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_4115646
_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           146
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'P 3*'
_symmetry_space_group_name_H-M   'R 3 :R'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.930(10)
_cell_angle_beta                 97.930(10)
_cell_angle_gamma                97.930(10)
_cell_formula_units_Z            1
_cell_length_a                   9.4424(15)
_cell_length_b                   9.4424(15)
_cell_length_c                   9.4424(15)
_cell_measurement_temperature    393(2)
_cell_volume                     815.2(2)
_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      393(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '2o phi 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  0.0800
_diffrn_reflns_av_sigmaI/netI    0.1117
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4386
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_T_max  0.9543
_exptl_absorpt_correction_T_min  0.9543
_exptl_absorpt_correction_type   Scalepack
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       prism
_exptl_crystal_F_000             302
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(7)
_refine_ls_extinction_coef       0.041(8)
_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   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2257
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0291P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                1650
_reflns_number_total             2257
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0162616_s1.cif
_cod_data_source_block           ppbypa(trigonal_K[Ph3SiH2]18C6)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4115646