Synthesis and Structure of m-Terphenyl Thio-, Seleno-, and Telluroethers
Uzma I. Zakai; Anna Błoch-Mechkour; Neil E. Jacobsen; Leif Abrell; Guangxin Lin; Gary S. Nichol; Thomas Bally; Richard S. Glass; Journal of Organic Chemistry 75 (2010) 8363–8371; doi:10.1021/jo101299x

data_4025859
_publ_section_title
;
 Synthesis and Structure of m-Terphenyl Thio-, Seleno-, and Telluroethers
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8363
_journal_page_last               8371
_journal_paper_doi               10.1021/jo101299x
_journal_volume                  75
_journal_year                    2010
_chemical_formula_moiety         'C21 H20 O2 S'
_chemical_formula_sum            'C21 H20 O2 S'
_chemical_formula_weight         336.43
_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                 111.354(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.805(5)
_cell_length_b                   7.535(2)
_cell_length_c                   14.901(5)
_cell_measurement_reflns_used    2978
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      2.60
_cell_volume                     1757.3(9)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10573
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.60
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_T_max  0.9726
_exptl_absorpt_correction_T_min  0.9119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 2006'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.0016(4)
_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_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         2969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0154P)^2^+1.4642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0947
_reflns_number_gt                1972
_reflns_number_total             2969
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo101299x_si_001.cif
_cod_data_source_block           rsg105
_cod_original_cell_volume        1757.2(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4025859