Synthesis for the Mesomer and Racemate of Thiophene-Based Double Helicene under Irradiation
Xinming Liu; Panpan Yu; Li Xu; Juanjuan Yang; Jianwu Shi; Zhihua Wang; Yanxiang Cheng; Hua Wang; Journal of Organic Chemistry 78 (2013) 6316–6321; doi:10.1021/jo400691s

data_4028340
_publ_section_title
;
 Synthesis for the Mesomer and Racemate of Thiophene-Based Double Helicene
 under Irradiation
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6316
_journal_page_last               6321
_journal_paper_doi               10.1021/jo400691s
_journal_volume                  78
_journal_year                    2013
_chemical_formula_sum            'C46 H40 S12 Si4'
_chemical_formula_weight         1089.86
_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                98.69(3)
_cell_angle_beta                 100.69(3)
_cell_angle_gamma                99.92(3)
_cell_formula_units_Z            2
_cell_length_a                   10.348(9)
_cell_length_b                   14.739(7)
_cell_length_c                   18.510(7)
_cell_measurement_reflns_used    1170
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.67
_cell_measurement_theta_min      2.43
_cell_volume                     2683(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0672
_diffrn_reflns_av_sigmaI/netI    0.1909
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14660
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_T_max  0.9088
_exptl_absorpt_correction_T_min  0.8725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         10354
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.1988
_refine_ls_R_factor_gt           0.0825
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0161P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1570
_refine_ls_wR_factor_ref         0.1985
_reflns_number_gt                4257
_reflns_number_total             10354
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo400691s_si_001.cif
_cod_data_source_block           a
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4028340