Derivatization of Deltahedral Zintl Ions by Nucleophilic Addition: [Ph-Ge9-SbPh2]2-and [Ph2Sb-Ge9-Ge9-SbPh2]4-
Angel Ugrinov; Slavi C. Sevov; Journal of the American Chemical Society 125 (2003) 14059–14064; doi:10.1021/ja037007b

data_4114354
_publ_section_title
;
 Derivatization of Deltahedral Zintl Ions by Nucleophilic Addition:
 [Ph-Ge9-SbPh2]2-and [Ph2Sb-Ge9-Ge9-SbPh2]4-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14059
_journal_page_last               14064
_journal_paper_doi               10.1021/ja037007b
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C26 H61 Ge9 K3 N10 O6'
_chemical_formula_weight         1380.46
_chemical_name_systematic
; 
(K-crypt)2K4[Ge9-Ge9].8en
;
_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                84.5220(10)
_cell_angle_beta                 81.3900(10)
_cell_angle_gamma                80.1760(10)
_cell_formula_units_Z            2
_cell_length_a                   9.3854(5)
_cell_length_b                   13.5391(7)
_cell_length_c                   19.4560(10)
_cell_measurement_temperature    100(2)
_cell_volume                     2402.4(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL-V5.1'
_computing_molecular_graphics    'Bruker SHELXTL-V5.1'
_computing_publication_material  'Bruker SHELXTL-V5.1'
_computing_structure_refinement  'Bruker SHELXTL-V5.1'
_computing_structure_solution    'Bruker SHELXTL-V5.1'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0784
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26489
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    5.852
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6762
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.721
_refine_diff_density_min         -1.717
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     467
_refine_ls_number_reflns         11921
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.055
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0724P)^2^+8.3368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1467
_reflns_number_gt                8639
_reflns_number_total             11921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja037007bsi20030701_034647_3.cif
_cod_data_source_block           p-1
_cod_database_code               4114354