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_4103089
_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         K14[(UO2)20(O2)24(P2O7)6](H2o)2
_chemical_formula_sum            'K14 O132 P12 U20'
_chemical_formula_weight         7791.64
_chemical_name_common            U20Py6b
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 115.851(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   35.968(5)
_cell_length_b                   18.094(2)
_cell_length_c                   31.033(5)
_cell_measurement_reflns_used    13778
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      23.81
_cell_measurement_theta_min      1.29
_cell_volume                     18175(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      273(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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    0.1164
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13778
_diffrn_reflns_theta_full        23.81
_diffrn_reflns_theta_max         23.81
_diffrn_reflns_theta_min         1.29
_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    18.265
_exptl_absorpt_correction_T_max  0.373
_exptl_absorpt_correction_T_min  0.267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.847
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             13368
_exptl_crystal_size_max          0.076
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.054
_refine_diff_density_max         4.099
_refine_diff_density_min         -2.792
_refine_diff_density_rms         0.331
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         13778
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1600
_reflns_number_gt                8007
_reflns_number_total             13778
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1048219_si_004.cif
_cod_data_source_block           c2c
_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               4103089