Hybrid Uranyl-Carboxyphosphonate Cage Clusters
Pius O. Adelani; Michael Ozga; Christine M. Wallace; Jie Qiu; Jennifer E. S. Szymanowski; Ginger E. Sigmon; Peter C. Burns; Inorganic Chemistry 52 (2013) 7673–7679; doi:10.1021/ic4008262

data_4335382
_publ_section_title
;
 Hybrid Uranyl-Carboxyphosphonate Cage Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7673
_journal_page_last               7679
_journal_paper_doi               10.1021/ic4008262
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C70 H40 K18 Li4 O167 P10 U20'
_chemical_formula_sum            'C70 H40 K18 Li4 O167 P10 U20'
_chemical_formula_weight         9354.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.498(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.975(3)
_cell_length_b                   34.567(5)
_cell_length_c                   21.848(3)
_cell_measurement_reflns_used    9802
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.24
_cell_volume                     13253(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0584
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            103701
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.605
_exptl_absorpt_correction_T_max  0.6057
_exptl_absorpt_correction_T_min  0.2286
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SHELXPREP
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.344
_exptl_crystal_description       tablet
_exptl_crystal_F_000             8280
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.192
_platon_squeeze_details
;
;
_refine_diff_density_max         7.626
_refine_diff_density_min         -6.533
_refine_diff_density_rms         0.538
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.665
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1303
_refine_ls_number_reflns         29825
_refine_ls_number_restraints     353
_refine_ls_restrained_S_all      1.660
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0749P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1951
_refine_ls_wR_factor_ref         0.2078
_reflns_number_gt                21796
_reflns_number_total             29825
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4008262_si_002_1.cif
_cod_data_source_block           p21c
_cod_original_cell_volume        13253(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4335382