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_4103094
_publ_section_title
;
 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         K20[(UO2)26(O2)28(P2O7)11]
_chemical_formula_sum            'K20 O185 P22 U26'
_chemical_formula_weight         10612.12
_chemical_name_common            U26Py11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_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                 95.2100(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   25.225(2)
_cell_length_b                   19.7976(19)
_cell_length_c                   27.139(3)
_cell_measurement_reflns_used    9324
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.76
_cell_measurement_theta_min      0.75
_cell_volume                     13497(2)
_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      100(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    0.0440
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9324
_diffrn_reflns_theta_full        17.76
_diffrn_reflns_theta_max         17.76
_diffrn_reflns_theta_min         0.75
_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    16.060
_exptl_absorpt_correction_T_max  0.598
_exptl_absorpt_correction_T_min  0.297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.611
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flake
_exptl_crystal_F_000             9164
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.032
_refine_diff_density_max         3.152
_refine_diff_density_min         -1.052
_refine_diff_density_rms         0.260
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         9324
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0866P)^2^+52.4907P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1299
_reflns_number_gt                7632
_reflns_number_total             9324
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1048219_si_009.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               4103094