Methyl 2,3-(3,6,9-trioxaundecane-1,11-diyldithio)-1,4,5,8-tetrathiafulvalene-6-carboxylate
Hou, Rui-bin; Li, Bao; Yin, Bing-zhu; Wu, Li-xin; Acta Crystallographica Section E 65 (2009) o1057–; doi:10.1107/S1600536809013154

data_2221630
_publ_section_title
;Methyl
 2,3-(3,6,9-trioxaundecane-1,11-diyldithio)-1,4,5,8-tetrathiafulvalene-6-carboxylate
;
_journal_coeditor_code           CV2536
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1057
_journal_paper_doi               10.1107/S1600536809013154
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C16 H20 O5 S6'
_chemical_formula_moiety         'C16 H20 O5 S6'
_chemical_formula_sum            'C16 H20 O5 S6'
_chemical_formula_weight         484.68
_chemical_name_systematic
;
Methyl 2,3-(3,6,9-trioxaundecane-1,11-diyldithio)-1,4,5,8-
tetrathiafulvalene-6-carboxylate
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.65(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.604(5)
_cell_length_b                   5.2048(10)
_cell_length_c                   17.801(4)
_cell_measurement_reflns_used    7343
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.09
_cell_measurement_theta_min      3.44
_cell_volume                     2094.1(8)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_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  0.1012
_diffrn_reflns_av_sigmaI/netI    0.1315
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9505
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_max  0.9230
_exptl_absorpt_correction_T_min  0.8763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.455
_refine_ls_abs_structure_details 'Flack (1983), 1855 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.12(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4254
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0878P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1720
_reflns_number_gt                3370
_reflns_number_total             4254
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv2536.cif
_cod_data_source_block           I
_cod_original_cell_volume        2094.1(7)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2221630
_cod_database_fobs_code          2221630