Redetermination of tetramethyl tetrathiafulvalene-2,3,6,7-tetracarboxylate
Katzsch, Felix; Weber, Edwin; Acta Crystallographica Section E 68 (2012) o2354–o2355; doi:10.1107/S1600536812029534

data_2235867
_publ_section_title
;
 Redetermination of tetramethyl
 tetrathiafulvalene-2,3,6,7-tetracarboxylate
;
_journal_coeditor_code           IM2387
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2354
_journal_page_last               o2355
_journal_paper_doi               10.1107/S1600536812029534
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C14 H12 O8 S4'
_chemical_formula_moiety         'C14 H12 O8 S4'
_chemical_formula_sum            'C14 H12 O8 S4'
_chemical_formula_weight         436.48
_chemical_name_systematic
;
Tetramethyl tetrathiafulvalene-2,3,6,7-tetracarboxylate
;
_space_group_IT_number           2
_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                100.2210(10)
_cell_angle_beta                 99.2550(10)
_cell_angle_gamma                99.3280(10)
_cell_formula_units_Z            1
_cell_length_a                   6.8666(2)
_cell_length_b                   7.8783(2)
_cell_length_c                   8.4335(2)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      45.31
_cell_measurement_theta_min      2.50
_cell_volume                     434.53(2)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'phi and omega 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  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0120
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10884
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    0.588
_exptl_absorpt_correction_T_max  0.9169
_exptl_absorpt_correction_T_min  0.7046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             224
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+0.2220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0540
_refine_ls_wR_factor_ref         0.0545
_reflns_number_gt                1471
_reflns_number_total             1534
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            im2387.cif
_cod_data_source_block           I
_cod_database_code               2235867
_cod_database_fobs_code          2235867