# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_lkc007 _database_code_depnum_ccdc_archive 'CCDC 893212' #TrackingRef 'LKC Dalton revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(2,6-bis(pyrid-2-yl)pyrazine]iron(II) ditetrafluoroborate nitromethane solvate ; _chemical_name_common ; Bis(2,6-bis(pyrid-2-yl)pyrazine)iron(ii) ditetrafluoroborate nitromethane solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C28 H20 Fe N8, 2[B F4], C H3 N O2' _chemical_formula_sum 'C29 H23 B2 F8 Fe N9 O2' _chemical_formula_weight 759.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.8102(4) _cell_length_b 8.8297(4) _cell_length_c 39.8492(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.181(2) _cell_angle_gamma 90.00 _cell_volume 3099.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 64966 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 25.10 _exptl_crystal_description lath _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.581 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 0.85 _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. The crystals only showed significant diffraction below 2\q = 50 \%. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 64966 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.10 _reflns_number_total 5504 _reflns_number_gt 5030 _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 'X-SEED (Barbour, 2001)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Both BF~4~^-^ ions are disordered, each over two equally occupied sites labelled 'A' and 'B'. The refined restraints B---F = 1.38(2) and F...F = 2.25(2) \%A were applied to these residues. The two O atoms of the nitromethane molecule were also disordered over two equally occupied orientations, which were modelled without restraints. All fully-occupied non-H atoms were refined anisotropically, and H atoms were placed in calculated positions and refined using a riding model. The highest residual Fourier peak of +1.4 e.\%A^-3^ lies within the disordered anion centred on B38. ; _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^)+(0.0531P)^2^+18.3584P] 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 5504 _refine_ls_number_parameters 450 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0715 _refine_ls_wR_factor_ref 0.1713 _refine_ls_wR_factor_gt 0.1680 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.113 _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 0.88460(6) 0.02541(7) 0.138199(14) 0.01471(18) Uani 1 1 d . . . N2 N 0.8826(4) -0.0154(4) 0.18447(9) 0.0168(7) Uani 1 1 d . . . C3 C 1.0050(5) -0.0797(5) 0.19939(11) 0.0190(9) Uani 1 1 d . . . C4 C 1.0030(5) -0.1048(6) 0.23392(12) 0.0290(11) Uani 1 1 d . . . H4 H 1.0899 -0.1480 0.2443 0.035 Uiso 1 1 calc R . . N5 N 0.8828(5) -0.0701(5) 0.25292(10) 0.0312(10) Uani 1 1 d . . . C6 C 0.7614(5) -0.0090(6) 0.23754(11) 0.0280(11) Uani 1 1 d . . . H6 H 0.6740 0.0144 0.2505 0.034 Uiso 1 1 calc R . . C7 C 0.7598(5) 0.0212(5) 0.20318(11) 0.0194(9) Uani 1 1 d . . . C8 C 0.6411(5) 0.0926(5) 0.18269(11) 0.0197(9) Uani 1 1 d . . . N9 N 0.6783(4) 0.1044(4) 0.14941(9) 0.0195(8) Uani 1 1 d . . . C10 C 0.5793(5) 0.1720(5) 0.12870(12) 0.0236(10) Uani 1 1 d . . . H10 H 0.6028 0.1781 0.1055 0.028 Uiso 1 1 calc R . . C11 C 0.4430(5) 0.2337(6) 0.13996(14) 0.0299(11) Uani 1 1 d . . . H11 H 0.3752 0.2814 0.1247 0.036 Uiso 1 1 calc R . . C12 C 0.4076(5) 0.2245(6) 0.17368(14) 0.0314(11) Uani 1 1 d . . . H12 H 0.3162 0.2676 0.1819 0.038 Uiso 1 1 calc R . . C13 C 0.5074(5) 0.1515(6) 0.19542(13) 0.0266(10) Uani 1 1 d . . . H13 H 0.4843 0.1423 0.2186 0.032 Uiso 1 1 calc R . . C14 C 1.1277(5) -0.1070(5) 0.17532(11) 0.0182(9) Uani 1 1 d . . . N15 N 1.0931(4) -0.0581(4) 0.14339(9) 0.0164(7) Uani 1 1 d . . . C16 C 1.2008(5) -0.0701(5) 0.11973(11) 0.0204(9) Uani 1 1 d . . . H16 H 1.1795 -0.0337 0.0978 0.024 Uiso 1 1 calc R . . C17 C 1.3426(5) -0.1338(5) 0.12619(12) 0.0251(10) Uani 1 1 d . . . H17 H 1.4163 -0.1403 0.1089 0.030 Uiso 1 1 calc R . . C18 C 1.3750(5) -0.1875(6) 0.15798(12) 0.0268(10) Uani 1 1 d . . . H18 H 1.4701 -0.2339 0.1626 0.032 Uiso 1 1 calc R . . C19 C 1.2662(5) -0.1728(5) 0.18316(12) 0.0233(10) Uani 1 1 d . . . H19 H 1.2868 -0.2072 0.2053 0.028 Uiso 1 1 calc R . . N20 N 0.8891(4) 0.0655(4) 0.09170(9) 0.0175(8) Uani 1 1 d . . . C21 C 0.8417(5) -0.0405(5) 0.06958(11) 0.0214(9) Uani 1 1 d . . . C22 C 0.8494(6) -0.0086(6) 0.03519(11) 0.0280(11) Uani 1 1 d . . . H22 H 0.8156 -0.0829 0.0196 0.034 Uiso 1 1 calc R . . N23 N 0.9028(5) 0.1226(5) 0.02364(10) 0.0305(10) Uani 1 1 d . . . C24 C 0.9494(6) 0.2253(6) 0.04601(11) 0.0269(10) Uani 1 1 d . . . H24 H 0.9877 0.3195 0.0382 0.032 Uiso 1 1 calc R . . C25 C 0.9438(5) 0.1987(5) 0.08057(11) 0.0201(9) Uani 1 1 d . . . C26 C 0.7876(5) -0.1770(5) 0.08652(11) 0.0197(9) Uani 1 1 d . . . N27 N 0.8012(4) -0.1699(4) 0.12075(9) 0.0180(8) Uani 1 1 d . . . C28 C 0.7552(5) -0.2917(5) 0.13870(12) 0.0213(9) Uani 1 1 d . . . H28 H 0.7667 -0.2898 0.1624 0.026 Uiso 1 1 calc R . . C29 C 0.6926(5) -0.4181(5) 0.12398(13) 0.0265(10) Uani 1 1 d . . . H29 H 0.6602 -0.5006 0.1375 0.032 Uiso 1 1 calc R . . C30 C 0.6769(6) -0.4248(6) 0.08938(13) 0.0302(11) Uani 1 1 d . . . H30 H 0.6324 -0.5107 0.0789 0.036 Uiso 1 1 calc R . . C31 C 0.7274(5) -0.3039(6) 0.07048(12) 0.0265(10) Uani 1 1 d . . . H31 H 0.7211 -0.3072 0.0467 0.032 Uiso 1 1 calc R . . C32 C 0.9911(5) 0.2974(5) 0.10823(10) 0.0184(9) Uani 1 1 d . . . N33 N 0.9687(4) 0.2347(4) 0.13928(9) 0.0164(7) Uani 1 1 d . . . C34 C 1.0087(5) 0.3170(5) 0.16638(11) 0.0189(9) Uani 1 1 d . . . H34 H 0.9934 0.2750 0.1881 0.023 Uiso 1 1 calc R . . C35 C 1.0711(5) 0.4602(5) 0.16382(12) 0.0224(10) Uani 1 1 d . . . H35 H 1.0977 0.5152 0.1835 0.027 Uiso 1 1 calc R . . C36 C 1.0946(5) 0.5227(5) 0.13251(12) 0.0252(10) Uani 1 1 d . . . H36 H 1.1390 0.6203 0.1304 0.030 Uiso 1 1 calc R . . C37 C 1.0523(5) 0.4409(5) 0.10409(11) 0.0221(10) Uani 1 1 d . . . H37 H 1.0652 0.4826 0.0823 0.026 Uiso 1 1 calc R . . B38A B 0.3890(15) 0.2464(17) 0.0456(3) 0.037(5) Uiso 0.50 1 d PD A 1 F39A F 0.5374(9) 0.1905(11) 0.0491(2) 0.066(2) Uiso 0.50 1 d PD A 1 F40A F 0.3502(8) 0.2707(9) 0.01249(16) 0.0350(19) Uiso 0.50 1 d PD A 1 F41A F 0.2921(9) 0.1412(9) 0.06077(19) 0.061(2) Uiso 0.50 1 d PD A 1 F42A F 0.3614(9) 0.3765(9) 0.06330(19) 0.057(2) Uiso 0.50 1 d PD A 1 B38B B 0.3964(14) 0.2136(17) 0.0453(3) 0.028(4) Uiso 0.50 1 d PD B 2 F39B F 0.5432(7) 0.2594(9) 0.05137(16) 0.0370(16) Uiso 0.50 1 d PD B 2 F40B F 0.3617(9) 0.2206(10) 0.01175(18) 0.045(2) Uiso 0.50 1 d PD B 2 F41B F 0.3616(15) 0.0753(13) 0.0563(3) 0.115(4) Uiso 0.50 1 d PD B 2 F42B F 0.3065(15) 0.3151(16) 0.0648(3) 0.128(5) Uiso 0.50 1 d PD B 2 B43A B 0.6641(17) 0.5201(14) 