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_4104616
_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
;
 2(C18 H36 K N2 O6 ), C8 H14 Ge9, 3(C2 N2)
;
_chemical_formula_sum            'C50 H86 Ge9 K2 N10 O12'
_chemical_formula_weight         1750.98
_chemical_name_systematic
;
 (K-crypt)2[Ge9-(CH2CH(CH2)2)2] 3en
;
_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                 93.8900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9391(3)
_cell_length_b                   25.7127(5)
_cell_length_c                   19.0906(4)
_cell_measurement_temperature    100(2)
_cell_volume                     7316.3(3)
_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  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0178
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            57546
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    3.813
_exptl_absorpt_correction_T_max  0.284
_exptl_absorpt_correction_T_min  0.136
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             3526
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         12889
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0232P)^2^+14.1596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                11448
_reflns_number_total             12889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9025962_si_002_2.cif
_cod_data_source_block           ge9-methylcyclopropane
_cod_database_code               4104616