Alkylation of Deltahedral Zintl Clusters: Synthesis of [R-Ge9-Ge9-R]4- (R = tBu, sBu, nBu, tAm) and Structure of [tBu-Ge9-Ge9-tBu]4-
Michael W. Hull; Angel Ugrinov; Ivaylo Petrov; Slavi C. Sevov; Inorganic Chemistry 46 (2007) 2704–2708; doi:10.1021/ic0623314

data_4307840
_publ_section_title
;
Alkylation of Deltahedral Zintl Clusters: Synthesis of
[R-Ge9-Ge9-R]4- (R = tBu, sBu, nBu, tAm) and Structure of
[tBu-Ge9-Ge9-tBu]4-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2704
_journal_page_last               2708
_journal_paper_doi               10.1021/ic0623314
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety
'4(C18 H36 K N2 O6), C12 H18 Ge18, 7(C2 H8 N2)'
_chemical_formula_sum            'C94 H182 Ge18 K4 N22 O24'
_chemical_formula_weight         3467.64
_chemical_name_systematic
; 
 (K-crypt)4[tBu-Ge9-Ge9-tBu]*7en 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 94.0136(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   35.0914(10)
_cell_length_b                   24.8161(6)
_cell_length_c                   16.8782(5)
_cell_measurement_temperature    100(2)
_cell_volume                     14662.0(7)
_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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            47916
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.01
_exptl_absorpt_coefficient_mu    3.804
_exptl_absorpt_correction_T_max  0.49804
_exptl_absorpt_correction_T_min  0.32903
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             6976
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.219
_refine_diff_density_max         2.186
_refine_diff_density_min         -1.276
_refine_diff_density_rms         .347
_refine_ls_extinction_coef       0.00034(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     747
_refine_ls_number_reflns         12925
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0918P)^2^+165.5306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1644
_refine_ls_wR_factor_ref         0.1779
_reflns_number_gt                9900
_reflns_number_total             12925
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0623314si20070118_121123.cif
_cod_data_source_block           c2c
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4307840