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_4122459
_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         'C39 H108 Ge9 Si12 Sn'
_chemical_formula_sum            'C39 H108 Ge9 Si12 Sn'
_chemical_formula_weight         1686.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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            42
_cell_length_a                   64.496(14)
_cell_length_b                   64.496(14)
_cell_length_c                   22.031(5)
_cell_measurement_reflns_used    9823
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.27
_cell_measurement_theta_min      2.36
_cell_volume                     79365(3)
_computing_cell_refinement       'Bruker SAINT v7.60A'
_computing_data_collection       'Bruker APEX-II v2008-6'
_computing_data_reduction        'Bruker SAINT v7.60A'
_computing_molecular_graphics    SHELXL-XP
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_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  0.1896
_diffrn_reflns_av_sigmaI/netI    0.1020
_diffrn_reflns_limit_h_max       76
_diffrn_reflns_limit_h_min       -76
_diffrn_reflns_limit_k_max       76
_diffrn_reflns_limit_k_min       -76
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            295701
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.63
_exptl_absorpt_coefficient_mu    4.062
_exptl_absorpt_correction_T_max  0.6868
_exptl_absorpt_correction_T_min  0.2933
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sheldrick, 2008'
_exptl_crystal_colour            Black-reddish
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             35616
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.621
_refine_diff_density_min         -1.706
_refine_diff_density_rms         0.298
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1282
_refine_ls_number_reflns         31076
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.2022
_refine_ls_R_factor_gt           0.1028
_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^)+(0.1339P)^2^+6161.0615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2420
_refine_ls_wR_factor_ref         0.2883
_reflns_number_gt                16020
_reflns_number_total             31076
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja505826x_si_004.cif
_cod_data_source_block           mo_lf041_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4122457--4122459.cif.
;
_cod_original_cell_volume        79366(29)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4122459