#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:43:06 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179152 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/13/4311301.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_4311301
loop_
_publ_author_name
'Yukinari Sunatsuki'
'Hiromi Ohta'
'Masaaki Kojima'
'Yuichi Ikuta'
'Yoshiyuki Goto'
'Naohide Matsumoto'
'Seiichiro Iijima'
'Haruo Akashi'
'Sumio Kaizaki'
'Françoise Dahan'
'Jean-Pierre Tuchagues'
_publ_contact_author_address     Japan
_publ_contact_author_email       kojima@cc.okayama-u.ac.jp
_publ_contact_author_fax         +81-86-251-7842
_publ_contact_author_name        'Masaaki KOJIMA'
_publ_contact_author_phone       +81-86-251-7842
_publ_section_title
;
 Supramolecular Spin-Crossover Iron Complexes Based on
 Imidazole-Imidazolate Hydrogen Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4154
_journal_page_last               4171
_journal_paper_doi               10.1021/ic0498384
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C36 H45 B2 F8 Fe2 N20'
_chemical_formula_weight         1043.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           143
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3'
_symmetry_space_group_name_H-M   'P 3'
_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                120.00
_cell_formula_units_Z            1
_cell_length_a                   11.8047(7)
_cell_length_b                   11.8047(7)
_cell_length_c                   9.3705(4)
_cell_measurement_temperature    100(2)
_cell_volume                     1130.85(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0144
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9692
_diffrn_reflns_theta_full        30.38
_diffrn_reflns_theta_max         30.38
_diffrn_reflns_theta_min         3.99
_exptl_absorpt_coefficient_mu    0.729
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Dark-Red
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             535
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4025
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0165P)²+1.1533P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0704
_reflns_number_gt                3937
_reflns_number_total             4025
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0498384si20040401_112019_05.cif
_cod_data_source_block           bf100
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0165P)^2^+1.1533P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0165P)^2^+1.1533P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1130.85(10)
_cod_database_code               4311301
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.3333 0.6667 -0.47746(4) 0.01029(10) Uani 1 d S . .
N1 N 0.21440(16) 0.50182(16) -0.58014(17) 0.0132(3) Uani 1 d . . .
N2 N 0.35419(16) 0.54395(16) -0.35705(17) 0.0136(3) Uani 1 d . . .
N3 N 0.36359(19) 0.41942(19) -0.18577(19) 0.0214(4) Uani 1 d . . .
N4 N 0.3333 0.6667 -0.8298(4) 0.0204(7) Uani 1 d S . .
C1 C 0.1977(2) 0.3960(2) -0.5213(2) 0.0145(4) Uani 1 d . . .
H1 H 0.1401 0.3118 -0.5594 0.016 Uiso 1 calc R . .
C2 C 0.2731(2) 0.41491(19) -0.3929(2) 0.0154(3) Uani 1 d . . .
C3 C 0.2784(2) 0.3371(2) -0.2865(2) 0.0205(4) Uani 1 d . . .
H3 H 0.2318 0.2442 -0.2837 0.023 Uiso 1 calc R . .
C4 C 0.4067(2) 0.5417(2) -0.2318(2) 0.0177(4) Uani 1 d . . .
H4 H 0.4675 0.6178 -0.1812 0.019 Uiso 1 calc R . .
C5 C 0.13763(19) 0.4910(2) -0.7080(2) 0.0155(3) Uani 1 d . . .
H5A H 0.0957 0.5450 -0.6955 0.017 Uiso 1 calc R . .
H5B H 0.0676 0.3989 -0.7205 0.017 Uiso 1 calc R . .
C6 C 0.2239(2) 0.5362(2) -0.8415(2) 0.0171(4) Uani 1 d . . .
H6A H 0.2569 0.4752 -0.8600 0.019 Uiso 1 calc R . .
H6B H 0.1700 0.5321 -0.9243 0.019 Uiso 1 calc R . .
Fe2 Fe 0.6667 0.3333 0.37350(4) 0.01066(10) Uani 1 d S . .
