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_4104898
_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)69'
_chemical_formula_sum            'C252 H462 Cl36 Co32 O141 S24'
_chemical_formula_weight         9679.62
_chemical_name_common
'[Co32(C40H44S4O4)6(u3-O)24(H2O)24](CHCl3)12(H2O)69'
_chemical_name_systematic        ?
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/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                   25.1839(18)
_cell_length_b                   25.1839(18)
_cell_length_c                   35.168(3)
_cell_measurement_reflns_used    9707
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.04
_cell_measurement_theta_min      2.29
_cell_volume                     22305(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-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  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            93784
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.99
_exptl_absorpt_coefficient_mu    1.554
_exptl_absorpt_correction_T_max  0.6974
_exptl_absorpt_correction_T_min  0.6615
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       Block
_exptl_crystal_F_000             9924
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
P. van der Sluis and A. L. Spek, Acta Crystallogr., 1990, A46, 194.
;
_refine_diff_density_max         3.297
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       0.00012(3)
_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   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         10002
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0847
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1915P)^2^+61.8676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2610
_refine_ls_wR_factor_ref         0.2731
_reflns_number_gt                7727
_reflns_number_total             10002
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9034939_si_002_2.cif
_cod_data_source_block           compound_1b
_cod_original_sg_symbol_Hall     '-I 4 '
_cod_database_code               4104898