5,5-Dimethyl-2,8-diphenyl-5<i>H</i>-dibenzo[<i>b</i>,<i>f</i>]silepine: a synchrotron study
Clegg, William; Harrington, Ross W.; Mercier, Lauren G.; Piers, Warren E.; Acta Crystallographica Section C 69 (2013) 436–438; doi:10.1107/S0108270113005659

data_2018916
_publ_section_title
;
 5,5-Dimethyl-2,8-diphenyl-5<i>H</i>-dibenzo[<i>b</i>,<i>f</i>]silepine: a
 synchrotron study
;
_journal_coeditor_code           KY3030
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              436
_journal_page_last               438
_journal_paper_doi               10.1107/S0108270113005659
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C28 H24 Si'
_chemical_formula_moiety         'C28 H24 Si'
_chemical_formula_sum            'C28 H24 Si'
_chemical_formula_weight         388.56
_chemical_name_systematic
;
5,5-Dimethyl-2,8-diphenyl-5<i>H</i>-dibenzo[<i>b</i>,<i>f</i>]silepine
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   24.234(6)
_cell_length_b                   51.149(12)
_cell_length_c                   6.952(2)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.24
_cell_volume                     8617(4)
_computing_cell_refinement       'APEX2 (Bruker, 2008)'
_computing_data_collection       'CrystalClear (Rigaku, 2008)'
_computing_data_reduction        'APEX2 (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)and local programs'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type
'Rigaku 724+ CCD diffractometer with Crystal Logic Kappa goniometer'
_diffrn_measurement_method       'thick-slice \w scans'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_radiation_source         'Diamond beamline I19'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       63
_diffrn_reflns_limit_k_min       -63
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            18302
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3296
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.149
_refine_diff_density_min         -0.134
_refine_ls_abs_structure_details 'Flack (1983), with 1600 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.01(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         3935
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0372P)^2^+2.9619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                3604
_reflns_number_total             3935
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ky3030.cif
_cod_data_source_block           I
_cod_database_code               2018916
_cod_database_fobs_code          2018916