"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_4106071
_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         '(sb2 Ge16), 4(C18 H36 K N2 O6), 3(C2 H8 N2)'
_chemical_formula_sum            'C78 H166 Ge16 K4 N14 O24 Sb2'
_chemical_formula_weight         3245.93
_chemical_name_systematic
; 
 (Kcrypt)4[SbGe8-Ge8Sb] 3en 
;
_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                 95.935(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.6545(18)
_cell_length_b                   24.5738(14)
_cell_length_c                   17.0791(11)
_cell_measurement_reflns_used    23662
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.21
_cell_measurement_theta_min      2.21
_cell_volume                     11961.8(13)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0840
_diffrn_reflns_av_sigmaI/netI    0.1063
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            93390
_diffrn_reflns_theta_full        26.21
_diffrn_reflns_theta_max         26.21
_diffrn_reflns_theta_min         0.71
_exptl_absorpt_coefficient_mu    4.600
_exptl_absorpt_correction_T_max  0.8374
_exptl_absorpt_correction_T_min  0.6822
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sheldrick, 2008'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_description       rod
_exptl_crystal_F_000             6456
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.952
_refine_diff_density_min         -2.311
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1270
_refine_ls_number_reflns         23662
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1403
_refine_ls_R_factor_gt           0.0745
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+180.7525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1826
_refine_ls_wR_factor_ref         0.2159
_reflns_number_gt                13964
_reflns_number_total             23662
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja200520c_si_002.cif
_cod_data_source_block           cmpd1a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C78 H166 K4 N14 O24 Ge16 Sb2'
_cod_database_code               4106071