1,1,4,4-Tetra-<i>tert</i>-butyl-1,4-dichloro-2,2,3,3-tetraphenyltetrasilane
Otsuka, Kyohei; Ishida, Shintaro; Kyushin, Soichiro; Acta Crystallographica Section E 68 (2012) o424–; doi:10.1107/S1600536812000669

data_2233523
_publ_section_title
;
 1,1,4,4-Tetra-<i>tert</i>-butyl-1,4-dichloro-2,2,3,3-tetraphenyltetrasilane
;
_journal_coeditor_code           IS5036
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o424
_journal_paper_doi               10.1107/S1600536812000669
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C40 H56 Cl2 Si4'
_chemical_formula_moiety         'C40 H56 Cl2 Si4'
_chemical_formula_sum            'C40 H56 Cl2 Si4'
_chemical_formula_weight         720.11
_chemical_melting_point_gt       517
_chemical_melting_point_lt       520
_chemical_name_systematic
;
1,1,4,4-Tetra-<i>tert</i>-butyl-1,4-dichloro-2,2,3,3-tetraphenyltetrasilane
;
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 105.7717(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   9.6981(8)
_cell_length_b                   15.3893(11)
_cell_length_c                   13.8546(11)
_cell_measurement_reflns_used    9597
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.2812
_cell_measurement_theta_min      1.3231
_cell_volume                     1989.9(3)
_computing_cell_refinement       '<i>CrystalClear</i> (Rigaku, 2003)'
_computing_data_collection       '<i>CrystalClear</i> (Rigaku, 2003)'
_computing_data_reduction        '<i>CrystalClear</i> (Rigaku, 2003)'
_computing_molecular_graphics    '<i>ORTEP-3</i> (Farrugia, 1997)'
_computing_publication_material
;
<i>SHELXL97</i> (Sheldrick, 2008) and
<i>Yadokari-XG 2009</i> (Kabuto <i>et al.</i>, 2009)
;
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SIR2004</i> (Burla <i>et al.</i>, 2005)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku RAXIS-IV imaging plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12290
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.311
_exptl_absorpt_correction_T_max  0.9696
_exptl_absorpt_correction_T_min  0.9126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>REQAB</i>; Jacobson, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.320
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0373P)^2^+1.7041P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                4826
_reflns_number_total             4895
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            is5036.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2233523
_cod_database_fobs_code          2233523