3,4-[2,2-Bis(methoxyethoxymethoxymethyl)propylenedithio]-3',4'-(ethylenedithio)tetrathiafulvalene: a spiro-substituted BEDT–TTF analogue
Brooks, Andrew C.; Day, Peter; Wallis, John D.; Acta Crystallographica Section C 64 (2008) o245–o247; doi:10.1107/S0108270108005933

data_2016622
_publ_section_title
;3,4-[2,2-Bis(methoxyethoxymethoxymethyl)propylenedithio]-3',4'-(ethylenedithio)tetrathiafulvalene:
 a spiro-substituted BEDT--TTF analogue
;
_journal_coeditor_code           SU3017
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o245
_journal_page_last               o247
_journal_paper_doi               10.1107/S0108270108005933
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C21 H30 O6 S8'
_chemical_formula_moiety         'C21 H30 O6 S8'
_chemical_formula_sum            'C21 H30 O6 S8'
_chemical_formula_weight         634.93
_chemical_melting_point          .356E-305
_chemical_name_common
;
3,4-[2,2-Bis(methoxyethoxymethoxymethyl)propylenedithio]-
3',4'-(ethylenedithio)tetrathiafulvalene
;
_chemical_name_systematic
;
2-(1,3-dithiolo[4,5-b][1,4]dithiin-2-ylidene)-6,6-
bis(methoxyethoxymethoxymethyl)-1,3-dithiolo[4,5-b][1,4]dithiepine
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.9050(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.8227(10)
_cell_length_b                   19.7775(4)
_cell_length_c                   20.3661(4)
_cell_measurement_reflns_used    6442
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.9
_cell_volume                     2738.1(4)
_computing_cell_refinement
;
DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)
;
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction
;
DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)
;
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            45147
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.2
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         6272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0191P)^2^+1.4275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0634
_reflns_number_gt                5278
_reflns_number_total             6272
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su3017.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2016622
_cod_database_fobs_code          2016622