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_7106233
_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(WO4)8Cl6](OH)2(CHCl3)12(CH3CH2OH)21
_chemical_formula_sum            'C294 H404 Cl42 Co24 O79 S24 W8'
_chemical_formula_weight         10345.63
_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                   27.0337(11)
_cell_length_b                   27.0337(11)
_cell_length_c                   29.0885(13)
_cell_measurement_reflns_used    9662
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0461
_cell_measurement_theta_min      2.2310
_cell_volume                     21258.5(15)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            71340
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.03
_exptl_absorpt_coefficient_mu    3.504
_exptl_absorpt_correction_T_max  0.5265
_exptl_absorpt_correction_T_min  0.4868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10276
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         3.405
_refine_diff_density_min         -4.543
_refine_diff_density_rms         0.374
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         5221
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0981
_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^)+(0.2000P)^2^+263.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2756
_refine_ls_wR_factor_ref         0.2858
_reflns_number_gt                4413
_reflns_number_total             5221
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc05574c.txt
_cod_data_source_block           Compound_2
_cod_original_sg_symbol_H-M      ' I4/mmm'
_cod_database_code               7106233
_platon_compound_2_details
;
SQUEEZE removed two (OH)- anions, 12 disordered CHCl3,
and 21 disordered CH3CH2OH
per formula unit. This valueis calculated based upon charge balance
considerations and 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 21 disordered CH3CH2OH omitted by SQUEEZE.

_PLAT043_ALERT_1_A
PROBLEM: Check Reported Molecular Weight ................ 10345.63
RESPONSE: This is caused by the given molecular weight being increased
from the atom count to account for two (OH)- anions, 12 disordered CHCl3,
26 disordered CH3CH2OH and 91 H2O omitted by SQUEEZE.

PLAT220_ALERT_2_A
PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.93 Ratio
PLAT201_ALERT_2_B
PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 6
RESPONSE: These are caused by the weak high-angle diffractions
and the disorder of tert-butyl atoms.

PLAT430_ALERT_2_A
PROBLEM1: Short Inter D...A Contact O3 .. O5' .. 2.35 Ang
PROBLEM2: Short Inter D...A Contact O4 .. O5' .. 2.32 Ang
RESPONSE: These are caused by the disorder of {WO4} group.

PLAT051_ALERT_1_B
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by........6.93 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 21 disordered CH3CH2OH
;