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_4324629
_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
'6(C18 H36 N2 O6 K), 2(Ni Sn9), 3(C2 H8 N2), C7 H8'
_chemical_formula_sum            'C121 H249 K6 N18 Ni2 O36 Sn18'
_chemical_formula_weight         5020.82
_chemical_name_systematic
; 
(K-crypt)6(Ni@Sn9)2(en)3(tol)
;
_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                 93.561(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.0012(14)
_cell_length_b                   23.3701(10)
_cell_length_c                   27.6515(14)
_cell_measurement_temperature    100(2)
_cell_volume                     18060.0(15)
_computing_cell_refinement       'Bruker SAINT v7.68A'
_computing_data_collection       'Bruker APEX-II v2010-3'
_computing_data_reduction        'Bruker SAINT v7.68A'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0960
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            344154
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    2.846
_exptl_absorpt_correction_T_max  0.9220
_exptl_absorpt_correction_T_min  0.8478
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_description       block
_exptl_crystal_F_000             9836
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         7.096
_refine_diff_density_min         -4.439
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1820
_refine_ls_number_reflns         31810
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.057
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+12.3038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1565
_reflns_number_gt                21626
_reflns_number_total             31810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102152e_si_002_2.cif
_cod_data_source_block           p21c
_cod_original_cell_volume        18059.9(15)
_cod_database_code               4324629