Soluble Zintl Phases A14ZnGe16 (A= K, Rb) Featuring [(η3-Ge4)Zn(η2-Ge4)]6- and [Ge4]4- Clusters and the Isolation of [(MesCu)2(η3,η3-Ge4)]4-: The Missing Link in the Solution Chemistry of Tetrahedral Group 14 Element Zintl Clusters
Saskia Stegmaier; Markus Waibel; Alexander Henze; Laura-Alice Jantke; Antti J. Karttunen; Thomas F. Fässler; Journal of the American Chemical Society 134 (2012) 14450–14460; doi:10.1021/ja304251t

data_4118563
_publ_contact_author_address
;Department Chemie
Technische Universit\"at M\"unchen
Lichtenbergstr. 4
85747 Garching
Germany
;
_publ_contact_author_email       thomas.faessler@lrz.tu-muenchen.de
_publ_contact_author_fax         '+49 89 28913186'
_publ_contact_author_name        'Prof. Dr. Thomas F. F\"assler'
_publ_contact_author_phone       '+49 89 28913134'
_publ_section_title
;
 Soluble Zintl Phases A14ZnGe16 (A= K, Rb) Featuring
 [(\h3-Ge4)Zn(\h2-Ge4)]6- and [Ge4]4- Clusters and the Isolation of
 [(MesCu)2(\h3,\h3-Ge4)]4-: The Missing Link in the Solution Chemistry of
 Tetrahedral Group 14 Element Zintl Clusters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14450
_journal_page_last               14460
_journal_paper_doi               10.1021/ja304251t
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'Ge16 K14 Zn'
_chemical_formula_weight         1774.21
_space_group_IT_number           31
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      31
_symmetry_space_group_name_Hall  'P 2ac -2'
_symmetry_space_group_name_H-M   'P m n 21'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL-97 cif-file'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.1357(5)
_cell_length_b                   6.9934(2)
_cell_length_c                   14.0398(5)
_cell_measurement_temperature    150
_cell_volume                     1977.04(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT A'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13760
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.77
_diffrn_source                   'rotating anode'
_diffrn_source_type              'BRUKER NONIUS FR591'
_exptl_absorpt_coefficient_mu    14.025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker 2007, APEX2, SADABS and SAINT, Bruker AXSInc., Madison, Wisconsin (USA)'
_exptl_crystal_colour            'lustrous black'
_exptl_crystal_density_diffrn    2.980
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.161(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         4992
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0168
_refine_ls_R_factor_gt           0.0138
_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^)+(0.0030P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0186
_refine_ls_wR_factor_ref         0.0189
_reflns_number_gt                4710
_reflns_number_total             4992
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja304251t_si_002.cif
_cod_data_source_block           K14ZnGe16
_cod_database_code               4118563