#------------------------------------------------------------------------------ #$Date: 2016-03-26 02:00:26 +0200 (Sat, 26 Mar 2016) $ #$Revision: 180118 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/10/16/7101685.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7101685 loop_ _publ_author_name 'Pritchard, Ruth' 'Kilner, Colin A' 'Halcrow, Malcolm A' _publ_section_title ; Iron(II) complexes with a terpyridine embrace packing motif show remarkably consistent cooperative spin-transitions. ; _journal_issue 6 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 577 _journal_page_last 579 _journal_paper_doi 10.1039/b613402e _journal_year 2007 _chemical_formula_moiety 'C22 H14 Cl4 Fe N10, 2[B F4]' _chemical_formula_sum 'C22 H14 B2 Cl4 F8 Fe N10' _chemical_formula_weight 789.70 _chemical_name_common ;Bis(2,6-di(4-chloropyrazol-1-yl)pyridine)iron(ii) ditetrafluoroborate ; _chemical_name_systematic ; Bis[2,6-di(4-chloropyrazol-1-yl)pyridine]iron(II) ditetrafluoroborate ; _space_group_IT_number 114 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'P -4 2n' _symmetry_space_group_name_H-M 'P -4 21 c' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 9.5613(1) _cell_length_b 9.5613(1) _cell_length_c 17.3177(3) _cell_measurement_reflns_used 24687 _cell_measurement_temperature 300(2) _cell_measurement_theta_max 27.46 _cell_measurement_theta_min 2.35 _cell_volume 1583.16(4) _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 300(2) _diffrn_detector_area_resol_mean 9.091 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 24687 _diffrn_reflns_theta_full 27.46 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_min 2.35 _exptl_absorpt_coefficient_mu 0.895 _exptl_absorpt_correction_T_max 0.832 _exptl_absorpt_correction_T_min 0.608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'Rectangular prism' _exptl_crystal_F_000 784 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.24 _refine_diff_density_max 0.312 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.074 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_extinction_coef 0.037(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 127 _refine_ls_number_reflns 1824 _refine_ls_number_restraints 20 _refine_ls_restrained_S_all 1.098 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0424 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+0.2717P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1166 _refine_ls_wR_factor_ref 0.1209 _reflns_number_gt 1693 _reflns_number_total 1824 _reflns_threshold_expression >2sigma(I) _cod_data_source_file b613402e.txt _cod_data_source_block rp25rt _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 7101685 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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.0000 1.0000 1.0000 0.0500(2) Uani 1 4 d S . . N2 N 0.0000 1.0000 0.87671(16) 0.0502(6) Uani 1 2 d S . . C3 C 0.0469(3) 0.8900(3) 0.83715(15) 0.0549(6) Uani 1 1 d . . . C4 C 0.0499(4) 0.8842(4) 0.75750(18) 0.0736(9) Uani 1 1 d . . . H4 H 0.0846 0.8045 0.7309 0.088 Uiso 1 1 calc R . . C5 C 0.0000 1.0000 0.7182(2) 0.0789(13) Uani 1 2 d S . . H5 H 0.0000 1.0000 0.6633 0.095 Uiso 1 2 calc SR . . N6 N 0.0928(2) 0.7807(2) 0.88512(13) 0.0552(5) Uani 1 1 d . . . N7 N 0.0755(2) 0.7947(2) 0.96300(13) 0.0536(5) Uani 1 1 d . . . C8 C 0.1223(3) 0.6763(3) 0.99300(18) 0.0597(6) Uani 1 1 d . . . H8 H 0.1238 0.6551 1.0466 0.072 Uiso 1 1 calc R . . C9 C 0.1694(3) 0.5866(3) 0.9343(2) 0.0642(7) Uani 1 1 d . . . C10 C 0.1504(4) 0.6553(3) 0.86688(19) 0.0666(7) Uani 1 1 d . . . H10 H 0.1730 0.6223 0.8167 0.080 Uiso 1 1 calc R . . Cl11 Cl 0.23932(11) 0.42421(9) 0.94551(8) 0.0957(4) Uani 1 1 d . . . B12A B 0.0368(14) 0.4630(12) 0.6824(7) 0.080(3) Uiso 0.35 1 d PD . 