) B18 0.0277(3) 0.0408(4) 0.0231(3) 0.0052(3) 0.0090(3) 0.0004(3) F19 0.0575(14) 0.121(2) 0.0744(15) -0.0497(16) 0.0342(12) -0.0530(15) F20 0.0506(11) 0.0542(13) 0.0402(10) 0.0024(9) 0.0048(9) 0.0165(10) F21 0.0636(13) 0.0390(12) 0.0830(15) -0.0147(11) 0.0414(12) -0.0054(11) F22 0.0759(16) 0.160(3) 0.0463(12) 0.0570(15) 0.0332(11) 0.0606(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.1808(16) . ? Fe1 N9 2.1951(18) . ? Fe1 N14 2.2297(19) . ? N2 C3 1.339(3) . ? N2 C7 1.340(3) . ? C3 C4 1.397(3) . ? C3 N8 1.417(3) . ? C4 C5 1.390(3) . ? C5 C6 1.398(3) . ? C6 C7 1.394(3) . ? C7 N13 1.419(3) . ? N8 C12 1.370(3) . ? N8 N9 1.378(2) . ? N9 C10 1.335(3) . ? C10 C11 1.418(3) . ? C11 C12 1.370(3) . ? N13 C17 1.371(3) . ? N13 N14 1.380(2) . ? N14 C15 1.336(3) . ? C15 C16 1.414(3) . ? C16 C17 1.369(3) . ? Cl18 O22 1.421(2) . ? Cl18 O19 1.422(2) . ? Cl18 O20 1.432(2) . ? Cl18 O21 1.443(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N2 155.69(10) . 2 ? N2 Fe1 N9 127.82(7) . 2 ? N2 Fe1 N9 72.35(7) . . ? N9 Fe1 N9 85.20(10) 2 . ? N2 Fe1 N14 72.13(6) . . ? N9 Fe1 N14 141.81(6) . . ? N2 Fe1 N14 90.17(6) . 2 ? N9 Fe1 N14 106.05(7) . 2 ? N14 Fe1 N14 87.62(10) . 2 ? C3 N2 C7 118.51(17) . . ? C3 N2 Fe1 120.42(14) . . ? C7 N2 Fe1 121.07(13) . . ? N2 C3 C4 123.4(2) . . ? N2 C3 N8 112.93(17) . . ? C4 C3 N8 123.60(19) . . ? C5 C4 C3 116.4(2) . . ? C4 C5 C6 121.81(19) . . ? C7 C6 C5 116.3(2) . . ? N2 C7 C6 123.5(2) . . ? N2 C7 N13 112.93(17) . . ? C6 C7 N13 123.6(2) . . ? C12 N8 N9 111.23(17) . . ? C12 N8 C3 129.86(17) . . ? N9 N8 C3 117.80(16) . . ? C10 N9 N8 104.80(17) . . ? C10 N9 Fe1 139.72(14) . . ? N8 N9 Fe1 115.48(13) . . ? N9 C10 C11 111.50(19) . . ? C12 C11 C10 105.2(2) . . ? N8 C12 C11 107.29(18) . . ? C17 N13 N14 111.31(18) . . ? C17 N13 C7 130.53(19) . . ? N14 N13 C7 118.16(18) . . ? C15 N14 N13 104.69(18) . . ? C15 N14 Fe1 138.93(15) . . ? N13 N14 Fe1 114.47(13) . . ? N14 C15 C16 111.4(2) . . ? C17 C16 C15 105.6(2) . . ? C16 C17 N13 107.0(2) . . ? O22 Cl18 O19 111.01(17) . . ? O22 Cl18 O20 107.76(12) . . ? O19 Cl18 O20 109.58(17) . . ? O22 Cl18 O21 110.74(17) . . ? O19 Cl18 O21 109.19(13) . . ? O20 Cl18 O21 108.51(13) . . ? _diffrn_measured_fraction_theta_max 0.885 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.885 _refine_diff_density_max 0.468 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.053