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_4131726
_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         'C84 H60 F6 O38 Th6'
_chemical_formula_sum            'C84 H60 F6 O38 Th6'
_chemical_formula_weight         3183.56
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-02-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.8409(11)
_cell_length_b                   23.8409(11)
_cell_length_c                   19.7162(10)
_cell_measurement_reflns_used    9438
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.11
_cell_measurement_theta_min      2.39
_cell_volume                     11206.5(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0581
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            273809
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        28.250
_diffrn_reflns_theta_max         28.365
_diffrn_reflns_theta_min         2.172
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.007
_exptl_absorpt_correction_T_max  0.3343
_exptl_absorpt_correction_T_min  0.2159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1351 before and 0.0541 after correction.
The Ratio of minimum to maximum transmission is 0.6458.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.943
_exptl_crystal_description       needle
_exptl_crystal_F_000             2924
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.488
_refine_diff_density_min         -1.600
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         7531
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0502P)^2^+32.3372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6173
_reflns_number_total             7531
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b09496_si_008.cif
_cod_data_source_block           h17_1_1m_sq
_cod_original_cell_volume        11206.5(12)
_cod_database_code               4131726
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.326
_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
 C13-C13_$3
 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
 C15-C16
 1.45 with sigma of 0.015
 F2-C16 = F1-C16
 1.35 with sigma of 0.01
 C14-C12
 1.54 with sigma of 0.02
 C8-C4
 1.54 with sigma of 0.01
 C11-C14 \\sim C13-C14
 with sigma of 0.015
3. Restrained planarity
 C9, C10, C11, C12, C13
 with sigma of 0.01
 C13, C14, C12, C11, C10
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uiso(C9) = Uiso(C10) = Uiso(C11) = Uiso(C12) = Uiso(C13)
5. Others
 Fixed Sof: C11(0.5) H11(0.5) C12(0.5) H12(0.25) C14(0.25) H14A(0.25)
 H14B(0.25) H14C(0.25) F1(0.25) F2(0.5)
 Fixed Uiso: C14(0.2) C16(0.15) F1(0.2) F2(0.2)
6.a Riding coordinates:
 C11(H11), C12(H12), C14(H14A,H14B,H14C)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C6(H6)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              78395
_shelx_hkl_checksum              92915
_shelx_fab_checksum              34905
_olex2_submission_special_instructions 'No special instructions were received'