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_7106235
_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][HPW12O40](CHCl3)6(CH3CH2OH)2(H2O)2
_chemical_formula_sum            'C250 H287 Cl24 Co24 O100 P S24 W20'
_chemical_formula_weight         11634.33
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.7610(10)
_cell_angle_beta                 109.4100(10)
_cell_angle_gamma                115.4390(10)
_cell_formula_units_Z            1
_cell_length_a                   21.1491(3)
_cell_length_b                   24.0930(3)
_cell_length_c                   24.4639(5)
_cell_measurement_reflns_used    9865
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0451
_cell_measurement_theta_min      2.3954
_cell_volume                     9877.6(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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            86095
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         0.95
_exptl_absorpt_coefficient_mu    7.127
_exptl_absorpt_correction_T_max  0.5664
_exptl_absorpt_correction_T_min  0.5078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.956
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5522
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.129
_refine_diff_density_min         -2.308
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1861
_refine_ls_number_reflns         34820
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0990
_reflns_number_gt                24293
_reflns_number_total             34820
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc05574c.txt
_cod_data_source_block           Compound_4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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      P-1
_cod_database_code               7106235
_platon_compound_4_details
;
In order to subtract the contribution from the disordered solvent molecules,
the SQUEEZE command was applied.
SQUEEZE removed six disordered CHCl3, two CH3CH2OH, and two H20
per formula unit. This valueis calculated based upon
volume/count_electrons analysis.
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.

PLAT220_ALERT_2_A
PROBLEM1: Large Non-Solvent C Ueq(max)/Ueq(min) ... 10.00 Ratio
PROBLEM2: Large Non-Solvent H Uiso(max)/Uso(min) ... 10.00 Ratio
RESPONSE: These are caused by the weak high-angle diffractions
and the disorder of tert-butyl atoms.

PLAT220_ALERT_2_B
PROBLEM: Large Non-Solvent O Ueq(max)/Ueq(min) ... 4.14 Ratio
RESPONSE: This is caused by the disorder of [PW12O40]3- anion.

CHEMW03_ALERT_2_B
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 six disordered CHCl3, two CH3CH2OH,
and two H20 omitted by SQUEEZE.

PLAT043_ALERT_1_B
PROBLEM: Check Reported Molecular Weight ................ 11634.33
RESPONSE:This is caused by the given molecular weight being increased
from the atom count to account for 6 disordered CHCl3 and
2 CH3CH2OH molecules, and tow H2O omitted by SQUEEZE.
;