0.2189(3) 0.020(5) Uiso 0.50 1 d PD C 1 F44A F 0.7179(10) 0.4294(10) 0.1928(2) 0.045(3) Uiso 0.50 1 d PD C 1 F45A F 0.7688(15) 0.6347(14) 0.2239(3) 0.110(5) Uiso 0.50 1 d PD C 1 F46A F 0.5347(9) 0.5958(10) 0.2095(2) 0.061(2) Uiso 0.50 1 d PD C 1 F47A F 0.6360(11) 0.4475(11) 0.2478(2) 0.057(3) Uiso 0.50 1 d PD C 1 B43B B 0.6415(17) 0.5119(17) 0.2187(4) 0.038(7) Uiso 0.50 1 d PD D 2 F44B F 0.7483(10) 0.4411(10) 0.1988(2) 0.046(3) Uiso 0.50 1 d PD D 2 F45B F 0.7167(14) 0.6418(12) 0.2304(3) 0.087(4) Uiso 0.50 1 d PD D 2 F46B F 0.5082(7) 0.5449(8) 0.20211(17) 0.0368(16) Uiso 0.50 1 d PD D 2 F47B F 0.6119(9) 0.4111(9) 0.24452(17) 0.033(2) Uiso 0.50 1 d PD D 2 C48 C 0.6578(8) 0.3049(11) -0.0228(2) 0.076(3) Uani 1 1 d . E . H48A H 0.5859 0.3731 -0.0340 0.114 Uiso 1 1 calc R . . H48B H 0.6559 0.3233 0.0014 0.114 Uiso 1 1 calc R . . H48C H 0.6290 0.1996 -0.0273 0.114 Uiso 1 1 calc R . . N49 N 0.8115(5) 0.3328(5) -0.03565(11) 0.0379(11) Uani 1 1 d . . . O50A O 0.8217(14) 0.2759(13) -0.0624(3) 0.059(3) Uiso 0.50 1 d P E 1 O51A O 0.9119(10) 0.4107(10) -0.0235(2) 0.033(2) Uiso 0.50 1 d P E 1 O50B O 0.8753(10) 0.2579(9) -0.0593(2) 0.032(2) Uiso 0.50 1 d P E 2 O51B O 0.8685(11) 0.4361(11) -0.0188(2) 0.040(2) Uiso 0.50 1 d P E 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 0.0138(3) 0.0153(3) 0.0151(3) 0.0009(2) -0.0013(2) -0.0014(2) N2 0.0143(17) 0.0170(18) 0.0191(18) -0.0011(15) -0.0008(14) -0.0034(14) C3 0.018(2) 0.019(2) 0.020(2) 0.0009(17) -0.0042(17) -0.0027(17) C4 0.025(2) 0.040(3) 0.022(2) 0.004(2) -0.0040(19) 0.000(2) N5 0.027(2) 0.046(3) 0.021(2) 0.0018(19) -0.0004(17) -0.0027(19) C6 0.024(2) 0.039(3) 0.021(2) -0.002(2) 0.0041(19) -0.003(2) C7 0.018(2) 0.021(2) 0.020(2) -0.0024(18) 0.0033(17) -0.0041(18) C8 0.018(2) 0.018(2) 0.022(2) -0.0029(18) 0.0001(17) -0.0034(18) N9 0.0181(18) 0.0158(19) 0.0246(19) -0.0001(15) -0.0027(15) -0.0033(15) C10 0.021(2) 0.022(2) 0.028(2) 0.0027(19) -0.0059(18) -0.0042(19) C11 0.020(2) 0.024(2) 0.045(3) 0.001(2) -0.011(2) 0.000(2) C12 0.015(2) 0.030(3) 0.049(3) -0.005(2) 0.000(2) 0.002(2) C13 0.019(2) 0.028(3) 0.032(3) -0.004(2) 0.0025(19) -0.004(2) C14 0.019(2) 0.014(2) 0.022(2) -0.0007(17) -0.0047(17) -0.0027(17) N15 0.0165(17) 0.0128(18) 0.0200(18) -0.0012(14) -0.0003(14) -0.0043(14) C16 0.022(2) 0.017(2) 0.022(2) -0.0006(18) 0.0026(18) -0.0038(18) C17 0.018(2) 0.024(2) 0.033(3) -0.005(2) 0.0052(19) -0.0031(19) C18 0.016(2) 0.025(2) 0.039(3) -0.004(2) -0.0009(19) 0.0014(19) C19 0.022(2) 0.022(2) 0.026(2) -0.0009(19) -0.0049(18) -0.0010(19) N20 0.0174(17) 0.0167(18) 0.0183(18) 0.0010(14) -0.0040(14) -0.0008(14) C21 0.021(2) 0.022(2) 0.021(2) -0.0030(18) -0.0031(17) -0.0036(19) C22 0.040(3) 0.025(3) 0.019(2) -0.0017(19) -0.003(2) -0.004(2) N23 0.042(2) 0.031(2) 0.019(2) -0.0007(17) -0.0026(18) -0.0063(19) C24 0.034(3) 0.026(3) 0.020(2) 0.0042(19) -0.0012(19) -0.006(2) C25 0.021(2) 0.018(2) 0.021(2) 0.0038(18) 0.0002(17) -0.0005(18) C26 0.018(2) 0.020(2) 0.022(2) -0.0020(18) -0.0025(17) 0.0003(18) N27 0.0142(17) 0.0198(19) 0.0201(18) 0.0020(15) -0.0003(14) 0.0022(15) C28 0.017(2) 0.020(2) 0.027(2) 0.0027(19) -0.0006(17) 0.0004(18) C29 0.022(2) 0.021(2) 0.036(3) 0.003(2) 0.001(2) -0.0043(19) C30 0.028(3) 0.024(2) 0.038(3) -0.005(2) -0.006(2) -0.004(2) C31 0.029(2) 0.027(3) 0.024(2) -0.003(2) -0.0050(19) -0.005(2) C32 0.015(2) 0.023(2) 0.018(2) 0.0022(18) -0.0006(16) 0.0020(18) N33 0.0122(17) 0.0171(18) 0.0199(18) 0.0024(15) -0.0007(14) 0.0008(14) C34 0.017(2) 0.021(2) 0.019(2) 0.0004(18) 0.0005(17) 0.0019(17) C35 0.022(2) 0.018(2) 0.027(2) -0.0022(19) -0.0055(18) 0.0012(18) C36 0.024(2) 0.017(2) 0.035(3) -0.001(2) -0.001(2) -0.0036(19) C37 0.022(2) 0.021(2) 0.023(2) 0.0034(18) 0.0019(18) -0.0039(18) C48 0.039(4) 0.123(7) 0.066(5) 0.040(5) -0.002(3) -0.012(4) N49 0.048(3) 0.040(3) 0.025(2) 0.004(2) -0.007(2) -0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.879(4) . ? Fe1 N20 1.887(4) . ? Fe1 N15 1.989(4) . ? Fe1 N33 1.992(4) . ? Fe1 N27 1.998(4) . ? Fe1 N9 1.998(4) . ? N2 C3 1.355(6) . ? N2 C7 1.355(5) . ? C3 C4 1.394(6) . ? C3 C14 1.467(6) . ? C4 N5 1.339(6) . ? N5 C6 1.344(6) . ? C6 C7 1.395(6) . ? C7 C8 1.467(6) . ? C8 N9 1.371(6) . ? C8 C13 1.385(6) . ? N9 C10 1.339(6) . ? C10 C11 1.395(7) . ? C11 C12 1.383(8) . ? C12 C13 1.391(7) . ? C14 N15 1.377(5) . ? C14 C19 1.386(6) . ? N15 C16 1.344(6) . ? C16 C17 1.393(6) . ? C17 C18 1.381(7) . ? C18 C19 1.396(7) . ? N20 C25 1.346(6) . ? N20 C21 1.351(6) . ? C21 C22 1.401(6) . ? C21 C26 1.462(6) . ? C22 N23 1.333(6) . ? N23 C24 1.335(6) . ? C24 C25 1.398(6) . ? C25 C32 1.465(6) . ? C26 N27 1.370(6) . ? C26 C31 1.394(6) . ? N27 C28 1.355(6) . ? C28 C29 1.375(7) . ? C29 C30 1.387(7) . ? C30 C31 1.381(7) . ? C32 N33 1.370(5) . ? C32 C37 1.387(6) . ? N33 C34 1.347(6) . ? C34 C35 1.383(6) . ? C35 C36 1.381(7) . ? C36 C37 1.393(7) . ? B38A F42A 1.370(14) . ? B38A F40A 1.379(13) . ? B38A F41A 1.400(14) . ? B38A F39A 1.405(14) . ? B38B F41B 1.333(14) . ? B38B F40B 1.371(12) . ? B38B F39B 1.376(12) . ? B38B F42B 1.427(14) . ? B43A F47A 1.340(13) . ? B43A F46A 1.374(13) . ? B43A F45A 1.384(15) . ? B43A F44A 1.396(12) . ? B43B F46B 1.376(14) . ? B43B F44B 1.383(14) . ? B43B F47B 1.386(14) . ? B43B F45B 1.403(15) . ? C48 N49 1.470(8) . ? N49 O50A 1.181(12) . ? N49 O51A 1.220(9) . ? N49 O51B 1.238(10) . ? N49 O50B 1.282(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N20 179.31(16) . . ? N2 Fe1 N15 80.70(15) . . ? N20 Fe1 N15 98.60(15) . . ? N2 Fe1 N33 99.30(15) . . ? N20 Fe1 N33 80.69(15) . . ? N15 Fe1 N33 89.90(14) . . ? N2 Fe1 N27 99.86(15) . . ? N20 Fe1 N27 80.15(15) . . ? N15 Fe1 N27 93.12(14) . . ? N33 Fe1 N27 160.84(14) . . ? N2 Fe1 N9 80.57(15) . . ? N20 Fe1 N9 100.12(15) . . ? N15 Fe1 N9 161.09(15) . . ? N33 Fe1 N9 90.57(14) . . ? N27 Fe1 N9 92.61(14) . . ? C3 N2 C7 119.6(4) . . ? C3 N2 Fe1 120.1(3) . . ? C7 N2 Fe1 120.3(3) . . ? N2 C3 C4 119.1(4) . . ? N2 C3 C14 111.7(4) . . ? C4 C3 C14 129.1(4) . . ? N5 C4 C3 122.3(4) . . ? C4 N5 C6 117.6(4) . . ? N5 C6 C7 122.0(4) . . ? N2 C7 C6 119.3(4) . . ? N2 C7 C8 111.4(4) . . ? C6 C7 C8 129.3(4) . . ? N9 C8 C13 122.1(4) . . ? N9 C8 C7 113.5(4) . . ? C13 C8 C7 124.3(4) . . ? C10 N9 C8 118.2(4) . . ? C10 N9 Fe1 127.5(3) . . ? C8 N9 Fe1 114.2(3) . . ? N9 C10 C11 122.4(4) . . ? C12 C11 C10 119.1(5) . . ? C11 C12 C13 119.3(4) . . ? C8 C13 C12 118.8(5) . . ? N15 C14 C19 122.1(4) . . ? N15 C14 C3 113.0(4) . . ? C19 C14 C3 124.8(4) . . ? C16 N15 C14 118.0(4) . . ? C16 N15 Fe1 127.6(3) . . ? C14 N15 Fe1 114.5(3) . . ? N15 C16 C17 122.4(4) . . ? C18 C17 C16 119.4(4) . . ? C17 C18 C19 119.1(4) . . ? C14 C19 C18 118.9(4) . . ? C25 N20 C21 120.0(4) . . ? C25 N20 Fe1 119.7(3) . . ? C21 N20 Fe1 120.2(3) . . ? N20 