[Ph2Bi-(Ge9)-BiPh2]2-: A Deltahedral Zintl Ion Functionalized by Exo-Bonded Ligands
Angel Ugrinov; Slavi C. Sevov; Journal of the American Chemical Society 124 (2002) 2442–2443; doi:10.1021/ja017813n

data_4114686
_publ_section_title
;
 [Ph2Bi-(Ge9)-BiPh2]2-: A Deltahedral Zintl Ion Functionalized by
 Exo-Bonded Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2442
_journal_page_last               2443
_journal_paper_doi               10.1021/ja017813n
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C62 H100 Bi2 Ge9 K2 N6 O12'
_chemical_formula_weight         2270.95
_chemical_name_systematic
; 
(K-2,2,2-crypt)2[Ge9(BiPh2)2].en
;
_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                79.7000(10)
_cell_angle_beta                 77.0030(10)
_cell_angle_gamma                65.8810(10)
_cell_formula_units_Z            2
_cell_length_a                   13.5216(9)
_cell_length_b                   13.6028(9)
_cell_length_c                   24.4984(17)
_cell_measurement_temperature    193(2)
_cell_volume                     3988.1(5)
_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      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0557
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33572
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    7.894
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5997
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.891
_exptl_crystal_description       plate
_exptl_crystal_F_000             2204
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.767
_refine_diff_density_min         -1.407
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     826
_refine_ls_number_reflns         14005
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+15.7432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1175
_reflns_number_gt                11680
_reflns_number_total             14005
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja017813n_s1.cif
_cod_data_source_block           Ge9Bi2Ph4
_cod_database_code               4114686