Synthesis and Properties of Conjugated Oligoyne-Centered π-Extended Tetrathiafulvalene Analogues and Related Macromolecular Systems
Guang Chen; Ilias Mahmud; Louise N. Dawe; Lee M. Daniels; Yuming Zhao; Journal of Organic Chemistry 76 (2011) 2701–2715; doi:10.1021/jo2000447

data_4026215
_publ_contact_author_email       yuming@mun.ca
_publ_contact_author_fax         '(709) 737-3471'
_publ_contact_author_name        'Yuming Zhao'
_publ_contact_author_phone       '(709) 737-8747'
_publ_section_title
;
 Synthesis and Properties of Conjugated Oligoyne-Centered \p-Extended
 Tetrathiafulvalene Analogues and Related Macromolecular Systems
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2701
_journal_page_last               2715
_journal_paper_doi               10.1021/jo2000447
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C32 H22 S8, 0.5(C6 H6)'
_chemical_formula_sum            'C35 H25 S8'
_chemical_formula_weight         702.06
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                91.643(11)
_cell_angle_beta                 90.138(14)
_cell_angle_gamma                95.741(10)
_cell_formula_units_Z            2
_cell_length_a                   7.827(4)
_cell_length_b                   8.897(4)
_cell_length_c                   23.452(10)
_cell_measurement_reflns_used    6184
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.7720
_cell_measurement_theta_min      2.4365
_cell_volume                     1624.2(13)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_publication_material  'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite - Rigaku SHINE'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            13568
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.9658
_exptl_absorpt_correction_T_min  0.8963
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(T. Higashi, 2000)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             726
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6576
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0937P)^2^+1.7105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1791
_refine_ls_wR_factor_ref         0.1926
_reflns_number_gt                5567
_reflns_number_total             6576
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo2000447_si_003.cif
_cod_data_source_block           GC443
_cod_database_code               4026215