Metal-Centered Deltahedral Zintl Ions: Synthesis of [Ni@Sn9]4- by direct Extraction from Intermetallic Precursors and of the Vertex-Fused Dimer [{Ni@Sn8(μ-Ge)1/2}2]4-
Miriam M. Gillett-Kunnath; Joseph I. Paik; Sara M. Jensen; Jacob D. Taylor; Slavi C. Sevov; Inorganic Chemistry 50 (2011) 11695–11701; doi:10.1021/ic2016963

data_4326901
_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
;
 Metal-Centered Deltahedral Zintl Ions: Synthesis of [Ni@Sn9]4- by direct
 Extraction from Intermetallic Precursors and of the Vertex-Fused Dimer
 [{Ni@Sn8(\m-Ge)1/2}2]4-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11695
_journal_page_last               11701
_journal_paper_doi               10.1021/ic2016963
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         '(Ni Sn9), 3(C18 H36 K N2 O6), K'
_chemical_formula_sum            'C54 H108 K4 N6 Ni O18 Sn9'
_chemical_formula_weight         2412.78
_chemical_name_systematic
; 
 (K-crypt)3(KSn9) 
;
_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                98.7140(10)
_cell_angle_beta                 104.4690(10)
_cell_angle_gamma                118.3890(10)
_cell_formula_units_Z            2
_cell_length_a                   15.8028(8)
_cell_length_b                   16.2350(9)
_cell_length_c                   20.1760(12)
_cell_measurement_reflns_used    15561
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.57
_cell_measurement_theta_min      2.18
_cell_volume                     4181.5(4)
_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      120(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0701
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            94056
_diffrn_reflns_theta_full        25.57
_diffrn_reflns_theta_max         25.57
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    3.116
_exptl_absorpt_correction_T_max  0.4652
_exptl_absorpt_correction_T_min  0.4085
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sheldrick, 2008'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_description       block
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.796
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         15561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0209P)^2^+13.4671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                11800
_reflns_number_total             15561
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2016963_si_001_3.cif
_cod_data_source_block           compd1b
_cod_database_code               4326901