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_4103087
_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
K11U0.5[(UO2)18(O2)18(OH)2(CH2P2O6)6(P2O7)2](H2O)3
_chemical_formula_sum            'C6 K11 O127 P16 U18.5'
_chemical_formula_weight         7433.24
_chemical_name_common            U18Py2PCP6
_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                89.4810(10)
_cell_angle_beta                 79.9640(10)
_cell_angle_gamma                62.3540(10)
_cell_formula_units_Z            2
_cell_length_a                   18.4363(9)
_cell_length_b                   19.1408(10)
_cell_length_c                   31.0479(16)
_cell_measurement_reflns_used    27827
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.40
_cell_measurement_theta_min      1.21
_cell_volume                     9524.5(8)
_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    0.0613
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27827
_diffrn_reflns_theta_full        23.40
_diffrn_reflns_theta_max         23.40
_diffrn_reflns_theta_min         1.21
_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    16.124
_exptl_absorpt_correction_T_max  0.476
_exptl_absorpt_correction_T_min  0.383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.592
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6406
_exptl_crystal_size_max          0.062
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.046
_refine_diff_density_max         5.268
_refine_diff_density_min         -1.679
_refine_diff_density_rms         0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     947
_refine_ls_number_reflns         27827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0494P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                20461
_reflns_number_total             27827
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1048219_si_002.cif
_cod_data_source_block           p-1
_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_original_formula_sum        'C6 K11 O127 P16 U18.50'
_cod_database_code               4103087