Uranium Pyrophosphate/Methylenediphosphonate Polyoxometalate Cage Clusters
Jie Ling; Jie Qiu; Ginger E. Sigmon; Matthew Ward; Jennifer E. S. Szymanowski; Peter C. Burns; Journal of the American Chemical Society 132 (2010) 13395–13402; doi:10.1021/ja1048219

data_4103095
_publ_section_title
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 Uranium Pyrophosphate/Methylenediphosphonate Polyoxometalate Cage
 Clusters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13395
_journal_page_last               13402
_journal_paper_doi               10.1021/ja1048219
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         Na4[(UO2)32(O2)32(P2O7)16]
_chemical_formula_sum            'Na4 O240 P32 U32'
_chemical_formula_weight         12539.96
_chemical_name_common            U32Py16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           107
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4 -2'
_symmetry_space_group_name_H-M   'I 4 m m'
_atom_sites_solution_hydrogens   none
_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                   28.456(3)
_cell_length_b                   28.456(3)
_cell_length_c                   28.080(7)
_cell_measurement_reflns_used    2954
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      15.71
_cell_measurement_theta_min      1.43
_cell_volume                     22738(7)
_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      273(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    0.0638
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            2954
_diffrn_reflns_theta_full        15.71
_diffrn_reflns_theta_max         15.71
_diffrn_reflns_theta_min         1.43
_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    11.531
_exptl_absorpt_correction_T_max  0.512
_exptl_absorpt_correction_T_min  0.433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10776
_exptl_crystal_size_max          0.076
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.436(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         2954
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0691
_reflns_number_gt                2595
_reflns_number_total             2954
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1048219_si_010.cif
_cod_data_source_block           i4mm
_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 
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_cod_database_code               4103095