#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:36:42 +0100 (vie 25 de mar de 2016) $
#$Revision: 179756 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/52/7005252.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_7005252
loop_
_publ_author_name
'Carbonera, Chiara'
'Kilner, Colin A.'
'Létard, Jean-François'
'Halcrow, Malcolm A.'
_publ_section_title
;
 Anion doping as a probe of cooperativity in the molecular
 spin-crossover compound [FeL2][BF4]2 (L =
 2,6-di{pyrazol-1-yl}pyridine).
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1284
_journal_page_last               1292
_journal_paper_doi               10.1039/b618480d
_journal_year                    2007
_chemical_formula_moiety         'C22 H18 Fe N10, 0.32[B F4], 1.68[Cl O4]'
_chemical_formula_sum            'C22 H18 B0.32 Cl1.68 F1.28 Fe N10 O6.72'
_chemical_formula_weight         673.17
_chemical_name_systematic
;
Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) 0.32:1.68 tetrafluoroborate:
perchlorate salt
;
_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                 99.320(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4602(17)
_cell_length_b                   9.3419(11)
_cell_length_c                   20.202(2)
_cell_measurement_reflns_used    5419
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      2.61
_cell_volume                     2693.0(5)
_computing_cell_refinement       'APEX 2 software, Bruker Nonius 2004'
_computing_data_collection       'APEX 2 software, Bruker Nonius 2004'
_computing_data_reduction        'SAINT, Bruker Nonius 2004'
_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 '120 microns'
_diffrn_measured_fraction_theta_full 0.885
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_device_type  'Bruker X8 Apex diffractometer'
_diffrn_measurement_method       'Rotation images'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5419
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_T_max  1.040
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2002). SADABS v. 2.03. University of
G/ottingen, Germany.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Square prism'
_exptl_crystal_F_000             1370
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0268P)²+7.0562P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0776
_reflns_number_gt                2150
_reflns_number_total             2365
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b618480d.txt
_cod_data_source_block           c:\datasets\leeds\mh140c\mh140c
_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               7005252
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 0.69648(5) 0.2500 0.01778(13) Uani 1 2 d S . .
N2 N 0.01422(12) 0.7456(2) 0.35670(8) 0.0187(4) Uani 1 1 d . . .
C3 C -0.03026(14) 0.6664(2) 0.39696(10) 0.0191(4) Uani 1 1 d . . .
C4 C -0.02808(16) 0.6960(3) 0.46495(10) 0.0246(5) Uani 1 1 d . . .
H4 H -0.0625 0.6406 0.4920 0.029 Uiso 1 1 calc R . .
C5 C 0.02712(17) 0.8111(3) 0.49086(10) 0.0275(5) Uani 1 1 d . . .
H5 H 0.0303 0.8353 0.5368 0.033 Uiso 1 1 calc R . .
C6 C 0.07813(16) 0.8921(3) 0.45112(10) 0.0261(5) Uani 1 1 d . . .
H6 H 0.1178 0.9684 0.4692 0.031 Uiso 1 1 calc R . .
C7 C 0.06762(15) 0.8548(2) 0.38353(10) 0.0210(5) Uani 1 1 d . . .
N8 N -0.07734(12) 0.5470(2) 0.36382(8) 0.0194(4) Uani 1 1 d . . .
N9 N -0.06791(12) 0.5235(2) 0.29788(8) 0.0208(4) Uani 1 1 d . . .
C10 C -0.10464(15) 0.3939(2) 0.28356(10) 0.0240(5) Uani 1 1 d . . .
H10 H -0.1082 0.3484 0.2412 0.029 Uiso 1 1 calc R . .
C11 C -0.13771(16) 0.3327(3) 0.33958(11) 0.0265(5) Uani 1 1 d . . .
H11 H -0.1667 0.2420 0.3419 0.032 Uiso 1 1 calc R . .
C12 C -0.11884(15) 0.4326(3) 0.38964(10) 0.0246(5) Uani 1 1 d . . .
H12 H -0.1321 0.4240 0.4340 0.029 Uiso 1 1 calc R . .
N13 N 0.11352(12) 0.9267(2) 0.33618(9) 0.0220(4) Uani 1 1 d . . .
N14 N 0.10717(13) 0.8687(2) 0.27277(8) 0.0223(4) Uani 1 1 d . . .
C15 C 0.15588(15) 0.9582(3) 0.23998(11) 0.0258(5) Uani 1 1 d . . .
H15 H 0.1643 0.9461 0.1946 0.031 Uiso 1 1 calc R . .
C16 C 0.19332(16) 1.0732(3) 0.28130(12) 0.0292(5) Uani 1 1 d . . .
H16 H 0.2303 1.1503 0.2695 0.035 Uiso 1 1 calc R . .
C17 C 0.16510(16) 1.0505(2) 0.34195(12) 0.0277(5) Uani 1 1 d . . .
