#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:24:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179326 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/23/4322307.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_4322307
loop_
_publ_author_name
'Mohammed Fettouhi'
'Mohammed Morsy'
'Abdel Waheed'
'Stéphane Golhen'
'Lahcène Ouahab'
'Jean-Pascal Sutter'
'Olivier Kahn'
'Nieves Menendez'
'François Varret'
_publ_section_title
;
 Spin-Crossover in the Complex Bis(cis-1,2-dicyano-1,2-ethylenedithiolato)
 [2-(p-pyridyl)-4,4,5,5-tetramethylimidazolinium]iron(III)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4910
_journal_page_last               4912
_journal_paper_doi               10.1021/ic990299q
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C26 H32 Fe N9 O2 S4'
_chemical_formula_weight         686.70
_chemical_name_systematic
; 
 ? 
;
_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                 100.04(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.755(16)
_cell_length_b                   13.620(4)
_cell_length_c                   13.832(17)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.312
_cell_measurement_theta_min      5.976
_cell_volume                     3294(5)
_computing_cell_refinement       'Enraf Nonius CAD4'
_computing_data_collection       'Enraf Noinius CAD4'
_computing_data_reduction        MolEN
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.481
_diffrn_measured_fraction_theta_max 0.481
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       θ-2θ
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.1190
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4917
_diffrn_reflns_theta_full        29.90
_diffrn_reflns_theta_max         29.90
_diffrn_reflns_theta_min         1.90
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  0.999993
_exptl_absorpt_correction_T_min  0.957889
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         4766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1785
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0502P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1288
_reflns_number_gt                2182
_reflns_number_total             4766
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990299q.cif
_cod_data_source_block           990299Q
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Psi scan' changed to
'psi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.0000P] 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^)+(0.0502P)^2^+0.0000P] 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        3293(5)
_cod_database_code               4322307
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.08623(5) 0.2500 0.03686(19) Uani 1 d S . .
S1 S -0.03989(5) 0.11911(6) 0.09100(6) 0.0467(2) Uani 1 d . . .
S2 S -0.11916(5) 0.10945(7) 0.27708(7) 0.0506(2) Uani 1 d . . .
C7 C 0.0000 -0.2780(3) 0.2500 0.0366(10) Uani 1 d S . .
N4 N -0.03894(16) -0.44052(19) 0.1807(2) 0.0515(8) Uani 1 d . . .
H4 H -0.0697 -0.4156 0.1288 0.062 Uiso 1 calc R . .
C6 C 0.0326(2) -0.2270(2) 0.1828(3) 0.0510(9) Uani 1 d . . .
H6 H 0.0550 -0.2598 0.1361 0.061 Uiso 1 calc R . .
C5 C 0.0315(2) -0.1255(2) 0.1858(3) 0.0494(9) Uani 1 d . . .
H5 H 0.0540 -0.0911 0.1402 0.059 Uiso 1 calc R . .
N3 N 0.0000 -0.0747(2) 0.2500 0.0341(8) Uani 1 d S . .
C10 C 0.0143(3) -0.5859(4) 0.1173(3) 0.1082(19) Uani 1 d . . .
H10A H -0.0179 -0.5769 0.0546 0.162 Uiso 1 calc R . .
H10B H 0.0250 -0.6546 0.1279 0.162 Uiso 1 calc R . .
H10C H 0.0615 -0.5509 0.1186 0.162 Uiso 1 calc R . .
C11 C -0.1016(3) -0.5973(4) 0.1914(4) 0.117(2) Uani 1 d . . .
H11A H -0.1303 -0.5670 0.2360 0.176 Uiso 1 calc R . .
H11B H -0.0933 -0.6653 0.2083 0.176 Uiso 1 calc R . .
H11C H -0.1295 -0.5921 0.1256 0.176 Uiso 1 calc R . .
C8 C 0.0000 -0.3877(3) 0.2500 0.0381(10) Uani 1 d S . .
N1 N -0.3194(2) 0.1188(3) 0.1485(3) 0.0921(13) Uani 1 d . . .
C2 C -0.13951(19) 0.1259(2) 0.0803(2) 0.0445(8) Uani 1 d . . .
C1 C -0.17334(19) 0.1198(2) 0.1605(3) 0.0452(8) Uani 1 d . . .
N2 N -0.2133(2) 0.1399(3) -0.0960(3) 0.0886(12) Uani 1 d . . .
C4 C -0.1821(2) 0.1346(3) -0.0171(3) 0.0603(10) Uani 1 d . . .
C9 C -0.0262(2) -0.5467(2) 0.1979(3) 0.0497(9) Uani 1 d . . .
C3 C -0.2544(2) 0.1212(3) 0.1525(3) 0.0606(10) Uani 1 d . . .
