# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Barrett, Simon' 'Kilner, Colin' 'Halcrow, Malcolm A.' _publ_contact_author_name 'Halcrow, Malcolm A.' _publ_contact_author_email M.A.Halcrow@leeds.ac.uk _publ_section_title ; Spin-Crossover in [Fe(3-bpp)2][BF4]2 in Different Solvents - a Dramatic Stabilisation of the Low-Spin State in Water ; # Attachment '- Solvent dependence Dalton.CIF' data_mh360 _database_code_depnum_ccdc_archive 'CCDC 821509' #TrackingRef '- Solvent dependence Dalton.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-di(pyrazol-3-yl)pyridine]iron(II) ditetrafluoroborate tris-diethyl ether solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H18 Fe N10, 2[B F4], 3[C4 H10 O]' _chemical_formula_sum 'C34 H48 B2 F8 Fe N10 O3' _chemical_formula_weight 874.29 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 '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 23.953(5) _cell_length_b 9.962(2) _cell_length_c 36.531(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.25(3) _cell_angle_gamma 90.00 _cell_volume 8485(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 61922 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.48 _exptl_crystal_description Fragment _exptl_crystal_colour Orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3632 _exptl_absorpt_coefficient_mu 0.436 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.537 _exptl_absorpt_correction_T_max 0.709 _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 61922 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9680 _reflns_number_gt 7576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 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. No disorder was included in the model, and no restraints were applied. All non-H atoms were refined anisotropically, while H atoms were placed in calculated positions and refined 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^)+(0.0731P)^2^+16.4964P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 9680 _refine_ls_number_parameters 530 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1643 _refine_ls_wR_factor_gt 0.1498 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.602769(14) 0.35943(4) 0.885389(9) 0.03150(11) Uani 1 1 d . . . N2 N 0.53713(9) 0.4381(2) 0.90696(6) 0.0372(5) Uani 1 1 d . . . C3 C 0.50605(11) 0.5416(3) 0.88943(8) 0.0419(6) Uani 1 1 d . . . C4 C 0.46076(13) 0.5959(3) 0.90304(10) 0.0519(7) Uani 1 1 d . . . H4 H 0.4387 0.6687 0.8906 0.062 Uiso 1 1 calc R . . C5 C 0.44901(14) 0.5402(4) 0.93523(10) 0.0577(8) Uani 1 1 d . . . H5 H 0.4186 0.5751 0.9451 0.069 Uiso 1 1 calc R . . C6 C 0.48133(13) 0.4342(3) 0.95301(9) 0.0512(7) Uani 1 1 d . . . H6 H 0.4736 0.3961 0.9752 0.061 Uiso 1 1 calc R . . C7 C 0.52529(12) 0.3844(3) 0.93803(8) 0.0410(6) Uani 1 1 d . . . C8 C 0.52460(11) 0.5869(3) 0.85621(8) 0.0412(6) Uani 1 1 d . . . N9 N 0.57030(9) 0.5218(2) 0.84886(6) 0.0386(5) Uani 1 1 d . . . N10 N 0.57960(11) 0.5814(3) 0.81767(6) 0.0472(6) Uani 1 1 d . . . H10 H 0.6074 0.5592 0.8067 0.057 Uiso 1 1 calc R . . C11 C 0.54106(17) 0.6791(3) 0.80537(9) 0.0592(9) Uani 1 1 d . . . H11 H 0.5393 0.7334 0.7837 0.071 Uiso 1 1 calc R . . C12 C 0.50494(15) 0.6870(3) 0.82929(9) 0.0558(8) Uani 1 1 d . . . H12 H 0.4736 0.7467 0.8280 0.067 Uiso 1 1 calc R . . C13 C 0.56272(13) 0.2723(3) 0.95297(8) 0.0462(7) Uani 1 1 d . . . N14 N 0.60245(10) 0.2390(3) 0.93375(7) 0.0502(6) Uani 1 1 d . . . N15 N 0.62964(13) 0.1317(3) 0.95308(11) 0.0741(10) Uani 1 1 d . . . H15 H 0.6581 0.0882 0.9469 0.089 Uiso 1 1 calc R . . C16 C 0.6076(2) 0.0998(4) 0.98305(12) 0.0808(13) Uani 1 1 d . . . H16 H 0.6199 0.0286 1.0003 0.097 Uiso 1 1 calc R . . C17 C 0.56519(18) 0.1874(4) 0.98374(10) 0.0660(10) Uani 1 1 d . . . H17 H 0.5418 0.1909 1.0015 0.079 Uiso 1 1 calc R . . N18 N 0.66743(9) 0.2968(2) 0.86030(6) 0.0348(5) Uani 1 1 d . . . C19 C 0.72056(11) 0.3506(3) 0.87130(7) 0.0393(6) Uani 1 1 d . . . C20 C 0.76367(13) 0.3156(4) 0.85341(9) 0.0530(8) Uani 1 1 d . . . H20 H 0.8009 0.3533 0.8612 0.064 Uiso 1 1 calc R . . C21 C 0.75146(14) 0.2245(4) 0.82398(10) 0.0613(9) Uani 1 1 d . . . H21 H 0.7805 0.1999 0.8114 0.074 Uiso 1 1 calc R . . C22 C 0.69709(14) 0.1690(3) 0.81280(9) 0.0529(8) Uani 1 1 d . . . H22 H 0.6884 0.1060 0.7928 0.063 Uiso 1 1 calc R . . C23 C 0.65573(12) 0.2086(3) 0.83187(7) 0.0386(6) Uani 1 1 d . . . C24 C 0.72472(11) 0.4445(3) 0.90244(7) 0.0401(6) Uani 1 1 d . . . N25 N 0.67621(10) 0.4648(2) 0.91406(6) 0.0405(5) Uani 1 1 d . . . N26 N 0.69031(13) 0.5510(3) 0.94299(7) 0.0551(7) Uani 1 1 d . . . H26 H 0.6661 0.5809 0.9559 0.066 Uiso 1 1 calc R . . C27 C 0.74591(17) 0.5857(4) 0.94974(9) 0.0648(10) Uani 1 1 d . . . H27 H 0.7651 0.6456 0.9687 0.078 Uiso 1 1 calc R . . C28 C 0.76975(14) 0.5196(4) 0.92443(8) 0.0547(8) Uani 1 1 d . . . H28 H 0.8084 0.5235 0.9222 0.066 Uiso 1 1 calc R . . C29 C 0.59630(12) 0.1614(3) 0.82423(7) 0.0406(6) Uani 1 1 d . . . N30 N 0.56414(9) 0.2107(3) 0.84651(6) 0.0440(6) Uani 1 1 d . . . N31 N 0.51240(11) 0.1498(3) 0.83457(7) 0.0595(8) Uani 1 1 d . . . H31 H 0.4825 0.1640 0.8443 0.071 Uiso 1 1 calc R . . C32 C 0.51284(15) 0.0652(4) 0.80608(9) 0.0665(11) Uani 1 1 d . . . H32 H 0.4815 0.0116 0.7935 0.080 Uiso 1 1 calc R . . C33 C 0.56541(15) 0.0692(4) 0.79831(8) 0.0576(9) Uani 1 1 d . . . H33 H 0.5785 0.0204 0.7795 0.069 Uiso 1 1 calc R . . B34 B 0.63109(15) 0.8995(5) 0.71766(11) 0.0561(9) Uani 1 1 d . . . F35 F 0.58777(9) 0.8516(2) 0.73399(5) 0.0612(5) Uani 1 1 d . . . F36 F 0.62738(14) 1.0390(3) 0.71656(11) 0.1228(12) Uani 1 1 d . . . F37 F 0.62302(12) 0.8545(4) 0.68209(7) 0.1104(11) Uani 1 1 d . . . F38 F 0.68397(11) 0.8716(4) 0.73796(9) 0.1185(12) Uani 1 1 d . . . B39 B 0.61540(16) 0.7304(4) 0.99786(10) 0.0495(8) Uani 1 1 d . . . F40 F 0.65606(9) 0.7899(2) 0.98089(6) 0.0677(6) Uani 1 1 d . . . F41 F 0.61322(10) 0.5945(2) 0.99050(7) 0.0785(7) Uani 1 1 d . . . F42 F 0.63400(12) 0.7477(3) 1.03544(6) 0.1050(10) Uani 1 1 d . . . F43 F 0.56287(11) 0.7845(3) 0.98668(11) 0.1332(14) Uani 1 1 d . . . C44 C 0.37579(19) 0.3130(5) 0.84925(12) 0.0810(12) Uani 1 1 d . . . H44A H 0.4116 0.3644 0.8538 0.122 Uiso 1 1 calc R . . H44B H 0.3440 0.3730 0.8509 0.122 Uiso 1 1 calc R . . H44C H 0.3685 0.2727 0.8241 0.122 Uiso 1 1 calc R . . C45 C 0.38061(16) 0.2065(5) 0.87766(11) 0.0799(13) Uani 1 1 d . . . H45A H 0.3773 0.2457 0.9020 0.096 Uiso 1 1 calc R . . H45B H 0.3493 0.1405 0.8697 0.096 Uiso 1 1 calc R . . O46 O 0.43518(10) 0.1411(3) 0.88190(7) 0.0647(7) Uani 1 1 d . . . C47 C 0.44163(18) 0.0296(5) 0.90794(11) 0.0792(13) Uani 1 1 d . . . H47A H 0.4088 -0.0326 0.9004 0.095 Uiso 1 1 calc R . . H47B H 0.4424 0.0630 0.9336 0.095 Uiso 1 1 calc R . . C48 C 0.49549(18) -0.0413(4) 0.90768(11) 0.0736(11) Uani 1 1 d . . . H48A H 0.4931 -0.0806 0.8828 0.110 Uiso 1 1 calc R . . H48B H 0.5016 -0.1128 0.9266 0.110 Uiso 1 1 calc R . . H48C H 0.5276 0.0222 0.9135 0.110 Uiso 1 1 calc R . . C49 C 0.5749(2) 0.3955(5) 0.73878(11) 0.0870(14) Uani 1 1 d . . . H49A H 0.5722 0.3408 0.7606 0.130 Uiso 1 1 calc R . . H49B H 0.5620 0.3427 0.7158 0.130 Uiso 1 1 calc R . . H49C H 0.5506 0.4752 0.7377 0.130 Uiso 1 1 calc R . . C50 C 0.6360(2) 0.4380(6) 0.74220(12) 0.0925(15) Uani 1 1 d . . . H50A H 