Experimental and Computational Study of a New Wheel-Shaped {[W5O21]3[(UVIO2)2(μ-O2)]3}30- Polyoxometalate
Pere Miró; Jie Ling; Jie Qiu; Peter C. Burns; Laura Gagliardi; Christopher J. Cramer; Inorganic Chemistry 51 (2012) 8784–8790; doi:10.1021/ic3005536

data_4330024
_publ_section_title
;
 Experimental and Computational Study of a New Wheel-Shaped
 {[W5O21]3[(UVIO2)2(\m-O2)]3}30- Polyoxometalate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8784
_journal_page_last               8790
_journal_paper_doi               10.1021/ic3005536
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         Na[(UO2)6(O2)3(W5O21)3](H2O)38
_chemical_formula_sum            'Na O119 U6 W15'
_chemical_formula_weight         6112.92
_chemical_name_common            U6w15
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                65.962(2)
_cell_angle_beta                 87.062(2)
_cell_angle_gamma                85.706(2)
_cell_formula_units_Z            4
_cell_length_a                   18.675(3)
_cell_length_b                   25.903(5)
_cell_length_c                   29.294(5)
_cell_measurement_reflns_used    42635
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.53
_cell_measurement_theta_min      1.32
_cell_volume                     12902(4)
_computing_cell_refinement       'SMART SAINT'
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELCIF-97 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '0.3 wide w/ exposures'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.4772
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            42635
_diffrn_reflns_theta_full        24.53
_diffrn_reflns_theta_max         24.53
_diffrn_reflns_theta_min         1.32
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count N/A
_diffrn_standards_interval_time  N/A
_diffrn_standards_number         N/A
_exptl_absorpt_coefficient_mu    20.920
_exptl_absorpt_correction_T_max  0.631
_exptl_absorpt_correction_T_min  0.401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.147
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             10500
_exptl_crystal_size_max          0.046
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.022
_refine_diff_density_max         3.749
_refine_diff_density_min         -5.867
_refine_diff_density_rms         0.857
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1369
_refine_ls_number_reflns         42635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.3056
_refine_ls_R_factor_gt           0.1385
_refine_ls_shift/su_max          0.117
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1548P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2985
_refine_ls_wR_factor_ref         0.3576
_reflns_number_gt                17045
_reflns_number_total             42635
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3005536_si_001.cif
_cod_data_source_block           test
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4330024