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_4031714
_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_moiety         'C44 H40 S14 Si5'
_chemical_formula_sum            'C51.3 H47.3 Cl21.9 S14 Si5'
_chemical_formula_weight         2029.44
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           50
_space_group_name_Hall           '-P 2ab 2b'
_space_group_name_H-M_alt        'P b a n :2'
_symmetry_space_group_name_Hall  '-P 2ab 2b'
_symmetry_space_group_name_H-M   'P b a n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-05-15
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.792(5)
_cell_length_b                   13.295(5)
_cell_length_c                   44.329(18)
_cell_measurement_reflns_used    3486
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.36
_cell_measurement_theta_min      2.48
_cell_volume                     6950(5)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
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_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0934
_diffrn_reflns_av_unetI/netI     0.1082
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            30333
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.82
_diffrn_reflns_theta_min         0.92
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1054 before and 0.0880 after correction.
The Ratio of minimum to maximum transmission is 0.7987.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.970
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2043
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.078
_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     144
_refine_ls_number_reflns         5834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1180
_refine_ls_R_factor_gt           0.0877
_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^)+(0.1566P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2543
_refine_ls_wR_factor_ref         0.2685
_reflns_number_gt                3370
_reflns_number_total             5834
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo5b01910_si_003.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_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.

2022-02-21
Space group name changed to comply with IUCR recomendations
                 miguel
;
_cod_original_sg_symbol_H-M   'P b a n :2'
_cod_original_cell_volume        6949(5)
_cod_original_formula_sum        'C51.30 H47.30 Cl21.90 S14 Si5'
_cod_database_code               4031714
_smtbx_masks_special_details
;
 Highly disordered solvent was located in the structures.
 Reflection contributions from this solvent were removed
 using program OLEX2, function MSAKS, which determined
 there to be 857.8 electrons in 4629.2 \%A^3^ removed per unit cell. 
 The disordered chloroform molecules were detected in the 13C NMR spectrum. 
 Thus, the total number of electrons [857.8] in the void per unit cell, 
 equivalent to about 857.8/2 = 428.8 per molecule unit, 
 which is attributed to about 7.3 disordered chloroform molecules.

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