Reactions of Hydridochlorosilanes with 2,2'-Bipyridine and 1,10-Phenanthroline: Complexation versus Dismutation and Metal-Catalyst-Free 1,4-Hydrosilylation
Gerrit W. Fester; Jana Eckstein; Daniela Gerlach; Jörg Wagler; Erica Brendler; Edwin Kroke; Inorganic Chemistry 49 (2010) 2667–2673; doi:10.1021/ic901620e

data_4315124
_publ_contact_author
;Wagler, J\"org 
 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 39-3556 '
_publ_section_title
;
 Reactions of Hydridochlorosilanes with 2,2'-Bipyridine and
 1,10-Phenanthroline: Complexation versus Dismutation and
 Metal-Catalyst-Free 1,4-Hydrosilylation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2667
_journal_page_last               2673
_journal_paper_doi               10.1021/ic901620e
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C10 H9 Cl3 N2 Si'
_chemical_formula_sum            'C10 H9 Cl3 N2 Si'
_chemical_formula_weight         291.63
_chemical_name_systematic
;
 trichlorosilane 2,2'-bipyridine complex
;
_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                 95.940(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4724(6)
_cell_length_b                   7.6648(3)
_cell_length_c                   12.9933(6)
_cell_measurement_reflns_used    3504
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      32.02
_cell_measurement_theta_min      2.39
_cell_volume                     1235.47(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep32 (Farugia)'
_computing_publication_material  'Shelx-97/ciftab(Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15199
_diffrn_reflns_theta_full        32.00
_diffrn_reflns_theta_max         32.00
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.811
_exptl_absorpt_correction_T_max  0.8678
_exptl_absorpt_correction_T_min  0.7897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       piece
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         4277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+1.8867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                3433
_reflns_number_total             4277
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901620e_si_002_2.cif
_cod_data_source_block           compound_2b
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               4315124