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_4127365
_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         'C80 H60 O37 Th6'
_chemical_formula_sum            'C80 H60 O37 Th6'
_chemical_formula_weight         3005.52
_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             2018-07-10
_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                   24.0205(8)
_cell_length_b                   24.0205(8)
_cell_length_c                   19.7574(6)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      26.140
_cell_measurement_theta_min      2.385
_cell_volume                     11399.7(6)
_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      301(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  0.1035
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            116021
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.410
_diffrn_reflns_theta_max         26.410
_diffrn_reflns_theta_min         2.158
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.933
_exptl_absorpt_correction_T_max  0.6198
_exptl_absorpt_correction_T_min  0.4251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1181 before and 0.0655 after correction.
The Ratio of minimum to maximum transmission is 0.6859.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.876
_exptl_crystal_description       needle
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.314
_refine_diff_density_min         -1.267
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         6309
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0460P)^2^+2.3044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4561
_reflns_number_total             6309
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04737_si_011.cif
_cod_data_source_block           th10meoh_rt_sq
_cod_original_cell_volume        11399.7(8)
_cod_database_code               4127365
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.859
_shelx_estimated_absorpt_t_min   0.538
_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. Shared sites
{C2A, C2B}
{C3A, C7B}
{C4A, C6B}
{C5A, C5B}
{C6A, C4B}
{C7A, C3B}
3. Restrained distances
 C8A-C4A = C8B-C4B
 1.54 with sigma of 0.02
 C13-C13_$1
 1.5 with sigma of 0.02
 C9-C10
 1.48 with sigma of 0.015
 C11-C10
 1.39 with sigma of 0.015
 C12-C11
 1.39 with sigma of 0.015
 C13-C12
 1.39 with sigma of 0.015
 C14-C12
 1.54 with sigma of 0.02
 C11-C14 \\sim C13-C14
 with sigma of 0.011
 C10-C12 \\sim C11-C13
 with sigma of 0.01
4. Restrained planarity
 C9, C10, C11, C12, C13, C14
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(C8A) \\sim Ueq, Uanis(C8B) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C5B)
\\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C6B) \\sim Ueq, Uanis(C3A) \\sim Ueq,
Uanis(C7B) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C2B) \\sim Ueq, Uanis(C7A)
\\sim Ueq, Uanis(C3B) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C4B) \\sim Ueq:
with sigma of 0.015 and sigma for terminal atoms of 0.03
Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C2A) = Uanis(C2B)
Uanis(C3A) = Uanis(C7B)
Uanis(C4A) = Uanis(C6B)
Uanis(C5A) = Uanis(C5B)
Uanis(C6A) = Uanis(C4B)
Uanis(C7A) = Uanis(C3B)
Uiso(C10) = Uiso(C11) = Uiso(C12) = Uiso(C13) = Uiso(C14)
6. Others
 Fixed Sof: C2A(0.5) C3A(0.5) H3A(0.5) C4A(0.5) C5A(0.5) C6A(0.5) H6A(0.5)
 C7A(0.5) H7A(0.5) C8A(0.5) H8AA(0.5) H8AB(0.5) H8AC(0.5) C2B(0.5) C3B(0.5)
 H3B(0.5) C4B(0.5) C5B(0.5) C6B(0.5) H6B(0.5) C7B(0.5) H7B(0.5) C8B(0.5)
 H8BA(0.5) H8BB(0.5) H8BC(0.5) C11(0.5) H11(0.5) C12(0.5) H12(0.25) C14(0.25)
 H14A(0.25) H14B(0.25) H14C(0.25) O7A(0.375) O7B(0.375) O7C(0.125)
7.a Riding coordinates:
 C11(H11), C12(H12), C14(H14A,H14B,H14C)
7.b Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C6A(H6A), C7A(H7A), C3B(H3B), C6B(H6B), C7B(H7B)
7.c Idealised Me refined as rotating group:
 C8A(H8AA,H8AB,H8AC), C8B(H8BA,H8BB,H8BC)
;
_shelx_res_checksum              8615
_shelx_hkl_checksum              90039
_shelx_fab_checksum              4153
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'