0.6605 0.3577 0.7426 0.111 Uiso 1 1 calc R . . H50B H 0.6389 0.4934 0.7202 0.111 Uiso 1 1 calc R . . O51 O 0.65566(12) 0.5136(3) 0.77594(7) 0.0681(7) Uani 1 1 d . . . C52 C 0.71046(19) 0.5757(6) 0.77938(14) 0.0911(15) Uani 1 1 d . . . H52A H 0.7115 0.6241 0.7559 0.109 Uiso 1 1 calc R . . H52B H 0.7409 0.5063 0.7837 0.109 Uiso 1 1 calc R . . C53 C 0.7208(2) 0.6719(7) 0.81170(14) 0.114(2) Uani 1 1 d . . . H53A H 0.6905 0.7401 0.8074 0.171 Uiso 1 1 calc R . . H53B H 0.7581 0.7156 0.8139 0.171 Uiso 1 1 calc R . . H53C H 0.7206 0.6231 0.8350 0.171 Uiso 1 1 calc R . . C54 C 0.6430(2) -0.1319(4) 0.88675(11) 0.0769(12) Uani 1 1 d . . . H54A H 0.6327 -0.1589 0.9101 0.115 Uiso 1 1 calc R . . H54B H 0.6360 -0.2068 0.8689 0.115 Uiso 1 1 calc R . . H54C H 0.6196 -0.0547 0.8759 0.115 Uiso 1 1 calc R . . C55 C 0.7047(2) -0.0944(5) 0.89486(11) 0.0770(11) Uani 1 1 d . . . H55A H 0.7285 -0.1734 0.9047 0.092 Uiso 1 1 calc R . . H55B H 0.7150 -0.0648 0.8714 0.092 Uiso 1 1 calc R . . O56 O 0.71561(11) 0.0115(3) 0.92195(7) 0.0667(7) Uani 1 1 d . . . C57 C 0.77440(19) 0.0455(5) 0.93375(15) 0.0900(14) Uani 1 1 d . . . H57A H 0.7882 0.0824 0.9123 0.108 Uiso 1 1 calc R . . H57B H 0.7971 -0.0359 0.9428 0.108 Uiso 1 1 calc R . . C58 C 0.7822(2) 0.1465(5) 0.96437(15) 0.0946(16) Uani 1 1 d . . . H58A H 0.7593 0.2265 0.9553 0.142 Uiso 1 1 calc R . . H58B H 0.8228 0.1713 0.9721 0.142 Uiso 1 1 calc R . . H58C H 0.7695 0.1085 0.9859 0.142 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02889(18) 0.0351(2) 0.03107(18) -0.00566(14) 0.00814(12) -0.00246(14) N2 0.0362(10) 0.0337(12) 0.0406(11) -0.0072(9) 0.0064(9) -0.0065(9) C3 0.0391(13) 0.0350(15) 0.0497(15) -0.0084(12) 0.0064(11) -0.0043(11) C4 0.0400(14) 0.0424(17) 0.074(2) -0.0104(15) 0.0135(14) -0.0001(13) C5 0.0473(16) 0.057(2) 0.075(2) -0.0196(17) 0.0267(15) -0.0082(15) C6 0.0540(17) 0.0506(19) 0.0546(16) -0.0117(14) 0.0238(14) -0.0131(14) C7 0.0433(14) 0.0373(16) 0.0414(13) -0.0076(11) 0.0077(11) -0.0134(11) C8 0.0403(13) 0.0337(14) 0.0462(14) -0.0039(11) 0.0030(11) -0.0021(11) N9 0.0441(12) 0.0363(13) 0.0348(10) -0.0001(9) 0.0081(9) -0.0079(9) N10 0.0632(15) 0.0434(14) 0.0352(11) 0.0005(10) 0.0117(10) -0.0104(12) C11 0.088(2) 0.0424(18) 0.0392(15) 0.0054(13) -0.0015(15) -0.0039(17) C12 0.067(2) 0.0401(17) 0.0514(17) 0.0007(13) -0.0049(15) 0.0058(15) C13 0.0517(16) 0.0376(16) 0.0452(14) -0.0060(12) 0.0026(12) -0.0110(12) N14 0.0435(13) 0.0363(14) 0.0614(15) -0.0103(11) -0.0076(11) -0.0019(10) N15 0.0577(17) 0.0411(17) 0.101(3) -0.0191(16) -0.0290(17) 0.0056(13) C16 0.098(3) 0.057(3) 0.069(2) 0.0135(19) -0.020(2) -0.023(2) C17 0.079(2) 0.053(2) 0.0542(19) 0.0068(16) -0.0092(17) -0.0207(19) N18 0.0369(10) 0.0367(12) 0.0315(10) 0.0025(9) 0.0096(8) -0.0049(9) C19 0.0387(13) 0.0413(15) 0.0396(13) 0.0042(11) 0.0125(10) -0.0073(11) C20 0.0411(15) 0.061(2) 0.0613(18) -0.0056(15) 0.0214(13) -0.0101(14) C21 0.0552(18) 0.070(2) 0.069(2) -0.0134(18) 0.0356(16) -0.0047(16) C22 0.0637(19) 0.0501(19) 0.0513(16) -0.0119(14) 0.0263(14) -0.0059(15) C23 0.0473(14) 0.0371(15) 0.0338(12) -0.0005(10) 0.0144(10) -0.0066(11) C24 0.0421(13) 0.0427(16) 0.0351(12) 0.0035(11) 0.0083(10) -0.0123(11) N25 0.0525(13) 0.0369(13) 0.0341(10) -0.0078(9) 0.0139(9) -0.0140(10) N26 0.0821(19) 0.0466(16) 0.0405(12) -0.0144(11) 0.0223(12) -0.0239(14) C27 0.086(2) 0.060(2) 0.0446(16) -0.0055(15) 0.0063(16) -0.0402(19) C28 0.0534(17) 0.062(2) 0.0466(15) 0.0028(14) 0.0059(13) -0.0271(15) C29 0.0486(14) 0.0414(16) 0.0313(12) 0.0012(10) 0.0079(10) -0.0113(12) N30 0.0359(11) 0.0614(17) 0.0333(11) 0.0034(10) 0.0053(9) -0.0127(11) N31 0.0385(12) 0.092(2) 0.0451(13) 0.0112(14) 0.0029(10) -0.0215(13) C32 0.065(2) 0.081(3) 0.0447(17) 0.0060(17) -0.0049(14) -0.0361(19) C33 0.077(2) 0.054(2) 0.0381(14) -0.0037(13) 0.0061(14) -0.0251(17) B34 0.0436(17) 0.068(3) 0.058(2) 0.0073(18) 0.0156(15) 0.0126(17) F35 0.0673(12) 0.0623(13) 0.0592(11) 0.0011(9) 0.0254(9) -0.0014(9) F36 0.123(2) 0.076(2) 0.192(3) 0.025(2) 0.080(2) 0.0030(17) F37 0.0882(17) 0.179(3) 0.0757(16) -0.0304(18) 0.0424(14) -0.0321(19) F38 0.0591(14) 0.172(3) 0.114(2) 0.043(2) -0.0021(14) 0.0117(17) B39 0.0553(19) 0.044(2) 0.0526(18) 0.0019(15) 0.0196(15) -0.0085(15) F40 0.0748(13) 0.0653(14) 0.0701(12) -0.0016(10) 0.0314(10) -0.0233(11) F41 0.0962(16) 0.0598(14) 0.0931(15) -0.0230(12) 0.0496(13) -0.0297(12) F42 0.112(2) 0.150(3) 0.0628(13) -0.0400(16) 0.0400(13) -0.0582(19) F43 0.0680(16) 0.109(3) 0.223(4) 0.087(3) 0.0335(19) 0.0175(15) C44 0.077(3) 0.087(3) 0.076(3) -0.003(2) 0.010(2) -0.021(2) C45 0.059(2) 0.122(4) 0.061(2) 0.001(2) 0.0188(17) -0.011(2) O46 0.0583(13) 0.0837(19) 0.0545(13) -0.0048(12) 0.0179(11) -0.0146(12) C47 0.075(2) 0.109(4) 0.055(2) 0.003(2) 0.0190(18) -0.028(2) C48 0.087(3) 0.067(3) 0.065(2) -0.0085(19) 0.0136(19) -0.024(2) C49 0.119(4) 0.083(3) 0.057(2) -0.012(2) 0.017(2) -0.017(3) C50 0.123(4) 0.102(4) 0.058(2) -0.009(2) 0.033(2) 0.009(3) O51 0.0801(16) 0.0746(18) 0.0549(13) 0.0036(12) 0.0264(12) -0.0025(14) C52 0.072(3) 0.117(4) 0.091(3) 0.034(3) 0.031(2) 0.001(3) C53 0.094(3) 0.150(6) 0.084(3) 0.035(3) -0.009(3) -0.060(4) C54 0.104(3) 0.057(2) 0.058(2) -0.0013(17) -0.007(2) -0.005(2) C55 0.100(3) 0.062(3) 0.065(2) 0.0039(19) 0.011(2) 0.008(2) O56 0.0675(15) 0.0516(15) 0.0709(15) 0.0074(12) -0.0053(12) 0.0017(12) C57 0.070(3) 0.084(3) 0.105(3) 0.016(3) -0.002(2) 0.001(2) C58 0.074(3) 0.073(3) 0.115(4) 0.009(3) -0.024(3) -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 2.068(2) . ? Fe1 N18 2.069(2) . ? Fe1 N25 2.109(2) . ? Fe1 N30 2.113(3) . ? Fe1 N9 2.127(2) . ? Fe1 N14 2.137(3) . ? N2 C7 1.343(3) . ? N2 C3 1.345(4) . ? C3 C4 1.401(4) . ? C3 C8 1.456(4) . ? C4 C5 1.386(5) . ? C5 C6 1.380(5) . ? C6 C7 1.385(4) . ? C7 C13 1.458(4) . ? C8 N9 1.351(4) . ? C8 C12 1.404(4) . ? N9 N10 1.348(3) . ? N10 C11 1.346(4) . ? C11 C12 1.365(5) . ? C13 N14 1.347(4) . ? C13 C17 1.397(5) . ? N14 N15 1.363(4) . ? N15 C16 1.358(6) . ? C16 C17 1.344(7) . ? N18 C23 1.340(3) . ? N18 C19 1.354(3) . ? C19 C20 1.387(4) . ? C19 C24 1.458(4) . ? C20 C21 1.386(5) . ? C21 C22 1.387(5) . ? C22 C23 1.392(4) . ? C23 C29 1.464(4) . ? C24 N25 1.341(4) . ? C24 C28 1.404(4) . ? N25 N26 1.343(3) . ? N26 C27 1.343(4) . ? C27 C28 1.363(5) . ? C29 N30 1.336(4) . ? C29 C33 1.403(4) . ? N30 N31 1.359(3) . ? N31 C32 1.341(5) . ? C32 C33 1.353(5) . ? B34 F38 1.342(4) . ? B34 F37 1.346(5) . ? B34 F36 1.393(5) . ? B34 F35 1.394(4) . ? B39 F43 1.343(5) . ? B39 F42 1.354(4) . ? B39 F41 1.379(4) . ? B39 F40 1.400(4) . ? C44 C45 1.470(6) . ? C45 O46 1.437(5) . ? O46 C47 1.448(5) . ? C47 C48 1.473(6) . ? C49 C50 1.502(7) . ? C50 O51 1.429(5) . ? O51 C52 1.430(5) . ? C52 C53 1.497(8) . ? C54 C55 1.487(6) . ? C55 O56 1.429(5) . ? O56 C57 1.416(5) . ? C57 C58 1.485(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N18 174.36(9) . . ? N2 Fe1 N25 104.03(9) . . ? N18 Fe1 N25 75.30(9) . . ? N2 Fe1 N30 105.54(9) . . ? N18 Fe1 N30 75.39(9) . . ? N25 Fe1 N30 150.41(9) . . ? N2 Fe1 N9 75.54(9) . . ? N18 Fe1 N9 98.89(9) . . ? N25 Fe1 N9 94.38(9) . . ? N30 Fe1 N9 94.04(9) . . ? N2 Fe1 N14 75.56(10) . . ? N18 Fe1 N14 109.99(9) . . ? N25 Fe1 N14 91.69(9) . . ? N30 Fe1 N14 94.49(9) . . ? N9 Fe1 N14 