Triclinic polymorph of bis(triphenylsilyl) oxide toluene disolvate
Purdy, Andrew P.; Smoot, Emily; Butcher, Ray J.; Kerr, Andrew; Acta Crystallographica Section E 68 (2012) o588–; doi:10.1107/S160053681200356X

data_2233977
_publ_section_title
;
 Triclinic polymorph of bis(triphenylsilyl) oxide toluene disolvate
;
_journal_coeditor_code           RZ2678
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o588
_journal_paper_doi               10.1107/S160053681200356X
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C36 H30 O Si2, 2C7 H8'
_chemical_formula_moiety         'C36 H30 O Si2, 2(C7 H8)'
_chemical_formula_sum            'C50 H46 O Si2'
_chemical_formula_weight         719.05
_chemical_name_common
;
bis(triphenylsilyl) oxide toluene disolvate
;
_chemical_name_systematic
;
triphenyl[(triphenylsilyl)oxy]silane toluene disolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                62.638(4)
_cell_angle_beta                 61.356(4)
_cell_angle_gamma                61.795(4)
_cell_formula_units_Z            1
_cell_length_a                   10.756(3)
_cell_length_b                   11.062(3)
_cell_length_c                   11.156(3)
_cell_measurement_reflns_used    8183
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.28
_cell_volume                     978.9(5)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \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  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16663
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         28.54
_diffrn_reflns_theta_min         2.18
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             382
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.378
_refine_diff_density_min         -0.521
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0884
_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^)+(0.1084P)^2^+2.5305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2367
_refine_ls_wR_factor_ref         0.2590
_reflns_number_gt                3344
_reflns_number_total             4819
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz2678.cif
_cod_data_source_block           I
_cod_original_cell_volume        978.8(4)
_cod_database_code               2233977
_cod_database_fobs_code          2233977