A {Co32} Nanosphere Supported by p-tert-Butylthiacalix[4]arene
Yanfeng Bi; Xiu-Teng Wang; Wuping Liao; Xiaofei Wang; Xinwu Wang; Hongjie Zhang; Song Gao; Journal of the American Chemical Society 131 (2009) 11650–11651; doi:10.1021/ja9034939

data_4104897
_publ_contact_author             'Prof Dr Wuping Liao'
_publ_contact_author_address
;     State Key Lab of Rare Earth Resource Utilization
      Changchun Institute of Applied Chemistry
      CAS, Changchun 130022
      P.R. China
;
_publ_contact_author_email       wpliao@ciac.jl.cn
_publ_section_title
;
 A {Co32} Nanosphere Supported by p-tert-Butylthiacalix[4]arene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11650
_journal_page_last               11651
_journal_paper_doi               10.1021/ja9034939
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety
'[Co32(C40H44S4O4)6(u3-O)24(H2O)24](CHCl3)12(H2O)110'
_chemical_formula_sum            'C252 H544 Cl36 Co32 O182 S24'
_chemical_formula_weight         10418.27
_chemical_name_common
'[Co32(C40H44S4O4)6(u3-O)24(H2O)24](CHCl3)12(H2O)110'
_chemical_name_systematic        ?
_space_group_IT_number           139
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_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            2
_cell_length_a                   27.0173(4)
_cell_length_b                   27.0173(4)
_cell_length_c                   29.0170(5)
_cell_measurement_reflns_used    19661
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.37
_cell_volume                     21180.5(6)
_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-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 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  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0101
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            280751
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.03
_exptl_absorpt_coefficient_mu    1.649
_exptl_absorpt_correction_T_max  0.7900
_exptl_absorpt_correction_T_min  0.6930
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       block
_exptl_crystal_F_000             10744
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
P. van der Sluis and A. L. Spek, Acta Crystallogr., 1990, A46, 194.
;
_refine_diff_density_max         2.272
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.248
_refine_ls_extinction_coef       0.00026(5)
_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   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         5156
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0962
_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^)+(0.1810P)^2^+130.6189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2726
_refine_ls_wR_factor_ref         0.2793
_reflns_number_gt                4798
_reflns_number_total             5156
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9034939_si_002_1.cif
_cod_data_source_block           compound_1a
_cod_database_code               4104897