O1 O 0.35236(18) -0.1218(2) 0.5273(2) 0.0855(10) Uani 1 d . . .
N6 N 0.23101(18) -0.1337(2) 0.4468(2) 0.0605(9) Uani 1 d . . .
C13 C 0.2463(3) -0.1628(4) 0.3547(3) 0.0956(16) Uani 1 d . . .
H13A H 0.2362 -0.1090 0.3094 0.143 Uiso 1 calc R . .
H13B H 0.2140 -0.2172 0.3307 0.143 Uiso 1 calc R . .
H13C H 0.2989 -0.1819 0.3609 0.143 Uiso 1 calc R . .
C12 C 0.2843(3) -0.1130(3) 0.5242(3) 0.0767(13) Uani 1 d . . .
H12 H 0.2679 -0.0901 0.5804 0.092 Uiso 1 calc R . .
C14 C 0.1519(3) -0.1257(3) 0.4577(4) 0.0855(14) Uani 1 d . . .
H14A H 0.1490 -0.1017 0.5222 0.128 Uiso 1 calc R . .
H14B H 0.1280 -0.1891 0.4486 0.128 Uiso 1 calc R . .
H14C H 0.1259 -0.0809 0.4095 0.128 Uiso 1 calc R . .
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'
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'
S S 0.1246 0.1234 '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'
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
N3 Fe1 S2 98.14(3) . 2 ?
N3 Fe1 S2 98.14(3) . . ?
S2 Fe1 S2 163.73(6) 2 . ?
N3 Fe1 S1 101.56(3) . 2 ?
S2 Fe1 S1 89.42(7) 2 2 ?
S2 Fe1 S1 87.33(7) . 2 ?
N3 Fe1 S1 101.56(3) . . ?
S2 Fe1 S1 87.33(7) 2 . ?
S2 Fe1 S1 89.42(7) . . ?
S1 Fe1 S1 156.88(6) 2 . ?
C2 S1 Fe1 103.64(13) . . ?
C1 S2 Fe1 104.11(14) . . ?
C6 C7 C6 118.9(4) 2 . ?
C6 C7 C8 120.6(2) 2 . ?
C6 C7 C8 120.6(2) . . ?
C8 N4 C9 112.1(3) . . ?
C7 C6 C5 118.5(3) . . ?
N3 C5 C6 123.5(3) . . ?
C5 N3 C5 117.0(4) . 2 ?
C5 N3 Fe1 121.52(19) . . ?
C5 N3 Fe1 121.52(19) 2 . ?
N4 C8 N4 112.7(4) . 2 ?
N4 C8 C7 123.7(2) . . ?
N4 C8 C7 123.7(2) 2 . ?
C1 C2 C4 122.7(3) . . ?
C1 C2 S1 120.9(3) . . ?
C4 C2 S1 116.4(3) . . ?
C2 C1 C3 121.5(3) . . ?
C2 C1 S2 120.9(3) . . ?
C3 C1 S2 117.6(3) . . ?
N2 C4 C2 177.0(5) . . ?
N4 C9 C11 109.4(3) . . ?
N4 C9 C10 107.6(3) . . ?
C11 C9 C10 109.0(4) . . ?
N4 C9 C9 101.39(17) . 2 ?
C11 C9 C9 115.9(4) . 2 ?
C10 C9 C9 112.9(4) . 2 ?
N1 C3 C1 177.1(4) . . ?
C12 N6 C13 124.5(4) . . ?
C12 N6 C14 118.0(4) . . ?
C13 N6 C14 117.5(4) . . ?
O1 C12 N6 125.1(5) . . ?
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 N3 2.192(3) . ?
Fe1 S2 2.234(2) 2 ?
Fe1 S2 2.234(2) . ?
Fe1 S1 2.235(3) 2 ?
Fe1 S1 2.235(3) . ?
S1 C2 1.752(4) . ?
S2 C1 1.733(4) . ?
C7 C6 1.367(4) 2 ?
C7 C6 1.367(4) . ?
C7 C8 1.494(6) . ?
N4 C8 1.297(3) . ?
N4 C9 1.477(4) . ?
C6 C5 1.382(4) . ?
C5 N3 1.324(4) . ?
N3 C5 1.324(4) 2 ?
C10 C9 1.526(6) . ?
C11 C9 1.493(5) . ?
C8 N4 1.297(3) 2 ?
N1 C3 1.146(5) . ?
C2 C1 1.353(5) . ?
C2 C4 1.431(5) . ?
C1 C3 1.424(5) . ?
N2 C4 1.136(5) . ?
C9 C9 1.573(7) 2 ?
O1 C12 1.207(5) . ?
N6 C12 1.330(5) . ?
N6 C13 1.405(5) . ?
N6 C14 1.443(5) . ?
