[2-(<i>tert</i>-Butyldimethylsilyl)phenyl]diphenyl(2,2,4,4-tetramethylpent-3-yloxy)silane and its Disilane Precursor, 1-<i>tert</i>-Butyl-1,1-dimethyl-2,2,2-triphenyldisilane
Stark, Joseph L.; Whitmire, Kenton H.; Acta Crystallographica Section C 53 (1997) IUC9700006–; doi:10.1107/S0108270197099496

data_2006249
_publ_section_title
;[2-(<i>tert</i>-Butyldimethylsilyl)phenyl]diphenyl(2,2,4,4-tetramethylpent-3-yloxy)silane
 and its Disilane Precursor,
 1-<i>tert</i>-Butyl-1,1-dimethyl-2,2,2-triphenyldisilane
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9700006
_journal_paper_doi               10.1107/S0108270197099496
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C24 H30 Si2'
_chemical_formula_sum            'C24 H30 Si2'
_chemical_formula_weight         374.66
_chemical_melting_point          .355E-305
_chemical_name_systematic
;
 1,1-dimethyl-1-tert-butyl-2,2,2-triphenyldisilane
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 105.76(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.602(4)
_cell_length_b                   14.924(5)
_cell_length_c                   22.770(6)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      4.7
_cell_volume                     4448(2)
_computing_cell_refinement       'XSCANS (Siemens)'
_computing_data_collection       'XSCANS (Siemens)'
_computing_data_reduction        'XSCANS (Siemens)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1995)'
_computing_publication_material  'SHELXTL (Sheldrick, 1995)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1995)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1995)'
_diffrn_ambient_temperature      299(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Siemens rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            4824
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.165
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
empirical via \y scans
applied in SHELXTL/XPREP (Sheldrick,1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_meas      ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.345
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.821
_refine_ls_goodness_of_fit_obs   0.806
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         3903
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.821
_refine_ls_restrained_S_obs      0.806
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_obs          .0614
_refine_ls_shift/esd_max         -0.046
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1929P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2228
_refine_ls_wR_factor_obs         .1781
_reflns_number_observed          2644
_reflns_number_total             3903
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            qb0006.cif
_cod_data_source_block           1c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1929P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1929P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4448.(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2006249
_cod_database_fobs_code          2006249