1 F13A F -0.1009(14) 0.4692(16) 0.6859(9) 0.171(6) Uiso 0.35 1 d PD . 1 F14A F 0.0856(8) 0.3814(8) 0.6242(4) 0.0952(18) Uiso 0.35 1 d PD A 1 F15A F 0.0888(11) 0.4078(10) 0.7532(5) 0.102(2) Uiso 0.35 1 d PD . 1 F16A F 0.0946(12) 0.5925(9) 0.6739(5) 0.102(3) Uiso 0.35 1 d PD . 1 B12B B 0.070(2) 0.4642(18) 0.6960(11) 0.067(7) Uiso 0.15 1 d PD . 2 F13B F -0.0418(17) 0.518(2) 0.7445(10) 0.121(6) Uiso 0.15 1 d PD . 2 F14B F 0.013(2) 0.3896(17) 0.6383(9) 0.100(5) Uiso 0.15 1 d PD . 2 F15B F 0.137(2) 0.374(2) 0.7460(11) 0.133(8) Uiso 0.15 1 d PD . 2 F16B F 0.1530(12) 0.5784(12) 0.6805(6) 0.054(2) Uiso 0.15 1 d PD . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0523(3) 0.0523(3) 0.0454(3) 0.000 0.000 0.000 N2 0.0581(15) 0.0443(13) 0.0481(12) 0.000 0.000 0.0066(16) C3 0.0631(14) 0.0490(13) 0.0525(13) -0.0023(10) -0.0011(11) 0.0090(10) C4 0.099(2) 0.0662(18) 0.0560(14) -0.0106(13) 0.0006(14) 0.0199(16) C5 0.111(4) 0.081(3) 0.0449(15) 0.000 0.000 0.023(4) N6 0.0633(12) 0.0464(10) 0.0560(11) -0.0033(9) -0.0035(10) 0.0071(10) N7 0.0536(11) 0.0521(11) 0.0552(11) 0.0035(9) -0.0007(9) 0.0005(9) C8 0.0530(13) 0.0555(13) 0.0706(16) 0.0111(13) -0.0047(13) -0.0005(10) C9 0.0536(14) 0.0464(12) 0.092(2) 0.0055(14) -0.0018(14) 0.0035(10) C10 0.0692(17) 0.0496(14) 0.0810(17) -0.0066(13) 0.0035(15) 0.0086(13) Cl11 0.0959(7) 0.0558(4) 0.1355(9) 0.0223(5) 0.0122(6) 0.0226(4) 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' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N2 Fe1 N2 180.00 . 2_467 N2 Fe1 N7 72.97(6) . . N7 Fe1 N7 145.94(11) 3_575 . N2 Fe1 N7 107.03(6) . 2_467 N7 Fe1 N7 94.92(3) . 2_467 C3 N2 C3 118.1(3) 3_575 . C3 N2 Fe1 120.94(15) . . N2 C3 C4 123.5(2) . . N2 C3 N6 112.8(2) . . C4 C3 N6 123.6(2) . . C3 C4 C5 116.9(3) . . C4 C5 C4 121.1(4) 3_575 . C10 N6 N7 111.4(2) . . C10 N6 C3 130.3(2) . . N7 N6 C3 118.3(2) . . C8 N7 N6 105.3(2) . . C8 N7 Fe1 139.8(2) . . N6 N7 Fe1 114.65(15) . . N7 C8 C9 110.3(3) . . C10 C9 C8 106.6(2) . . C10 C9 Cl11 126.5(3) . . C8 C9 Cl11 127.0(2) . . C9 C10 N6 106.4(3) . . F13A B12A F14A 113.7(13) . . F13A B12A F16A 111.6(11) . . F14A B12A F16A 107.6(9) . . F13A B12A F15A 109.0(12) . . F14A B12A F15A 107.9(9) . . F16A B12A F15A 106.8(10) . . F14B B12B F15B 109.0(14) . . F14B B12B F16B 120.7(15) . . F15B B12B F16B 110.7(15) . . F14B B12B F13B 108.3(15) . . F15B B12B F13B 101.4(14) . . F16B B12B F13B 104.9(13) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Fe1 N2 2.135(3) Fe1 N7 2.188(2) N2 C3 1.333(3) C3 C4 1.381(4) C3 N6 1.406(3) C4 C5 1.384(4) N6 C10 1.357(4) N6 N7 1.365(3) N7 C8 1.323(3) C8 C9 1.404(4) C9 C10 1.353(5) C9 Cl11 1.701(3) B12A F13A 1.320(13) B12A F14A 1.358(12) B12A F16A 1.363(13) B12A F15A 1.424(14) B12B F14B 1.345(17) B12B F15B 1.374(18) B12B F16B 1.374(17) B12B F13B 1.456(17)