151.09(9) . . ? C7 N2 C3 120.5(2) . . ? C7 N2 Fe1 119.82(19) . . ? C3 N2 Fe1 119.71(18) . . ? N2 C3 C4 121.1(3) . . ? N2 C3 C8 113.1(2) . . ? C4 C3 C8 125.8(3) . . ? C5 C4 C3 118.1(3) . . ? C6 C5 C4 120.3(3) . . ? C5 C6 C7 118.9(3) . . ? N2 C7 C6 121.2(3) . . ? N2 C7 C13 113.0(3) . . ? C6 C7 C13 125.8(3) . . ? N9 C8 C12 111.0(3) . . ? N9 C8 C3 115.7(3) . . ? C12 C8 C3 133.3(3) . . ? N10 N9 C8 104.8(2) . . ? N10 N9 Fe1 139.3(2) . . ? C8 N9 Fe1 115.88(18) . . ? C11 N10 N9 111.5(3) . . ? N10 C11 C12 108.3(3) . . ? C11 C12 C8 104.3(3) . . ? N14 C13 C17 111.5(3) . . ? N14 C13 C7 116.1(3) . . ? C17 C13 C7 132.4(3) . . ? C13 N14 N15 103.5(3) . . ? C13 N14 Fe1 115.4(2) . . ? N15 N14 Fe1 141.0(3) . . ? C16 N15 N14 111.9(4) . . ? C17 C16 N15 107.4(4) . . ? C16 C17 C13 105.7(4) . . ? C23 N18 C19 120.3(2) . . ? C23 N18 Fe1 119.76(17) . . ? C19 N18 Fe1 119.81(18) . . ? N18 C19 C20 120.7(3) . . ? N18 C19 C24 112.2(2) . . ? C20 C19 C24 127.1(3) . . ? C21 C20 C19 118.9(3) . . ? C20 C21 C22 120.4(3) . . ? C21 C22 C23 117.9(3) . . ? N18 C23 C22 121.8(3) . . ? N18 C23 C29 112.3(2) . . ? C22 C23 C29 125.9(3) . . ? N25 C24 C28 110.2(3) . . ? N25 C24 C19 115.8(2) . . ? C28 C24 C19 134.0(3) . . ? C24 N25 N26 105.4(2) . . ? C24 N25 Fe1 116.87(17) . . ? N26 N25 Fe1 137.69(19) . . ? N25 N26 C27 111.7(3) . . ? N26 C27 C28 107.6(3) . . ? C27 C28 C24 105.0(3) . . ? N30 C29 C33 111.3(3) . . ? N30 C29 C23 115.9(2) . . ? C33 C29 C23 132.7(3) . . ? C29 N30 N31 104.5(2) . . ? C29 N30 Fe1 116.26(17) . . ? N31 N30 Fe1 139.1(2) . . ? C32 N31 N30 111.2(3) . . ? N31 C32 C33 108.5(3) . . ? C32 C33 C29 104.5(3) . . ? F38 B34 F37 111.9(3) . . ? F38 B34 F36 105.6(4) . . ? F37 B34 F36 108.1(4) . . ? F38 B34 F35 113.2(3) . . ? F37 B34 F35 110.0(3) . . ? F36 B34 F35 107.8(3) . . ? F43 B39 F42 109.0(3) . . ? F43 B39 F41 110.1(3) . . ? F42 B39 F41 108.2(3) . . ? F43 B39 F40 113.2(3) . . ? F42 B39 F40 107.1(3) . . ? F41 B39 F40 109.2(3) . . ? O46 C45 C44 109.0(3) . . ? C45 O46 C47 112.1(3) . . ? O46 C47 C48 109.0(3) . . ? O51 C50 C49 110.0(3) . . ? C50 O51 C52 114.7(3) . . ? O51 C52 C53 109.2(4) . . ? O56 C55 C54 109.8(4) . . ? C57 O56 C55 113.5(4) . . ? O56 C57 C58 109.6(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N10 H10 O51 0.88 1.84 2.715(4) 169.8 . N15 H15 O56 0.88 1.97 2.836(5) 167.0 . N26 H26 F41 0.88 1.99 2.843(3) 163.5 . N31 H31 O46 0.88 1.99 2.808(4) 155.1 . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.703 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.063 #=END data_mh362 _database_code_depnum_ccdc_archive 'CCDC 821510' #TrackingRef '- Solvent dependence Dalton.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-di(pyrazol-3-yl)pyridine]iron(II) ditetrafluoroborate bis-nitromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H18 Fe N10, 2[B F4], 2[C H3 N O2]' _chemical_formula_sum 'C24 H24 B2 F8 Fe N12 O4' _chemical_formula_weight 774.02 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 '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 11.721(2) _cell_length_b 22.987(5) _cell_length_c 12.442(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.26(3) _cell_angle_gamma 90.00 _cell_volume 3346.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 29057 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 28.44 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour orange _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.546 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.689 _exptl_absorpt_correction_T_max 0.731 _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 29057 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 28.44 _reflns_number_total 4108 _reflns_number_gt 3610 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 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 asymmetric unit contains half a complex dication with Fe1, N2, C5, N11 and C14 all lying on the crystallographic C~2~ axis [0.5, y, 0.75]; and, one BF~4~^-^ anion and one nitromethane molecule, both occupying general lattice sites. The anion is disordered over two orientations, which were refined with the refined restraints B---F = 1.40(2) and F...F = 2.29(2) \%A. The occupancy ratio of the 'A' and 'B' anion disorder sites refined to 0.67:0.33. All non-H atoms except the minor anion disorder site were refined anistropically, 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^)+(0.0524P)^2^+4.7045P] 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 4108 _refine_ls_number_parameters 256 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1108 _refine_ls_wR_factor_gt 0.1050 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.047 _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 0.5000 0.720827(14) 0.7500 0.01961(11) Uani 1 2 d S . . N2 N 0.5000 0.63548(9) 0.7500 0.0245(4) Uani 1 2 d S . . C3 C 0.53955(15) 0.60565(8) 0.84042(15) 0.0292(4) Uani 1 1 d . . . C4 C 0.54096(17) 0.54460(9) 0.84294(19) 0.0397(5) Uani 1 1 d . . . H4 H 0.5687 0.5242 0.9055 0.048 Uiso 1 1 calc R . . C5 C 0.5000 0.51427(13) 0.7500 0.0459(8) Uani 1 2 d S . . H5 H 0.5000 0.4729 0.7500 0.055 Uiso 1 2 calc SR . . C6 C 0.57565(15) 0.64701(9) 0.92698(14) 0.0293(4) Uani 1 1 d . . . N7 N 0.56535(12) 0.70420(7) 0.89862(11) 0.0252(3) Uani 1 1 d . . . N8 N 0.59937(13) 0.73560(8) 0.98791(12) 0.0319(3) Uani 1 1 d . . . H8 H 0.6008 0.7738 0.9910 0.038 Uiso 1 1 calc R . . C9 C 0.63111(18) 0.69941(12) 1.07210(16) 0.0427(5) Uani 1 1 d . . . H9 H 0.6576 0.7114 1.1422 0.051 Uiso 1 1 calc R . . C10 C 0.61784(18) 0.64249(11) 1.03718(16) 0.0420(5) Uani 1 1 d . . . H10 H 0.6333 0.6080 1.0774 0.050 Uiso 1 1 calc R . . N11 N 0.5000 0.80638(9) 0.7500 0.0245(4) Uani 1 2 d S . . C12 C 0.40810(16) 0.83612(8) 0.78645(13) 0.0279(4) Uani 1 1 d . . . C13 C 0.4053(2) 0.89724(9) 0.78695(17) 0.0414(5) Uani 1 1 d . . . H13 H 0.3413 0.9176 0.8116 0.050 Uiso 1 1 calc R . . C14 C 0.5000 0.92750(13) 0.7500 0.0500(8) Uani 1 2 d S . . H14 H 0.5000 0.9688 0.7500 0.060 Uiso 1 2 calc SR . . C15 C 0.31974(15) 0.79519(8) 0.82109(13) 0.0259(3) Uani 1 1 d . . . N16 N 0.34650(12) 0.73772(7) 0.80745(11) 0.0238(3) Uani 1 1 d . . . N17 N 0.25582(13) 0.70702(7) 0.84155(12) 0.0284(3) Uani 1 1 d . . . H17 H 0.2512 0.6688 0.8415 0.034 Uiso 1 1 calc R . . C18 C 0.17299(17) 0.74342(10) 0.87581(15) 0.0349(4) Uani 1 1 d . . . H18 H 0.1023 0.7318 0.9027 0.042 Uiso 1 1 calc R . . C19 C 0.21019(16) 0.80045(9) 0.86444(14) 0.0332(4) Uani 1 1 d . . . H19 H 0.1713 0.8352 0.8817 0.040 Uiso 1 1 calc R . . B20A B 0.2482(4) 0.5494(2) 0.9290(3) 0.0331(9) Uani 0.67 1 d PD A 1 F21A F 0.3179(4) 0.5661(2) 1.0191(3) 0.0714(13) Uani 0.67 1 d PD A 1 F22A F 0.1326(2) 0.55696(14) 0.9528(3) 0.0815(9) Uani 0.67 1 d PD A 1 F23A F 0.2684(5) 0.5854(2) 0.8372(4) 0.0414(9) Uani 0.67 1 d PD A 1 F24A F 0.2698(2) 0.49224(8) 0.9030(2) 0.0591(6) Uani 0.67 1 d PD A 1 B20B B 0.2232(10) 0.5613(5) 0.9273(10) 0.045(4) Uiso 0.33 1 d PD B 2 F21B F 0.3004(10) 0.5520(5) 1.0146(9) 0.080(4) Uiso 0.33 1 d PD B 2 F22B F 0.1404(5) 0.6010(3) 0.9572(4) 0.0673(13) Uiso 0.33 1 d PD B 2 F23B F 0.2859(10) 0.5905(5) 0.8502(9) 0.039(2) Uiso 0.33 1 d PD B 2 F24B F 0.1738(6) 0.5116(3) 0.8861(5) 0.0886(18) Uiso 0.33 1 d PD B 2 C25 C 0.6249(2) 0.93989(11) 1.1087(2) 