Thermodynamics and Electronic Properties of Heterometallic Multinuclear Actinide-Containing Metal-Organic Frameworks with "Structural Memory".
Ejegbavwo, Otega A.; Martin, Corey R.; Olorunfemi, Oyindamola A.; Leith, Gabrielle A.; Ly, Richard T.; Rice, Allison M.; Dolgopolova, Ekaterina A.; Smith, Mark D.; Karakalos, Stavros G.; Birkner, Nancy; Powell, Brian A.; Pandey, Shubham; Koch, Robert J.; Misture, Scott T.; Loye, Hans-Conrad Zur; Phillpot, Simon R.; Brinkman, Kyle S.; Shustova, Natalia B.; Journal of the American Chemical Society 141 (2019) 11628–11640; doi:10.1021/jacs.9b04737

data_4127363
_publ_section_title
;
 Thermodynamics and Electronic Properties of Heterometallic Multinuclear
 Actinide-Containing Metal-Organic Frameworks with &quot;Structural
 Memory&quot;.
;
_journal_issue                   29
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11628
_journal_page_last               11640
_journal_paper_doi               10.1021/jacs.9b04737
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '0.5(C128 H96 O68 Th12)'
_chemical_formula_sum            'C64 H48 O34 Th6'
_chemical_formula_weight         2753.26
_space_group_crystal_system      tetragonal
_space_group_IT_number           131
_space_group_name_Hall           '-P 4c 2'
_space_group_name_H-M_alt        'P 42/m m c'
_symmetry_space_group_name_Hall  '-P 4c 2'
_symmetry_space_group_name_H-M   'P 42/m m c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   25.5223(17)
_cell_length_b                   25.5223(17)
_cell_length_c                   14.6275(11)
_cell_measurement_reflns_used    9677
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      2.26
_cell_volume                     9528.2(11)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX3 v2016.5-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker PHOTON-100 area detector'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1546
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            182288
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.167
_diffrn_reflns_theta_max         25.167
_diffrn_reflns_theta_min         2.118
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.699
_exptl_absorpt_correction_T_max  0.6936
_exptl_absorpt_correction_T_min  0.5224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0956 before and 0.0720 after correction.
The Ratio of minimum to maximum transmission is 0.7532.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.960
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.260
_refine_diff_density_min         -2.615
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         4669
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1223
_refine_ls_R_factor_gt           0.0895
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1150P)^2^+186.6628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2378
_refine_ls_wR_factor_ref         0.2657
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3016
_reflns_number_total             4669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04737_si_003.cif
_cod_data_source_block           oae123a_sq
_cod_original_cell_volume        9528.2(15)
_cod_database_code               4127363
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.766
_shelx_estimated_absorpt_t_min   0.559
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2-C1
 1.5 with sigma of 0.02
 C8-C4
 1.5 with sigma of 0.02
 C5-C5_$1
 1.5 with sigma of 0.02
 O3-C1 \\sim O4-C1
 with sigma of 0.01
 C3-C8 \\sim C5-C8
 with sigma of 0.01
3. Restrained planarity
 O3, C1, O4, C2, C7, C6, C5, C4, C3
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq,
Uanis(O6) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O7) \\sim
Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O3) = Uanis(C1) = Uanis(O4) = Uanis(C2) = Uanis(C7) = Uanis(C5) =
Uanis(C6) = Uanis(C4) = Uanis(C3) = Uanis(C8)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C3(H3)
5.b Fitted hexagon refined as free rotating group:
 C2(C7,C6,C5,C4,C3)
5.c Idealised Me refined with riding coordinates:
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              72643
_shelx_hkl_checksum              50904
_shelx_fab_checksum              19932
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'