N5 N 0.50218(16) 0.21437(16) 0.47639(17) 0.0135(3) Uani 1 d . . .
N6 N 0.54372(16) 0.35433(16) 0.25296(17) 0.0134(3) Uani 1 d . . .
N7 N 0.41978(19) 0.36404(19) 0.08101(19) 0.0209(4) Uani 1 d . . .
H7N H 0.3972 0.3865 0.0010 0.023 Uiso 1 calc R . .
N8 N 0.6667 0.3333 0.7272(5) 0.0267(8) Uani 1 d S . .
C7 C 0.3946(2) 0.1971(2) 0.4168(2) 0.0150(4) Uani 1 d . . .
H7 H 0.3102 0.1392 0.4543 0.016 Uiso 1 calc R . .
C8 C 0.41508(19) 0.2734(2) 0.2892(2) 0.0155(3) Uani 1 d . . .
C9 C 0.3369(2) 0.2786(2) 0.1818(2) 0.0203(4) Uani 1 d . . .
H9 H 0.2440 0.2321 0.1788 0.022 Uiso 1 calc R . .
C10 C 0.5423(2) 0.4068(2) 0.1280(2) 0.0179(4) Uani 1 d . . .
H10 H 0.6188 0.4674 0.0777 0.020 Uiso 1 calc R . .
C11 C 0.4909(2) 0.13734(19) 0.6040(2) 0.0168(4) Uani 1 d . . .
H11A H 0.5449 0.0954 0.5916 0.018 Uiso 1 calc R . .
H11B H 0.3988 0.0673 0.6162 0.018 Uiso 1 calc R . .
C12 C 0.5361(2) 0.2240(2) 0.7375(2) 0.0179(4) Uani 1 d . . .
H12A H 0.4751 0.2570 0.7554 0.020 Uiso 1 calc R . .
H12B H 0.5313 0.1699 0.8205 0.020 Uiso 1 calc R . .
B1 B 0.0000 0.0000 0.3404(17) 0.058(4) Uani 0.50 d SPD . 1
F1 F 0.0000 0.0000 0.4849(13) 0.159(7) Uani 0.50 d SPD A 1
F2 F 0.0998(4) -0.0176(4) 0.2895(7) 0.0814(17) Uani 0.50 d PD B 1
B2 B 0.0000 0.0000 0.6657(15) 0.054(3) Uani 0.50 d SPD . 2
F3 F 0.0000 0.0000 0.8106(10) 0.115(4) Uani 0.50 d SPD C 2
F4 F 0.1175(4) 0.0173(4) 0.6146(6) 0.0773(16) Uani 0.50 d PD D 2
B3 B 0.1930(14) -0.0063(10) -0.0291(15) 0.088(7) Uani 0.33 d PD E 3
F5 F 0.0832(13) -0.1195(12) -0.0597(13) 0.168(8) Uani 0.33 d PD . 3
F6 F 0.1815(13) 0.0998(10) -0.0621(10) 0.105(4) Uani 0.33 d PD E 3
F7 F 0.3057(12) 0.0101(14) -0.0722(14) 0.141(5) Uani 0.33 d PD E 3
F8 F 0.2002(10) -0.0057(10) 0.1251(9) 0.116(4) Uani 0.33 d PD E 3
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 89.77(7) 3_565 2_665 ?
N2 Fe1 N2 89.77(7) 3_565 . ?
N2 Fe1 N2 89.77(7) 2_665 . ?
N2 Fe1 N1 80.93(7) 3_565 3_565 ?
N2 Fe1 N1 90.72(7) 2_665 3_565 ?
N2 Fe1 N1 170.68(7) . 3_565 ?
N2 Fe1 N1 90.72(7) 3_565 . ?
N2 Fe1 N1 170.68(7) 2_665 . ?
N2 Fe1 N1 80.93(7) . . ?
N1 Fe1 N1 98.54(6) 3_565 . ?
