Facile synthesis of 2,5-bis(silyl)selenophene-1,1-dioxide and its photophysical properties
Masuda, Toshiyuki; Inagaki, Yusuke; Momma, Hiroyuki; Kwon, Eunsang; Setaka, Wataru; New J. Chem. 40 (2016) 8593–; doi:10.1039/C6NJ01886F

data_7055729
_publ_section_title
;
 Facile synthesis of 2,5-bis(silyl)selenophene-1,1-dioxide and its
 photophysical properties
;
_journal_issue                   10
_journal_name_full               'New J. Chem.'
_journal_page_first              8593
_journal_paper_doi               10.1039/C6NJ01886F
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C10 H20 Se Si2'
_chemical_formula_sum            'C10 H20 Se Si2'
_chemical_formula_weight         275.40
_chemical_melting_point          325.1(10)
_chemical_name_common            1,4-bisTMSselenophene
_chemical_name_systematic        1,4-bisTMSselenophene
_space_group_IT_number           59
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      59
_symmetry_space_group_name_Hall  '-P 2ab 2a'
_symmetry_space_group_name_H-M   'P m m n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc1lfjm5
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-04-07 deposited with the CCDC.
2016-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.
_cell_angle_beta                 90.
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   14.666(4)
_cell_length_b                   14.776(4)
_cell_length_c                   6.4741(16)
_cell_measurement_reflns_used    3416
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.88
_cell_measurement_theta_min      2.76
_cell_volume                     1403.0(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker SMART-APEX CCD'
_diffrn_measurement_method       'phi and omega 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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6412
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.89
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    2.810
_exptl_absorpt_correction_T_max  0.7664
_exptl_absorpt_correction_T_min  0.3994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             568
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0238
_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^)+(0.0319P)^2^+0.5938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0600
_reflns_number_gt                1408
_reflns_number_total             1550
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6nj01886f2.cif
_cod_data_source_block           TMS2Seleno100K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '51-53 deg.C' was changed to
'325.1(10)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7055728--7055729.cif.
;
_cod_original_sg_symbol_H-M      Pmmn
_cod_database_code               7055729
_solvent_exptl_crystal_recrystallization_method EtOH