#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:22:20 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179787 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/83/7008365.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_7008365
loop_
_publ_author_name
'Elhaik, Jerome'
'Evans, David J.'
'Kilner, Colin A.'
'Halcrow, Malcolm A.'
_publ_section_title
;
 A structural, magnetic and Mössbauer spectroscopic study of an
 unusual angular Jahn-Teller distortion in a series of high-spin
 iron(II) complexes.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1693
_journal_page_last               1700
_journal_paper_doi               10.1039/b502175h
_journal_year                    2005
_chemical_formula_moiety         'C22 H18 Fe N10, 2[Sb F6]'
_chemical_formula_sum            'C22 H18 F12 Fe N10 Sb2'
_chemical_formula_weight         949.81
_chemical_name_systematic
;
Bis-[2,6-dipyrazol-1-ylpyridine]iron(II) di(hexafluoroantimonate)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 100.0021(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6737(2)
_cell_length_b                   9.5610(2)
_cell_length_c                   21.1182(4)
_cell_measurement_reflns_used    20739
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.37
_cell_volume                     2917.75(9)
_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      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD 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  0.1207
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20739
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    2.441
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_correction_T_min  0.668
_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    2.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Rectangular Prism'
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       0.0018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0291
_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/[σ²(Fo²)+(0.0247P)²+4.0634P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0734
_reflns_number_gt                3046
_reflns_number_total             3330
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b502175h.txt
_cod_data_source_block           c:\datasets\leeds\mh115\mh115
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7008365
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'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.82756(5) 0.2500 0.02134(13) Uani 1 2 d S . .
N2 N 0.00907(13) 0.7772(2) 0.35127(9) 0.0216(4) Uani 1 1 d . . .
C3 C -0.03574(16) 0.8539(3) 0.38856(11) 0.0238(5) Uani 1 1 d . . .
C4 C -0.03949(17) 0.8201(3) 0.45176(11) 0.0292(5) Uani 1 1 d . . .
H4 H -0.0730 0.8759 0.4770 0.035 Uiso 1 1 calc R . .
C5 C 0.00800(17) 0.7007(3) 0.47672(11) 0.0294(5) Uani 1 1 d . . .
H5 H 0.0066 0.6732 0.5198 0.035 Uiso 1 1 calc R . .
C6 C 0.05728(17) 0.6217(3) 0.43915(11) 0.0273(5) Uani 1 1 d . . .
H6 H 0.0911 0.5411 0.4558 0.033 Uiso 1 1 calc R . .
C7 C 0.05526(16) 0.6647(2) 0.37671(11) 0.0228(5) Uani 1 1 d . . .
N8 N -0.07682(15) 0.9741(2) 0.35778(9) 0.0242(4) Uani 1 1 d . . .
N9 N -0.06698(15) 0.9964(2) 0.29532(10) 0.0262(4) Uani 1 1 d . . .
C10 C -0.10179(18) 1.1238(3) 0.28142(12) 0.0308(5) Uani 1 1 d . . .
H10 H -0.1053 1.1681 0.2408 0.037 Uiso 1 1 calc R . .
C11 C -0.13264(19) 1.1840(3) 0.33466(12) 0.0355(6) Uani 1 1 d . . .
H11 H -0.1597 1.2737 0.3369 0.043 Uiso 1 1 calc R . .
C12 C -0.11568(18) 1.0868(3) 0.38215(12) 0.0320(6) Uani 1 1 d . . .
H12 H -0.1286 1.0958 0.4245 0.038 Uiso 1 1 calc R . .
N13 N 0.10347(14) 0.5970(2) 0.33316(9) 0.0234(4) Uani 1 1 d . . .
N14 N 0.10237(14) 0.6560(2) 0.27411(9) 0.0242(4) Uani 1 1 d . . .
C15 C 0.15179(18) 0.5703(3) 0.24433(12) 0.0292(5) Uani 1 1 d . . .
H15 H 0.1628 0.5841 0.2018 0.035 Uiso 1 1 calc R . .
C16 C 0.1859(2) 0.4566(3) 0.28336(14) 0.0307(6) Uani 1 1 d . . .
H16 H 0.2231 0.3817 0.2729 0.037 Uiso 1 1 calc R . .
C17 C 0.15404(19) 0.4766(2) 0.33968(13) 0.0282(5) Uani 1 1 d . . .
H17 H 0.1650 0.4178 0.3765 0.034 Uiso 1 1 calc R . .
Sb18 Sb 0.228324(11) 1.035730(18) 0.420511(7) 0.02729(10) Uani 1 1 d . . .
