The Largest Supertetrahedral Oxychalcogenide Nanocluster and Its Unique Assembly.
Yang, Huajun; Zhang, Jiaxu; Luo, Min; Wang, Wei; Lin, Haiping; Li, Youyong; Li, Dongsheng; Feng, Pingyun; Wu, Tao; Journal of the American Chemical Society 140 (2018) 11189–11192; doi:10.1021/jacs.8b07349

data_4132900
_publ_section_title
;
 The Largest Supertetrahedral Oxychalcogenide Nanocluster and Its Unique
 Assembly.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11189
_journal_page_last               11192
_journal_paper_doi               10.1021/jacs.8b07349
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C6 In35 N4 O8 S48'
_chemical_formula_sum            'C6 In35 N4 O8 S48'
_chemical_formula_weight         5813.68
_space_group_crystal_system      trigonal
_space_group_IT_number           151
_space_group_name_Hall           'P 31 2 (0 0 4)'
_space_group_name_H-M_alt        'P 31 1 2'
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.5809(19)
_cell_length_b                   21.5809(19)
_cell_length_c                   41.108(4)
_cell_measurement_reflns_used    3686
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.1916
_cell_measurement_theta_min      2.1794
_cell_volume                     16580(3)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1326
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            43052
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        17.223
_diffrn_reflns_theta_max         17.223
_diffrn_reflns_theta_min         2.132
_exptl_absorpt_coefficient_mu    4.035
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_description       block
_exptl_crystal_F_000             7833.0
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 2054 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.701
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         6707
_refine_ls_number_restraints     561
_refine_ls_restrained_S_all      0.673
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0314
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.873
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5180
_reflns_number_total             6707
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07349_si_003.cif
_cod_data_source_block           IOS-2M
_cod_original_cell_volume        16580(4)
_cod_original_sg_symbol_Hall     'P 31 2c (0 0 1)'
_cod_database_code               4132900
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              31732
_shelx_hkl_checksum              12002
_shelx_fab_checksum              97008