0.0497(6) Uani 1 1 d . . . H25A H 0.5543 0.9618 1.0923 0.075 Uiso 1 1 calc R . . H25B H 0.6857 0.9551 1.0657 0.075 Uiso 1 1 calc R . . H25C H 0.6475 0.9439 1.1854 0.075 Uiso 1 1 calc R . . N26 N 0.60529(15) 0.87726(8) 1.08237(14) 0.0389(4) Uani 1 1 d . . . O27 O 0.59595(16) 0.86312(8) 0.98635(13) 0.0546(4) Uani 1 1 d . . . O28 O 0.5987(3) 0.84234(10) 1.15560(16) 0.0889(8) 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 0.02070(17) 0.02325(17) 0.01475(16) 0.000 -0.00030(11) 0.000 N2 0.0227(9) 0.0269(10) 0.0243(10) 0.000 0.0040(8) 0.000 C3 0.0246(8) 0.0324(9) 0.0311(9) 0.0069(7) 0.0063(7) 0.0034(6) C4 0.0354(10) 0.0322(10) 0.0526(12) 0.0132(9) 0.0129(9) 0.0062(8) C5 0.0427(16) 0.0257(14) 0.071(2) 0.000 0.0208(15) 0.000 C6 0.0230(8) 0.0403(10) 0.0249(8) 0.0085(7) 0.0022(6) 0.0047(7) N7 0.0227(7) 0.0353(8) 0.0174(6) -0.0002(5) -0.0004(5) 0.0001(5) N8 0.0274(8) 0.0490(10) 0.0189(7) -0.0046(6) -0.0029(6) -0.0016(6) C9 0.0359(10) 0.0712(15) 0.0202(9) 0.0045(9) -0.0058(7) 0.0040(10) C10 0.0342(10) 0.0639(14) 0.0275(9) 0.0176(9) -0.0014(8) 0.0099(9) N11 0.0301(10) 0.0265(10) 0.0167(9) 0.000 -0.0008(7) 0.000 C12 0.0361(9) 0.0282(9) 0.0194(8) -0.0004(6) 0.0006(7) 0.0047(7) C13 0.0588(13) 0.0282(10) 0.0380(11) -0.0005(8) 0.0114(10) 0.0094(9) C14 0.077(2) 0.0217(14) 0.0532(19) 0.000 0.0186(17) 0.000 C15 0.0306(9) 0.0313(8) 0.0156(7) -0.0009(6) -0.0014(6) 0.0066(7) N16 0.0243(7) 0.0300(7) 0.0170(6) 0.0007(5) -0.0002(5) -0.0001(5) N17 0.0260(7) 0.0370(8) 0.0225(7) 0.0002(6) 0.0028(6) -0.0028(6) C18 0.0273(9) 0.0514(12) 0.0264(9) -0.0009(8) 0.0049(7) 0.0031(8) C19 0.0319(9) 0.0449(11) 0.0227(8) -0.0019(7) 0.0021(7) 0.0117(8) B20A 0.0284(19) 0.038(2) 0.033(2) 0.0096(15) 0.0080(15) 0.0050(18) F21A 0.106(3) 0.067(3) 0.0374(14) -0.0048(14) -0.0276(15) 0.033(2) F22A 0.0419(13) 0.093(2) 0.114(2) 0.0377(18) 0.0408(14) 0.0210(12) F23A 0.046(2) 0.0392(17) 0.0387(16) 0.0117(13) 0.0026(16) 0.0003(14) F24A 0.0814(16) 0.0249(9) 0.0735(15) 0.0030(9) 0.0254(12) -0.0031(9) C25 0.0573(14) 0.0420(13) 0.0493(13) 0.0010(10) -0.0027(11) -0.0042(10) N26 0.0383(9) 0.0435(10) 0.0340(9) 0.0028(7) -0.0053(7) -0.0047(7) O27 0.0652(11) 0.0633(12) 0.0347(8) -0.0087(8) -0.0021(8) 0.0022(9) O28 0.163(2) 0.0562(13) 0.0435(11) 0.0143(9) -0.0242(13) -0.0381(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.962(2) . ? Fe1 N11 1.967(2) . ? Fe1 N7 1.9977(15) . ? Fe1 N16 2.0111(15) . ? N2 C3 1.375(2) . ? C3 C4 1.404(3) . ? C3 C6 1.480(3) . ? C4 C5 1.411(3) . ? C6 N7 1.365(2) . ? C6 C10 1.435(3) . ? N7 N8 1.365(2) . ? N8 C9 1.372(3) . ? C9 C10 1.385(4) . ? N11 C12 1.374(2) . ? C12 C13 1.405(3) . ? C12 C15 1.481(3) . ? C13 C14 1.409(3) . ? C15 N16 1.370(2) . ? C15 C19 1.426(3) . ? N16 N17 1.363(2) . ? N17 C18 1.368(2) . ? C18 C19 1.391(3) . ? B20A F24A 1.380(6) . ? B20A F21A 1.402(6) . ? B20A F22A 1.414(5) . ? B20A F23A 1.441(5) . ? B20B F24B 1.366(12) . ? B20B F21B 1.390(13) . ? B20B F22B 1.399(11) . ? B20B F23B 1.411(13) . ? C25 N26 1.491(3) . ? N26 O28 1.220(3) . ? N26 O27 1.237(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 N11 180.00 . . ? N2 Fe1 N7 78.97(5) . . ? N11 Fe1 N7 101.03(5) . . ? N7 Fe1 N7 157.94(9) 2_656 . ? N7 Fe1 N16 93.57(6) . 2_656 ? N2 Fe1 N16 101.13(4) . . ? N11 Fe1 N16 78.87(4) . . ? N7 Fe1 N16 90.67(6) . . ? N16 Fe1 N16 157.73(9) 2_656 . ? C3 N2 C3 120.2(2) 2_656 . ? C3 N2 Fe1 119.91(11) . . ? N2 C3 C4 121.31(19) . . ? N2 C3 C6 110.12(17) . . ? C4 C3 C6 128.56(18) . . ? C3 C4 C5 118.2(2) . . ? C4 C5 C4 120.8(3) . 2_656 ? N7 C6 C10 109.73(18) . . ? N7 C6 C3 114.41(15) . . ? C10 C6 C3 135.85(19) . . ? C6 N7 N8 106.34(15) . . ? C6 N7 Fe1 116.57(12) . . ? N8 N7 Fe1 136.97(13) . . ? N7 N8 C9 110.77(18) . . ? N8 C9 C10 108.21(18) . . ? C9 C10 C6 104.94(18) . . ? C12 N11 C12 120.3(2) 2_656 . ? C12 N11 Fe1 119.83(11) . . ? N11 C12 C13 121.17(19) . . ? N11 C12 C15 110.74(16) . . ? C13 C12 C15 128.09(18) . . ? C12 C13 C14 118.2(2) . . ? C13 C14 C13 120.8(3) 2_656 . ? N16 C15 C19 110.24(17) . . ? N16 C15 C12 114.05(15) . . ? C19 C15 C12 135.70(17) . . ? N17 N16 C15 105.81(14) . . ? N17 N16 Fe1 137.69(12) . . ? C15 N16 Fe1 116.47(12) . . ? N16 N17 C18 111.10(16) . . ? N17 C18 C19 108.21(17) . . ? C18 C19 C15 104.64(17) . . ? F24A B20A F21A 110.1(4) . . ? F24A B20A F22A 110.9(3) . . ? F21A B20A F22A 108.7(4) . . ? F24A B20A F23A 108.6(4) . . ? F21A B20A F23A 111.2(4) . . ? F22A B20A F23A 107.3(4) . . ? F24B B20B F21B 114.2(9) . . ? F24B B20B F22B 111.0(9) . . ? F21B B20B F22B 108.8(9) . . ? F24B B20B F23B 111.7(9) . . ? F21B B20B F23B 105.3(10) . . ? F22B B20B F23B 105.4(9) . . ? O28 N26 O27 122.9(2) . . ? O28 N26 C25 119.1(2) . . ? O27 N26 C25 118.02(19) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N8 H8 O27 0.88 2.05 2.932(3) 175.2 . N17 H17 F23A 0.88 1.93 2.800(6) 170.2 . N17 H17 F23B 0.88 1.85 2.702(12) 163.6 . _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 28.44 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.597 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.072 #=END data_mh363 _database_code_depnum_ccdc_archive 'CCDC 821511' #TrackingRef '- Solvent dependence Dalton.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-di(pyrazol-3-yl)pyridine]iron(II) diterafluoroborate dinitromethane bis(diisopropylether) solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H18 Fe N10, 2[B F4], 2[C H3 N O2], 2[C6 H14 O]' _chemical_formula_sum 'C36 H52 B2 F8 Fe N12 O6' _chemical_formula_weight 978.37 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/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.035(3) _cell_length_b 13.729(3) _cell_length_c 26.943(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.22(3) _cell_angle_gamma 90.00 _cell_volume 4712.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 76956 _cell_measurement_theta_min 1.67 _cell_measurement_theta_max 28.60 _exptl_crystal_description fragment _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 0.407 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_T_max 1.152 _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 76956 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 28.60 _reflns_number_total 12045 _reflns_number_gt 9042 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 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 BF~4~^-^ ion B39-F43 is disordered, over three sites labelled 'A' (occupancy 0.4), 'B' (0.4) and 'C' (0.2). The refined restraints B---F = 1.37(2) and F...F = 2.24(2)\%A were applied to this anion. The nitromethane molecule C62-O65 is also disordered, over two orientations with a 0.60:0.40 occupancy ratio. These two partial solvent sites share a common wholly occupied O atom O65 (which accepts a hydrogen bond form the complex cation). This was modelled using the fixed restraints C---N = 1.47(2), N---O = 1.21(2), O...O = 2.10(2) and C...O = 2.30(2)\%A. All wholly occupied non-H atoms were refined anistropically, and all H atoms were placed in calculated positions and refined using a riding model. The highest residual Fourier peak of 1.0e.