Crystal growth and characterization of solvated organic charge-transfer complexes built on TTF and 9-dicyanomethylenefluorene derivatives
Salmerón-Valverde, Amparo; Bernès, Sylvain; CrystEngComm 17 (2015) 6227–; doi:10.1039/C5CE01059D

data_7221126
_publ_section_title
;
 Crystal growth and characterization of solvated organic charge-transfer
 complexes built on TTF and 9-dicyanomethylenefluorene derivatives
;
_journal_issue                   32
_journal_name_full               CrystEngComm
_journal_page_first              6227
_journal_paper_doi               10.1039/C5CE01059D
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C16 H5 N5 O6, C6 H4 S4, 0.5(C3 H6 O)'
_chemical_formula_sum            'C23.5 H12 N5 O6.5 S4'
_chemical_formula_weight         596.62
_chemical_melting_point          499
_chemical_name_systematic
'Tetrathiafulvalene 9-dicyanomethylene-2,4,7-trinitrofluorene acetone hemisolvate'
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-06
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-03-23 deposited with the CCDC.
2015-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.1682(15)
_cell_length_b                   19.902(6)
_cell_length_c                   37.805(9)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      11.95
_cell_measurement_theta_min      3.83
_cell_volume                     5393(2)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics
;
SHELXTL-Plus (Siemens, 1996) and MERCURY (Macrae et al., 2008)
;
_computing_publication_material  SHELXL-2014/7
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         X-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1049
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            8389
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        22.534
_diffrn_reflns_theta_max         22.534
_diffrn_reflns_theta_min         2.047
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30
_diffrn_source_power             1.5
_diffrn_source_type              FN4
_diffrn_source_voltage           50
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.403
_exptl_absorpt_correction_T_max  0.24470
_exptl_absorpt_correction_T_min  0.21349
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   ' XSCANS (Siemens, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       plate
_exptl_crystal_F_000             2432
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetone'
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.00053(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     399
_refine_ls_number_reflns         3545
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0787P)^2^+0.8174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1848
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1984
_reflns_number_total             3545
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01059d2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7221123--7221128.cif.'
_cod_original_formula_sum        'C23.50 H12 N5 O6.50 S4'
_cod_database_code               7221126
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              52580