H17 H 0.1787 1.1093 0.3807 0.033 Uiso 1 1 calc R . .
Cl18 Cl 0.29708(4) 0.95932(8) 0.08960(3) 0.02998(18) Uani 0.84 1 d P A 1
O19 O 0.21857(16) 0.8692(3) 0.09230(12) 0.0818(9) Uani 0.84 1 d P A 1
O20 O 0.38171(14) 0.8784(2) 0.10646(9) 0.0486(5) Uani 0.84 1 d P A 1
O21 O 0.29769(15) 1.0733(2) 0.13786(12) 0.0586(6) Uani 0.84 1 d P A 1
O22 O 0.29502(17) 1.0156(4) 0.02400(11) 0.0913(10) Uani 0.84 1 d P A 1
B18 B 0.29708(4) 0.95932(8) 0.08960(3) 0.02998(18) Uani 0.16 1 d P B 2
F20 F 0.38171(14) 0.8784(2) 0.10646(9) 0.0486(5) Uani 0.16 1 d P B 2
F22 F 0.29502(17) 1.0156(4) 0.02400(11) 0.0913(10) Uani 0.16 1 d P B 2
F21 F 0.29769(15) 1.0733(2) 0.13786(12) 0.0586(6) Uani 0.16 1 d P B 2
F19 F 0.21857(16) 0.8692(3) 0.09230(12) 0.0818(9) Uani 0.16 1 d P B 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 155.69(10) . 2 ?
N2 Fe1 N9 127.82(7) . 2 ?
N2 Fe1 N9 72.35(7) . . ?
N9 Fe1 N9 85.20(10) 2 . ?
N2 Fe1 N14 72.13(6) . . ?
N9 Fe1 N14 141.81(6) . . ?
N2 Fe1 N14 90.17(6) . 2 ?
N9 Fe1 N14 106.05(7) . 2 ?
N14 Fe1 N14 87.62(10) . 2 ?
C3 N2 C7 118.51(17) . . ?
C3 N2 Fe1 120.42(14) . . ?
C7 N2 Fe1 121.07(13) . . ?
N2 C3 C4 123.4(2) . . ?
N2 C3 N8 112.93(17) . . ?
C4 C3 N8 123.60(19) . . ?
C5 C4 C3 116.4(2) . . ?
C4 C5 C6 121.81(19) . . ?
C7 C6 C5 116.3(2) . . ?
N2 C7 C6 123.5(2) . . ?
N2 C7 N13 112.93(17) . . ?
C6 C7 N13 123.6(2) . . ?
C12 N8 N9 111.23(17) . . ?
C12 N8 C3 129.86(17) . . ?
N9 N8 C3 117.80(16) . . ?
C10 N9 N8 104.80(17) . . ?
C10 N9 Fe1 139.72(14) . . ?
N8 N9 Fe1 115.48(13) . . ?
N9 C10 C11 111.50(19) . . ?
C12 C11 C10 105.2(2) . . ?
N8 C12 C11 107.29(18) . . ?
C17 N13 N14 111.31(18) . . ?
C17 N13 C7 130.53(19) . . ?
N14 N13 C7 118.16(18) . . ?
C15 N14 N13 104.69(18) . . ?
C15 N14 Fe1 138.93(15) . . ?
N13 N14 Fe1 114.47(13) . . ?
N14 C15 C16 111.4(2) . . ?
C17 C16 C15 105.6(2) . . ?
C16 C17 N13 107.0(2) . . ?
O22 Cl18 O19 111.01(17) . . ?
O22 Cl18 O20 107.76(12) . . ?
O19 Cl18 O20 109.58(17) . . ?
O22 Cl18 O21 110.74(17) . . ?
O19 Cl18 O21 109.19(13) . . ?
O20 Cl18 O21 108.51(13) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.1808(16) . ?
Fe1 N9 2.1951(18) . ?
Fe1 N14 2.2297(19) . ?
N2 C3 1.339(3) . ?
N2 C7 1.340(3) . ?
C3 C4 1.397(3) . ?
C3 N8 1.417(3) . ?
C4 C5 1.390(3) . ?
C5 C6 1.398(3) . ?
C6 C7 1.394(3) . ?
C7 N13 1.419(3) . ?
N8 C12 1.370(3) . ?
N8 N9 1.378(2) . ?
N9 C10 1.335(3) . ?
C10 C11 1.418(3) . ?
C11 C12 1.370(3) . ?
N13 C17 1.371(3) . ?
N13 N14 1.380(2) . ?
N14 C15 1.336(3) . ?
C15 C16 1.414(3) . ?
C16 C17 1.369(3) . ?
Cl18 O22 1.421(2) . ?
Cl18 O19 1.422(2) . ?
Cl18 O20 1.432(2) . ?
Cl18 O21 1.443(2) . ?
