Heteroatomic Deltahedral Zintl Ions of Group 14 and their Alkenylation
Miriam M. Gillett-Kunnath; Ivaylo Petrov; Slavi C. Sevov; Inorganic Chemistry 49 (2010) 721–729; doi:10.1021/ic9019487

data_4314566
_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
;
 Heteroatomic Deltahedral Zintl Ions of Group 14 and their Alkenylation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              721
_journal_page_last               729
_journal_paper_doi               10.1021/ic9019487
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety
'(C2 H3 Ge Sn8), 3(C18 H36 K N2 O6), C2 H8 N2, C7 H8'
_chemical_formula_sum            'C61.5 H123 Ge K3 N8 O18 Sn8'
_chemical_formula_weight         2402.09
_chemical_name_systematic
; 
 (K-crypt)3[GeSn8-CHCH2] 1en 1tol 
;
_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                94.2580(10)
_cell_angle_beta                 98.5210(10)
_cell_angle_gamma                98.4890(10)
_cell_formula_units_Z            2
_cell_length_a                   13.9220(3)
_cell_length_b                   14.9788(3)
_cell_length_c                   21.5892(5)
_cell_measurement_reflns_used    9316
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.73
_cell_measurement_theta_min      2.25
_cell_volume                     4382.31(17)
_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 0.899
_diffrn_measured_fraction_theta_max 0.899
_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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26993
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    2.781
_exptl_absorpt_correction_T_max  0.3369
_exptl_absorpt_correction_T_min  0.1818
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sheldrick, 2008'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2362
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.63
_exptl_crystal_size_min          0.50
_refine_diff_density_max         1.568
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         16713
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+13.3074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                13115
_reflns_number_total             16713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9019487_si_002_2.cif
_cod_data_source_block           cmpd1
_cod_original_cell_volume        4382.31(16)
_cod_original_formula_sum        'C61.50 H123 Ge K3 N8 O18 Sn8'
_cod_database_code               4314566