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_4000023
_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         'C18 H14 S12, GaCl4, (C4H8O)0.5'
_chemical_formula_sum            'C20 H18 Cl4 Ga O0.5 S12'
_chemical_formula_weight         862.58
_chemical_name_common            'Bis(EDT)ethane, GaCl4, 0.5 THF'
_chemical_name_systematic
;
1,2-bis(ethylenedithiotetrathiafulvalenyl)ethane, tetrachlorogallate,
1/2 tetrahydrofurane
;
_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                 90.804(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.5016(14)
_cell_length_b                   13.9153(14)
_cell_length_c                   31.139(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      2
_cell_volume                     6283.0(11)
_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_measurement_device       'area detector'
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'rotation, phi incr. 0.8&#x00A1;'
_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  0.0780
_diffrn_reflns_av_sigmaI/netI    0.0649
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            24222
_diffrn_reflns_theta_max         23.92
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.031
_exptl_absorpt_correction_T_max  0.9249
_exptl_absorpt_correction_T_min  0.5789
_exptl_absorpt_correction_type   'numerical [FACEIT, Stoe-IPDS]'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             3464
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.933
_refine_ls_goodness_of_fit_obs   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_restrained_S_obs      1.084
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_obs          0.0479
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1138
_refine_ls_wR_factor_obs         0.1006
_reflns_number_observed          2868
_reflns_number_total             4630
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            cm0001511.cif
_cod_data_source_block           cp102mono
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0579P)^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^)+(0.0579P)^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 Ga O0.50 S12'
_cod_database_code               4000023