Mixed-Valence, Layered, Cation Radical Salts of the Ethane-Bridged Dimeric Tetrathiafulvalene [(EDT-TTF‒CH~2^‒^~)~2~^•+^][X^-^][THF]~0.5~, X^-^ = FeCl~4~^-^, GaCl~4~^-^
Mézière, Cécile; Fourmigué, Marc; Canadell, Enric; Clérac, Rodolphe; Bechgaard, Klaus; Auban-Senzier, Pascale; Chemistry of Materials 12 (2000) 2250–2256; doi:10.1021/cm0001511

data_4000022
_publ_section_title
;
 Mixed-Valence, Layered, Cation Radical Salts of the Ethane-Bridged Dimeric
 Tetrathiafulvalene [(EDT-TTF--CH~2^--^~)~2~^&#x2022;+^][X^-^][THF]~0.5~,
 X^-^ = FeCl~4~^-^, GaCl~4~^-^
;
_journal_coden_ASTM              CMATEX
_journal_issue                   8
_journal_name_full               'Chemistry of Materials'
_journal_page_first              2250
_journal_page_last               2256
_journal_paper_doi               10.1021/cm0001511
_journal_volume                  12
_journal_year                    2000
_chemical_formula_moiety         C18H14S12,FeCl4,0.5(C4H8O)
_chemical_formula_sum            'C20 H18 Cl4 Fe O0.5 S12'
_chemical_formula_weight         848.71
_chemical_name_common            'Bis(EDT-TTF)ethane,FeCl4,0.5 THF'
_chemical_name_systematic
;
1,2-Bis(ethylenedithiotetrathiafulvalene)ethane cation, tetrachloroferrate, THF solvate
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.644(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.5030(14)
_cell_length_b                   13.9152(14)
_cell_length_c                   31.148(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.8
_cell_measurement_theta_min      2.1
_cell_volume                     6285.6(10)
_computing_cell_refinement       'SELECT [Stoe IPDS]'
_computing_data_collection       'EXPOSE [Stoe IPDS]'
_computing_data_reduction        'INTEGRATE [Stoe IPDS]'
_computing_molecular_graphics    'ORTEP [Johnson, 1976]'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'rotation, Df = 0.8&#x00A1;'
_diffrn_radiation_detector       'area detector'
_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  0.1522
_diffrn_reflns_av_sigmaI/netI    0.2387
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            17155
_diffrn_reflns_theta_max         23.96
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.635
_exptl_absorpt_correction_T_max  0.9720
_exptl_absorpt_correction_T_min  0.7733
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT, Stoe-IPDS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'parallelepipedic plate'
_exptl_crystal_F_000             3424
_exptl_crystal_size_max          0.086
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.008
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.686
_refine_ls_goodness_of_fit_obs   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.719
_refine_ls_restrained_S_obs      0.962
_refine_ls_R_factor_all          0.2077
_refine_ls_R_factor_obs          0.0458
_refine_ls_shift/esd_max         0.014
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0070P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0728
_refine_ls_wR_factor_obs         0.0489
_reflns_number_observed          1414
_reflns_number_total             4811
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            cm0001511.cif
_cod_data_source_block           monofac
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0070P)^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^)+(0.0070P)^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_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C20 H18 Cl4 Fe O0.50 S12'
_cod_database_code               4000022