The Formal Combination of Three Singlet Biradicaloid Entities to a Singlet Hexaradicaloid Metalloid Ge14[Si(SiMe3)3]5[Li(THF)2]3 Cluster
Christian Schenk; Andreas Kracke; Karin Fink; Adam Kubas; Wim Klopper; Marco Neumaier; Hansgeorg Schnöckel; Andreas Schnepf; Journal of the American Chemical Society 133 (2011) 2518–2524; doi:10.1021/ja107446z

data_4105673
_publ_section_title
;
 The Formal Combination of Three Singlet Biradicaloid Entities to a
 Singlet Hexaradicaloid Metalloid Ge14[Si(SiMe3)3]5[Li(THF)2]3 Cluster
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2518
_journal_page_last               2524
_journal_paper_doi               10.1021/ja107446z
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C81.5 H219.5 Ge14 Li3 O7 Si25'
_chemical_formula_weight         3051.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   20.1775(6)
_cell_length_b                   20.1775(6)
_cell_length_c                   21.9148(7)
_cell_measurement_reflns_used    40898
_cell_measurement_temperature    149(2)
_cell_measurement_theta_max      26.10
_cell_measurement_theta_min      2.45
_cell_volume                     7726.9(4)
_computing_cell_refinement       'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_data_collection       'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)'
_computing_data_reduction        'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_molecular_graphics    'SHELXTL 6.12 (BrukerAXS Inc., 2003)'
_computing_publication_material  'SHELXTL 6.12 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.12 (BrukerAXS Inc., 2003)'
_computing_structure_solution    'SHELXTL 6.12 (BrukerAXS Inc., 2003)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.80000
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21115
_diffrn_reflns_theta_full        26.08
_diffrn_reflns_theta_max         26.08
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    2.909
_exptl_absorpt_correction_T_max  0.5992
_exptl_absorpt_correction_T_min  0.4403
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       rod
_exptl_crystal_F_000             3143
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         3611
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0348P)^2^+5.3449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.0975
_reflns_number_gt                3389
_reflns_number_total             3611
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107446z_si_001.cif
_cod_data_source_block           ak10p63m
_cod_original_formula_sum        'C81.50 H219.50 Ge14 Li3 O7 Si25'
_cod_database_code               4105673