Addition of a Thallium Vertex to Empty and Centered Nine-Atom Deltahedral Zintl Ions of Germanium and Tin
Daniel Rios; Miriam M. Gillett-Kunnath; Jacob D. Taylor; Allen G. Oliver; Slavi C. Sevov; Inorganic Chemistry 50 (2011) 2373–2377; doi:10.1021/ic102152e

data_4324628
_publ_section_title
;
 Addition of a Thallium Vertex to Empty and Centered Nine-Atom Deltahedral
 Zintl Ions of Germanium and Tin
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2373
_journal_page_last               2377
_journal_paper_doi               10.1021/ic102152e
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         '3(C18 H36 K N2 O6), 2(C5 H5 N), Ge9 Tl'
_chemical_formula_sum            'C64 H118 Ge9 K3 N8 O18 Tl'
_chemical_formula_weight         2262.64
_chemical_name_common            '[K-crypt]3[Ge9Tl].2py'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.9176(4)
_cell_length_b                   21.9176(4)
_cell_length_c                   36.9948(8)
_cell_measurement_reflns_used    9389
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.25
_cell_measurement_theta_min      2.20
_cell_volume                     17771.6(6)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'APEX-II D8 diffractometer'
_diffrn_measurement_method       'combination of omega and phi-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  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            265074
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    5.007
_exptl_absorpt_correction_T_max  0.2393
_exptl_absorpt_correction_T_min  0.1886
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Sheldrick, 2008'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_description       block
_exptl_crystal_F_000             9024
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.759
_refine_diff_density_min         -1.720
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.531(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     930
_refine_ls_number_reflns         18259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+37.5304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                17201
_reflns_number_total             18259
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102152e_si_002_1.cif
_cod_data_source_block           dr26
_cod_database_code               4324628