C21 C22 118.9(4) . . ? N20 C21 C26 111.7(4) . . ? C22 C21 C26 129.3(4) . . ? N23 C22 C21 122.0(4) . . ? C22 N23 C24 117.9(4) . . ? N23 C24 C25 122.1(4) . . ? N20 C25 C24 119.0(4) . . ? N20 C25 C32 111.9(4) . . ? C24 C25 C32 129.1(4) . . ? N27 C26 C31 121.7(4) . . ? N27 C26 C21 113.2(4) . . ? C31 C26 C21 125.1(4) . . ? C28 N27 C26 117.6(4) . . ? C28 N27 Fe1 127.7(3) . . ? C26 N27 Fe1 114.7(3) . . ? N27 C28 C29 122.6(4) . . ? C28 C29 C30 119.8(4) . . ? C31 C30 C29 118.6(4) . . ? C30 C31 C26 119.6(4) . . ? N33 C32 C37 122.3(4) . . ? N33 C32 C25 113.4(4) . . ? C37 C32 C25 124.3(4) . . ? C34 N33 C32 117.9(4) . . ? C34 N33 Fe1 127.9(3) . . ? C32 N33 Fe1 114.2(3) . . ? N33 C34 C35 122.5(4) . . ? C36 C35 C34 119.5(4) . . ? C35 C36 C37 119.2(4) . . ? C32 C37 C36 118.7(4) . . ? F42A B38A F40A 108.6(11) . . ? F42A B38A F41A 103.0(10) . . ? F40A B38A F41A 111.5(10) . . ? F42A B38A F39A 114.2(11) . . ? F40A B38A F39A 112.1(10) . . ? F41A B38A F39A 107.0(11) . . ? F41B B38B F40B 108.1(11) . . ? F41B B38B F39B 115.4(12) . . ? F40B B38B F39B 111.4(9) . . ? F41B B38B F42B 105.6(11) . . ? F40B B38B F42B 112.3(11) . . ? F39B B38B F42B 104.0(10) . . ? F47A B43A F46A 108.2(11) . . ? F47A B43A F45A 110.6(11) . . ? F46A B43A F45A 103.6(10) . . ? F47A B43A F44A 115.4(10) . . ? F46A B43A F44A 111.0(10) . . ? F45A B43A F44A 107.4(11) . . ? F46B B43B F44B 113.7(11) . . ? F46B B43B F47B 109.3(11) . . ? F44B B43B F47B 105.4(10) . . ? F46B B43B F45B 112.8(11) . . ? F44B B43B F45B 103.8(11) . . ? F47B B43B F45B 111.6(11) . . ? O50A N49 O51A 122.8(8) . . ? O50A N49 C48 108.4(8) . . ? O51A N49 C48 128.6(7) . . ? O51B N49 O50B 126.9(7) . . ? O51B N49 C48 107.9(7) . . ? O50B N49 C48 125.1(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.432 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.101 data_lkc018 _database_code_depnum_ccdc_archive 'CCDC 893213' #TrackingRef 'LKC Dalton revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-di(pyrazinyl)pyridine]cobalt(II) ditetrafluoroborate ; _chemical_name_common 'Bis(2,6-di(pyrazinyl)pyridine)cobalt(ii) ditetrafluoroborate' _chemical_melting_point ? _chemical_formula_moiety 'C26 H18 Co N10, 2[B F4]' _chemical_formula_sum 'C26 H18 B2 Co F8 N10' _chemical_formula_weight 703.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 8.7106(11) _cell_length_b 8.7106(11) _cell_length_c 19.178(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1455.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 29757 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 30.24 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 706 _exptl_absorpt_coefficient_mu 0.679 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 29757 _diffrn_reflns_av_R_equivalents 0.0634 _diffrn_reflns_av_sigmaI/netI 0.0221 _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 -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 30.24 _reflns_number_total 2176 _reflns_number_gt 2102 _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 'X-SEED (Barbour, 2001)' _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 compound was originally solved in P1, then transformed up to P-421c using the ADSYMM routine in PLATON. The crystal was refined as a racemic twin. The asymmetric unit contains 1/4 of a complex dication, with Co1 occupying the crystallographic S4 site [0, 0, 0] and N2 and N5 lying on the C2 axis [0, 0, z]; and, half a BF~4~^-^ anion spanning the C~2~ axis [0, 0.5, z]. This half-anion was refined subject to the refined restraints B---F = 1.41(2)\%A and F...F = 2.30(2)\%A. All non-H atoms were refined 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^)+(0.0000P)^2^+4.1099P] 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 0.48(4) _refine_ls_number_reflns 2176 _refine_ls_number_parameters 132 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.1314 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.131 _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 Co1 Co 0.0000 0.0000 0.0000 0.02726(19) Uani 1 4 d S . . N2 N 0.0000 0.0000 0.10074(19) 0.0301(7) Uani 1 2 d S . . C3 C 0.0553(4) 0.1250(4) 0.1352(2) 0.0285(7) Uani 1 1 d . . . C4 C 0.0582(5) 0.1271(6) 0.2094(2) 0.0436(10) Uani 1 1 d . . . H4 H 0.0986 0.2127 0.2340 0.052 Uiso 1 1 calc R . . C5 C 0.0000 0.0000 0.2450(3) 0.0557(15) Uani 1 2 d S . . H5 H 0.0000 0.0000 0.2945 0.067 Uiso 1 2 calc SR . . C6 C 0.1113(4) 0.2471(4) 0.0889(2) 0.0287(7) Uani 1 1 d . . . N7 N 0.0990(3) 0.2155(3) 0.01923(15) 0.0256(6) Uani 1 1 d . . . C8 C 0.1466(4) 0.3226(5) -0.0260(2) 0.0357(8) Uani 1 1 d . . . H8 H 0.1380 0.3039 -0.0747 0.043 Uiso 1 1 calc R . . C9 C 0.2089(5) 0.4620(4) -0.0027(3) 0.0442(10) Uani 1 1 d . . . H9 H 0.2438 0.5342 -0.0363 0.053 Uiso 1 1 calc R . . N10 N 0.2214(4) 0.4982(5) 0.0666(2) 0.0475(8) Uani 1 1 d . . . C11 C 0.1739(5) 0.3888(5) 0.1113(2) 0.0386(9) Uani 1 1 d . . . H11 H 0.1827 0.4074 0.1600 0.046 Uiso 1 1 calc R . . B12 B -0.0112(17) 0.5206(13) 0.3108(3) 0.031(3) Uani 0.50 1 d PD . . F13 F -0.0327(13) 0.3687(12) 0.3354(5) 0.069(3) Uani 0.50 1 d PD . . F14 F 0.0504(7) 0.5174(12) 0.2439(3) 0.073(2) Uani 0.50 1 d PD . . F15 F -0.1594(6) 0.5869(7) 0.3069(3) 0.0505(14) Uani 0.50 1 d PD . . F16 F 0.0769(10) 0.6063(11) 0.3571(4) 0.051(2) Uani 0.50 1 d PD . . 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 Co1 0.0222(2) 0.0222(2) 0.0373(4) 0.000 0.000 0.000 N2 0.0209(19) 0.031(2) 0.0384(19) 0.000 0.000 0.004(3) C3 0.0244(15) 0.0248(16) 0.0362(18) -0.0033(14) 0.0014(14) 0.0018(12) C4 0.043(2) 0.049(3) 0.038(2) -0.0105(19) 0.0000(18) -0.0071(19) C5 0.066(5) 0.065(5) 0.037(3) 0.000 0.000 -0.016(7) C6 0.0266(16) 0.0215(16) 0.0380(19) -0.0007(14) 0.0008(15) 0.0011(13) N7 0.0229(13) 0.0245(13) 0.0294(15) -0.0011(11) -0.0025(11) 0.0032(10) C8 0.0272(18) 0.040(2) 0.0403(19) 0.0074(17) -0.0040(16) 0.0024(16) C9 0.041(2) 0.0306(18) 0.061(3) 0.016(2) -0.004(2) -0.0059(13) N10 0.047(2) 0.0299(15) 0.065(2) -0.007(2) -0.0039(17) -0.0073(19) C11 0.035(2) 0.0274(19) 0.053(2) -0.0093(17) 0.0025(18) -0.0032(16) B12 0.051(6) 0.017(8) 0.024(3) 0.000(3) 0.003(4) 0.015(6) F13 0.100(10) 0.057(4) 0.049(5) -0.005(4) -0.001(4) -0.004(5) F14 0.081(5) 0.095(5) 0.043(2) -0.018(4) 0.014(3) 0.000(5) F15 0.041(3) 0.062(4) 0.049(3) 0.012(3) 0.001(2) -0.003(3) F16 0.045(4) 0.056(5) 0.051(5) -0.026(4) 0.002(3) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N2 1.932(4) . ? Co1 N7 2.099(3) . ? N2 C3 1.362(4) . ? C3 C4 1.422(6) . ? C3 C6 1.469(5) . ? C4 C5 1.396(5) . ? C6 N7 1.368(5) . ? C6 C11 1.416(5) . ? N7 C8 1.340(5) . ? C8 C9 1.403(6) . ? C9 N10 1.372(7) . ? N10 C11 1.347(6) . ? B12 F14 1.390(9) . ? B12 F16 1.391(13) . ? B12 F15 1.416(13) . ? B12 F13 1.417(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 N2 Co1 N2 180.00 2 . ? N2 Co1 N7 79.88(8) . . ? N7 Co1 N7 159.76(16) 3 . ? N2 Co1 N7 100.12(8) . 