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_4324630
_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_sum            'C112 H232 K6 N16 Ni2 O36 Sn18 Tl0.88'
_chemical_formula_weight         5046.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 93.2360(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.2574(11)
_cell_length_b                   23.4554(9)
_cell_length_c                   27.7372(10)
_cell_measurement_reflns_used    9829
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.26
_cell_volume                     18354.6(12)
_computing_cell_refinement       'Bruker SAINT v7.66A'
_computing_data_collection       'Bruker APEX-II v2009-9'
_computing_data_reduction        'Bruker SAINT v7.66A'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa X8-APEX-II'
_diffrn_measurement_method       'combination of \w and \f-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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            268161
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.13
_exptl_absorpt_coefficient_mu    3.561
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick (2008)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_description       plate
_exptl_crystal_F_000             9780
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         6.446
_refine_diff_density_min         -5.239
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1783
_refine_ls_number_reflns         37468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.073
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+231.5553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1641
_refine_ls_wR_factor_ref         0.1727
_reflns_number_gt                29918
_reflns_number_total             37468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102152e_si_002_3.cif
_cod_data_source_block           dr28
_cod_original_sg_symbol_Hall     '-P 2yc'
_cod_database_code               4324630