\%A^-3^ lies within the disordered anion B39-F43. ; _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^)+(0.0693P)^2^+6.5449P] 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 12045 _refine_ls_number_parameters 609 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0815 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1593 _refine_ls_wR_factor_gt 0.1429 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.026 _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 0.01005(2) 0.78989(2) 0.156983(12) 0.01776(9) Uani 1 1 d . . . N2 N -0.06388(15) 0.88981(14) 0.11245(7) 0.0205(4) Uani 1 1 d . . . C3 C -0.16978(18) 0.89829(18) 0.10629(9) 0.0220(5) Uani 1 1 d . . . C4 C -0.2257(2) 0.96894(19) 0.07414(9) 0.0272(5) Uani 1 1 d . . . H4 H -0.2995 0.9750 0.0703 0.033 Uiso 1 1 calc R . . C5 C -0.1704(2) 1.0301(2) 0.04798(10) 0.0309(6) Uani 1 1 d . . . H5 H -0.2069 1.0785 0.0258 0.037 Uiso 1 1 calc R . . C6 C -0.0616(2) 1.02112(19) 0.05401(9) 0.0277(5) Uani 1 1 d . . . H6 H -0.0237 1.0628 0.0362 0.033 Uiso 1 1 calc R . . C7 C -0.00970(19) 0.94949(18) 0.08679(9) 0.0228(5) Uani 1 1 d . . . C8 C -0.21008(18) 0.82713(17) 0.13752(9) 0.0210(4) Uani 1 1 d . . . N9 N -0.13581(15) 0.76989(14) 0.16625(7) 0.0205(4) Uani 1 1 d . . . N10 N -0.18801(16) 0.71071(15) 0.19248(8) 0.0240(4) Uani 1 1 d . . . H10 H -0.1580 0.6660 0.2142 0.029 Uiso 1 1 calc R . . C11 C -0.29250(19) 0.72900(19) 0.18103(10) 0.0282(5) Uani 1 1 d . . . H11 H -0.3443 0.6965 0.1950 0.034 Uiso 1 1 calc R . . C12 C -0.31070(19) 0.80295(19) 0.14563(10) 0.0262(5) Uani 1 1 d . . . H12 H -0.3762 0.8313 0.1302 0.031 Uiso 1 1 calc R . . C13 C 0.10215(19) 0.92568(18) 0.09890(9) 0.0235(5) Uani 1 1 d . . . N14 N 0.12679(15) 0.84867(15) 0.13080(7) 0.0216(4) Uani 1 1 d . . . N15 N 0.23137(15) 0.83642(16) 0.13691(8) 0.0252(4) Uani 1 1 d . . . H15 H 0.2676 0.7908 0.1559 0.030 Uiso 1 1 calc R . . C16 C 0.2735(2) 0.9035(2) 0.11001(10) 0.0296(5) Uani 1 1 d . . . H16 H 0.3454 0.9088 0.1084 0.036 Uiso 1 1 calc R . . C17 C 0.1930(2) 0.9626(2) 0.08542(10) 0.0285(5) Uani 1 1 d . . . H17 H 0.1979 1.0166 0.0640 0.034 Uiso 1 1 calc R . . N18 N 0.08455(14) 0.68672(15) 0.19886(7) 0.0208(4) Uani 1 1 d . . . C19 C 0.09362(18) 0.59768(18) 0.17800(9) 0.0237(5) Uani 1 1 d . . . C20 C 0.1478(2) 0.5222(2) 0.20689(11) 0.0310(6) Uani 1 1 d . . . H20 H 0.1539 0.4601 0.1922 0.037 Uiso 1 1 calc R . . C21 C 0.1925(2) 0.5399(2) 0.25769(11) 0.0344(6) Uani 1 1 d . . . H21 H 0.2298 0.4894 0.2779 0.041 Uiso 1 1 calc R . . C22 C 0.1832(2) 0.6309(2) 0.27917(10) 0.0307(6) Uani 1 1 d . . . H22 H 0.2137 0.6431 0.3139 0.037 Uiso 1 1 calc R . . C23 C 0.12792(18) 0.70396(19) 0.24849(9) 0.0241(5) Uani 1 1 d . . . C24 C 0.03876(18) 0.59619(18) 0.12477(10) 0.0244(5) Uani 1 1 d . . . N25 N -0.00607(15) 0.68239(15) 0.10787(7) 0.0229(4) Uani 1 1 d . . . N26 N -0.05629(17) 0.66728(18) 0.05925(8) 0.0297(5) Uani 1 1 d . . . H26 H -0.0924 0.7119 0.0395 0.036 Uiso 1 1 calc R . . C27 C -0.0435(2) 0.5739(2) 0.04506(11) 0.0386(7) Uani 1 1 d . . . H27 H -0.0714 0.5465 0.0126 0.046 Uiso 1 1 calc R . . C28 C 0.0167(2) 0.5257(2) 0.08574(11) 0.0360(6) Uani 1 1 d . . . H28 H 0.0387 0.4596 0.0873 0.043 Uiso 1 1 calc R . . C29 C 0.10780(18) 0.80407(19) 0.26217(9) 0.0242(5) Uani 1 1 d . . . N30 N 0.05395(15) 0.85862(15) 0.22336(7) 0.0217(4) Uani 1 1 d . . . N31 N 0.04294(16) 0.94740(16) 0.24344(8) 0.0268(4) Uani 1 1 d . . . H31 H 0.0107 0.9971 0.2262 0.032 Uiso 1 1 calc R . . C32 C 0.0881(2) 0.9498(2) 0.29359(10) 0.0341(6) Uani 1 1 d . . . H32 H 0.0901 1.0043 0.3155 0.041 Uiso 1 1 calc R . . C33 C 0.1305(2) 0.8594(2) 0.30727(10) 0.0328(6) Uani 1 1 d . . . H33 H 0.1671 0.8389 0.3399 0.039 Uiso 1 1 calc R . . B34 B 0.4420(3) 0.7356(3) 0.21444(14) 0.0403(8) Uani 1 1 d . . . F35 F 0.34025(13) 0.69661(14) 0.20134(8) 0.0482(5) Uani 1 1 d . . . F36 F 0.46248(15) 0.78301(17) 0.17253(9) 0.0655(7) Uani 1 1 d . . . F37 F 0.51108(14) 0.65903(18) 0.22894(10) 0.0685(7) Uani 1 1 d . . . F38 F 0.4466(4) 0.7994(2) 0.25364(13) 0.1275(14) Uani 1 1 d . . . B39A B -0.1870(11) 0.7515(10) -0.0549(5) 0.044(6) Uiso 0.40 1 d PD A 1 F40A F -0.1669(7) 0.6576(6) -0.0644(3) 0.092(2) Uiso 0.40 1 d PD A 1 F41A F -0.2138(5) 0.7573(6) -0.0061(2) 0.0754(17) Uiso 0.40 1 d PD A 1 F42A F -0.0979(6) 0.8059(6) -0.0432(3) 0.097(2) Uiso 0.40 1 d PD A 1 F43A F -0.2628(6) 0.7976(4) -0.0923(2) 0.0375(15) Uiso 0.40 1 d PD A 1 B39B B -0.1955(11) 0.7421(10) -0.0572(5) 0.032(11) Uiso 0.40 1 d PD B 2 F40B F -0.1027(5) 0.6939(5) -0.0625(2) 0.0673(16) Uiso 0.40 1 d PD B 2 F41B F -0.1711(4) 0.8006(4) -0.01266(18) 0.0439(11) Uiso 0.40 1 d PD B 2 F42B F -0.2659(6) 0.6736(5) -0.0504(3) 0.089(2) Uiso 0.40 1 d PD B 2 F43B F -0.2236(5) 0.8010(4) -0.0987(2) 0.0512(15) Uiso 0.40 1 d PD B 2 B39C B -0.1995(14) 0.7452(14) -0.0567(7) 0.04(2) Uiso 0.20 1 d PD C 3 F40C F -0.1503(7) 0.6817(7) -0.0849(4) 0.040(2) Uiso 0.20 1 d PD C 3 F41C F -0.1276(6) 0.8078(5) -0.0236(3) 0.0223(14) Uiso 0.20 1 d PD C 3 F42C F -0.2453(6) 0.6933(6) -0.0236(3) 0.0352(18) Uiso 0.20 1 d PD C 3 F43C F -0.2834(10) 0.7948(10) -0.0856(5) 0.056(5) Uiso 0.20 1 d PD C 3 C44 C 0.2883(4) 0.1884(4) 0.4877(2) 0.0807(14) Uani 1 1 d . . . H44A H 0.3267 0.1844 0.5231 0.121 Uiso 1 1 calc R . . H44B H 0.2473 0.2487 0.4827 0.121 Uiso 1 1 calc R . . H44C H 0.3382 0.1879 0.4652 0.121 Uiso 1 1 calc R . . C45 C 0.1597(5) 0.1033(5) 0.42019(18) 0.111(2) Uani 1 1 d . . . H45A H 0.1198 0.1640 0.4126 0.166 Uiso 1 1 calc R . . H45B H 0.1116 0.0477 0.4134 0.166 Uiso 1 1 calc R . . H45C H 0.2115 0.0987 0.3987 0.166 Uiso 1 1 calc R . . C46 C 0.2158(3) 0.1026(3) 0.47585(16) 0.0615(10) Uani 1 1 d . . . H46 H 0.2579 0.0414 0.4829 0.074 Uiso 1 1 calc R . . O47 O 0.1351(2) 0.1015(2) 0.50478(9) 0.0579(7) Uani 1 1 d . . . C48 C 0.1653(3) 0.0557(3) 0.55403(13) 0.0597(10) Uani 1 1 d . . . H48 H 0.2397 0.0728 0.5697 0.072 Uiso 1 1 calc R . . C49 C 0.0930(5) 0.0982(4) 0.58573(16) 0.0849(15) Uani 1 1 d . . . H49A H 0.0203 0.0806 0.5706 0.127 Uiso 1 1 calc R . . H49B H 0.1001 0.1693 0.5868 0.127 Uiso 1 1 calc R . . H49C H 0.1120 0.0721 0.6203 0.127 Uiso 1 1 calc R . . C50 C 0.1539(4) -0.0537(3) 0.55004(18) 0.0710(12) Uani 1 1 d . . . H50A H 0.1958 -0.0786 0.5266 0.106 Uiso 1 1 calc R . . H50B H 0.0800 -0.0705 0.5373 0.106 Uiso 1 1 calc R . . H50C H 0.1786 -0.0830 0.5836 0.106 Uiso 1 1 calc R . . C51 C -0.1433(3) 0.4515(2) 0.19166(12) 0.0423(7) Uani 1 1 d . . . H51A H -0.1736 0.5042 0.1687 0.063 Uiso 1 1 calc R . . H51B H -0.1704 0.3888 0.1771 0.063 Uiso 1 1 calc R . . H51C H -0.0667 0.4524 0.1963 0.063 Uiso 1 1 calc R . . C52 C -0.1734(2) 0.46531(19) 0.24264(10) 0.0295(5) Uani 1 1 d . . . H52 H -0.1372 0.4147 0.2668 0.035 Uiso 1 1 calc R . . C53 C -0.2916(2) 0.4573(2) 0.23868(12) 0.0400(7) Uani 1 1 d . . . H53A H -0.3078 0.4697 0.2720 0.060 Uiso 1 1 calc R . . H53B H -0.3151 0.3916 0.2273 0.060 Uiso 1 1 calc R . . H53C H -0.3278 0.5052 0.2142 0.060 Uiso 1 1 calc R . . O54 O -0.13538(15) 0.56098(13) 0.26103(7) 0.0294(4) Uani 1 1 d . . . C55 C -0.0215(2) 0.5356(3) 0.34440(11) 0.0441(7) Uani 1 1 d . . . H55A H -0.0133 0.4680 0.3342 0.066 Uiso 1 1 calc R . . H55B H -0.0198 0.5380 0.3809 0.066 Uiso 1 1 calc R . . H55C H 0.0358 0.5752 0.3368 0.066 Uiso 1 1 calc R . . C56 C -0.1261(2) 0.5753(2) 0.31526(10) 0.0338(6) Uani 1 1 d . . . H56 H -0.1845 0.5399 0.3263 0.041 Uiso 1 1 calc R . . C57 C -0.1379(4) 0.6838(3) 0.32354(14) 