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_4118565
_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            'C42 H92.5 Cu2 Ge4 K4 N7.5 O12'
_chemical_formula_weight         1468.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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           'manual editing of SHELXL-97 cif-file'
_cell_angle_alpha                98.230(4)
_cell_angle_beta                 111.166(4)
_cell_angle_gamma                107.105(4)
_cell_formula_units_Z            2
_cell_length_a                   13.5093(6)
_cell_length_b                   15.8892(7)
_cell_length_c                   17.7605(8)
_cell_measurement_temperature    120(2)
_cell_volume                     3262.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0577
_diffrn_reflns_av_sigmaI/netI    0.1171
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40591
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    2.769
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       block
_exptl_crystal_F_000             1510
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.120
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.866
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         14901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.866
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1079
_reflns_number_gt                8614
_reflns_number_total             14901
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja304251t_si_004.cif
_cod_data_source_block           C42H92.50Cu2Ge4K4N7.50O12
_cod_original_formula_sum        'C42 H92.50 Cu2 Ge4 K4 N7.50 O12'
_cod_database_code               4118565