A Multiunit Catalyst with Synergistic Stability and Reactivity: A Polyoxometalate-Metal Organic Framework for Aerobic Decontamination
Jie Song; Zhen Luo; David K. Britt; Hiroyasu Furukawa; Omar M. Yaghi; Kenneth I. Hardcastle; Craig L. Hill; Journal of the American Chemical Society 133 (2011) 16839–16846; doi:10.1021/ja203695h

data_4106985
_publ_section_title
;
 A Multiunit Catalyst with Synergistic Stability and Reactivity: A
 Polyoxometalate-Metal Organic Framework for Aerobic Decontamination
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16839
_journal_page_last               16846
_journal_paper_doi               10.1021/ja203695h
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C88 H153 Cu13 N4 O127 P W11'
_chemical_formula_sum            'C77 H30 Cu13 N1.25 O110.56 P W11'
_chemical_formula_weight         5620.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           225
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 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            4
_cell_length_a                   26.307(2)
_cell_length_b                   26.307(2)
_cell_length_c                   26.307(2)
_cell_measurement_reflns_used    4584
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.98
_cell_measurement_theta_min      2.19
_cell_volume                     18206(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1396
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            78158
_diffrn_reflns_theta_full        27.85
_diffrn_reflns_theta_max         27.85
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    8.500
_exptl_absorpt_correction_T_max  0.5876
_exptl_absorpt_correction_T_min  0.3824
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.051
_exptl_crystal_description       block
_exptl_crystal_F_000             10365
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
_vrf_PLAT601_ALERT_2_A 

 PROBLEM:  Structure Contains Solvent Accessible VOIDS of  879 A**3. 
 Electron density could be identified within these voids. These voids
 contain water and disordered [(CH3)4N] cations that are only partially
 resolved and too disordered to be modelled effectively. 
 The data were therefore treated by using PLATON/SQUEEZE.

 PLAT041_ALERT_1_C Calc. and Reported SumFormula Strings Differ ?
 The _chemical_formula_moiety is that from chemical analysis whereas
 the _chemical_formula_sum does not contain the squeezed material.
 
 PLATON/SQUEEZE - An Effective Tool for Taking the Contribution 
 of Disordered Solvent into Account in Crystal Structure Refinement. 
 Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13.

;
_refine_diff_density_max         3.005
_refine_diff_density_min         -2.793
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1148
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0567
_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^)+(0.1900P)^2^+19.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1788
_refine_ls_wR_factor_ref         0.2468
_reflns_number_gt                811
_reflns_number_total             1148
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja203695h_si_002.cif
_cod_data_source_block           js100118n
_cod_original_cell_volume        18207(3)
_cod_database_code               4106985