Rotational isomerism and crystal structures of 2,2′-diphenyl-2,2′-bi-1,3-dithianyl and 2,2′-diphenyl-2,2′-bi-1,3-dioxolanyl †
Lam, Yulin; Wah Wong, Ming; Huang, Hsing-Hua; Liang, Eping; Journal of the Chemical Society, Perkin Transactions 2  (2000) 2090–; doi:10.1039/b003961f

data_7213374
_publ_section_title
;
 Rotational isomerism and crystal structures of
 2,2&#x2032;-diphenyl-2,2&#x2032;-bi-1,3-dithianyl and
 2,2&#x2032;-diphenyl-2,2&#x2032;-bi-1,3-dioxolanyl&#x200A;&#x2020;
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              2090
_journal_paper_doi               10.1039/b003961f
_journal_year                    2000
_chemical_compound_source        'see text'
_chemical_formula_sum            'C20 H22 S4'
_chemical_formula_weight         390.62
_chemical_melting_point          478.15
_chemical_name_systematic
; 
 2,2'-diphenyl-2,2'-bis(1,3-dithianyl) 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 101.341(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4890(3)
_cell_length_b                   7.7878(1)
_cell_length_c                   15.7930(3)
_cell_measurement_reflns_used    6739
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.30
_cell_measurement_theta_min      2.63
_cell_volume                     1867.84(6)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1996)'
_computing_publication_material  'SHELXTL (Siemens, 1996)'
_computing_structure_refinement  'SHELXTL (Siemens, 1996)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens SMART CCD System'
_diffrn_measurement_method       'frames \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  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11341
_diffrn_reflns_theta_max         29.30
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  0.9111
_exptl_absorpt_correction_T_min  0.7940
_exptl_absorpt_correction_type   'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'hexagonal blocks'
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.0020(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.045
_refine_ls_goodness_of_fit_obs   1.089
_refine_ls_hydrogen_treatment
; 
riding models
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_restrained_S_obs      1.089
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_obs          0.0484
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+1.9758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1153
_refine_ls_wR_factor_obs         0.1079
_reflns_number_observed          3713
_reflns_number_total             4566
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b003961fsup1.cif
_cod_data_source_block           2,2'-diphenyl-2,2'-bis(1,3-dithianyl)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '205.0oC' was changed to '478.15' -
it was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+1.9758P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+1.9758P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7213374