N2 Fe1 N1 170.68(7) 3_565 2_665 ?
N2 Fe1 N1 80.93(7) 2_665 2_665 ?
N2 Fe1 N1 90.72(7) . 2_665 ?
N1 Fe1 N1 98.54(6) 3_565 2_665 ?
N1 Fe1 N1 98.54(6) . 2_665 ?
C1 N1 C5 118.45(17) . . ?
C1 N1 Fe1 115.66(14) . . ?
C5 N1 Fe1 125.69(13) . . ?
C4 N2 C2 105.40(17) . . ?
C4 N2 Fe1 139.30(15) . . ?
C2 N2 Fe1 113.94(13) . . ?
C4 N3 C3 106.94(18) . . ?
C6 N4 C6 119.43(5) 3_565 . ?
C6 N4 C6 119.43(5) 3_565 2_665 ?
C6 N4 C6 119.43(5) . 2_665 ?
N1 C1 C2 115.03(19) . . ?
N1 C1 H1 122.5 . . ?
C2 C1 H1 122.5 . . ?
N2 C2 C3 108.86(18) . . ?
N2 C2 C1 114.06(17) . . ?
C3 C2 C1 136.8(2) . . ?
N3 C3 C2 106.75(19) . . ?
N3 C3 H3 126.6 . . ?
C2 C3 H3 126.6 . . ?
N2 C4 N3 112.1(2) . . ?
N2 C4 H4 124.0 . . ?
N3 C4 H4 124.0 . . ?
N1 C5 C6 111.23(15) . . ?
N1 C5 H5A 109.4 . . ?
C6 C5 H5A 109.4 . . ?
N1 C5 H5B 109.4 . . ?
C6 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
N4 C6 C5 113.4(2) . . ?
N4 C6 H6A 108.9 . . ?
C5 C6 H6A 108.9 . . ?
N4 C6 H6B 108.9 . . ?
C5 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
N6 Fe2 N6 89.82(7) 2_655 3_665 ?
N6 Fe2 N6 89.82(7) 2_655 . ?
N6 Fe2 N6 89.82(7) 3_665 . ?
N6 Fe2 N5 81.05(7) 2_655 2_655 ?
N6 Fe2 N5 90.67(7) 3_665 2_655 ?
N6 Fe2 N5 170.86(7) . 2_655 ?
N6 Fe2 N5 90.67(7) 2_655 . ?
N6 Fe2 N5 170.86(7) 3_665 . ?
N6 Fe2 N5 81.05(7) . . ?
N5 Fe2 N5 98.43(6) 2_655 . ?
N6 Fe2 N5 170.86(7) 2_655 3_665 ?
N6 Fe2 N5 81.05(7) 3_665 3_665 ?
N6 Fe2 N5 90.67(7) . 3_665 ?
N5 Fe2 N5 98.43(6) 2_655 3_665 ?
N5 Fe2 N5 98.43(6) . 3_665 ?
C7 N5 C11 118.13(17) . . ?
C7 N5 Fe2 115.68(14) . . ?
C11 N5 Fe2 125.97(13) . . ?
C10 N6 C8 105.94(17) . . ?
C10 N6 Fe2 138.89(15) . . ?
C8 N6 Fe2 113.79(12) . . ?
C10 N7 C9 106.75(17) . . ?
C10 N7 H7N 126.6 . . ?
C9 N7 H7N 126.6 . . ?
C12 N8 C12 119.55(5) 2_655 . ?
C12 N8 C12 119.55(5) 2_655 3_665 ?
C12 N8 C12 119.55(5) . 3_665 ?
N5 C7 C8 114.23(19) . . ?
N5 C7 H7 122.9 . . ?
C8 C7 H7 122.9 . . ?
N6 C8 C9 108.62(18) . . ?
N6 C8 C7 114.87(17) . . ?
C9 C8 C7 136.2(2) . . ?
N7 C9 C8 106.65(18) . . ?
N7 C9 H9 126.7 . . ?
C8 C9 H9 126.7 . . ?
