Functionalization of Nine-Atom Deltahedral Zintl Ions with Organic Substituents: Detailed Studies of the Reactions
Michael W. Hull; Slavi C. Sevov; Journal of the American Chemical Society 131 (2009) 9026–9037; doi:10.1021/ja9025962

data_4104615
_publ_contact_author_address
;Department of Chemistry and Biochemistry
251 Nieuwland Science Hall
University of Notre Dame
Notre Dame, Indiana 46556
;
_publ_contact_author_email       ssevov@nd.edu
_publ_contact_author_name        'Sevov, S. C.'
_publ_section_title
;
 Functionalization of Nine-Atom Deltahedral Zintl Ions with Organic
 Substituents: Detailed Studies of the Reactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9026
_journal_page_last               9037
_journal_paper_doi               10.1021/ja9025962
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety
;
 3(C18 H36 K N2 O6) C5 H7 Ge9 0.21(C6 H6)
;
_chemical_formula_sum            'C60.25 H116.1 Ge9 K3 N6 O18'
_chemical_formula_weight         1983.53
_chemical_name_systematic
;
 (K-crypt)3[Ge9-(C(CH3)=CHCH2CH3)]0.5[Ge9-(C(CH2CH3)=CHCH3)]0.5 0.4bz
;
_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                94.688(2)
_cell_angle_beta                 94.819(2)
_cell_angle_gamma                102.300(2)
_cell_formula_units_Z            2
_cell_length_a                   14.2449(4)
_cell_length_b                   14.3354(4)
_cell_length_c                   20.8288(6)
_cell_measurement_temperature    100(2)
_cell_volume                     4119.3(2)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_measurement_method       'Phi and Omega 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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            63370
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.99
_exptl_absorpt_coefficient_mu    3.449
_exptl_absorpt_correction_T_max  0.7028
_exptl_absorpt_correction_T_min  0.4793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2025
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.355
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     945
_refine_ls_number_reflns         14490
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+16.8975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1217
_reflns_number_gt                11520
_reflns_number_total             14490
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9025962_si_002_1.cif
_cod_data_source_block           ge9-pentyne
_cod_original_formula_sum        'C60.25 H116.10 Ge9 K3 N6 O18'
_cod_database_code               4104615