Oxidative Coupling of Deltahedral [Ge9]4- Zintl Ions
Li Xu; Slavi C. Sevov; Journal of the American Chemical Society 121 (1999) 9245–9246; doi:10.1021/ja992269s

data_4116558
_publ_section_title
;
 Oxidative Coupling of Deltahedral [Ge9]4- Zintl Ions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9245
_journal_page_last               9246
_journal_paper_doi               10.1021/ja992269s
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C24 H60 Cs2 Ge9 K N8 O6'
_chemical_formula_weight         1515.03
_chemical_name_systematic
;
 Cs4(K-crypt)2[(Ge9)-(Ge9)](en)6
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.804(9)
_cell_angle_beta                 100.032(7)
_cell_angle_gamma                98.682(8)
_cell_formula_units_Z            2
_cell_length_a                   11.0058(8)
_cell_length_b                   12.6150(10)
_cell_length_c                   18.518(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      15
_cell_volume                     2431.3(4)
_computing_cell_refinement       'CAD4-ARGUS, (Enraf-Nonius, 1994)'
_computing_data_collection       'CAD4-ARGUS, (Enraf-Nonius, 1994)'
_computing_data_reduction        'xcad4 (Harms, 1996)'
_computing_molecular_graphics    'SHELXTL-V5.1 (Siemens, 1994)'
_computing_publication_material  'SHELXTL-V5.1 (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       omega-2theta
_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  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8978
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.082
_exptl_absorpt_correction_T_max  0.422
_exptl_absorpt_correction_T_min  0.309
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    2.069
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             1450
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.509
_refine_diff_density_min         -2.272
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         8494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0882P)^2^+11.9099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1722
_reflns_number_gt                6113
_reflns_number_total             8494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja992269s.cif
_cod_data_source_block           KcrGe18
_cod_database_code               4116558