Mixed Si/Ge Nine-Atom Zintl Clusters: ESI Mass Spectrometric Investigations and Single-Crystal Structure Determination of Paramagnetic [Si9-xGex]3-
Markus Waibel; Thomas F. Fässler; Inorganic Chemistry 52 (2013) 5861–5866; doi:10.1021/ic302802h

data_4334841
_publ_contact_author_address
;Department Chemie, 
Technische Universitaet Muenchen,
D-85747 Garching
Germany
;
_publ_contact_author_email       thomas.faessler@lrz.tum.de
_publ_contact_author_fax         '(+49) 89-289-13186'
_publ_contact_author_name        'Thomas F. Faessler'
_publ_contact_author_phone       '(+49) 89-289-13131'
_publ_section_title
;
 Mixed Si/Ge Nine-Atom Zintl Clusters: ESI Mass Spectrometric
 Investigations and Single-Crystal Structure Determination of Paramagnetic
 [Si9-xGex]3-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5861
_journal_page_last               5866
_journal_paper_doi               10.1021/ic302802h
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C54 H132 Ge6.81 N14 O18 Rb3 Si2.2'
_chemical_formula_weight         2077.78
_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           SHELXL-97
_cell_angle_alpha                80.251(3)
_cell_angle_beta                 84.862(3)
_cell_angle_gamma                66.630(4)
_cell_formula_units_Z            2
_cell_length_a                   14.1713(5)
_cell_length_b                   15.1574(6)
_cell_length_c                   22.9195(9)
_cell_measurement_temperature    120(2)
_cell_volume                     4452.6(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  0.1415
_diffrn_reflns_av_sigmaI/netI    0.2630
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44245
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    3.987
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59670
_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            orange
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_description       block
_exptl_crystal_F_000             2115
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.997
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.826
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     900
_refine_ls_number_reflns         15574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.826
_refine_ls_R_factor_all          0.1716
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.1039
_reflns_number_gt                6947
_reflns_number_total             15574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302802h_si_001_2.cif
_cod_data_source_block           compound2
_cod_original_formula_sum        'C54 H132 Ge6.81 N14 O18 Rb3 Si2.20'
_cod_database_code               4334841