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_4130526
_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 K N2 O6), 0.660(Bi7 Pb7 U), 0.340(Bi9 Pb4 U),
 2(C7 H8)
;
_chemical_formula_sum            'C68 H124 Bi7.68 K3 N6 O18 Pb5.98 U'
_chemical_formula_weight         4512.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 96.032(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1698(3)
_cell_length_b                   23.0713(5)
_cell_length_c                   30.3293(7)
_cell_measurement_reflns_used    53051
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      2.48
_cell_volume                     10556.1(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'IPDS/2T (Stoe)'
_diffrn_measurement_method       omega-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0981
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            93332
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.811
_diffrn_reflns_theta_min         2.476
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    23.946
_exptl_absorpt_correction_T_max  0.079
_exptl_absorpt_correction_T_min  0.034
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'Coppens et al. (1965)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.840
_exptl_crystal_description       block
_exptl_crystal_F_000             7979
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.098
_refine_diff_density_max         1.921
_refine_diff_density_min         -2.230
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1027
_refine_ls_number_reflns         22367
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0653
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13792
_reflns_number_total             22367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04363_si_003.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4130526
_shelxl_version_number           2013-4
_shelx_res_checksum              8745