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_4314567
_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
'2(C4 H6 Ge2 Sn7),  4(C18 H36 K N2 O6), 0.5(C4 H16 N4)'
_chemical_formula_sum            'C82 H164 Ge4 K4 N10 O24 Sn14'
_chemical_formula_weight         3783.01
_chemical_name_systematic
; 
 (K-crypt)4[Ge2Sn7-(CHCH2)2]2 1en 
;
_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                 90.052(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   48.1883(15)
_cell_length_b                   12.1551(4)
_cell_length_c                   21.4824(7)
_cell_measurement_reflns_used    9440
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      2.30
_cell_volume                     12583.0(7)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker X8-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  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            151693
_diffrn_reflns_theta_full        27.27
_diffrn_reflns_theta_max         27.27
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    3.855
_exptl_absorpt_correction_T_max  0.6144
_exptl_absorpt_correction_T_min  0.2943
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sheldrick, 2008'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.997
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7288
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.770
_refine_diff_density_min         -3.753
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1236
_refine_ls_number_reflns         27885
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+121.0850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1197
_reflns_number_gt                23385
_reflns_number_total             27885
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9019487_si_002_3.cif
_cod_data_source_block           cmpd2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4314567