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_4117539
_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         'C40 Cd13 In22 N4 S52'
_chemical_formula_sum            'C40 Cd13 In22 N4 S52'
_chemical_formula_weight         6190.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           141
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2'
_symmetry_space_group_name_H-M   'I 41/a m d :2'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.0877(4)
_cell_length_b                   28.0877(4)
_cell_length_c                   26.7025(4)
_cell_measurement_temperature    150(2)
_cell_volume                     21066.1(5)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1078
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40812
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    4.166
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.952
_exptl_crystal_description       'elongated square bipyramid'
_exptl_crystal_F_000             11208
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.114
_refine_diff_density_min         -6.611
_refine_diff_density_rms         0.642
_refine_ls_extinction_coef       0.00021(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2601
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.2824
_refine_ls_R_factor_gt           0.1946
_refine_ls_shift/su_max          0.500
_refine_ls_shift/su_mean         0.102
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+20000.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4616
_refine_ls_wR_factor_ref         0.6185
_reflns_number_gt                1236
_reflns_number_total             2601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210039u_si_002_6.cif
_cod_data_source_block           ISC-9-No-SQ
_cod_original_sg_symbol_H-M      'I 41/a m d'
_cod_database_code               4117539