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_7106234
_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][HPMo12O40](CHCl3)12(CH3CH2OH)7
_chemical_formula_sum            'C266 H319 Cl42 Co24 Mo20 O103 P S24'
_chemical_formula_weight         10786.64
_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                   24.6357(3)
_cell_length_b                   24.6357(3)
_cell_length_c                   36.1032(5)
_cell_measurement_reflns_used    9731
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0011
_cell_measurement_theta_min      2.2564
_cell_volume                     21911.7(5)
_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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            93902
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    1.867
_exptl_absorpt_correction_T_max  0.6044
_exptl_absorpt_correction_T_min  0.5611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10680
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_refine_diff_density_max         3.230
_refine_diff_density_min         -1.570
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         9843
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1551P)^2^+110.3081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2161
_refine_ls_wR_factor_ref         0.2275
_reflns_number_gt                7764
_reflns_number_total             9843
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc05574c.txt
_cod_data_source_block           compound_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      ' I4/m'
_cod_database_code               7106234
_platon_compound_3_details
;
SQUEEZE removed 12 disordered CHCl3 and 7 CH3CH2OH molecules
per formula unit. This valueis calculated based upon charge balance
considerations, volume/count_electrons analysis and 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 12 disordered CHCl3 and
7 CH3CH2OH molecules omitted by SQUEEZE.

_PLAT043_ALERT_1_A
PROBLEM: Check Reported Molecular Weight ................10786.64
RESPONSE: This is caused by the given molecular weight being increased
from the atom count to account for 12 disordered CHCl3 and
7 CH3CH2OH molecules omitted by SQUEEZE.

_PLAT051_ALERT_1_A
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by........12.24 Perc
RESPONSE: This is caused by the given molecular weight being increased
from the atom count to account for 12 disordered CHCl3 and
7 CH3CH2OH molecules omitted by SQUEEZE.

_PLAT220_ALERT_2_A
PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.27 Ratio
RESPONSE: These is caused by the weak high-angle diffractions
and the disorder of tert-butyl atoms.

PLAT241_ALERT_2_A
PROBLEM: Check High Ueq as Compared to Neighbors for O11
PROBLEM: Check Low Ueq as Compared to Neighbors for Mo2
PLAT430_ALERT_2_B
PROBLEM: Short Inter D...A Contact O11 .. O12 .. 2.82 Ang.
PROBLEM: Short Inter D...A Contact O12 .. O13 .. 2.77 Ang.
PROBLEM: Short Inter D...A Contact O12 .. O13 .. 2.77 Ang.
RESPONSE: These is caused by the disorder of [PW12O40]3- anion and it can not be
solved appropriately.
;