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_7213375
_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            'C18 H18 O4'
_chemical_formula_weight         298.32
_chemical_melting_point          503.15
_chemical_name_systematic
; 
 2,2'-diphenyl-2,2'-bis(1,3-dioxolanyl)  
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.023(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.0592(3)
_cell_length_b                   6.9442(4)
_cell_length_c                   17.666(1)
_cell_measurement_reflns_used    2739
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.97
_cell_measurement_theta_min      2.31
_cell_volume                     741.49(7)
_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      296(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  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            4412
_diffrn_reflns_theta_max         28.97
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.9778
_exptl_absorpt_correction_T_min  0.7594
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'long thin plates cut'
_exptl_crystal_F_000             316
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.156
_refine_diff_density_rms         0.031
_refine_ls_extinction_coef       0.0075(38)
_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   1.059
_refine_ls_goodness_of_fit_obs   1.123
_refine_ls_hydrogen_treatment
;
riding models
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_restrained_S_obs      1.123
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_obs          0.0389
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.1433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1021
_refine_ls_wR_factor_obs         0.0956
_reflns_number_observed          1415
_reflns_number_total             1789
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b003961fsup1.cif
_cod_data_source_block           2,2'-diphenyl-2,2'-bis(1,3-dioxolanyl)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '230.0oC' was changed to '503.15' -
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^)+(0.0425P)^2^+0.1433P] 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^)+(0.0425P)^2^+0.1433P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        741.50(7)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7213375