Syntheses and crystal structures of 2-methyl-1,1,2,3,3-pentaphenyl-2-silapropane and 2-methyl-1,1,3,3-tetraphenyl-2-silapropan-2-ol
Williams, Alexandra; Brown, Michelle; Staples, Richard J.; Biros, Shannon M.; Winchester, William R.; Acta Crystallographica Section E 75 (2019) 1339–1343; doi:10.1107/S2056989019011265

data_2243070
_publ_section_title
;
 Syntheses and crystal structures of
 2-methyl-1,1,2,3,3-pentaphenyl-2-silapropane and
 2-methyl-1,1,3,3-tetraphenyl-2-silapropan-2-ol
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1339
_journal_page_last               1343
_journal_paper_doi               10.1107/S2056989019011265
_journal_volume                  75
_journal_year                    2019
_chemical_formula_moiety         'C33 H30 Si'
_chemical_formula_sum            'C33 H30 Si'
_chemical_formula_weight         454.66
_chemical_name_systematic
;
2-Methyl-1,1,2,3,3-pentaphenyl-2-silapropane
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_cell_angle_alpha                68.8212(7)
_cell_angle_beta                 70.6364(7)
_cell_angle_gamma                84.7947(8)
_cell_formula_units_Z            2
_cell_length_a                   10.3879(7)
_cell_length_b                   10.5037(7)
_cell_length_c                   13.6350(9)
_cell_measurement_reflns_used    6620
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.393
_cell_measurement_theta_min      2.170
_cell_volume                     1308.06(15)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009; Bourhis <i>et al.</i>,
2015)
;
_computing_publication_material
;
CrystalMaker (Palmer, 2007)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16773
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.393
_diffrn_reflns_theta_min         1.692
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       block
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.174
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4803
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0521P)^2^+0.3536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1204
_reflns_number_gt                3734
_reflns_number_total             4803
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5509sup1.cif
_cod_data_source_block           I
_cod_database_code               2243070
_cod_database_fobs_code          2243070
_shelx_estimated_absorpt_t_min   0.978
_shelx_estimated_absorpt_t_max   0.981
_shelx_hkl_checksum              3177
_shelx_res_checksum              25352