Silicon Spiro Double Helicene-like Compounds Based on Dithieno[2,3-b:3',2'-d]thiophene: Syntheses and Crystal Structures.
Li, Chunli; Wu, Longlong; Xu, Wan; Song, Jinsheng; Shi, Jianwu; Yu, Panpan; Kan, Yuhe; Wang, Hua; The Journal of organic chemistry 80 (2015) 11156–11161; doi:10.1021/acs.joc.5b01910

data_4031713
_publ_section_title
;
 Silicon Spiro Double Helicene-like Compounds Based on
 Dithieno[2,3-b:3',2'-d]thiophene: Syntheses and Crystal Structures.
;
_journal_issue                   21
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              11156
_journal_page_last               11161
_journal_paper_doi               10.1021/acs.joc.5b01910
_journal_volume                  80
_journal_year                    2015
_chemical_formula_sum            'C46.5 H42.5 Cl7.5 S14 Si5'
_chemical_formula_weight         1456.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.949(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.032(3)
_cell_length_b                   29.029(5)
_cell_length_c                   21.783(3)
_cell_measurement_reflns_used    6485
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.41
_cell_measurement_theta_min      2.17
_cell_volume                     13268(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0906
_diffrn_reflns_av_sigmaI/netI    0.1210
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            67500
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.883
_exptl_absorpt_correction_T_max  0.9408
_exptl_absorpt_correction_T_min  0.6665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5944
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1315
_refine_ls_number_reflns         23325
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.2095
_refine_ls_R_factor_gt           0.0925
_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^)+(0.0300P)^2^+60.2136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1852
_refine_ls_wR_factor_ref         0.2344
_reflns_number_gt                9544
_reflns_number_total             23325
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo5b01910_si_004.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4031713--4031715.cif.
;
_cod_original_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               4031713