Structure and Bonding of KSiH3 and Its 18-Crown-6 Derivatives: Unusual Ambidentate Behavior of the SiH3- Anion
David J. Wolstenholme; Paul D. Prince; G. Sean McGrady; Michael J. Landry; Jonathan W. Steed; Inorganic Chemistry 50 (2011) 11222–11227; doi:10.1021/ic201774x

data_4326757
_publ_section_title
;
 Structure and Bonding of KSiH3 and Its 18-Crown-6 Derivatives: Unusual
 Ambidentate Behavior of the SiH3- Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11222
_journal_page_last               11227
_journal_paper_doi               10.1021/ic201774x
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C30 H43 K O6 Si2'
_chemical_formula_weight         594.92
_space_group_IT_number           160
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'P 3* -2'
_symmetry_space_group_name_H-M   'R 3 m :R'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.201(10)
_cell_angle_beta                 98.201(10)
_cell_angle_gamma                98.201(10)
_cell_formula_units_Z            1
_cell_length_a                   9.4687(10)
_cell_length_b                   9.4687(10)
_cell_length_c                   9.4687(10)
_cell_measurement_temperature    115(2)
_cell_volume                     820.06(16)
_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      115(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '2o phi scans 7.5s/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  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4204
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_T_max  0.8757
_exptl_absorpt_correction_T_min  0.8757
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       prism
_exptl_crystal_F_000             318
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.31(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1303
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0455P)^2^+0.2873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0966
_reflns_number_gt                1232
_reflns_number_total             1303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201774x_si_003.cif
_cod_data_source_block           22.CIF
_cod_original_cell_volume        820.06(15)
_cod_original_sg_symbol_H-M      'R 3 m:R'
_cod_database_code               4326757