The First Structurally Characterized Hypervalent Silicon Hydride: Unexpected Molecular Geometry and Si-H...K Interactions
Michael J. Bearpark; G. Sean McGrady; Paul D. Prince; Jonathan W. Steed; Journal of the American Chemical Society 123 (2001) 7736–7737; doi:10.1021/ja0162616

data_4115647
_publ_section_title
;
 The First Structurally Characterized Hypervalent Silicon Hydride:
 Unexpected Molecular Geometry and Si-H...K Interactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7736
_journal_page_last               7737
_journal_paper_doi               10.1021/ja0162616
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C30 H41 K O6 Si'
_chemical_formula_weight         564.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.540(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3861(5)
_cell_length_b                   20.2252(10)
_cell_length_c                   16.5969(10)
_cell_measurement_temperature    125(2)
_cell_volume                     3063.1(3)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'XSeed (Barbour, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '1.6 phi + omega scans 6s/o'
_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  0.0810
_diffrn_reflns_av_sigmaI/netI    0.0999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16817
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.8846
_exptl_absorpt_correction_T_min  0.7871
_exptl_absorpt_correction_type   Scalepack
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          1.00
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.0013(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         6802
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0451P)^2^+0.9529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1232
_reflns_number_gt                4249
_reflns_number_total             6802
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0162616_s2.cif
_cod_data_source_block           ppsilyl1(monoclinic_K[Ph3SiH2]18C6)
_cod_database_code               4115647