Multifaceted Modularity: A Key for Stepwise Building of Hierarchical Complexity in Actinide Metal-Organic Frameworks.
Dolgopolova, Ekaterina A.; Ejegbavwo, Otega A.; Martin, Corey R.; Smith, Mark D.; Setyawan, Wahyu; Karakalos, Stavros G.; Henager, Charles H.; Zur Loye, Hans-Conrad; Shustova, Natalia B.; Journal of the American Chemical Society 139 (2017) 16852–16861; doi:10.1021/jacs.7b09496

data_4131732
_publ_section_title
;
 Multifaceted Modularity: A Key for Stepwise Building of Hierarchical
 Complexity in Actinide Metal-Organic Frameworks.
;
_journal_issue                   46
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16852
_journal_page_last               16861
_journal_paper_doi               10.1021/jacs.7b09496
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C120 H90 N6 O38 Th6'
_chemical_formula_sum            'C120 H90 N6 O38 Th6'
_chemical_formula_weight         3616.21
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.0484(16)
_cell_length_b                   34.0484(16)
_cell_length_c                   34.0484(16)
_cell_measurement_reflns_used    9179
_cell_measurement_temperature    302(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.39
_cell_volume                     39472(3)
_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      302(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  0.1065
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            79586
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.036
_diffrn_reflns_theta_max         25.036
_diffrn_reflns_theta_min         2.608
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.278
_exptl_absorpt_correction_T_max  0.3526
_exptl_absorpt_correction_T_min  0.2770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0850 before and 0.0716 after correction.
The Ratio of minimum to maximum transmission is 0.7856.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.609
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             6784
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         1779
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0384P)^2^+455.2714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1530
_reflns_number_total             1779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b09496_si_009.cif
_cod_data_source_block           p131_4b_sq
_cod_original_cell_volume        39472(6)
_cod_database_code               4131732
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.839
_shelx_estimated_absorpt_t_min   0.839
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C7_$1
 1.4 with sigma of 0.015
 N1-C7
 1.4 with sigma of 0.015
 C3-C2 \\sim C5-C4 \\sim C7-C6
 with sigma of 0.015
 N1-C6 \\sim N1-C7_$1
 with sigma of 0.02
3. Restrained planarity
 C6, C7, C7_$1, C6_$2, C7_$3, C7_$4, N1
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C6) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.0175 and sigma
for terminal atoms of 0.025
5. Others
 Fixed Sof: O3(0.125) C7(0.5) H7(0.875) N1(0.125)
 Fixed Uiso: O3(0.1) C7(0.15) N1(0.15)
6.a Riding coordinates:
 C7(H7)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
;
_shelx_res_checksum              19610
_shelx_hkl_checksum              29017
_shelx_fab_checksum              47105
_olex2_submission_special_instructions 'No special instructions were received'