A facile synthesis of dithieno[3,2-b:6,7-b]fluorenes via a tandem annulation–reduction
Xiong, Xiaoli; Liu, Qiancai; Zhang, Jun; Zhu, Min; Wang, Yanmei; Deng, Shiming; RSC Advances 3 (2013) 17707–; doi:10.1039/c3ra41927d

data_7239096
_publ_section_title
;
 A facile synthesis of dithieno[3,2-b:6,7-b]fluorenes via a tandem
 annulation--reduction
;
_journal_issue                   39
_journal_name_full               'RSC Advances'
_journal_page_first              17707
_journal_paper_doi               10.1039/c3ra41927d
_journal_volume                  3
_journal_year                    2013
_chemical_formula_sum            'C27 H30 S2'
_chemical_formula_weight         418.63
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                67.639(3)
_cell_angle_beta                 84.037(4)
_cell_angle_gamma                81.169(4)
_cell_formula_units_Z            2
_cell_length_a                   7.6535(9)
_cell_length_b                   11.5648(14)
_cell_length_c                   13.8466(17)
_cell_measurement_temperature    296(2)
_cell_volume                     1118.6(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13113
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.249
_exptl_absorpt_correction_T_max  0.9472
_exptl_absorpt_correction_T_min  0.9157
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.137
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0498P)^2^+0.2675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.1006
_reflns_number_gt                3127
_reflns_number_total             3920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra41927d.txt
_cod_data_source_block           z
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               7239096