2 ? N7 Co1 N7 91.77(3) . 2 ? C3 N2 C3 121.9(4) . 3 ? C3 N2 Co1 119.0(2) . . ? N2 C3 C4 120.1(4) . . ? N2 C3 C6 113.7(3) . . ? C4 C3 C6 126.1(4) . . ? C5 C4 C3 118.2(4) . . ? C4 C5 C4 121.4(5) 3 . ? N7 C6 C11 120.1(4) . . ? N7 C6 C3 114.8(3) . . ? C11 C6 C3 125.1(4) . . ? C8 N7 C6 117.9(3) . . ? C8 N7 Co1 129.5(3) . . ? C6 N7 Co1 112.6(2) . . ? N7 C8 C9 121.1(4) . . ? N10 C9 C8 122.6(4) . . ? C11 N10 C9 115.5(4) . . ? N10 C11 C6 122.8(4) . . ? F14 B12 F16 112.7(12) . . ? F14 B12 F15 108.2(7) . . ? F16 B12 F15 108.5(7) . . ? F14 B12 F13 109.9(8) . . ? F16 B12 F13 111.2(7) . . ? F15 B12 F13 106.1(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.24 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.367 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.085 data_lkc045 _database_code_depnum_ccdc_archive 'CCDC 893214' #TrackingRef 'LKC Dalton revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(2,6-bis(pyrimidin-4-yl)pyridine]iron(II) ditetrafluoroborate tri-nitromethane solvate ; _chemical_name_common ; Bis(2,6-bis(pyrimidin-4-yl)pyridine)iron(ii) ditetrafluoroborate tri-nitromethane solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C26 H18 Fe N10, 2[B F4], 3[C H3 N O2]' _chemical_formula_sum 'C29 H27 B2 F8 Fe N13 O6' _chemical_formula_weight 883.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.506(2) _cell_length_b 14.577(3) _cell_length_c 23.349(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.533(9) _cell_angle_gamma 90.00 _cell_volume 3890.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 116433 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 30.10 _exptl_crystal_description fragment _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.485 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 116433 _diffrn_reflns_av_R_equivalents 0.0861 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 30.10 _reflns_number_total 11369 _reflns_number_gt 7058 _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 'X-SEED (Barbour, 2001)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One of the BF~4~^-^ ions in the asymmetric unit, and two of the three nitromethane molecules, are disordered. The anion B43-F47 was refined over two orientations, labelled 'A' and 'B', with refined occupancies of 0.56:0.44. The refined restraints B---F = 1.39(2) and F...F = 2.27(2) \%A were applied to this residue. The solvent molecule C52-O55 was modelled over two sites, also labelled 'A' and 'B', with refined occupancies of 0.69:0.31. Three orientations were refined for solvent molecule C56-O59 with fixed occupancies of 0.50, 0.25 and 0.25. The quarter-occupied 'B' and 'C' sites shared a common half-occupied N atom, N57B. The disordered solvent was refined using the fixed restraints C---N = 1.45(2), N---O = 1.22(2), O...O = 2.09(2) and C...O = 2.30(2) \%A. All non-H atoms with occupancy >0.5 were refined anisotropically, and all H atoms were placed in calculated positions and refined using a riding model. The highest residual Fourier peak of +1.2 e.\%A^-3^ is 0.8 \%A from Fe1. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1274P)^2^+3.6896P] 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 11369 _refine_ls_number_parameters 579 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.1171 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.2344 _refine_ls_wR_factor_gt 0.1944 _refine_ls_goodness_of_fit_ref 1.034 _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 0.09856(3) 0.27079(3) 0.353562(15) 0.03259(15) Uani 1 1 d . . . N2 N 0.1533(2) 0.37772(19) 0.31681(9) 0.0341(5) Uani 1 1 d . . . C3 C 0.1638(3) 0.3755(3) 0.25833(11) 0.0384(7) Uani 1 1 d . . . C4 C 0.2064(3) 0.4526(3) 0.23076(13) 0.0472(8) Uani 1 1 d . . . H4 H 0.2155 0.4505 0.1909 0.057 Uiso 1 1 calc R . . C5 C 0.2354(3) 0.5328(3) 0.26319(14) 0.0495(9) Uani 1 1 d . . . H5 H 0.2655 0.5847 0.2452 0.059 Uiso 1 1 calc R . . C6 C 0.2197(3) 0.5360(3) 0.32256(13) 0.0437(8) Uani 1 1 d . . . H6 H 0.2360 0.5903 0.3444 0.052 Uiso 1 1 calc R . . C7 C 0.1793(2) 0.4563(2) 0.34815(11) 0.0370(7) Uani 1 1 d . . . C8 C 0.1245(3) 0.2855(2) 0.23240(12) 0.0377(7) Uani 1 1 d . . . N9 N 0.0911(2) 0.2229(2) 0.27224(10) 0.0355(6) Uani 1 1 d . . . C10 C 0.0569(3) 0.1384(3) 0.25193(12) 0.0415(7) Uani 1 1 d . . . H10 H 0.0355 0.0951 0.2793 0.050 Uiso 1 1 calc R . . N11 N 0.0506(3) 0.1104(2) 0.19623(11) 0.0497(7) Uani 1 1 d . . . C12 C 0.0804(3) 0.1739(3) 0.15750(13) 0.0520(9) Uani 1 1 d . . . H12 H 0.0743 0.1575 0.1179 0.062 Uiso 1 1 calc R . . C13 C 0.1196(3) 0.2620(3) 0.17362(13) 0.0477(9) Uani 1 1 d . . . H13 H 0.1420 0.3044 0.1460 0.057 Uiso 1 1 calc R . . C14 C 0.1587(2) 0.4427(2) 0.41002(12) 0.0377(7) Uani 1 1 d . . . N15 N 0.1243(2) 0.3545(2) 0.42240(10) 0.0374(6) Uani 1 1 d . . . C16 C 0.1079(3) 0.3358(3) 0.47852(12) 0.0417(8) Uani 1 1 d . . . H16 H 0.0855 0.2751 0.4872 0.050 Uiso 1 1 calc R . . N17 N 0.1211(3) 0.3973(2) 0.52279(11) 0.0490(7) Uani 1 1 d . . . C18 C 0.1521(3) 0.4841(3) 0.50910(13) 0.0494(9) Uani 1 1 d . . . H18 H 0.1606 0.5291 0.5387 0.059 Uiso 1 1 calc R . . C19 C 0.1720(3) 0.5101(3) 0.45285(13) 0.0448(8) Uani 1 1 d . . . H19 H 0.1937 0.5711 0.4444 0.054 Uiso 1 1 calc R . . N20 N 0.0408(2) 0.1628(2) 0.38756(9) 0.0357(6) Uani 1 1 d . . . C21 C -0.0781(3) 0.1503(3) 0.38642(11) 0.0396(7) Uani 1 1 d . . . C22 C -0.1236(3) 0.0687(3) 0.40697(12) 0.0461(9) Uani 1 1 d . . . H22 H -0.2056 0.0610 0.4068 0.055 Uiso 1 1 calc R . . C23 C -0.0460(3) -0.0017(3) 0.42789(13) 0.0470(9) Uani 1 1 d . . . H23 H -0.0757 -0.0577 0.4411 0.056 Uiso 1 1 calc R . . C24 C 0.0766(3) 0.0113(3) 0.42922(12) 0.0435(8) Uani 1 1 d . . . H24 H 0.1298 -0.0353 0.4437 0.052 Uiso 1 1 calc R . . C25 C 0.1178(3) 0.0946(2) 0.40856(12) 0.0387(7) Uani 1 1 d . . . C26 C -0.1440(3) 0.2321(3) 0.36220(12) 0.0389(7) Uani 1 1 d . . . N27 N -0.0734(2) 0.3013(2) 0.34505(10) 0.0358(6) Uani 1 1 d . . . C28 C -0.1266(3) 0.3807(3) 0.32562(13) 0.0419(7) Uani 1 1 d . . . H28 H -0.0780 0.4287 0.3146 0.050 Uiso 1 1 calc R . . N29 N -0.2441(2) 0.3966(3) 0.32074(13) 0.0527(8) Uani 1 1 d . . . C30 C -0.3116(3) 0.3265(3) 0.33619(15) 0.0549(10) Uani 1 1 d . . . H30 H -0.3940 0.3350 0.3325 0.066 Uiso 1 1 calc R . . C31 C -0.2664(3) 0.2428(3) 0.35721(14) 0.0478(9) Uani 1 1 d . . . H31 H -0.3159 0.1951 0.3677 0.057 Uiso 1 1 calc R . . C32 C 0.2410(3) 0.1213(3) 0.40316(12) 0.0416(7) Uani 1 1 d . . . N33 N 0.2519(2) 0.2050(2) 0.37567(11) 0.0410(6) Uani 1 1 d . . . C34 C 0.3615(3) 0.2328(3) 0.36782(17) 0.0545(10) Uani 1 1 d . . . H34 H 0.3686 0.2884 0.3473 0.065 Uiso 1 1 calc R . . N35 N 0.4615(3) 0.1881(3) 0.38661(18) 0.0732(12) Uani 1 1 d . . . C36 C 0.4502(3) 0.1073(4) 0.4143(2) 0.0685(13) Uani 1 1 d . . . H36 H 0.5190 0.0741 0.4278 0.082 Uiso 1 1 calc R . . C37 C 0.3411(3) 0.0705(3) 0.42377(16) 0.0545(9) Uani 1 1 d . . . H37 H 0.3351 0.0138 0.4433 0.065 Uiso 1 1 calc R . . B38 B 0.8288(4) 0.2684(3) 0.02821(17) 0.0501(10) Uani 1 1 d . . . F39 F 0.7489(2) 0.34156(18) 0.01226(11) 0.0651(6) Uani 1 1 d . . . F40 F 0.8249(2) 0.20330(18) -0.01674(9) 0.0658(7) Uani 1 1 d . . . F41 F 0.7971(3) 0.22624(17) 0.07874(9) 0.0679(7) Uani 1 1 d . . . F42 F 0.9431(2) 0.30448(19) 0.03864(12) 0.0709(7) Uani 1 1 d . . . B43A B 0.3634(5) 0.3562(5) 0.0779(3) 0.0328(13) Uani 0.56 1 d PD A 1 F44A F 0.3321(6) 0.4307(5) 0.1106(4) 0.106(2) Uani 0.56 1 d PD A 1 F45A F 0.3957(6) 0.2831(4) 0.1140(3) 0.0893(19) Uani 0.56 1 d PD A 1 F46A F 0.2700(5) 0.3297(6) 0.0395(3) 0.118(3) Uani 0.56 1 d PD A 1 F47A F 0.4629(8) 0.3763(9) 0.0520(4) 0.112(5) Uani 0.56 1 d PD A 1 B43B B 0.3775(11) 0.3808(9) 0.0924(5) 0.055(4) Uiso 0.44 1 d PD B 2 F44B F 0.3750(9) 0.4632(7) 0.1241(4) 0.101(3) Uiso 0.44 1 d PD B 2 F45B F 0.3890(8) 0.3199(6) 0.1383(4) 0.099(3) Uiso 0.44 1 d PD B 2 F46B F 0.2689(8) 0.3684(6) 0.0602(4) 0.095(3) Uiso 0.44 1 d PD B 2 F47B F 0.4655(9) 0.3863(6) 0.0560(5) 0.057(3) Uiso 0.44 1 d PD B 2 C48 C 0.6683(4) 0.3525(4) 0.16468(19) 0.0740(14) Uani 1 1 d . . . H48A H 0.6628 0.3533 0.1225 0.111 Uiso 1 1 calc R . . H48B H 0.6416 0.4115 0.1785 0.111 Uiso 1 1 calc R . . H48C H 0.6192 0.3032 0.1772 0.111 Uiso 1 1 calc R . . N49 N 0.7933(3) 0.3366(3) 0.18910(12) 0.0558(8) Uani 1 1 d . . . O50 O 0.8188(3) 0.2620(2) 0.21182(11) 0.0632(8) Uani 1 1 d . . . O51 O 0.8640(3) 0.3994(3) 0.18510(14) 0.0771(9) Uani 1 1 d . . . C52A C 0.4936(9) 0.8318(6) -0.0027(4) 0.083(2) Uani 0.69 1 d PD C 1 H52A H 0.5670 0.7975 0.0050 0.124 Uiso 0.69 1 calc PR C 1 H52B H 0.4900 0.8608 -0.0407 0.124 Uiso 0.69 1 calc PR C 1 H52C H 0.4274 0.7897 -0.0020 0.124 Uiso 0.69 1 calc PR C 1 N53A N 0.4882(4) 0.9040(4) 0.0424(3) 0.0506(12) Uani 0.69 1 d PD C 1 O54A O 0.5686(5) 0.9099(4) 0.0821(3) 0.100(2) Uani 0.69 1 d PD C 1 O55A O 0.4062(4) 0.9529(4) 0.0421(3) 0.0940(18) Uani 0.69 1 d PD C 1 C52B C 0.4402(13) 0.8334(12) -0.0163(8) 0.067(5) Uiso 0.31 1 d PD D 2 H52D H 0.4741 0.7981 -0.0460 0.101 Uiso 0.31 1 calc PR D 2 H52E H 0.3822 0.8766 -0.0347 0.101 Uiso 0.31 1 calc PR D 2 H52F H 0.4022 0.7915 0.0086 0.101 Uiso 0.31 1 calc PR D 2 N53B N 0.5320(14) 0.8839(12) 0.0181(7) 0.081(4) Uiso 0.31 1 d PD D 2 O54B O 0.6312(13) 0.8735(12) 0.0066(8) 0.132(6) Uiso 0.31 1 d PD D 2 O55B O 0.509(2) 0.9359(16) 0.0546(10) 0.145(11) Uiso 0.31 1 d PD D 2 C56A C 0.4177(10) 0.0893(8) 0.1712(4) 0.061(3) Uiso 0.50 1 d PD E 1 H56A H 0.4945 0.0817 0.1574 0.092 Uiso 0.50 1 calc PR E 1 H56B H 0.3656 0.1227 0.1423 0.092 Uiso 0.50 1 calc PR E 1 H56C H 0.3843 0.0288 0.1777 0.092 Uiso 0.50 1 calc PR E 1 N57A N 0.4307(7) 0.1408(6) 0.2251(3) 0.0662(18) Uiso 0.50 1 d PD E 1 O58A O 0.3475(8) 0.1575(8) 0.2481(4) 0.101(3) Uiso 0.50 1 d PD E 1 O59A O 0.5272(7) 0.1742(6) 0.2409(4) 0.098(2) Uiso 0.50 1 d PD E 1 C56B C 0.433(4) 0.119(3) 0.1783(12) 0.18(2) Uiso 0.25 1 d PD F 2 H56D H 0.3623 0.1458 0.1577 0.269 Uiso 0.25 1 calc PR F 2 H56E H 0.4684 0.0764 0.1525 0.269 Uiso 0.25 1 calc PR F 2 H56F H 0.4889 0.1672 0.1908 0.269 Uiso 0.25 1 calc PR F 2 N57B N 0.4030(9) 0.0694(8) 0.2274(4) 0.104(3) Uiso 0.50 1 d PD . . O58B O 0.3340(11) 0.1138(14) 0.2579(5) 0.050(3) Uiso 0.25 1 d PD F 2 O59B O 0.4797(17) 0.0297(15) 0.2601(9) 0.126(7) Uiso 0.25 1 d PD F 2 C56C C 0.3808(19) 0.0912(13) 0.1619(6) 0.058(5) Uiso 0.25 1 d PD F 3 H56G H 0.3112 0.1300 0.1544 0.087 Uiso 0.25 1 calc PR F 3 H56H H 0.3684 0.0338 0.1402 0.087 Uiso 0.25 1 calc PR F 3 H56I H 0.4487 0.1234 0.1498 0.087 Uiso 0.25 1 calc PR F 3 O58C O 0.3289(15) 0.0860(13) 0.2579(7) 0.085(8) Uiso 0.25 1 d PD F 3 O59C O 0.4679(14) -0.0012(11) 0.2370(8) 0.099(5) Uiso 0.25 1 d PD F 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0241(2) 0.0575(3) 0.01560(18) 0.00404(16) -0.00004(13) -0.00766(17) N2 0.0249(11) 0.0580(16) 0.0186(10) 0.0077(10) -0.0008(8) -0.0042(10) C3 0.0301(14) 0.066(2) 0.0194(11) 0.0091(12) 0.0020(10) 0.0051(13) C4 0.0447(17) 0.073(2) 0.0240(13) 0.0140(15) 0.0062(12) 0.0026(16) C5 0.0481(18) 0.067(2) 0.0338(16) 0.0190(16) 0.0067(13) -0.0071(17) C6 0.0378(16) 0.063(2) 0.0296(14) 0.0087(14) -0.0006(12) -0.0106(15) C7 0.0257(13) 0.064(2) 0.0206(12) 0.0051(12) -0.0026(10) -0.0084(13) C8 0.0294(13) 0.065(2) 0.0188(11) 0.0051(12) 0.0029(10) 0.0051(13) N9 0.0264(11) 0.0615(18) 0.0181(10) 0.0020(10) 0.0003(8) 0.0035(11) C10 0.0350(15) 0.066(2) 0.0236(13) -0.0004(13) 0.0028(11) 0.0019(14) N11 0.0501(16) 0.072(2) 0.0264(12) -0.0084(13) 0.0034(11) 0.0089(15) C12 0.057(2) 0.077(3) 0.0224(13) -0.0017(15) 0.0068(13) 0.0164(19) C13 0.0503(19) 0.074(3) 0.0197(13) 0.0048(14) 0.0071(12) 0.0119(17) C14 0.0275(13) 0.062(2) 0.0223(12) 0.0044(12) -0.0027(10) -0.0107(13) N15 0.0260(11) 0.0659(18) 0.0195(10) 0.0028(11) -0.0016(8) -0.0123(11) C16 0.0384(16) 0.066(2) 0.0201(12) 0.0051(13) 0.0001(11) -0.0155(14) N17 0.0498(16) 0.075(2) 0.0214(11) -0.0013(12) 0.0014(11) -0.0174(15) C18 0.0455(18) 0.077(3) 0.0249(14) -0.0062(15) 0.0022(12) -0.0184(17) C19 0.0411(17) 0.063(2) 0.0290(14) 0.0005(14) -0.0009(12) -0.0190(15) N20 0.0316(12) 0.0588(17) 0.0165(9) -0.0007(10) 0.0016(8) -0.0153(11) C21 0.0317(14) 0.070(2) 0.0177(11) -0.0110(13) 0.0036(10) -0.0137(14) C22 0.0394(16) 0.077(2) 0.0227(12) -0.0101(14) 0.0087(12) -0.0249(16) C23 0.055(2) 0.062(2) 0.0242(13) -0.0021(14) 0.0074(13) -0.0237(17) C24 0.0516(19) 0.056(2) 0.0229(13) 0.0008(13) 0.0027(12) -0.0147(15) C25 0.0377(15) 0.059(2) 0.0185(11) 0.0030(12) -0.0008(10) -0.0092(14) C26 0.0307(14) 0.068(2) 0.0180(11) -0.0103(12) 0.0033(10) -0.0136(14) N27 0.0284(11) 0.0608(17) 0.0181(10) -0.0043(10) 0.0017(8) -0.0065(11) C28 0.0304(14) 0.069(2) 0.0259(13) -0.0062(14) 0.0012(11) -0.0018(14) N29 0.0312(14) 0.086(2) 0.0409(15) -0.0064(15) 0.0015(11) 0.0078(14) C30 0.0287(15) 0.097(3) 0.0396(17) -0.0124(19) 0.0048(13) -0.0028(18) C31 0.0286(14) 0.087(3) 0.0285(14) -0.0098(16) 0.0046(12) -0.0138(16) C32 0.0354(15) 0.063(2) 0.0251(13) 0.0085(13) -0.0028(11) -0.0063(14) N33 0.0297(12) 0.0662(18) 0.0257(11) 0.0147(11) -0.0024(9) -0.0079(12) C34 0.0292(15) 0.080(3) 0.053(2) 0.0300(19) -0.0021(14) -0.0080(16) N35 0.0309(15) 0.105(3) 0.081(3) 0.046(2) -0.0046(15) -0.0042(17) C36 0.0372(19) 0.095(3) 0.070(3) 0.032(2) -0.0094(18) 0.002(2) C37 0.0431(18) 0.075(3) 0.0427(18) 0.0194(18) -0.0060(14) 0.0006(17) B38 0.059(2) 0.061(3) 0.0302(17) 0.0036(17) 0.0081(16) 0.019(2) F39 0.0573(13) 0.0720(16) 0.0657(15) 0.0167(12) 0.0050(11) 0.0157(12) F40 