"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_4106075
_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         '(Ge16 Bi2), 4(C12 H24 K O6), 5(C2 H8 N2)'
_chemical_formula_sum            'C58 H136 Bi2 Ge16 K4 N10 O24'
_chemical_formula_weight         3093.87
_chemical_name_systematic
; 
 (K(18-crown-6))4[BiGe8-Ge8Bi] 5en   
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.963(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.347(3)
_cell_length_b                   21.923(5)
_cell_length_c                   17.287(3)
_cell_measurement_reflns_used    10206
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.36
_cell_volume                     5815(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1836
_diffrn_reflns_av_sigmaI/netI    0.1232
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            66753
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    7.278
_exptl_absorpt_correction_T_max  0.8390
_exptl_absorpt_correction_T_min  0.5604
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sheldrick, 2008'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_description       rod
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.785
_refine_diff_density_min         -2.626
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         10206
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1446
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0713P)^2^+60.0672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1381
_refine_ls_wR_factor_ref         0.1822
_reflns_number_gt                5420
_reflns_number_total             10206
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja200520c_si_006.cif
_cod_data_source_block           cmpd3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4106075