Hypervalent hydridosilicates: synthesis, structure and hydride bridging
Prince, Paul D.; Bearpark, Michael J.; McGrady, G. Sean; Steed, Jonathan W.; Dalton Transactions  (2008) 271–282; doi:10.1039/b713427d

data_7003171
_publ_section_title
;
 Hypervalent hydridosilicates: synthesis, structure and hydride
 bridging
;
_journal_issue                   2
_journal_name_full               'Dalton Transactions'
_journal_page_first              271
_journal_page_last               282
_journal_paper_doi               10.1039/b713427d
_journal_year                    2008
_chemical_formula_sum            'C30 H41 K O6 Si'
_chemical_formula_weight         564.82
_space_group_IT_number           160
_symmetry_cell_setting           trigonal
_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                97.956(6)
_cell_angle_beta                 97.956(6)
_cell_angle_gamma                97.956(6)
_cell_formula_units_Z            1
_cell_length_a                   9.4377(12)
_cell_length_b                   9.4377(12)
_cell_length_c                   9.4377(12)
_cell_measurement_temperature    100(2)
_cell_volume                     813.80(18)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    X-Seed
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_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  0.0506
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4637
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         3.36
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.237
_exptl_absorpt_correction_T_max  0.9432
_exptl_absorpt_correction_T_min  0.9432
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   scalepack
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             302
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.54(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         1043
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0230P)^2^+0.2182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0705
_reflns_number_gt                1000
_reflns_number_total             1043
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b713427d.txt
_cod_data_source_block           R3M1.CIF
_cod_original_sg_symbol_H-M      R3mr
_cod_database_code               7003171