0.0960(19) 0.0765(16) 0.0249(9) 0.0044(9) 0.0067(10) 0.0128(13) F41 0.102(2) 0.0719(16) 0.0320(10) 0.0064(10) 0.0193(12) 0.0185(14) F42 0.0535(14) 0.0769(17) 0.0822(18) -0.0095(14) 0.0072(12) 0.0200(12) B43A 0.025(3) 0.038(4) 0.035(3) -0.001(3) -0.001(2) 0.001(3) F44A 0.090(5) 0.081(4) 0.157(7) -0.034(4) 0.055(5) 0.022(4) F45A 0.103(4) 0.055(3) 0.113(5) 0.039(3) 0.029(4) 0.026(3) F46A 0.077(4) 0.192(8) 0.083(4) -0.038(5) -0.006(3) -0.070(5) F47A 0.046(3) 0.232(12) 0.061(4) -0.036(5) 0.023(2) -0.010(4) C48 0.062(3) 0.108(4) 0.049(2) 0.005(2) -0.0033(19) 0.030(3) N49 0.0585(19) 0.082(2) 0.0260(13) -0.0012(14) 0.0022(12) 0.0152(18) O50 0.0729(19) 0.082(2) 0.0318(13) -0.0018(13) -0.0067(12) 0.0201(16) O51 0.076(2) 0.102(3) 0.0541(18) 0.0015(17) 0.0126(15) -0.005(2) C52A 0.092(6) 0.083(6) 0.070(5) 0.002(4) -0.004(4) -0.017(5) N53A 0.040(2) 0.049(3) 0.060(3) 0.023(2) -0.009(2) -0.005(2) O54A 0.064(3) 0.075(3) 0.145(5) -0.024(3) -0.054(3) 0.004(3) O55A 0.044(2) 0.127(5) 0.107(4) -0.026(4) -0.009(2) 0.016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N20 1.915(3) . ? Fe1 N2 1.920(3) . ? Fe1 N15 2.013(3) . ? Fe1 N27 2.015(3) . ? Fe1 N9 2.016(2) . ? Fe1 N33 2.023(3) . ? N2 C7 1.374(4) . ? N2 C3 1.385(3) . ? C3 C4 1.410(5) . ? C3 C8 1.493(5) . ? C4 C5 1.412(6) . ? C5 C6 1.419(4) . ? C6 C7 1.408(5) . ? C7 C14 1.503(4) . ? C8 N9 1.388(4) . ? C8 C13 1.410(4) . ? N9 C10 1.362(5) . ? C10 N11 1.357(4) . ? N11 C12 1.365(5) . ? C12 C13 1.399(6) . ? C14 N15 1.385(4) . ? C14 C19 1.398(5) . ? N15 C16 1.372(3) . ? C16 N17 1.363(4) . ? N17 C18 1.363(5) . ? C18 C19 1.411(4) . ? N20 C21 1.377(4) . ? N20 C25 1.384(4) . ? C21 C22 1.406(5) . ? C21 C26 1.489(5) . ? C22 C23 1.410(6) . ? C23 C24 1.420(5) . ? C24 C25 1.408(5) . ? C25 C32 1.490(4) . ? C26 N27 1.382(4) . ? C26 C31 1.408(4) . ? N27 C28 1.363(5) . ? C28 N29 1.363(4) . ? N29 C30 1.357(5) . ? C30 C31 1.394(6) . ? C32 N33 1.391(5) . ? C32 C37 1.406(5) . ? N33 C34 1.357(4) . ? C34 N35 1.351(5) . ? N35 C36 1.357(6) . ? C36 C37 1.406(6) . ? B38 F42 1.411(6) . ? B38 F40 1.412(5) . ? B38 F41 1.415(5) . ? B38 F39 1.429(5) . ? B43A F46A 1.375(8) . ? B43A F45A 1.383(8) . ? B43A F47A 1.386(9) . ? B43A F44A 1.398(9) . ? B43B F45B 1.388(13) . ? B43B F46B 1.395(13) . ? B43B F47B 1.397(13) . ? B43B F44B 1.412(13) . ? C48 N49 1.503(5) . ? N49 O50 1.230(5) . ? N49 O51 1.235(5) . ? C52A N53A 1.495(10) . ? N53A O55A 1.182(7) . ? N53A O54A 1.236(7) . ? C52B N53B 1.452(14) . ? N53B O55B 1.192(15) . ? N53B O54B 1.211(14) . ? C56A N57A 1.458(11) . ? N57A O58A 1.175(9) . ? N57A O59A 1.231(9) . ? C56B N57B 1.428(16) . ? N57B O59B 1.243(14) . ? N57B O58B 1.297(13) . ? N57B O58C 1.195(13) . ? N57B O59C 1.277(13) . ? N57B C56C 1.555(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N20 Fe1 N2 177.87(10) . . ? N20 Fe1 N15 101.18(10) . . ? N2 Fe1 N15 80.71(11) . . ? N20 Fe1 N27 80.73(11) . . ? N2 Fe1 N27 98.35(11) . . ? N15 Fe1 N27 89.91(10) . . ? N20 Fe1 N9 97.27(11) . . ? N2 Fe1 N9 80.84(11) . . ? N15 Fe1 N9 161.55(11) . . ? N27 Fe1 N9 92.71(9) . . ? N20 Fe1 N33 80.69(11) . . ? N2 Fe1 N33 100.27(10) . . ? N15 Fe1 N33 92.25(11) . . ? N27 Fe1 N33 161.36(11) . . ? N9 Fe1 N33 91.06(11) . . ? C7 N2 C3 120.4(3) . . ? C7 N2 Fe1 120.11(18) . . ? C3 N2 Fe1 119.5(2) . . ? N2 C3 C4 120.4(3) . . ? N2 C3 C8 111.3(3) . . ? C4 C3 C8 128.3(3) . . ? C3 C4 C5 119.2(3) . . ? C4 C5 C6 120.2(3) . . ? C7 C6 C5 118.2(3) . . ? N2 C7 C6 121.6(3) . . ? N2 C7 C14 110.7(3) . . ? C6 C7 C14 127.8(3) . . ? N9 C8 C13 120.6(3) . . ? N9 C8 C3 113.6(2) . . ? C13 C8 C3 125.8(3) . . ? C10 N9 C8 116.9(2) . . ? C10 N9 Fe1 128.4(2) . . ? C8 N9 Fe1 114.7(2) . . ? N11 C10 N9 126.0(3) . . ? C10 N11 C12 116.2(3) . . ? N11 C12 C13 122.8(3) . . ? C12 C13 C8 117.5(3) . . ? N15 C14 C19 120.9(3) . . ? N15 C14 C7 113.8(3) . . ? C19 C14 C7 125.3(3) . . ? C16 N15 C14 117.2(3) . . ? C16 N15 Fe1 128.2(2) . . ? C14 N15 Fe1 114.56(18) . . ? N17 C16 N15 125.3(3) . . ? C18 N17 C16 116.2(3) . . ? N17 C18 C19 122.9(3) . . ? C14 C19 C18 117.4(3) . . ? C21 N20 C25 120.4(3) . . ? C21 N20 Fe1 119.4(2) . . ? C25 N20 Fe1 119.93(19) . . ? N20 C21 C22 120.8(3) . . ? N20 C21 C26 111.3(3) . . ? C22 C21 C26 127.9(3) . . ? C21 C22 C23 119.2(3) . . ? C22 C23 C24 119.9(3) . . ? C25 C24 C23 118.6(3) . . ? N20 C25 C24 121.0(3) . . ? N20 C25 C32 111.1(3) . . ? C24 C25 C32 127.9(3) . . ? N27 C26 C31 120.7(3) . . ? N27 C26 C21 113.8(3) . . ? C31 C26 C21 125.5(3) . . ? C28 N27 C26 117.3(3) . . ? C28 N27 Fe1 128.2(2) . . ? C26 N27 Fe1 114.4(2) . . ? N29 C28 N27 125.2(3) . . ? C30 N29 C28 116.2(3) . . ? N29 C30 C31 123.4(3) . . ? C30 C31 C26 117.1(3) . . ? N33 C32 C37 120.5(3) . . ? N33 C32 C25 113.8(3) . . ? C37 C32 C25 125.7(3) . . ? C34 N33 C32 117.2(3) . . ? C34 N33 Fe1 128.4(2) . . ? C32 N33 Fe1 114.4(2) . . ? N35 C34 N33 125.6(3) . . ? C34 N35 C36 116.7(3) . . ? N35 C36 C37 122.8(4) . . ? C36 C37 C32 117.1(4) . . ? F42 B38 F40 109.2(3) . . ? F42 B38 F41 110.0(3) . . ? F40 B38 F41 109.8(4) . . ? F42 B38 F39 109.0(4) . . ? F40 B38 F39 110.0(3) . . ? F41 B38 F39 108.8(3) . . ? F46A B43A F45A 108.5(7) . . ? F46A B43A F47A 113.5(7) . . ? F45A B43A F47A 104.6(7) . . ? F46A B43A F44A 110.1(6) . . ? F45A B43A F44A 109.5(7) . . ? F47A B43A F44A 110.6(8) . . ? F45B B43B F46B 109.5(9) . . ? F45B B43B F47B 119.7(11) . . ? F46B B43B F47B 110.2(10) . . ? F45B B43B F44B 98.3(9) . . ? F46B B43B F44B 108.9(10) . . ? F47B B43B F44B 109.3(10) . . ? O50 N49 O51 124.1(4) . . ? O50 N49 C48 118.1(4) . . ? O51 N49 C48 117.8(4) . . ? O55A N53A O54A 119.4(7) . . ? O55A N53A C52A 121.2(6) . . ? O54A N53A C52A 119.4(6) . . ? O55B N53B O54B 121.7(16) . . ? O55B N53B C52B 120.9(15) . . ? O54B N53B C52B 117.3(14) . . ? O58A N57A O59A 122.3(9) . . ? O58A N57A C56A 119.5(9) . . ? O59A N57A C56A 117.6(8) . . ? O59B N57B O58B 109.4(13) . . ? O59B N57B C56B 120.5(17) . . ? O58B N57B C56B 114.2(16) . . ? O58C N57B O59C 120.1(14) . . ? O58C N57B C56C 119.7(13) . . ? O59C N57B C56C 111.4(11) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.10 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.239 _refine_diff_density_min -0.790 _refine_diff_density_rms 0.101 data_lkc046 _database_code_depnum_ccdc_archive 'CCDC 893215' #TrackingRef 'LKC Dalton revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(2,6-bis(pyrimidin-4-yl)pyridine]cobalt(II) ditetrafluoroborate ; _chemical_name_common ;Bis(2,6-bis(pyrimidin-4-yl)pyridine)cobalt(ii) ditetrafluoroborate ; _chemical_melting_point ? _chemical_formula_moiety 'C26 H18 Co N10, 2[B F4]' _chemical_formula_sum 'C26 H18 B2 Co F8 N10' _chemical_formula_weight 703.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.672(4) _cell_length_b 10.146(2) _cell_length_c 15.074(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.816(9) _cell_angle_gamma 90.00 _cell_volume 2821.