F19 F 0.18491(14) 0.95508(17) 0.33978(8) 0.0451(4) Uani 1 1 d . A 1
F20 F 0.27502(12) 1.10802(19) 0.50210(7) 0.0437(4) Uani 1 1 d . A 1
F21 F 0.34455(13) 0.95842(16) 0.41789(9) 0.0424(4) Uani 1 1 d . A 1
F22 F 0.19089(18) 0.8780(3) 0.46056(10) 0.0789(8) Uani 1 1 d . A 1
F23 F 0.11245(13) 1.1177(3) 0.41960(9) 0.0686(7) Uani 1 1 d . A 1
F24 F 0.26327(12) 1.19585(16) 0.37944(8) 0.0392(4) Uani 1 1 d . A 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 154.41(10) 2 . ?
N2 Fe1 N9 71.90(7) . . ?
N2 Fe1 N9 129.54(7) . 2 ?
N9 Fe1 N9 85.25(12) 2 . ?
N2 Fe1 N14 89.16(7) . 2 ?
N9 Fe1 N14 107.87(8) . 2 ?
N2 Fe1 N14 71.80(7) . . ?
N9 Fe1 N14 141.18(7) . . ?
N14 Fe1 N14 84.88(10) 2 . ?
C3 N2 C7 118.3(2) . . ?
C3 N2 Fe1 120.55(15) . . ?
C7 N2 Fe1 121.00(15) . . ?
N2 C3 C4 123.3(2) . . ?
N2 C3 N8 113.2(2) . . ?
C4 C3 N8 123.5(2) . . ?
C3 C4 C5 117.1(2) . . ?
C6 C5 C4 120.4(2) . . ?
C7 C6 C5 117.3(2) . . ?
N2 C7 C6 123.5(2) . . ?
N2 C7 N13 112.6(2) . . ?
C6 C7 N13 123.9(2) . . ?
C12 N8 N9 111.2(2) . . ?
C12 N8 C3 130.3(2) . . ?
N9 N8 C3 117.74(19) . . ?
C10 N9 N8 104.7(2) . . ?
C10 N9 Fe1 139.42(18) . . ?
N8 N9 Fe1 115.83(15) . . ?
N9 C10 C11 111.2(2) . . ?
C12 C11 C10 105.5(2) . . ?
C11 C12 N8 107.3(2) . . ?
C17 N13 N14 111.1(2) . . ?
C17 N13 C7 130.3(2) . . ?
N14 N13 C7 118.55(19) . . ?
C15 N14 N13 104.94(19) . . ?
C15 N14 Fe1 138.79(17) . . ?
N13 N14 Fe1 114.47(14) . . ?
N14 C15 C16 111.7(2) . . ?
C17 C16 C15 105.2(2) . . ?
N13 C17 C16 107.1(2) . . ?
F22 Sb18 F21 92.05(11) . . ?
F22 Sb18 F23 90.28(12) . . ?
F21 Sb18 F23 177.31(9) . . ?
F22 Sb18 F20 88.32(9) . . ?
F21 Sb18 F20 89.04(7) . . ?
F23 Sb18 F20 92.38(8) . . ?
F22 Sb18 F24 178.71(9) . . ?
F21 Sb18 F24 89.14(8) . . ?
F23 Sb18 F24 88.52(10) . . ?
F20 Sb18 F24 92.21(8) . . ?
F22 Sb18 F19 89.97(9) . . ?
F21 Sb18 F19 88.75(8) . . ?
F23 Sb18 F19 89.91(9) . . ?
F20 Sb18 F19 177.15(7) . . ?
F24 Sb18 F19 89.55(7) . . ?
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 2.1736(18) . ?
Fe1 N9 2.194(2) . ?
Fe1 N14 2.223(2) . ?
N2 C3 1.330(3) . ?
N2 C7 1.334(3) . ?
C3 C4 1.384(3) . ?
C3 N8 1.404(3) . ?
C4 C5 1.392(4) . ?
C5 C6 1.387(4) . ?
C6 C7 1.377(3) . ?
C7 N13 1.411(3) . ?
N8 C12 1.361(3) . ?
N8 N9 1.368(3) . ?
N9 C10 1.333(3) . ?
C10 C11 1.406(4) . ?
C11 C12 1.358(4) . ?
N13 C17 1.363(3) . ?
N13 N14 1.366(3) . ?
N14 C15 1.323(3) . ?
C15 C16 1.403(4) . ?
C16 C17 1.365(4) . ?
Sb18 F22 1.8583(19) . ?
Sb18 F21 1.8684(17) . ?
Sb18 F23 1.8694(19) . ?
Sb18 F20 1.8724(15) . ?
Sb18 F24 1.8744(16) . ?
Sb18 F19 1.8787(16) . ?