0.0629(11) Uani 1 1 d . . . H57A H -0.0831 0.7192 0.3111 0.094 Uiso 1 1 calc R . . H57B H -0.1312 0.6966 0.3599 0.094 Uiso 1 1 calc R . . H57C H -0.2071 0.7054 0.3050 0.094 Uiso 1 1 calc R . . C58 C -0.0616(4) 0.2980(4) 0.5063(2) 0.0894(18) Uani 1 1 d . . . H58A H -0.0375 0.2303 0.5083 0.134 Uiso 1 1 calc R . . H58B H -0.1226 0.3051 0.4782 0.134 Uiso 1 1 calc R . . H58C H -0.0814 0.3160 0.5383 0.134 Uiso 1 1 calc R . . N59 N 0.0227(2) 0.3618(2) 0.49784(11) 0.0428(6) Uani 1 1 d . . . O60 O 0.0967(2) 0.3713(2) 0.53373(12) 0.0758(9) Uani 1 1 d . . . O61 O 0.0152(3) 0.4002(3) 0.45696(12) 0.0889(11) Uani 1 1 d . . . C62A C -0.0453(7) 1.2344(6) 0.1312(3) 0.078(2) Uiso 0.60 1 d PD D 1 H62A H -0.1202 1.2501 0.1249 0.117 Uiso 0.60 1 calc PR D 1 H62B H -0.0234 1.2280 0.0987 0.117 Uiso 0.60 1 calc PR D 1 H62C H -0.0050 1.2867 0.1512 0.117 Uiso 0.60 1 calc PR D 1 N63A N -0.0265(4) 1.1444(4) 0.15871(18) 0.0474(11) Uiso 0.60 1 d PD D 1 O64A O 0.0634(4) 1.1129(4) 0.1693(2) 0.0770(14) Uiso 0.60 1 d PD D 1 O65 O -0.0921(2) 1.0876(2) 0.17023(10) 0.0640(7) Uani 1 1 d D . . C62B C 0.0328(8) 1.1958(10) 0.1531(5) 0.090(4) Uiso 0.40 1 d PD D 2 H62D H 0.0325 1.2607 0.1380 0.135 Uiso 0.40 1 calc PR D 2 H62E H 0.0650 1.1491 0.1335 0.135 Uiso 0.40 1 calc PR D 2 H62F H 0.0733 1.1976 0.1882 0.135 Uiso 0.40 1 calc PR D 2 N63B N -0.0802(5) 1.1644(5) 0.1528(2) 0.0377(14) Uiso 0.40 1 d PD D 2 O64B O -0.1469(6) 1.2146(6) 0.1322(3) 0.078(2) Uiso 0.40 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 0.01711(15) 0.01872(16) 0.01690(16) 0.00088(12) 0.00234(11) 0.00375(12) N2 0.0226(9) 0.0206(10) 0.0175(9) -0.0002(7) 0.0026(7) 0.0050(7) C3 0.0213(11) 0.0243(12) 0.0197(11) -0.0018(9) 0.0031(8) 0.0056(9) C4 0.0264(12) 0.0299(13) 0.0244(12) 0.0016(10) 0.0029(9) 0.0106(10) C5 0.0354(14) 0.0305(14) 0.0255(12) 0.0084(10) 0.0037(10) 0.0135(11) C6 0.0348(13) 0.0261(13) 0.0232(12) 0.0069(10) 0.0088(10) 0.0064(10) C7 0.0253(11) 0.0242(12) 0.0194(11) 0.0006(9) 0.0062(9) 0.0033(9) C8 0.0211(10) 0.0213(11) 0.0196(10) -0.0027(9) 0.0021(8) 0.0046(9) N9 0.0217(9) 0.0204(10) 0.0193(9) 0.0006(7) 0.0039(7) 0.0032(7) N10 0.0250(10) 0.0217(10) 0.0258(10) 0.0038(8) 0.0062(8) 0.0018(8) C11 0.0219(11) 0.0282(13) 0.0354(14) 0.0003(10) 0.0082(10) 0.0002(10) C12 0.0197(11) 0.0289(13) 0.0298(12) -0.0017(10) 0.0045(9) 0.0048(9) C13 0.0282(12) 0.0219(12) 0.0209(11) 0.0010(9) 0.0062(9) 0.0032(9) N14 0.0204(9) 0.0234(10) 0.0208(9) -0.0002(8) 0.0039(7) 0.0033(8) N15 0.0186(9) 0.0300(11) 0.0265(10) 0.0008(9) 0.0034(8) 0.0021(8) C16 0.0233(12) 0.0358(14) 0.0300(13) -0.0005(11) 0.0060(10) -0.0035(10) C17 0.0313(13) 0.0280(13) 0.0268(12) 0.0029(10) 0.0079(10) -0.0014(10) N18 0.0163(8) 0.0230(10) 0.0231(10) 0.0035(8) 0.0045(7) 0.0018(7) C19 0.0186(10) 0.0226(12) 0.0316(12) 0.0027(10) 0.0092(9) 0.0027(9) C20 0.0260(12) 0.0240(13) 0.0442(15) 0.0093(11) 0.0102(11) 0.0086(10) C21 0.0273(13) 0.0335(15) 0.0418(15) 0.0178(12) 0.0062(11) 0.0080(11) C22 0.0240(12) 0.0392(15) 0.0279(13) 0.0133(11) 0.0031(10) 0.0035(11) C23 0.0184(10) 0.0306(13) 0.0232(11) 0.0061(10) 0.0039(8) 0.0010(9) C24 0.0219(11) 0.0218(12) 0.0312(12) -0.0005(10) 0.0095(9) 0.0039(9) N25 0.0205(9) 0.0259(10) 0.0213(9) -0.0026(8) 0.0025(7) 0.0046(8) N26 0.0286(11) 0.0357(12) 0.0223(10) -0.0068(9) -0.0003(8) 0.0063(9) C27 0.0412(15) 0.0405(16) 0.0331(14) -0.0158(12) 0.0058(12) 0.0023(13) C28 0.0414(15) 0.0273(14) 0.0414(16) -0.0091(12) 0.0136(12) 0.0037(12) C29 0.0196(10) 0.0328(14) 0.0198(11) 0.0030(9) 0.0029(8) -0.0017(9) N30 0.0195(9) 0.0229(10) 0.0222(9) -0.0014(8) 0.0038(7) 0.0010(8) N31 0.0257(10) 0.0250(11) 0.0295(11) -0.0059(9) 0.0054(8) 0.0001(8) C32 0.0319(13) 0.0400(16) 0.0294(13) -0.0118(12) 0.0045(11) -0.0037(12) C33 0.0298(13) 0.0449(16) 0.0210(12) -0.0034(11) -0.0002(10) -0.0046(12) B34 0.0302(16) 0.0391(19) 0.048(2) 0.0125(15) 0.0002(14) -0.0062(13) F35 0.0262(8) 0.0507(11) 0.0664(12) 0.0277(9) 0.0071(8) -0.0009(7) F36 0.0330(9) 0.0723(15) 0.0910(16) 0.0532(13) 0.0130(10) 0.0019(9) F37 0.0312(9) 0.0724(15) 0.1011(18) 0.0537(14) 0.0121(10) 0.0101(10) F38 0.202(4) 0.076(2) 0.093(2) -0.0341(18) 0.005(2) -0.027(2) C44 0.078(3) 0.080(3) 0.085(3) -0.009(3) 0.017(3) -0.022(3) C45 0.131(5) 0.148(6) 0.051(3) -0.001(3) 0.018(3) -0.055(4) C46 0.067(2) 0.054(2) 0.064(2) 0.0009(19) 0.016(2) 0.0011(19) O47 0.0631(16) 0.0576(16) 0.0471(14) 0.0077(12) -0.0014(12) -0.0011(13) C48 0.074(3) 0.055(2) 0.0396(18) 0.0036(16) -0.0097(17) -0.0005(19) C49 0.132(5) 0.074(3) 0.044(2) -0.006(2) 0.010(2) 0.013(3) C50 0.089(3) 0.051(2) 0.070(3) 0.008(2) 0.012(2) 0.003(2) C51 0.0463(17) 0.0391(17) 0.0446(17) -0.0100(13) 0.0168(14) -0.0062(13) C52 0.0308(13) 0.0219(12) 0.0357(14) 0.0014(10) 0.0069(11) -0.0014(10) C53 0.0330(14) 0.0396(17) 0.0473(17) -0.0013(13) 0.0081(12) -0.0025(12) O54 0.0397(10) 0.0225(9) 0.0253(9) 0.0031(7) 0.0056(7) -0.0031(8) C55 0.0410(16) 0.056(2) 0.0321(15) 0.0059(14) 0.0016(12) -0.0050(14) C56 0.0422(15) 0.0328(15) 0.0267(13) 0.0035(11) 0.0079(11) -0.0007(12) C57 0.110(3) 0.0380(19) 0.0385(18) -0.0070(15) 0.011(2) 0.008(2) C58 0.061(3) 0.095(4) 0.096(3) 0.043(3) -0.021(2) -0.044(3) N59 0.0380(14) 0.0408(15) 0.0488(15) -0.0065(12) 0.0072(11) -0.0096(11) O60 0.0581(17) 0.084(2) 0.077(2) -0.0168(16) -0.0050(14) -0.0315(15) O61 0.086(2) 0.120(3) 0.0632(19) 0.027(2) 0.0207(16) -0.019(2) O65 0.0787(19) 0.0622(17) 0.0527(15) -0.0056(13) 0.0176(13) -0.0158(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N18 1.939(2) . ? Fe1 N2 1.9394(19) . ? Fe1 N25 1.964(2) . ? Fe1 N14 1.980(2) . ? Fe1 N9 1.988(2) . ? Fe1 N30 1.996(2) . ? N2 C3 1.360(3) . ? N2 C7 1.362(3) . ? C3 C4 1.398(3) . ? C3 C8 1.458(3) . ? C4 C5 1.392(4) . ? C5 C6 1.399(4) . ? C6 C7 1.397(3) . ? C7 C13 1.462(3) . ? C8 N9 1.355(3) . ? C8 C12 1.414(3) . ? N9 N10 1.351(3) . ? N10 C11 1.355(3) . ? C11 C12 1.379(4) . ? C13 N14 1.358(3) . ? C13 C17 1.404(4) . ? N14 N15 1.349(3) . ? N15 C16 1.358(3) . ? C16 C17 1.380(4) . ? N18 C23 1.358(3) . ? N18 C19 1.361(3) . ? C19 C20 1.395(3) . ? C19 C24 1.461(4) . ? C20 C21 1.391(4) . ? C21 C22 1.393(4) . ? C22 C23 1.398(3) . ? C23 C29 1.461(4) . ? C24 N25 1.355(3) . ? C24 C28 1.413(4) . ? N25 N26 1.351(3) . ? N26 C27 1.358(4) . ? C27 C28 1.375(4) . ? C29 N30 1.355(3) . ? C29 C33 1.410(4) . ? N30 N31 1.353(3) . ? N31 C32 1.355(3) . ? C32 C33 1.376(4) . ? B34 F38 1.364(5) . ? B34 F36 1.378(4) . ? B34 F37 1.385(4) . ? B34 F35 1.404(4) . ? B39A F40A 1.350(13) . ? B39A F42A 1.360(14) . ? B39A F43A 1.403(13) . ? B39A F41A 1.435(13) . ? B39B F42B 1.352(13) . ? B39B F43B 1.367(12) . ? B39B F40B 1.413(15) . ? B39B F41B 1.423(13) . ? B39C F42C 1.372(18) . ? B39C F43C 1.381(17) . ? B39C F40C 1.399(17) . ? B39C F41C 1.433(17) . ? C44 C46 1.502(6) . ? C45 C46 1.523(6) . ? C46 O47 1.435(5) . ? O47 C48 1.445(4) . ? C48 C50 1.511(6) . ? C48 C49 1.516(6) . ? C51 C52 1.518(4) . ? C52 O54 1.453(3) . ? C52 C53 1.525(4) . ? O54 C56 1.454(3) . ? C55 C56 1.523(4) . ? C56 C57 1.518(4) . ? C58 N59 1.460(5) . ? N59 O61 1.206(4) . ? N59 O60 1.220(4) . ? C62A N63A 1.436(8) . ? N63A O64A 1.224(7) . ? N63A O65 1.245(5) . ? C62B N63B 1.534(11) . ? N63B O64B 1.155(9) . ? N63B O65 1.179(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N18 Fe1 N2 