Rational Synthesis of [Ge9{Si(SiMe3)3}3]- from Its Parent Zintl Ion Ge94-
Feng Li; Slavi C. Sevov; Inorganic Chemistry 51 (2012) 2706–2708; doi:10.1021/ic202744d

data_4328467
_publ_section_title
;
 Rational Synthesis of [Ge9{Si(SiMe3)3}3]- from Its Parent Zintl Ion Ge94-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2706
_journal_page_last               2708
_journal_paper_doi               10.1021/ic202744d
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C27 H81 Ge9 Si12, C18 H36 K N2 O6'
_chemical_formula_sum            'C45 H117 Ge9 K N2 O6 Si12'
_chemical_formula_weight         1812.30
_chemical_name_systematic
; 
 (K-crypt)[Ge9(Si(Si(CH3)3)3]
;
_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                 113.888(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.497(3)
_cell_length_b                   24.090(2)
_cell_length_c                   29.268(3)
_cell_measurement_reflns_used    9864
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      21.72
_cell_measurement_theta_min      2.27
_cell_volume                     17082(3)
_computing_cell_refinement       'Bruker SAINT v7.60A'
_computing_data_collection       'Bruker APEX-II v2008-6'
_computing_data_reduction        'Bruker SAINT v7.60A'
_computing_molecular_graphics    SHELXL-XP
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'combination of \w/2\q-scans and \f-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  0.1117
_diffrn_reflns_av_sigmaI/netI    0.0898
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            205527
_diffrn_reflns_theta_full        26.46
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         0.84
_exptl_absorpt_coefficient_mu    3.373
_exptl_absorpt_correction_T_max  0.4860
_exptl_absorpt_correction_T_min  0.1733
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sheldrick, 2008'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       block
_exptl_crystal_F_000             7392
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.192
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1351
_refine_ls_number_reflns         35096
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0395P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.1010
_reflns_number_gt                21529
_reflns_number_total             35096
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202744d_si_002.cif
_cod_data_source_block           lf027_0m
_cod_database_code               4328467