Complex nanoscale Cage Clusters Built from Uranyl Polyhedra and Phosphate Tetrahedra
Daniel K. Unruh; Jie Ling; Jie Qiu; Laura Pressprich; Melissa Baranay; Matthew Ward; Peter C. Burns; Inorganic Chemistry 50 (2011) 5509–5516; doi:10.1021/ic200065y

data_4325385
_publ_section_title
;
 Complex nanoscale Cage Clusters Built from Uranyl Polyhedra and Phosphate
 Tetrahedra
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5509
_journal_page_last               5516
_journal_paper_doi               10.1021/ic200065y
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'Ba15 O675 Rb29 U90'
_chemical_formula_weight         36759.57
_chemical_name_common            U30a
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           160
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   55.286(5)
_cell_length_b                   55.286(5)
_cell_length_c                   20.523(2)
_cell_measurement_reflns_used    9701
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      24.13
_cell_measurement_theta_min      2.21
_cell_volume                     54325(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CrystalMaker 8.3.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0770
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_max       65
_diffrn_reflns_limit_h_min       -65
_diffrn_reflns_limit_k_max       65
_diffrn_reflns_limit_k_min       -65
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            180085
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    22.888
_exptl_absorpt_correction_T_max  0.6134
_exptl_absorpt_correction_T_min  0.3664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.371
_exptl_crystal_description       blocky
_exptl_crystal_F_000             46779
_exptl_crystal_size_max          .120
_exptl_crystal_size_mid          .100
_exptl_crystal_size_min          .100
_refine_diff_density_max         3.211
_refine_diff_density_min         -2.094
_refine_diff_density_rms         0.286
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.004(6)
_refine_ls_extinction_coef       0.0000014(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         22208
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0945
_reflns_number_gt                18603
_reflns_number_total             22208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200065y_si_001_1.cif
_cod_data_source_block           ellip_r3m
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               4325385