177.46(8) . . ? N18 Fe1 N25 79.17(9) . . ? N2 Fe1 N25 98.42(8) . . ? N18 Fe1 N14 100.20(8) . . ? N2 Fe1 N14 79.04(8) . . ? N25 Fe1 N14 92.69(9) . . ? N18 Fe1 N9 101.56(8) . . ? N2 Fe1 N9 79.18(8) . . ? N25 Fe1 N9 90.69(8) . . ? N14 Fe1 N9 158.22(8) . . ? N18 Fe1 N30 79.08(8) . . ? N2 Fe1 N30 103.33(8) . . ? N25 Fe1 N30 158.24(8) . . ? N14 Fe1 N30 91.74(8) . . ? N9 Fe1 N30 93.05(8) . . ? C3 N2 C7 120.6(2) . . ? C3 N2 Fe1 119.64(16) . . ? C7 N2 Fe1 119.77(16) . . ? N2 C3 C4 121.1(2) . . ? N2 C3 C8 110.6(2) . . ? C4 C3 C8 128.2(2) . . ? C5 C4 C3 118.4(2) . . ? C4 C5 C6 120.6(2) . . ? C7 C6 C5 118.6(2) . . ? N2 C7 C6 120.7(2) . . ? N2 C7 C13 110.6(2) . . ? C6 C7 C13 128.7(2) . . ? N9 C8 C12 110.4(2) . . ? N9 C8 C3 114.7(2) . . ? C12 C8 C3 134.9(2) . . ? N10 N9 C8 105.63(19) . . ? N10 N9 Fe1 138.54(15) . . ? C8 N9 Fe1 115.76(16) . . ? N9 N10 C11 111.3(2) . . ? N10 C11 C12 108.1(2) . . ? C11 C12 C8 104.5(2) . . ? N14 C13 C17 110.2(2) . . ? N14 C13 C7 114.0(2) . . ? C17 C13 C7 135.8(2) . . ? N15 N14 C13 105.78(19) . . ? N15 N14 Fe1 137.65(16) . . ? C13 N14 Fe1 116.52(16) . . ? N14 N15 C16 111.3(2) . . ? N15 C16 C17 107.6(2) . . ? C16 C17 C13 105.1(2) . . ? C23 N18 C19 120.6(2) . . ? C23 N18 Fe1 119.91(17) . . ? C19 N18 Fe1 119.50(16) . . ? N18 C19 C20 121.0(2) . . ? N18 C19 C24 110.5(2) . . ? C20 C19 C24 128.5(2) . . ? C21 C20 C19 118.5(3) . . ? C20 C21 C22 120.7(2) . . ? C21 C22 C23 118.5(2) . . ? N18 C23 C22 120.8(2) . . ? N18 C23 C29 110.7(2) . . ? C22 C23 C29 128.5(2) . . ? N25 C24 C28 110.0(2) . . ? N25 C24 C19 113.8(2) . . ? C28 C24 C19 136.1(2) . . ? N26 N25 C24 106.1(2) . . ? N26 N25 Fe1 136.86(17) . . ? C24 N25 Fe1 116.93(16) . . ? N25 N26 C27 110.8(2) . . ? N26 C27 C28 108.2(2) . . ? C27 C28 C24 104.8(2) . . ? N30 C29 C33 110.3(2) . . ? N30 C29 C23 114.6(2) . . ? C33 C29 C23 135.1(2) . . ? N31 N30 C29 105.71(19) . . ? N31 N30 Fe1 138.55(16) . . ? C29 N30 Fe1 115.70(17) . . ? N30 N31 C32 111.1(2) . . ? N31 C32 C33 108.1(2) . . ? C32 C33 C29 104.8(2) . . ? F38 B34 F36 110.3(3) . . ? F38 B34 F37 110.4(3) . . ? F36 B34 F37 111.2(3) . . ? F38 B34 F35 108.9(3) . . ? F36 B34 F35 108.1(3) . . ? F37 B34 F35 107.8(3) . . ? F40A B39A F42A 112.2(11) . . ? F40A B39A F43A 115.6(10) . . ? F42A B39A F43A 110.9(10) . . ? F40A B39A F41A 108.7(10) . . ? F42A B39A F41A 96.8(9) . . ? F43A B39A F41A 111.1(10) . . ? F42B B39B F43B 116.7(11) . . ? F42B B39B F40B 107.9(10) . . ? F43B B39B F40B 106.4(10) . . ? F42B B39B F41B 108.4(10) . . ? F43B B39B F41B 109.2(10) . . ? F40B B39B F41B 107.8(10) . . ? F42C B39C F43C 102.8(13) . . ? F42C B39C F40C 109.9(14) . . ? F43C B39C F40C 113.6(14) . . ? F42C B39C F41C 103.0(12) . . ? F43C B39C F41C 113.0(14) . . ? F40C B39C F41C 113.3(13) . . ? O47 C46 C44 113.2(4) . . ? O47 C46 C45 106.3(4) . . ? C44 C46 C45 110.7(4) . . ? C46 O47 C48 114.5(3) . . ? O47 C48 C50 111.3(3) . . ? O47 C48 C49 105.6(3) . . ? C50 C48 C49 111.1(4) . . ? O54 C52 C51 106.7(2) . . ? O54 C52 C53 110.9(2) . . ? C51 C52 C53 112.2(2) . . ? C52 O54 C56 114.5(2) . . ? O54 C56 C57 106.9(2) . . ? O54 C56 C55 110.1(2) . . ? C57 C56 C55 112.5(3) . . ? O61 N59 O60 125.1(3) . . ? O61 N59 C58 119.1(3) . . ? O60 N59 C58 115.8(3) . . ? O64A N63A O65 113.2(5) . . ? O64A N63A C62A 118.3(6) . . ? O65 N63A C62A 128.1(6) . . ? O64B N63B O65 125.2(7) . . ? O64B N63B C62B 117.4(8) . . ? O65 N63B C62B 117.1(8) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N10 H10 O54 0.88 1.90 2.752(3) 163.0 . N15 H15 F35 0.88 1.89 2.769(3) 175.0 . N26 H26 F41B 0.88 1.97 2.849(5) 172.3 . N26 H26 F41A 0.88 1.89 2.704(7) 152.8 . N26 H26 F41C 0.88 2.12 2.948(8) 156.1 . N31 H31 O65 0.88 2.18 3.037(4) 163.9 . N31 H31 O64A 0.88 2.41 3.073(6) 132.8 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.60 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.014 _refine_diff_density_min -0.680 _refine_diff_density_rms 0.075 #=END data_mh361 _database_code_depnum_ccdc_archive 'CCDC 821512' #TrackingRef '- Solvent dependence Dalton.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-di(pyrazol-3-yl)pyridine]iron(II) ditetrafluoroborate bis-acetonitrile solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H18 Fe N10, 2[B F4], 2[C2 H3 N]' _chemical_formula_sum 'C26 H24 B2 F8 Fe N12' _chemical_formula_weight 734.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 11.8232(13) _cell_length_b 23.510(2) _cell_length_c 12.3117(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.191(6) _cell_angle_gamma 90.00 _cell_volume 3416.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30470 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 28.45 _exptl_crystal_description fragment _exptl_crystal_colour orange _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 0.523 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.631 _exptl_absorpt_correction_T_max 0.647 _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 30470 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 28.45 _reflns_number_total 4318 _reflns_number_gt 3481 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 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 asymmetric unit contains half a complex dication with Fe1, N2, C5, N11 and C14 all lying on the crystallographic C~2~ axis [0.5, y, 0.75]; and, one BF~4~^-^ anion and one acetonitrile molecule, both occupying general lattice sites. The anion is disordered over three equally occupied orientations, which were refined with the refined restraints B---F = 1.40(2) and F...F = 2.29(2) \%A. The acetonitrile molecule is also disordered, over two equally occupied sites. These were refined with the fixed restraints C-C = 1.46(2), C-N = 1.16(2) and 1,3-C...N = 2.62(2) \%A. All non-H atoms except the anion disorder sites were refined anistropically, 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^)+(0.0816P)^2^+4.4660P] 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 4318 _refine_ls_number_parameters 270 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1576 _refine_ls_wR_factor_gt 0.1431 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.067 _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 0.5000 0.710274(18) 0.7500 0.03227(16) Uani 1 2 d S . . N2 N 0.5000 0.62118(13) 0.7500 0.0412(6) Uani 1 2 d S . . C3 C 0.5387(2) 0.59197(13) 0.8413(2) 0.0493(6) Uani 1 1 d . . . C4 C 0.5404(3) 0.53234(15) 0.8431(3) 0.0687(9) Uani 1 1 d . . . H4 H 0.5684 0.5125 0.9062 0.082 Uiso 1 1 calc R . . C5 C 0.5000 0.5025(2) 0.7500 0.0805(16) Uani 1 2 d S . . H5 H 0.5000 0.4621 0.7500 0.097 Uiso 1 2 calc SR . . C6 C 0.5760(2) 0.63097(16) 0.9306(2) 0.0559(7) Uani 1 1 d . . . N7 N 0.56837(17) 0.68774(12) 0.90918(17) 0.0525(6) Uani 1 1 d . . . N8 N 0.6061(2) 0.71445(18) 1.0036(2) 0.0867(12) Uani 1 1 d . . . H8 H 0.6098 0.7516 1.0123 0.104 Uiso 1 1 calc R . . C9 C 0.6369(3) 0.6757(3) 1.0820(3) 0.119(2) Uani 1 1 d . . . H9 H 0.6660 0.6843 1.1536 0.142 Uiso 1 1 calc R . . C10 C 0.6188(3) 0.6225(3) 1.0404(3) 0.0961(17) Uani 1 1 d . . . H10 H 0.6319 0.5872 1.0767 0.115 Uiso 1 1 calc R . . N11 N 0.5000 0.79983(12) 0.7500 0.0410(6) Uani 1 2 d S . . C12 C 0.4099(2) 0.82878(11) 0.7884(2) 0.0482(6) Uani 1 1 d . . . C13 C 0.4070(4) 0.88871(13) 0.7892(3) 