A binaphthol-substituted tetrathiafulvalene with axial chirality and its enantiopure TCNQF4 charge-transfer salts
Saad, Ali; Jeannin, Olivier; Fourmigué, Marc; New Journal of Chemistry 35 (2011) 1004–; doi:10.1039/c1nj20034h

data_7052632
_publ_section_title
;
 A binaphthol-substituted tetrathiafulvalene with axial chirality and
 its enantiopure TCNQF4 charge-transfer salts
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1004
_journal_paper_doi               10.1039/c1nj20034h
_journal_volume                  35
_journal_year                    2011
_chemical_formula_moiety         'C30 H20 O2 S6, C12 F4 N4, C H2 Cl2'
_chemical_formula_sum            'C43 H22 Cl2 F4 N4 O2 S6'
_chemical_formula_weight         965.91
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.5700(10)
_cell_angle_beta                 90.8370(10)
_cell_angle_gamma                92.7430(10)
_cell_formula_units_Z            2
_cell_length_a                   8.5380(2)
_cell_length_b                   12.9927(3)
_cell_length_c                   18.7805(5)
_cell_measurement_reflns_used    8962
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.81
_cell_measurement_theta_min      2.26
_cell_volume                     1993.68(9)
_computing_cell_refinement       'Bruker SMART, 2006'
_computing_data_collection       'Bruker SMART, 2006'
_computing_data_reduction        'Bruker SAINT, 2006'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26784
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.13
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.157
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1137
_refine_ls_number_reflns         13579
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1243P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.1760
_reflns_number_gt                11819
_reflns_number_total             13579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1nj20034h.txt
_cod_data_source_block           -R--1-TCNQF4
_cod_original_cell_volume        1993.68(8)
_cod_original_sg_symbol_Hall     P1
_cod_original_sg_symbol_H-M      P1
_cod_database_code               7052632