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_4127367
_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 U12)'
_chemical_formula_sum            'C64 H48 O34 U6'
_chemical_formula_weight         2789.20
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   25.1420(15)
_cell_length_b                   25.1420(15)
_cell_length_c                   15.1163(9)
_cell_measurement_reflns_used    9778
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.123
_cell_measurement_theta_min      2.257
_cell_volume                     9555.3(10)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3 v2016.5-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1125
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            145182
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        22.212
_diffrn_reflns_theta_max         22.212
_diffrn_reflns_theta_min         2.107
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.100
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.5728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1266 before and 0.0648 after correction.
The Ratio of minimum to maximum transmission is 0.7690.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    0.969
_exptl_crystal_description       prism
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         3325
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0785P)^2^+76.1080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2325
_reflns_number_total             3325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04737_si_006.cif
_cod_data_source_block           oae_4_5a_sq
_cod_original_cell_volume        9555.3(13)
_cod_database_code               4127367
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.749
_shelx_estimated_absorpt_t_min   0.535
_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
 C6-C8
 1.5 with sigma of 0.02
 C8-C7
 2.5 with sigma of 0.02
 C8-C5
 2.5 with sigma of 0.02
 C5-C5_$1
 1.5 with sigma of 0.02
 C2-C1
 1.5 with sigma of 0.02
3. Restrained planarity
 O1, O2, C1, C2, C3, C4, C5, C6, C7, C8
 with sigma of 0.015
4. Uiso/Uaniso restraints and constraints
Uiso(C8) = Uiso(C6) = Uiso(C7) = Uiso(C2) = Uiso(C3) = Uiso(C4) = Uiso(C5) =
Uiso(C1)
5. Others
 Fixed Sof: O7(0.25)
6.a Riding coordinates:
 C8(H8A,H8B,H8C)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C4(H4), C3(H3)
6.c Fitted hexagon refined as free rotating group:
 C2(C7,C6,C5,C4,C3)
;
_shelx_res_checksum              70456
_shelx_hkl_checksum              58881
_shelx_fab_checksum              64190
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'