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_7055728
_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_compound_source        no
_chemical_formula_moiety         'C10 H20 O2 Se Si2'
_chemical_formula_sum            'C10 H20 O2 Se Si2'
_chemical_formula_weight         307.40
_chemical_name_common            bis(TMS)selenophenedioxide
_chemical_name_systematic        bis(TMS)selenophenedioxide
_chemical_properties_physical    ', Heat-sensitive,Photo-sensitive'
_chemical_temperature_decomposition 469.15
_space_group_crystal_system      tetragonal
_space_group_IT_number           81
_space_group_name_Hall           'P -4'
_space_group_name_H-M_alt        'P -4'
_symmetry_space_group_name_Hall  'P -4'
_symmetry_space_group_name_H-M   'P -4'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1lfjl4
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-08-17 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            2
_cell_length_a                   11.0742(16)
_cell_length_b                   11.0742(16)
_cell_length_c                   6.4127(9)
_cell_measurement_reflns_used    4115
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      3.18
_cell_volume                     786.44(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker SMART/APEX CCD'
_diffrn_measurement_method       '\f and \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  0.0261
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            4426
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.493
_diffrn_reflns_theta_min         3.177
_exptl_absorpt_coefficient_mu    2.523
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.4532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (bruker)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       plate
_exptl_crystal_F_000             316
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuran'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.24(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         1826
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0240
_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
w={1-exp[-9.0000(sin\q/\l)^2^)]}/[\s^2^(Fo^2^)+1.2676P]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0709
_reflns_Friedel_coverage         0.839
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.949
_reflns_number_gt                1803
_reflns_number_total             1826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj01886f2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been given
as '196 deg.C(decomp)'. The value '196 deg.C(decomp)' was changed to
'469.15' - it was converted from degrees Celsius(C) to Kelvins(K).

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

 Adding full bibliography for 7055728--7055729.cif.
;
_cod_original_cell_volume        786.4(3)
_cod_database_code               7055728
_shelx_estimated_absorpt_t_min   0.518
_shelx_estimated_absorpt_t_max   0.632
_shelxl_version_number           2013-4
_shelx_res_checksum              26836