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_4131728
_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         '0.5(C143.13 H96 O98.76 Th12 U8.09), 4(O1.2)'
_chemical_formula_sum            'C71.57 H48 O54.18 Th6 U4.05'
_chemical_formula_weight         4129.75
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-05-24 deposited with the CCDC.
2017-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.1119(14)
_cell_length_b                   24.1119(14)
_cell_length_c                   19.0718(11)
_cell_measurement_reflns_used    9217
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      2.45
_cell_volume                     11088.0(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0787
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            218890
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.405
_diffrn_reflns_theta_max         26.407
_diffrn_reflns_theta_min         2.136
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.992
_exptl_absorpt_correction_T_max  0.6939
_exptl_absorpt_correction_T_min  0.5248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0812 before and 0.0611 after correction.
The Ratio of minimum to maximum transmission is 0.7563.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       needle
_exptl_crystal_F_000             3646
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.644
_refine_diff_density_min         -3.568
_refine_diff_density_rms         0.317
_refine_ls_extinction_coef       0.00030(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         6167
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.239
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0980
_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^)+(0.0066P)^2^+591.1290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2063
_refine_ls_wR_factor_ref         0.2109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5487
_reflns_number_total             6167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b09496_si_002.cif
_cod_data_source_block           h17_u1_0m_sq
_cod_original_cell_volume        11088.0(14)
_cod_database_code               4131728
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.679
_shelx_estimated_absorpt_t_min   0.401
_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
 C4-C8
 1.54 with sigma of 0.02
 O8-C15
 1.25 with sigma of 0.02
 C16-C15
 1.54 with sigma of 0.02
 C9-C10
 1.54 with sigma of 0.02
 U3-O31 \\sim U1-O11 \\sim U2-O21 \\sim U4-O41 \\sim U5-O51 \\sim U6-O61
 with sigma of 0.015
 O5A-C9 \\sim O5B-C9
 with sigma of 0.015
3. Restrained planarity
 C1, C2, C3, C4, C5, C6, C7, C8
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C8) \\sim Ueq: with sigma of 0.015 and sigma for terminal atoms of 0.03
Uanis(U1) \\sim Ueq: with sigma of 0.0025 and sigma for terminal atoms of 0.005
Uanis(U2) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uiso(O7A) = Uiso(O7B)
Uiso(C9) = Uiso(C10)
Uiso(O51) = Uiso(U5)
Uiso(U6) = Uiso(O61)
5. Rigid body (RIGU) restrains
 O3, C1, O4, C2, C7, C6, C5, C4, C3, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(U1)=0.5*FVAR(2)
 Sof(O11)=FVAR(1)
 Sof(U2)=0.5*FVAR(3)
 Sof(O21)=FVAR(2)
 Sof(U3)=0.5*FVAR(4)
 Sof(O31)=FVAR(3)
 Sof(U4)=0.5*FVAR(5)
 Sof(O41)=FVAR(4)
 Sof(U5)=0.5*FVAR(6)
 Sof(O51)=FVAR(5)
 Sof(C15)=Sof(C16)=0.25*(1-FVAR(7))
 Sof(U6)=0.5*FVAR(7)
 Sof(O61)=FVAR(6)
 Fixed Sof: O5A(0.25) O5B(0.25) C9(0.25) C10(0.25) O7A(0.25) O7B(0.25) O72(0.25)
 Fixed Uiso: C15(0.08) C16(0.08) O71(0.1) O73(0.1) O74(0.1) O75(0.1)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7)
7.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              69115
_shelx_hkl_checksum              51635
_shelx_fab_checksum              75778
_olex2_submission_special_instructions 'No special instructions were received'