p-tert-Butylthiacalix[4]arene-surpported High-nuclearity {Co24M8} (M = Mo or W) Nanospheres and the Hybrids with Keggin Polyoxometalates
Yanfeng Bi; Shangchao Du; Wuping Liao; Chem.Commun. 47 (2011) 4724–; doi:10.1039/c0cc05574c

data_7106232
_publ_section_title
;
 p-tert-Butylthiacalix[4]arene-surpported High-nuclearity {Co24M8} (M = Mo
 or W) Nanospheres and the Hybrids with Keggin Polyoxometalates
;
_journal_name_full               Chem.Commun.
_journal_page_first              4724
_journal_paper_doi               10.1039/c0cc05574c
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety
Co24(C40H44O4S4)6(MoO4)8Cl6](OH)2(CHCl3)12(CH3CH2OH)12
_chemical_formula_sum            'C276 H350 Cl42 Co24 Mo8 O70 S24'
_chemical_formula_weight         9227.74
_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                   26.9672(15)
_cell_length_b                   26.9672(15)
_cell_length_c                   29.0503(15)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.9717
_cell_measurement_theta_min      2.3717
_cell_volume                     21126(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            76176
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.03
_exptl_absorpt_coefficient_mu    1.582
_exptl_absorpt_correction_T_max  0.7123
_exptl_absorpt_correction_T_min  0.6838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9296
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.668
_refine_diff_density_min         -1.590
_refine_diff_density_rms         0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         5153
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0870
_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^)+(0.1663P)^2^+247.3424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2481
_refine_ls_wR_factor_ref         0.2585
_reflns_number_gt                4415
_reflns_number_total             5153
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc05574c.txt
_cod_data_source_block           compound_1
_cod_original_sg_symbol_H-M      ' I4/mmm'
_cod_database_code               7106232
_platon_compound_1_details
;
SQUEEZE removed two (OH)- anions, 12 disordered CHCl3,
and 12 disordered CH3CH2OH
per formula unit. This valueis calculated based upon charge balance
considerations, volume/count_electrons analysis, and TG experiment.
See ref. Bi, Y. F.; Wang, X. T.; Liao, W. P.; Wang, X. F.; Wang, X. W.;
Zhang, H. J.; Gao, S. J. Am. Chem. Soc. 2009, 131, 11650.

CHEMW03_ALERT_2_A ALERT
PROBLEM: The ratio of given/expected molecular weight as
RESPONSE: This is caused by the given molecular weight being increased
from the atom count to account for two (OH)- anions, 12 disordered CHCl3,
and 12 disordered CH3CH2OH omitted by SQUEEZE.

_PLAT043_ALERT_1_A
PROBLEM: Check Reported Molecular Weight ................9227.74
RESPONSE: This is caused by the given molecular weight being increased
from the atom count to account for two (OH)- anions, 12 disordered CHCl3,
and 12 disordered CH3CH2OH omitted by SQUEEZE.

_PLAT051_ALERT_1_A
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by........15.13 Perc
RESPONSE: This is caused by the given molecular weight being increased
from the atom count to account for two (OH)- anions, 12 disordered CHCl3,
and 12 disordered CH3CH2OH omitted by SQUEEZE.

_PLAT220_ALERT_2_A
PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 7.43 Ratio
PLAT201_ALERT_2_B
PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 6
RESPONSE: These is caused by the weak high-angle diffractions
and the disorder of tert-butyl atoms.
;