Octahedral HSiCl3 and HSiCl2Me Adducts with Pyridines
Gerrit W. Fester; Jörg Wagler; Erica Brendler; Uwe Böhme; Daniela Gerlach; Edwin Kroke; Journal of the American Chemical Society 131 (2009) 6855–6864; doi:10.1021/ja901053w

data_4104379
_publ_contact_author
;Uwe B\"ohme 
 Institut f\"ur Anorganische Chemie  
 Technische Universit\"at Bergakademie Freiberg
 Leipziger Str. 29 
 09596 Freiberg 
 Bundesrepublik Deutschland
;
_publ_contact_author_fax         '03731 39-4058 '
_publ_contact_author_phone       '03731 39-2050 '
_publ_section_title
;
 Octahedral HSiCl3 and HSiCl2Me Adducts with Pyridines
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6855
_journal_page_last               6864
_journal_paper_doi               10.1021/ja901053w
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C22 H19 Cl3 N2 Si'
_chemical_formula_sum            'C22 H19 Cl3 N2 Si'
_chemical_formula_weight         445.83
_chemical_name_systematic
;
   Bis-(4-phenylpyridine)hydridotrichlorosilane
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.419(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.4028(10)
_cell_length_b                   7.2048(8)
_cell_length_c                   16.494(2)
_cell_measurement_reflns_used    1933
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      2.47
_cell_volume                     998.2(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP32 (Farugia)'
_computing_publication_material  'Ciftab (Sheldrick)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0891
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12843
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  0.9791
_exptl_absorpt_correction_T_min  0.7691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1912
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1200
_reflns_number_gt                1254
_reflns_number_total             1912
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja901053w_si_002.cif
_cod_data_source_block           1h
_cod_original_cell_volume        998.3(2)
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               4104379