Two Closely Related Organic Charge-Transfer Complexes Based on Tetrathiafulvalene and 9H-fluorenone Derivatives. Competition between Hydrogen Bonding and Stacking Interactions
Salmerón-Valverde, Amparo; Bernès, Sylvain; Crystals 5 (2015) 283–; doi:10.3390/cryst5030283

data_1529352
_publ_section_title
;
 Two Closely Related Organic Charge-Transfer Complexes Based on
 Tetrathiafulvalene and 9H-fluorenone Derivatives. Competition between
 Hydrogen Bonding and Stacking Interactions
;
_journal_issue                   3
_journal_name_full               Crystals
_journal_page_first              283
_journal_paper_doi               10.3390/cryst5030283
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         'C14 H5 N3 O9, C6 H4 S4'
_chemical_formula_sum            'C20 H9 N3 O9 S4'
_chemical_formula_weight         563.54
_chemical_melting_point          477
_chemical_name_systematic
;
2,2'-bis(1,3-Dithiolylidene) 4,5,7-trinitro-9-fluorenone-2-carboxylic acid
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-07-24
_audit_creation_method           SHELXTL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90.106(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0275(10)
_cell_length_b                   7.8676(13)
_cell_length_c                   34.961(5)
_cell_measurement_reflns_used    61
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      12.44
_cell_measurement_theta_min      4.80
_cell_volume                     2208.0(6)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  SHELXL2014
_computing_structure_refinement  'SHELXL2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_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  0.0257
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            5529
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.005
_diffrn_reflns_theta_min         2.330
_diffrn_source_current           30
_diffrn_source_power             1.5
_diffrn_source_type              FN4
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  0.514
_exptl_absorpt_correction_T_min  0.475
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'XSCANS (Bruker, 1996)'
_exptl_crystal_colour            dark_green
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.0028(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL2014
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     326
_refine_ls_number_reflns         3897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0665P)^2^+1.3679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1458
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2464
_reflns_number_total             3897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ASV_Crystals.cif
_cod_data_source_block           1
_cod_original_cell_volume        2208.0(5)
_cod_database_code               1529352
_shelxl_version_number           2014-3
_shelx_res_checksum              67388
_shelx_hkl_checksum              7872