Superbase Route to Supertetrahedral Chalcogenide Clusters
Tao Wu; Xianhui Bu; Puhong Liao; Le Wang; Shou-Tian Zheng; Richard Ma; Pingyun Feng; Journal of the American Chemical Society 134 (2012) 3619–3622; doi:10.1021/ja210039u

data_4117535
_publ_section_title
;
 Superbase Route to Supertetrahedral Chalcogenide Clusters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3619
_journal_page_last               3622
_journal_paper_doi               10.1021/ja210039u
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C21 H27 Ga10 N9 O3 S16'
_chemical_formula_sum            'C21 H27 Ga10 N9 O3 S16'
_chemical_formula_weight         1663.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_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            6
_cell_length_a                   21.70730(10)
_cell_length_b                   21.70730(10)
_cell_length_c                   28.5686(3)
_cell_measurement_temperature    150(2)
_cell_volume                     11658.19(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'Omega Scan'
_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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            34402
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    3.862
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       block
_exptl_crystal_F_000             4836
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.923
_refine_diff_density_min         -1.289
_refine_diff_density_rms         0.236
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         3382
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0892
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1694P)^2^+503.4629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2905
_refine_ls_wR_factor_ref         0.3203
_reflns_number_gt                2610
_reflns_number_total             3382
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210039u_si_002_2.cif
_cod_data_source_block           ISC-2
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4117535