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_4114358
_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            'C24 H34 Ge9 N9 O6 Rb3'
_chemical_formula_weight         1454.32
_chemical_name_systematic
; 
(Rb-crypt)2Rb4(Ge9)(Ge9).7en
;
_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                76.76(1)
_cell_angle_beta                 80.90(2)
_cell_angle_gamma                78.60(1)
_cell_formula_units_Z            2
_cell_length_a                   10.138(3)
_cell_length_b                   13.881(2)
_cell_length_c                   19.311(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2574.9(10)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977)
_computing_data_collection       CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction        SDS_Package_(Enraf-Nonius,_1985)
_computing_molecular_graphics    'SHELXTL (Siemens, 1994)'
_computing_publication_material  'SHELXTL (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  0.0859
_diffrn_reflns_av_sigmaI/netI    0.1690
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6542
_diffrn_reflns_theta_full        21.96
_diffrn_reflns_theta_max         21.96
_diffrn_reflns_theta_min         2.05
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.030
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.200
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         6298
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.2263
_refine_ls_R_factor_gt           0.0948
_refine_ls_shift/su_max          0.113
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1255P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2090
_refine_ls_wR_factor_ref         0.2541
_reflns_number_gt                2694
_reflns_number_total             6298
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja037007bsi20030701_034647_7.cif
_cod_data_source_block           tri
_cod_original_cell_volume        2575(1)
_cod_database_code               4114358