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_4131730
_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(C128 H96 O80.37 U1.76 Zr12)'
_chemical_formula_sum            'C64 H48 O40.08 U0.88 Zr6'
_chemical_formula_weight         2213.98
_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             2017-03-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.0528(9)
_cell_length_b                   24.0528(9)
_cell_length_c                   15.7060(7)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.70
_cell_measurement_theta_min      2.29
_cell_volume                     9086.5(6)
_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 0.998
_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  0.1721
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            83728
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.088
_diffrn_reflns_theta_max         25.088
_diffrn_reflns_theta_min         2.133
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0789 before and 0.0617 after correction.
The Ratio of minimum to maximum transmission is 0.8565.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.809
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             2146
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.089
_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     154
_refine_ls_number_reflns         4425
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0586
_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^)+(0.1243P)^2^+7.4385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.2046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2893
_reflns_number_total             4425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b09496_si_004.cif
_cod_data_source_block           oe_zru_sq
_cod_original_cell_volume        9086.5(8)
_cod_database_code               4131730
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.934
_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
 U1-O11 = U1-O12 = U2-O21 = U2-O22
 1.77 with sigma of 0.02
 C8-C4
 1.55 with sigma of 0.02
 O4-O21
 -2.7 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.015 and
sigma for terminal atoms of 0.03
4. Rigid body (RIGU) restrains
 O4, C1, O3, C2, C7, C6, C5, C4, C8, C3
 with sigma for 1-2 distances of 0.015 and sigma for 1-3 distances of 0.015
5. Others
 Fixed Uiso: O11(0.15) O12(0.15) O21(0.15) O22(0.15)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7)
6.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              44692
_shelx_hkl_checksum              77123
_shelx_fab_checksum              29967
_olex2_submission_special_instructions 'No special instructions were received'