0.0738(10) Uani 1 1 d . . . H13 H 0.3442 0.9087 0.8154 0.089 Uiso 1 1 calc R . . C14 C 0.5000 0.9180(2) 0.7500 0.0876(18) Uani 1 2 d S . . H14 H 0.5000 0.9584 0.7500 0.105 Uiso 1 2 calc SR . . C15 C 0.3201(2) 0.79024(11) 0.82420(19) 0.0435(5) Uani 1 1 d . . . N16 N 0.33959(17) 0.73344(10) 0.80998(15) 0.0420(5) Uani 1 1 d . . . N17 N 0.2453(2) 0.70673(12) 0.84394(18) 0.0557(6) Uani 1 1 d . . . H17 H 0.2353 0.6696 0.8431 0.067 Uiso 1 1 calc R . . C18 C 0.1684(3) 0.74500(18) 0.8794(2) 0.0662(9) Uani 1 1 d . . . H18 H 0.0970 0.7360 0.9069 0.079 Uiso 1 1 calc R . . C19 C 0.2122(3) 0.79877(16) 0.8682(2) 0.0602(8) Uani 1 1 d . . . H19 H 0.1782 0.8339 0.8859 0.072 Uiso 1 1 calc R . . B20A B 0.2426(12) 0.5555(6) 0.9333(12) 0.057(5) Uiso 0.34 1 d PD A 1 F21A F 0.3271(6) 0.5762(3) 1.0066(5) 0.0638(16) Uiso 0.34 1 d PD A 1 F22A F 0.1398(6) 0.5603(3) 0.9809(7) 0.082(2) Uiso 0.34 1 d PD A 1 F23A F 0.2361(10) 0.5906(5) 0.8342(9) 0.112(5) Uiso 0.34 1 d PD A 1 F24A F 0.2757(6) 0.4974(3) 0.9092(6) 0.0714(18) Uiso 0.34 1 d PD A 1 B20B B 0.2257(11) 0.5615(6) 0.9166(11) 0.054(4) Uiso 0.33 1 d PD B 2 F21B F 0.3147(8) 0.5494(4) 0.9924(8) 0.095(3) Uiso 0.33 1 d PD B 2 F22B F 0.1400(5) 0.5949(2) 0.9565(5) 0.0627(13) Uiso 0.33 1 d PD B 2 F23B F 0.2808(8) 0.5928(4) 0.8416(8) 0.073(4) Uiso 0.33 1 d PD B 2 F24B F 0.1764(6) 0.5104(3) 0.8765(6) 0.0840(18) Uiso 0.33 1 d PD B 2 B20C B 0.2346(11) 0.5499(6) 0.9155(11) 0.053(5) Uiso 0.33 1 d PD C 3 F21C F 0.2941(6) 0.5611(4) 1.0190(6) 0.0692(19) Uiso 0.33 1 d PD C 3 F22C F 0.1201(6) 0.5555(4) 0.9325(7) 0.089(2) Uiso 0.33 1 d PD C 3 F23C F 0.2644(10) 0.5867(3) 0.8279(7) 0.049(2) Uiso 0.33 1 d PD C 3 F24C F 0.2453(8) 0.4973(3) 0.8754(7) 0.084(2) Uiso 0.33 1 d PD C 3 C25A C 0.618(2) 0.9475(8) 1.114(2) 0.086(5) Uani 0.50 1 d PD D 1 H25A H 0.5727 0.9548 1.1766 0.128 Uiso 0.50 1 calc PR D 1 H25B H 0.5910 0.9720 1.0530 0.128 Uiso 0.50 1 calc PR D 1 H25C H 0.6976 0.9557 1.1327 0.128 Uiso 0.50 1 calc PR D 1 C26A C 0.605(3) 0.8871(10) 1.081(3) 0.076(6) Uani 0.50 1 d PD D 1 N27A N 0.5976(18) 0.8436(6) 1.0402(15) 0.096(5) Uani 0.50 1 d PD D 1 C25B C 0.6254(14) 0.9348(7) 1.0941(19) 0.075(4) Uani 0.50 1 d PD E 2 H25D H 0.6763 0.9510 1.0420 0.112 Uiso 0.50 1 calc PR E 2 H25E H 0.6562 0.9421 1.1684 0.112 Uiso 0.50 1 calc PR E 2 H25F H 0.5505 0.9524 1.0837 0.112 Uiso 0.50 1 calc PR E 2 C26B C 0.615(3) 0.8726(8) 1.0763(18) 0.072(5) Uani 0.50 1 d PD E 2 N27B N 0.6057(15) 0.8241(5) 1.0690(14) 0.079(3) Uani 0.50 1 d PD 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 0.0330(2) 0.0370(3) 0.0266(2) 0.000 0.00058(16) 0.000 N2 0.0325(13) 0.0566(17) 0.0347(14) 0.000 0.0034(10) 0.000 C3 0.0351(12) 0.0669(16) 0.0467(14) 0.0147(12) 0.0093(10) 0.0058(11) C4 0.0553(17) 0.0674(19) 0.086(2) 0.0270(17) 0.0283(16) 0.0145(15) C5 0.073(3) 0.058(3) 0.115(5) 0.000 0.047(3) 0.000 C6 0.0338(12) 0.099(2) 0.0353(13) 0.0106(13) 0.0020(10) 0.0057(13) N7 0.0346(10) 0.0891(18) 0.0336(11) -0.0213(11) -0.0007(8) -0.0037(11) N8 0.0406(13) 0.164(4) 0.0550(17) -0.058(2) 0.0024(11) -0.0122(16) C9 0.052(2) 0.269(8) 0.0337(17) -0.030(3) -0.0093(15) -0.005(3) C10 0.0519(19) 0.197(6) 0.0398(17) 0.032(3) 0.0008(14) 0.018(2) N11 0.0514(16) 0.0425(15) 0.0291(13) 0.000 0.0035(11) 0.000 C12 0.0621(16) 0.0456(13) 0.0373(12) 0.0002(10) 0.0061(11) 0.0092(12) C13 0.100(3) 0.0447(15) 0.079(2) -0.0011(15) 0.026(2) 0.0159(17) C14 0.123(5) 0.039(2) 0.105(4) 0.000 0.039(4) 0.000 C15 0.0470(13) 0.0551(14) 0.0282(11) 0.0034(9) 0.0020(9) 0.0117(11) N16 0.0418(10) 0.0536(12) 0.0306(9) 0.0045(8) 0.0018(8) -0.0036(9) N17 0.0523(13) 0.0810(17) 0.0337(11) 0.0096(10) 0.0012(9) -0.0178(12) C18 0.0423(14) 0.119(3) 0.0379(14) 0.0138(16) 0.0044(11) -0.0003(16) C19 0.0524(16) 0.094(2) 0.0349(13) 0.0078(13) 0.0066(11) 0.0244(16) C25A 0.105(12) 0.069(7) 0.081(10) -0.007(6) -0.006(6) 0.002(6) C26A 0.051(8) 0.090(8) 0.088(10) -0.023(6) 0.013(5) -0.001(8) N27A 0.089(7) 0.095(10) 0.105(12) -0.034(8) 0.012(8) 0.007(8) C25B 0.048(5) 0.087(11) 0.089(10) 0.012(8) 0.004(5) -0.010(6) C26B 0.047(6) 0.121(16) 0.047(7) -0.015(8) 0.005(5) 0.000(12) N27B 0.067(5) 0.083(8) 0.087(7) -0.005(5) 0.008(5) -0.016(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 2.095(3) . ? Fe1 N11 2.106(3) . ? Fe1 N16 2.143(2) . ? Fe1 N7 2.144(2) . ? N2 C3 1.373(3) . ? C3 C4 1.402(5) . ? C3 C6 1.481(4) . ? C4 C5 1.405(5) . ? C6 N7 1.363(4) . ? C6 C10 1.430(4) . ? N7 N8 1.374(3) . ? N8 C9 1.361(7) . ? C9 C10 1.365(8) . ? N11 C12 1.370(3) . ? C12 C13 1.409(4) . ? C12 C15 1.482(4) . ? C13 C14 1.405(4) . ? C15 N16 1.368(3) . ? C15 C19 1.427(4) . ? N16 N17 1.365(3) . ? N17 C18 1.368(4) . ? C18 C19 1.376(5) . ? B20A F22A 1.383(13) . ? B20A F21A 1.396(14) . ? B20A F24A 1.456(14) . ? B20A F23A 1.471(14) . ? B20B F23B 1.374(13) . ? B20B F22B 1.393(13) . ? B20B F21B 1.397(14) . ? B20B F24B 1.413(13) . ? B20C F24C 1.340(14) . ? B20C F22C 1.388(13) . ? B20C F23C 1.442(13) . ? B20C F21C 1.445(14) . ? C25A C26A 1.482(15) . ? C26A N27A 1.139(15) . ? C25B C26B 1.481(14) . ? C26B N27B 1.151(15) . ? 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 N11 180.00 . . ? N2 Fe1 N16 104.72(6) . . ? N11 Fe1 N16 75.28(6) . . ? N16 Fe1 N16 150.56(12) 2_656 . ? N2 Fe1 N7 75.70(7) . . ? N11 Fe1 N7 104.30(7) . . ? N16 Fe1 N7 94.69(8) 2_656 . ? N16 Fe1 N7 92.50(8) . . ? N7 Fe1 N7 151.40(15) 2_656 . ? C3 N2 C3 120.0(4) 2_656 . ? C3 N2 Fe1 120.00(18) . . ? N2 C3 C4 121.1(3) . . ? N2 C3 C6 111.7(3) . . ? C4 C3 C6 127.1(3) . . ? C3 C4 C5 118.8(3) . . ? C4 C5 C4 120.0(5) . 2_656 ? N7 C6 C10 109.6(4) . . ? N7 C6 C3 116.7(2) . . ? C10 C6 C3 133.7(4) . . ? C6 N7 N8 105.6(3) . . ? C6 N7 Fe1 115.89(17) . . ? N8 N7 Fe1 138.5(3) . . ? C9 N8 N7 110.8(4) . . ? N8 C9 C10 108.5(3) . . ? C9 C10 C6 105.4(4) . . ? C12 N11 C12 120.4(3) . 2_656 ? C12 N11 Fe1 119.78(16) . . ? N11 C12 C13 121.2(3) . . ? N11 C12 C15 112.5(2) . . ? C13 C12 C15 126.2(3) . . ? C14 C13 C12 117.8(3) . . ? C13 C14 C13 121.4(4) 2_656 . ? N16 C15 C19 110.3(3) . . ? N16 C15 C12 115.5(2) . . ? C19 C15 C12 134.2(3) . . ? N17 N16 C15 105.3(2) . . ? N17 N16 Fe1 137.89(19) . . ? C15 N16 Fe1 116.80(17) . . ? N16 N17 C18 111.3(3) . . ? N17 C18 C19 108.1(3) . . ? C18 C19 C15 105.0(3) . . ? F22A B20A F21A 108.2(11) . . ? F22A B20A F24A 114.5(10) . . ? F21A B20A F24A 105.5(10) . . ? F22A B20A F23A 107.4(11) . . ? F21A B20A F23A 110.1(10) . . ? F24A B20A F23A 111.1(11) . . ? F23B B20B F22B 108.5(10) . . ? F23B B20B F21B 101.0(9) . . ? F22B B20B F21B 114.5(10) . . ? F23B B20B F24B 115.0(11) . . ? F22B B20B F24B 108.0(9) . . ? F21B B20B F24B 110.0(10) . . ? F24C B20C F22C 104.8(10) . . ? F24C B20C F23C 104.3(10) . . ? F22C B20C F23C 109.7(11) . . ? F24C B20C F21C 116.3(11) . . ? F22C B20C F21C 106.3(10) . . ? F23C B20C F21C 115.0(10) . . ? N27A C26A C25A 170(3) . . ? N27B C26B C25B 176(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N8 H8 N27A 0.88 2.20 3.072(15) 172.9 . N8 H8 N27B 0.88 1.84 2.700(15) 163.9 . N17 H17 F23A 0.88 1.86 2.734(13) 171.4 . N17 H17 F23B 0.88 1.88 2.711(11) 155.7 . N17 H17 F23C 0.88 1.99 2.838(9) 161.4 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.45 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.482 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.063