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 54457 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 31.05 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 0.700 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.84 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 54457 _diffrn_reflns_av_R_equivalents 0.0815 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 31.05 _reflns_number_total 8904 _reflns_number_gt 6803 _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 'X-SEED (Barbour, 2001)' _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 anion B43-F47 is disordered over two equally occupied orientations, labelled 'A' and 'B'. This was modelled using the refined restraints B---F = 1.39(2) and F...F = 2.27(2) \%A. All non-H atoms were refined anisotropically, and 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^)+(0.1084P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8904 _refine_ls_number_parameters 470 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1529 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.755278(12) 0.66105(2) 0.690089(14) 0.01888(9) Uani 1 1 d . . . N2 N 0.66729(8) 0.78138(15) 0.64841(9) 0.0209(3) Uani 1 1 d . . . C3 C 0.66317(9) 0.90001(18) 0.68828(11) 0.0225(3) Uani 1 1 d . . . C4 C 0.59938(11) 0.9752(2) 0.67268(13) 0.0300(4) Uani 1 1 d . . . H4 H 0.5960 1.0570 0.7025 0.036 Uiso 1 1 calc R . . C5 C 0.54064(11) 0.9266(2) 0.61193(14) 0.0328(4) Uani 1 1 d . . . H5 H 0.4967 0.9753 0.6009 0.039 Uiso 1 1 calc R . . C6 C 0.54658(10) 0.8071(2) 0.56775(13) 0.0298(4) Uani 1 1 d . . . H6 H 0.5079 0.7749 0.5250 0.036 Uiso 1 1 calc R . . C7 C 0.61136(9) 0.73609(18) 0.58838(11) 0.0226(3) Uani 1 1 d . . . C8 C 0.73237(10) 0.94137(18) 0.74485(11) 0.0231(3) Uani 1 1 d . . . N9 N 0.78705(8) 0.85099(15) 0.74907(10) 0.0220(3) Uani 1 1 d . . . C10 C 0.85230(10) 0.88677(19) 0.79317(11) 0.0250(3) Uani 1 1 d . . . H10 H 0.8905 0.8247 0.7939 0.030 Uiso 1 1 calc R . . N11 N 0.86895(9) 1.00073(17) 0.83611(11) 0.0296(3) Uani 1 1 d . . . C12 C 0.81388(12) 1.0872(2) 0.83404(13) 0.0319(4) Uani 1 1 d . . . H12 H 0.8228 1.1685 0.8651 0.038 Uiso 1 1 calc R . . C13 C 0.74398(11) 1.0626(2) 0.78802(13) 0.0287(4) Uani 1 1 d . . . H13 H 0.7063 1.1258 0.7864 0.034 Uiso 1 1 calc R . . C14 C 0.62811(9) 0.60758(18) 0.54756(11) 0.0234(3) Uani 1 1 d . . . N15 N 0.69115(8) 0.54971(16) 0.58555(10) 0.0253(3) Uani 1 1 d . . . C16 C 0.70963(11) 0.4358(2) 0.54888(13) 0.0319(4) Uani 1 1 d . . . H16 H 0.7530 0.3944 0.5764 0.038 Uiso 1 1 calc R . . N17 N 0.67226(11) 0.3754(2) 0.47691(12) 0.0365(4) Uani 1 1 d . . . C18 C 0.61038(12) 0.4336(2) 0.43984(13) 0.0354(4) Uani 1 1 d . . . H18 H 0.5825 0.3936 0.3889 0.042 Uiso 1 1 calc R . . C19 C 0.58521(11) 0.5507(2) 0.47296(12) 0.0308(4) Uani 1 1 d . . . H19 H 0.5410 0.5899 0.4461 0.037 Uiso 1 1 calc R . . N20 N 0.84133(8) 0.55060(14) 0.75100(9) 0.0199(3) Uani 1 1 d . . . C21 C 0.90526(9) 0.55326(17) 0.71819(11) 0.0207(3) Uani 1 1 d . . . C22 C 0.96852(10) 0.50027(19) 0.76599(12) 0.0256(3) Uani 1 1 d . . . H22 H 1.0129 0.5034 0.7425 0.031 Uiso 1 1 calc R . . C23 C 0.96507(10) 0.44234(19) 0.84940(13) 0.0278(4) Uani 1 1 d . . . H23 H 1.0077 0.4072 0.8839 0.033 Uiso 1 1 calc R . . C24 C 0.89912(10) 0.43610(19) 0.88213(11) 0.0251(3) Uani 1 1 d . . . H24 H 0.8959 0.3948 0.9379 0.030 Uiso 1 1 calc R . . C25 C 0.83742(9) 0.49249(17) 0.83053(11) 0.0203(3) Uani 1 1 d . . . C26 C 0.90060(9) 0.62190(17) 0.63031(11) 0.0210(3) Uani 1 1 d . . . N27 N 0.83658(9) 0.68434(16) 0.60224(10) 0.0245(3) Uani 1 1 d . . . C28 C 0.83008(12) 0.7501(2) 0.52402(13) 0.0318(4) Uani 1 1 d . . . H28 H 0.7853 0.7938 0.5052 0.038 Uiso 1 1 calc R . . N29 N 0.88043(11) 0.76007(19) 0.47010(11) 0.0346(4) Uani 1 1 d . . . C30 C 0.94345(12) 0.6964(2) 0.49789(13) 0.0318(4) Uani 1 1 d . . . H30 H 0.9804 0.6996 0.4610 0.038 Uiso 1 1 calc R . . C31 C 0.95674(11) 0.6260(2) 0.57846(12) 0.0276(4) Uani 1 1 d . . . H31 H 1.0017 0.5830 0.5972 0.033 Uiso 1 1 calc R . . C32 C 0.76455(9) 0.50157(17) 0.85973(10) 0.0207(3) Uani 1 1 d . . . N33 N 0.71622(8) 0.58391(15) 0.80987(9) 0.0214(3) Uani 1 1 d . . . C34 C 0.65098(10) 0.6000(2) 0.83704(12) 0.0262(3) Uani 1 1 d . . . H34 H 0.6173 0.6568 0.8022 0.031 Uiso 1 1 calc R . . N35 N 0.62957(9) 0.54256(18) 0.90908(11) 0.0297(3) Uani 1 1 d . . . C36 C 0.67699(11) 0.4575(2) 0.95494(12) 0.0304(4) Uani 1 1 d . . . H36 H 0.6629 0.4118 1.0045 0.036 Uiso 1 1 calc R . . C37 C 0.74603(11) 0.4333(2) 0.93307(12) 0.0278(4) Uani 1 1 d . . . H37 H 0.7786 0.3733 0.9666 0.033 Uiso 1 1 calc R . . B38 B 0.88880(13) 1.2186(2) 0.62653(13) 0.0299(4) Uani 1 1 d . . . F39 F 0.96118(7) 1.24530(14) 0.66482(9) 0.0402(3) Uani 1 1 d . . . F40 F 0.87882(8) 1.08229(14) 0.61303(9) 0.0426(3) Uani 1 1 d . . . F41 F 0.84144(8) 1.26618(14) 0.68198(9) 0.0404(3) Uani 1 1 d . . . F42 F 0.87437(9) 1.28327(15) 0.54244(8) 0.0451(3) Uani 1 1 d . . . B43A B 0.5624(5) 0.3269(9) 0.6981(5) 0.023(3) Uani 0.50 1 d PD B 1 F44A F 0.4971(3) 0.2693(8) 0.7063(5) 0.069(2) Uani 0.50 1 d PD B 1 F45A F 0.5819(6) 0.2816(11) 0.6170(5) 0.063(3) Uani 0.50 1 d PD B 1 F46A F 0.6148(5) 0.2933(12) 0.7680(5) 0.0554(18) Uani 0.50 1 d PD B 1 F47A F 0.5528(11) 0.4631(10) 0.6914(12) 0.043(2) Uani 0.50 1 d PD B 1 B43B B 0.5652(7) 0.3294(12) 0.7005(8) 0.046(5) Uani 0.50 1 d PD A 2 F44B F 0.5152(4) 0.2519(7) 0.7373(5) 0.080(3) Uani 0.50 1 d PD A 2 F45B F 0.5693(5) 0.2813(10) 0.6149(5) 0.0438(18) Uani 0.50 1 d PD A 2 F46B F 0.6318(6) 0.3139(13) 0.7534(6) 0.090(4) Uani 0.50 1 d PD A 2 F47B F 0.5449(10) 0.4611(9) 0.6979(11) 0.042(2) Uani 0.50 1 d PD A 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 Co1 0.01436(13) 0.02319(14) 0.01878(12) 0.00052(7) 0.00155(8) 0.00271(8) N2 0.0163(6) 0.0241(7) 0.0225(6) 0.0018(5) 0.0034(5) 0.0030(5) C3 0.0184(8) 0.0244(8) 0.0256(7) 0.0015(6) 0.0061(6) 0.0032(6) C4 0.0234(9) 0.0303(9) 0.0372(9) 0.0021(7) 0.0077(7) 0.0103(7) C5 0.0194(8) 0.0400(11) 0.0392(10) 0.0071(8) 0.0053(7) 0.0114(8) C6 0.0170(8) 0.0389(10) 0.0326(9) 0.0058(7) 0.0012(6) 0.0043(7) C7 0.0160(7) 0.0281(8) 0.0233(7) 0.0039(6) 0.0020(5) 0.0024(6) C8 0.0212(8) 0.0250(8) 0.0241(7) 0.0011(6) 0.0068(6) 0.0015(6) N9 0.0189(7) 0.0247(7) 0.0226(6) -0.0009(5) 0.0040(5) 0.0009(5) C10 0.0205(8) 0.0279(9) 0.0267(7) -0.0010(6) 0.0042(6) -0.0002(7) N11 0.0244(8) 0.0325(8) 0.0317(7) -0.0047(6) 0.0043(6) -0.0050(6) C12 0.0350(10) 0.0273(9) 0.0340(9) -0.0065(7) 0.0072(8) -0.0028(8) C13 0.0278(9) 0.0257(9) 0.0337(8) -0.0028(7) 0.0080(7) 0.0019(7) C14 0.0183(8) 0.0292(9) 0.0225(7) 0.0019(6) 0.0021(6) 0.0000(7) N15 0.0199(7) 0.0301(8) 0.0255(6) -0.0031(5) 