N6 C10 N7 112.0(2) . . ?
N6 C10 H10 124.0 . . ?
N7 C10 H10 124.0 . . ?
N5 C11 C12 110.99(16) . . ?
N5 C11 H11A 109.4 . . ?
C12 C11 H11A 109.4 . . ?
N5 C11 H11B 109.4 . . ?
C12 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
N8 C12 C11 113.8(2) . . ?
N8 C12 H12A 108.8 . . ?
C11 C12 H12A 108.8 . . ?
N8 C12 H12B 108.8 . . ?
C11 C12 H12B 108.8 . . ?
H12A C12 H12B 107.7 . . ?
F1 B1 F2 110.2(6) . 3 ?
F1 B1 F2 110.2(6) . 2 ?
F2 B1 F2 108.7(6) 3 2 ?
F1 B1 F2 110.2(6) . . ?
F2 B1 F2 108.7(6) 3 . ?
F2 B1 F2 108.7(6) 2 . ?
F3 B2 F4 110.3(6) . 3 ?
F3 B2 F4 110.3(6) . . ?
F4 B2 F4 108.7(6) 3 . ?
F3 B2 F4 110.3(6) . 2 ?
F4 B2 F4 108.7(6) 3 2 ?
F4 B2 F4 108.7(6) . 2 ?
F7 B3 F5 118.9(12) . . ?
F7 B3 F6 110.8(13) . . ?
F5 B3 F6 112.0(11) . . ?
F7 B3 F8 104.7(10) . . ?
F5 B3 F8 104.1(12) . . ?
F6 B3 F8 104.8(9) . . ?
B3 F5 F6 139.0(16) . 3 ?
B3 F6 F5 158.3(13) . 2 ?
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 1.9465(17) 3_565 ?
Fe1 N2 1.9465(17) 2_665 ?
Fe1 N2 1.9465(17) . ?
Fe1 N1 1.9878(16) 3_565 ?
Fe1 N1 1.9878(16) . ?
Fe1 N1 1.9878(16) 2_665 ?
N1 C1 1.287(3) . ?
N1 C5 1.469(2) . ?
N2 C4 1.334(2) . ?
N2 C2 1.375(2) . ?
N3 C4 1.339(3) . ?
N3 C3 1.367(3) . ?
N4 C6 1.436(2) 3_565 ?
N4 C6 1.436(2) . ?
N4 C6 1.436(2) 2_665 ?
C1 C2 1.446(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.378(3) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 C6 1.531(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
Fe2 N6 1.9502(16) 2_655 ?
Fe2 N6 1.9502(16) 3_665 ?
Fe2 N6 1.9502(16) . ?
Fe2 N5 1.9862(16) 2_655 ?
Fe2 N5 1.9862(16) . ?
Fe2 N5 1.9862(16) 3_665 ?
N5 C7 1.306(3) . ?
N5 C11 1.467(2) . ?
N6 C10 1.329(2) . ?
N6 C8 1.372(3) . ?
N7 C10 1.345(3) . ?
N7 C9 1.371(3) . ?
N7 H7N 0.8800 . ?
N8 C12 1.436(2) 2_655 ?
N8 C12 1.436(2) . ?
N8 C12 1.436(2) 3_665 ?
C7 C8 1.444(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.387(3) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.533(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
B1 F1 1.354(15) . ?
B1 F2 1.379(6) 3 ?
B1 F2 1.379(6) 2 ?
B1 F2 1.379(6) . ?
B2 F3 1.358(14) . ?
B2 F4 1.382(5) 3 ?
B2 F4 1.382(5) . ?
B2 F4 1.382(5) 2 ?
B3 F7 1.309(14) . ?
B3 F5 1.347(12) . ?
B3 F6 1.362(12) . ?
B3 F8 1.447(14) . ?
F5 F6 1.703(17) 3 ?
F6 F5 1.703(17) 2 ?
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
N7 H7N N3 0.88 1.88 2.748(2) 169.6 .
