"n-Doping" of Deltahedral Zintl Ions
Miriam M. Gillett-Kunnath; Allen G. Oliver; Slavi C. Sevov; Journal of the American Chemical Society 133 (2011) 6560–6562; doi:10.1021/ja200520c

data_4106074
_publ_contact_author_address
;
University of Notre Dame
Department of Chemistry and Biochemistry
251 Nieuwland Science Hall
Notre Dame, Indiana 46556
;
_publ_contact_author_email       ssevov@nd.edu
_publ_contact_author_name        'Sevov, S. C.'
_publ_section_title
;
 "n-Doping" of Deltahedral Zintl Ions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6560
_journal_page_last               6562
_journal_paper_doi               10.1021/ja200520c
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         '(C12 H10 Sb2 Ge8), 2(C18 H36 K N2 O6)'
_chemical_formula_sum            'C48 H82 Ge8 K2 N4 O12 Sb2'
_chemical_formula_weight         1809.60
_chemical_name_systematic
; 
  (K-crypt)2[SbGe8-SbPh2] 
;
_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                81.879(3)
_cell_angle_beta                 69.709(2)
_cell_angle_gamma                84.921(3)
_cell_formula_units_Z            2
_cell_length_a                   12.9472(9)
_cell_length_b                   16.5696(9)
_cell_length_c                   16.5832(9)
_cell_measurement_reflns_used    11897
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.63
_cell_measurement_theta_min      1.32
_cell_volume                     3300.4(3)
_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 83.33
_diffrn_measured_fraction_theta_full 0.857
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'combination of \w/2\q-scans 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  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30864
_diffrn_reflns_theta_full        26.63
_diffrn_reflns_theta_max         26.63
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    4.572
_exptl_absorpt_correction_T_max  0.8382
_exptl_absorpt_correction_T_min  0.8036
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sheldrick, 2008'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_description       block
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         2.340
_refine_diff_density_min         -2.345
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         11897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.056
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+21.4284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1133
_reflns_number_gt                9217
_reflns_number_total             11897
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja200520c_si_005.cif
_cod_data_source_block           Cmpd1
_cod_database_code               4106074