Main Group Metal-Actinide Magnetic Coupling and Structural Response Upon U(4+) Inclusion Into Bi, Tl/Bi, or Pb/Bi Cages.
Lichtenberger, Niels; Wilson, Robert J.; Eulenstein, Armin R.; Massa, Werner; Clérac, Rodolphe; Weigend, Florian; Dehnen, Stefanie; Journal of the American Chemical Society 138 (2016) 9033–9036; doi:10.1021/jacs.6b04363

data_4130527
_publ_section_title
;
 Main Group Metal-Actinide Magnetic Coupling and Structural Response Upon
 U(4+) Inclusion Into Bi, Tl/Bi, or Pb/Bi Cages.
;
_journal_issue                   29
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9033
_journal_page_last               9036
_journal_paper_doi               10.1021/jacs.6b04363
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety
;
3(C18 H36 N2 O6 K), Bi12 U, C7 H8, 1.5(C2 H8 N2)
;
_chemical_formula_sum            'C64 H84 Bi12 K3 N9 O18 U'
_chemical_formula_weight         4130.49
_space_group_crystal_system      orthorhombic
_space_group_IT_number           32
_space_group_name_Hall           'P 2 -2ab'
_space_group_name_H-M_alt        'P b a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.7268(6)
_cell_length_b                   39.3976(12)
_cell_length_c                   16.6980(3)
_cell_measurement_reflns_used    38575
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.81
_cell_measurement_theta_min      1.33
_cell_volume                     20871.8(8)
_computing_cell_refinement       'XAREA 1.66 (Stoe 2013)'
_computing_data_collection       'XAREA 1.66 (Stoe 2013)'
_computing_data_reduction        'XAREA 1.66 (Stoe 2013)'
_computing_molecular_graphics    'DIAMOND 3.2k (Brandenburg 2014)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.7
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'IPDS-II (Stoe)'
_diffrn_measurement_method       omega-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_av_unetI/netI     0.1377
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            115730
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.384
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    21.871
_exptl_absorpt_correction_T_max  0.0767
_exptl_absorpt_correction_T_min  0.0229
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'Coppens et al. (1965)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.629
_exptl_crystal_description       block
_exptl_crystal_F_000             14560
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.384
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.256
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.539(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         35066
_refine_ls_number_restraints     187
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.1206
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0935
_reflns_Friedel_coverage         0.931
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                15911
_reflns_number_total             35066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04363_si_001.cif
_cod_data_source_block           shelx
_cod_database_code               4130527
_shelxl_version_number           2013-4
_shelx_res_checksum              38905