Chiral diethyl-EDT-TTF and tetraethyl-BEDT-TTF: synthesis, structural characterization, radical cation salt and charge transfer complexes
Mroweh, Nabil; Cauchy, Thomas; Vanthuyne, Nicolas; Avarvari, Narcis; CrystEngComm  (2022) –; doi:10.1039/D2CE00857B

data_7245324
_publ_section_title
;
 Chiral diethyl-EDT-TTF and tetraethyl-BEDT-TTF: synthesis, structural
 characterization, radical cation salt and charge transfer complexes
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00857B
_journal_year                    2022
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C12 H14 S6, F6 P'
_chemical_formula_sum            'C12 H14 F6 P S6'
_chemical_formula_weight         495.56
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-04-14T15:10:36-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2022-08-02 deposited with the CCDC.	2022-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                68.670(10)
_cell_angle_beta                 88.608(8)
_cell_angle_gamma                87.047(8)
_cell_formula_units_Z            4
_cell_length_a                   8.1638(4)
_cell_length_b                   15.558(3)
_cell_length_c                   16.203(3)
_cell_measurement_reflns_used    6081
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.011
_cell_measurement_theta_min      3.628
_cell_volume                     1914.4(5)
_computing_cell_refinement       'Dirax (Duisenberg, 1992)'
_computing_data_collection       'Collect (Hooft, 2008)'
_computing_data_reduction        'EvalCCD (Duisenberg et al., 2000)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, V2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30103
_diffrn_reflns_point_group_measured_fraction_full 0.789
_diffrn_reflns_point_group_measured_fraction_max 0.789
_diffrn_reflns_theta_full        27.011
_diffrn_reflns_theta_max         27.011
_diffrn_reflns_theta_min         3.628
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 '(SADABS (Sheldrick, Bruker, 2008))'
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_description       plate
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 3131 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     922
_refine_ls_number_reflns         13201
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+2.2050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.102
_refine_ls_wR_factor_ref         0.1157
_reflns_Friedel_coverage         0.589
_reflns_Friedel_fraction_full    0.585
_reflns_Friedel_fraction_max     0.585
_reflns_number_gt                9280
_reflns_number_total             13201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00857b3.cif
_cod_data_source_block           sad
_cod_database_code               7245324
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              49346