Chloropentaphenyldisiloxane—Model Study on Intermolecular Interactions in the Crystal Structure of a Monofunctionalized Disiloxane
Bauer, Jonathan O.; Götz, Tobias; Chemistry 3 (2021) 444–453; doi:10.3390/chemistry3020033

data_1561479
_publ_section_title
;
 Chloropentaphenyldisiloxane---Model Study on Intermolecular Interactions
 in the Crystal Structure of a Monofunctionalized Disiloxane
;
_journal_issue                   2
_journal_name_full               Chemistry
_journal_page_first              444
_journal_page_last               453
_journal_paper_doi               10.3390/chemistry3020033
_journal_volume                  3
_journal_year                    2021
_chemical_formula_moiety         'C30 H25 Cl O Si2'
_chemical_formula_sum            'C30 H25 Cl O Si2'
_chemical_formula_weight         493.13
_chemical_name_systematic        Chloropentaphenyldisiloxane
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)

SHELXL-2018/3
;
_cell_angle_alpha                90
_cell_angle_beta                 99.597(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6741(2)
_cell_length_b                   14.2858(2)
_cell_length_c                   17.5012(3)
_cell_measurement_reflns_used    11402
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      69.5930
_cell_measurement_theta_min      3.5930
_cell_volume                     2631.37(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'CrystalExplorer 17.5 (Turner et al., 2017)'
_computing_publication_material
'WinGX (Version 2018.3) (Farrugia, 2012), Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement
'SHELXL-2018/3 (Sheldrick, 2008; Sheldrick, 2015; Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 4.1818
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -22.00  28.00   1.00   44.09    --  -43.64  38.00  60.00   50
  2  \w     -5.00  34.00   1.00   44.09    --  -43.64  19.00 -90.00   39
  3  \w     58.00 131.00   1.00   44.09    --   43.64-178.00 -30.00   73
  4  \w     17.00  46.00   1.00  176.35    --   95.79 -15.00 -30.00   29
  5  \w     26.00  93.00   1.00  176.35    --   95.79 -61.00 -90.00   67
  6  \w     23.00  57.00   1.00  176.35    --   95.79 -30.00  90.00   34
  7  \w     23.00  57.00   1.00  176.35    --   95.79 -30.00   0.00   34
  8  \w     26.00  93.00   1.00  176.35    --   95.79 -61.00  60.00   67
  9  \w     16.00 175.00   1.00  176.35    --   95.79   0.00-180.00  159
 10  \w     18.00 113.00   1.00   44.09    --   43.64  57.00 -60.00   95
 11  \w     18.00 113.00   1.00   44.09    --   43.64  57.00  60.00   95
 12  \w     17.00  46.00   1.00  176.35    --   95.79 -15.00 120.00   29
 13  \w     71.00 166.00   1.00  176.35    --   95.79  45.00 -90.00   95
 14  \w     27.00  56.00   1.00  176.35    --   95.79-125.00 -90.00   29
 15  \w     17.00  46.00   1.00  176.35    --   95.79 -15.00 150.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\b'
_diffrn_radiation_wavelength     1.39222
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22059
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        56.650
_diffrn_reflns_theta_max         69.661
_diffrn_reflns_theta_min         3.627
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.690
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         6570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0347
_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/[\s^2^(Fo^2^)+(0.0503P)^2^+0.8830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.0994
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5823
_reflns_number_total             6570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tg199.cif
_cod_data_source_block           tg199
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1561479
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.773
_shelx_estimated_absorpt_t_max   0.871
_shelx_res_checksum              57908
_shelx_hkl_checksum              61225