Supramolecular Assembly of Geometrically Unstable Hybrid Organic-Inorganic Uranyl Peroxide Cage Clusters and Their Transformations.
Xu, Mengyu; Traustason, Hrafn; Bo, Fabrice Dal; Hickam, Sarah; Chong, Saehwa; Zhang, Lei; Oliver, Allen G.; Burns, Peter C.; Journal of the American Chemical Society 141 (2019) 12780–12788; doi:10.1021/jacs.9b05599

data_4127749
_publ_section_title
;
 Supramolecular Assembly of Geometrically Unstable Hybrid
 Organic-Inorganic Uranyl Peroxide Cage Clusters and Their
 Transformations.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12780
_journal_page_last               12788
_journal_paper_doi               10.1021/jacs.9b05599
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C24 H16 K22.69 O151.5 P8 U18.61'
_chemical_formula_weight         8293.04
_chemical_name_common            U19
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.374(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.099(4)
_cell_length_b                   25.697(5)
_cell_length_c                   19.253(4)
_cell_measurement_reflns_used    6639
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      21.49
_cell_measurement_theta_min      2.19
_cell_volume                     9446(3)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      160(2)
_diffrn_detector_area_resol_mean 8.33
_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       'combination of \w and \f-scans '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0959
_diffrn_reflns_av_unetI/netI     0.1069
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            81504
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        23.256
_diffrn_reflns_theta_max         23.256
_diffrn_reflns_theta_min         1.058
_diffrn_source                   'Incoatec micro-focus'
_exptl_absorpt_coefficient_mu    16.563
_exptl_absorpt_correction_T_max  0.0932
_exptl_absorpt_correction_T_min  0.0432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Krause 2015)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.916
_exptl_crystal_description       block
_exptl_crystal_F_000             7270
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.190
_refine_diff_density_min         -2.999
_refine_diff_density_rms         0.322
_refine_ls_abs_structure_details
;
 Flack x determined using 7759 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1124
_refine_ls_number_reflns         27147
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+56.4956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1438
_refine_ls_wR_factor_ref         0.1590
_reflns_Friedel_coverage         0.949
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                20793
_reflns_number_total             27147
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05599_si_002.cif
_cod_data_source_block           u19
_cod_original_formula_sum        'C24 H16 K22.69 O151.50 P8 U18.61'
_cod_database_code               4127749
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.190
_shelx_estimated_absorpt_t_max   0.636
_diffrn_source_monochromator     'MONTEL Multi-layer'
_shelx_res_checksum              83986
_shelx_hkl_checksum              71242