Synthesis, structures, and solution dynamics of tetrasubstituted nine-atom germanium deltahedral clusters.
Li, Feng; Sevov, Slavi C.; Journal of the American Chemical Society 136 (2014) 12056–12063; doi:10.1021/ja505826x

data_4122458
_publ_section_title
;
 Synthesis, structures, and solution dynamics of tetrasubstituted
 nine-atom germanium deltahedral clusters.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12056
_journal_page_last               12063
_journal_paper_doi               10.1021/ja505826x
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C29 H86 Ge9 Si12'
_chemical_formula_sum            'C29 H86 Ge9 Si12'
_chemical_formula_weight         1425.36
_chemical_name_common            EthyltrisupersilylGe9
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     vecmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 99.96(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.163(5)
_cell_length_b                   23.872(5)
_cell_length_c                   23.166(5)
_cell_measurement_reflns_used    6644
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.48
_cell_measurement_theta_min      2.27
_cell_volume                     12617(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXT (Sheldrick 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 83.33
_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_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            348772
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.234
_exptl_absorpt_coefficient_mu    4.472
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       thin-plate
_exptl_crystal_F_000             5728
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.462
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     902
_refine_ls_number_reflns         25807
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+31.4241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20296
_reflns_number_total             25807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja505826x_si_003.cif
_cod_data_source_block           LF081_0m
_cod_depositor_comments
'Adding full bibliography for 4122457--4122459.cif.'
_cod_database_code               4122458
_shelx_estimated_absorpt_t_min   0.468
_shelx_estimated_absorpt_t_max   0.807
_shelxl_version_number           2013-4
_shelx_res_checksum              47497
_shelx_hkl_checksum              88214