0.0021(5) 0.0040(6) C16 0.0289(10) 0.0300(9) 0.0363(9) -0.0071(7) 0.0032(7) 0.0051(8) N17 0.0376(10) 0.0371(9) 0.0354(8) -0.0109(7) 0.0073(7) -0.0014(8) C18 0.0335(10) 0.0449(12) 0.0276(8) -0.0087(8) 0.0046(7) -0.0093(9) C19 0.0233(9) 0.0425(11) 0.0253(8) -0.0003(7) -0.0007(6) -0.0034(8) N20 0.0168(6) 0.0227(7) 0.0202(6) -0.0008(5) 0.0034(5) -0.0004(5) C21 0.0180(7) 0.0222(8) 0.0225(7) -0.0012(5) 0.0045(5) 0.0001(6) C22 0.0169(8) 0.0293(9) 0.0308(8) 0.0005(6) 0.0039(6) 0.0026(7) C23 0.0191(8) 0.0299(9) 0.0327(8) 0.0048(7) -0.0013(6) 0.0033(7) C24 0.0214(8) 0.0273(9) 0.0256(7) 0.0048(6) 0.0010(6) 0.0015(7) C25 0.0188(7) 0.0208(7) 0.0211(6) -0.0001(5) 0.0022(5) 0.0004(6) C26 0.0187(8) 0.0225(7) 0.0222(7) -0.0013(6) 0.0044(5) -0.0001(6) N27 0.0235(7) 0.0287(7) 0.0219(6) 0.0026(5) 0.0054(5) 0.0039(6) C28 0.0336(10) 0.0363(10) 0.0263(8) 0.0072(7) 0.0068(7) 0.0070(8) N29 0.0399(10) 0.0399(10) 0.0262(7) 0.0045(6) 0.0118(7) 0.0012(8) C30 0.0315(10) 0.0400(11) 0.0267(8) -0.0025(7) 0.0128(7) -0.0041(9) C31 0.0233(9) 0.0335(9) 0.0275(8) -0.0028(7) 0.0082(6) -0.0007(7) C32 0.0181(7) 0.0224(8) 0.0213(7) -0.0015(5) 0.0027(5) -0.0020(6) N33 0.0167(7) 0.0241(7) 0.0237(6) -0.0006(5) 0.0038(5) -0.0005(5) C34 0.0185(8) 0.0324(9) 0.0281(8) -0.0026(6) 0.0052(6) -0.0014(7) N35 0.0218(7) 0.0372(9) 0.0316(7) -0.0035(6) 0.0094(6) -0.0052(7) C36 0.0286(9) 0.0378(10) 0.0265(8) 0.0006(7) 0.0098(7) -0.0066(8) C37 0.0264(9) 0.0324(9) 0.0250(7) 0.0026(7) 0.0051(6) -0.0029(7) B38 0.0311(11) 0.0350(11) 0.0234(8) -0.0022(7) 0.0038(7) 0.0055(9) F39 0.0321(7) 0.0442(8) 0.0425(7) -0.0049(5) 0.0007(5) 0.0019(6) F40 0.0425(8) 0.0368(7) 0.0448(7) -0.0073(5) -0.0048(6) 0.0045(6) F41 0.0401(7) 0.0449(7) 0.0400(7) -0.0041(5) 0.0184(5) 0.0035(6) F42 0.0546(9) 0.0525(8) 0.0277(6) 0.0058(5) 0.0045(5) 0.0081(7) B43A 0.023(5) 0.025(5) 0.020(4) 0.011(3) -0.002(3) 0.003(3) F44A 0.046(2) 0.058(3) 0.103(5) 0.012(3) 0.016(3) -0.027(2) F45A 0.095(6) 0.057(4) 0.042(4) 0.004(3) 0.028(4) -0.012(4) F46A 0.077(4) 0.048(3) 0.0328(16) -0.0020(18) -0.018(2) 0.022(3) F47A 0.044(4) 0.031(4) 0.050(4) 0.007(3) -0.005(3) 0.001(3) B43B 0.052(10) 0.042(8) 0.041(7) -0.021(5) 0.000(6) -0.002(6) F44B 0.122(7) 0.046(3) 0.091(5) -0.001(3) 0.075(5) -0.009(3) F45B 0.055(3) 0.048(4) 0.025(2) -0.010(2) -0.0067(18) 0.020(2) F46B 0.087(6) 0.055(5) 0.101(7) -0.031(5) -0.070(5) 0.032(4) F47B 0.047(5) 0.029(4) 0.044(3) -0.009(3) -0.011(3) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N20 2.0563(15) . ? Co1 N2 2.0659(15) . ? Co1 N15 2.1482(15) . ? Co1 N9 2.1666(15) . ? Co1 N27 2.1749(16) . ? Co1 N33 2.1928(15) . ? N2 C3 1.353(2) . ? N2 C7 1.353(2) . ? C3 C4 1.403(3) . ? C3 C8 1.495(2) . ? C4 C5 1.406(3) . ? C5 C6 1.396(3) . ? C6 C7 1.401(2) . ? C7 C14 1.495(3) . ? C8 N9 1.366(2) . ? C8 C13 1.393(3) . ? N9 C10 1.345(2) . ? C10 N11 1.338(2) . ? N11 C12 1.349(3) . ? C12 C13 1.403(3) . ? C14 N15 1.361(2) . ? C14 C19 1.401(2) . ? N15 C16 1.349(2) . ? C16 N17 1.344(3) . ? N17 C18 1.341(3) . ? C18 C19 1.397(3) . ? N20 C25 1.348(2) . ? N20 C21 1.360(2) . ? C21 C22 1.394(2) . ? C21 C26 1.487(2) . ? C22 C23 1.398(3) . ? C23 C24 1.396(3) . ? C24 C25 1.409(2) . ? C25 C32 1.496(2) . ? C26 N27 1.362(2) . ? C26 C31 1.401(2) . ? N27 C28 1.344(2) . ? C28 N29 1.338(3) . ? N29 C30 1.351(3) . ? C30 C31 1.398(3) . ? C32 N33 1.367(2) . ? C32 C37 1.392(2) . ? N33 C34 1.353(2) . ? C34 N35 1.346(2) . ? N35 C36 1.348(3) . ? C36 C37 1.400(3) . ? B38 F41 1.393(3) . ? B38 F40 1.406(3) . ? B38 F39 1.412(3) . ? B38 F42 1.416(2) . ? B43A F46A 1.366(9) . ? B43A F44A 1.375(9) . ? B43A F47A 1.395(10) . ? B43A F45A 1.406(10) . ? B43B F46B 1.380(13) . ? B43B F47B 1.387(12) . ? B43B F45B 1.393(11) . ? B43B F44B 1.399(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N20 Co1 N2 171.27(5) . . ? N20 Co1 N15 110.52(6) . . ? N2 Co1 N15 76.10(6) . . ? N20 Co1 N9 98.94(6) . . ? N2 Co1 N9 75.77(6) . . ? N15 Co1 N9 148.82(6) . . ? N20 Co1 N27 76.15(6) . . ? N2 Co1 N27 110.33(6) . . ? N15 Co1 N27 88.45(6) . . ? N9 Co1 N27 88.88(6) . . ? N20 Co1 N33 76.91(6) . . ? N2 Co1 N33 96.43(6) . . ? N15 Co1 N33 101.42(6) . . ? N9 Co1 N33 94.83(6) . . ? N27 Co1 N33 153.05(6) . . ? C3 N2 C7 120.58(15) . . ? C3 N2 Co1 119.17(11) . . ? C7 N2 Co1 119.93(12) . . ? N2 C3 C4 120.91(17) . . ? N2 C3 C8 113.59(15) . . ? C4 C3 C8 125.45(17) . . ? C3 C4 C5 118.41(19) . . ? C6 C5 C4 120.28(17) . . ? C5 C6 C7 118.03(18) . . ? N2 C7 C6 121.67(18) . . ? N2 C7 C14 112.51(15) . . ? C6 C7 C14 125.81(16) . . ? N9 C8 C13 120.61(17) . . ? N9 C8 C3 114.36(15) . . ? C13 C8 C3 124.98(16) . . ? C10 N9 C8 117.09(15) . . ? C10 N9 Co1 127.81(13) . . ? C8 N9 Co1 114.97(12) . . ? N11 C10 N9 126.72(18) . . ? C10 N11 C12 115.56(17) . . ? N11 C12 C13 122.93(18) . . ? C8 C13 C12 117.02(18) . . ? N15 C14 C19 120.74(17) . . ? N15 C14 C7 115.16(14) . . ? C19 C14 C7 124.03(16) . . ? C16 N15 C14 117.16(16) . . ? C16 N15 Co1 127.05(13) . . ? C14 N15 Co1 115.52(12) . . ? N17 C16 N15 125.98(19) . . ? C18 N17 C16 116.33(19) . . ? N17 C18 C19 122.73(18) . . ? C18 C19 C14 117.05(18) . . ? C25 N20 C21 120.15(14) . . ? C25 N20 Co1 119.36(11) . . ? C21 N20 Co1 119.73(11) . . ? N20 C21 C22 121.71(15) . . ? N20 C21 C26 113.47(15) . . ? C22 C21 C26 124.77(16) . . ? C21 C22 C23 118.34(17) . . ? C24 C23 C22 120.09(16) . . ? C23 C24 C25 118.51(16) . . ? N20 C25 C24 121.16(16) . . ? N20 C25 C32 114.24(14) . . ? C24 C25 C32 124.49(15) . . ? N27 C26 C31 120.60(16) . . ? N27 C26 C21 115.04(15) . . ? C31 C26 C21 124.35(16) . . ? C28 N27 C26 117.42(16) . . ? C28 N27 Co1 127.63(14) . . ? C26 N27 Co1 114.94(11) . . ? N29 C28 N27 126.40(19) . . ? C28 N29 C30 115.79(17) . . ? N29 C30 C31 122.94(18) . . ? C30 C31 C26 116.84(18) . . ? N33 C32 C37 121.13(16) . . ? N33 C32 C25 115.43(14) . . ? C37 C32 C25 123.43(16) . . ? C34 N33 C32 117.14(15) . . ? C34 N33 Co1 129.39(12) . . ? C32 N33 Co1 113.32(11) . . ? N35 C34 N33 125.77(18) . . ? C34 N35 C36 115.96(17) . . ? N35 C36 C37 123.18(17) . . ? C32 C37 C36 116.70(18) . . ? F41 B38 F40 110.21(19) . . ? F41 B38 F39 110.13(16) . . ? F40 B38 F39 110.19(17) . . ? F41 B38 F42 109.00(17) . . ? F40 B38 F42 108.86(16) . . ? F39 B38 F42 108.42(19) . . ? F46A B43A F44A 111.4(7) . . ? F46A B43A F47A 111.8(10) . . ? F44A B43A F47A 108.7(10) . . ? F46A B43A F45A 109.9(8) . . ? F44A B43A F45A 106.9(9) . . ? F47A B43A F45A 108.0(9) . . ? F46B B43B F47B 110.1(11) . . ? F46B B43B F45B 108.8(10) . . ? F47B B43B F45B 111.4(10) . . ? F46B B43B F44B 107.7(10) . . ? F47B B43B F44B 110.9(11) . . ? F45B B43B F44B 107.8(9) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 31.05 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.703 _refine_diff_density_min -0.927 _refine_diff_density_rms 0.135