Hybrid Molecular Materials Based upon Organic π-Electron Donors and Metal Complexes. Radical Salts of Bis(ethylenethia)tetrathiafulvalene (BET-TTF) with the Octahedral Anions Hexacyanoferrate(III) and Nitroprusside. The First Kappa Phase in the BET-TTF Family
Miguel Clemente-León; Eugenio Coronado; José R. Galán-Mascarós; Carlos Giménez-Saiz; Carlos J. Gómez-García; Elisabet Ribera; José Vidal-Gancedo; Concepció Rovira; E. Canadell; Vladimir Laukhin; Inorganic Chemistry 40 (2001) 3526–3533; doi:10.1021/ic001431l

data_4319943
_publ_section_title
;
 Hybrid Molecular Materials Based upon Organic \p-Electron Donors and
 Metal Complexes. Radical Salts of Bis(ethylenethia)tetrathiafulvalene
 (BET-TTF) with the Octahedral Anions Hexacyanoferrate(III) and
 Nitroprusside. The First Kappa Phase in the BET-TTF Family
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3526
_journal_page_last               3533
_journal_paper_doi               10.1021/ic001431l
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C31 H16 Fe0.5 N4 S12'
_chemical_formula_weight         857.12
_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                 90.994(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   38.867(7)
_cell_length_b                   8.438(8)
_cell_length_c                   11.239(6)
_cell_measurement_temperature    293(2)
_cell_volume                     3685(4)
_computing_cell_refinement       'CAD4 Software (Enraf-Nonius, 1988)'
_computing_data_collection       'CAD4 Software (Enraf-Nonius, 1988)'
_computing_data_reduction        'CAD4 Software (Enraf-Nonius, 1988)'
_computing_molecular_graphics    'PLATON (Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       'omega/2Theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.2148
_diffrn_reflns_av_sigmaI/netI    0.1623
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3362
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.88
_diffrn_standards_decay_%        '4.68 %'
_diffrn_standards_interval_count 400
_diffrn_standards_interval_time  '60 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_T_max  0.829
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.0000(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   0.945
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3182
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.2131
_refine_ls_R_factor_gt           0.0754
_refine_ls_shift/su_max          5.166
_refine_ls_shift/su_mean         0.087
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+34.7124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.2202
_reflns_number_gt                1388
_reflns_number_total             3182
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001431l_1.cif
_cod_data_source_block           for_(BET-TTF)4(NEt4)2[Fe(CN)6]
_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 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C31 H16 Fe0.50 N4 S12'
_cod_database_code               4319943