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_4131727
_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(C168 H112 O64 Zr12)'
_chemical_formula_sum            'C84 H56 O32 Zr6'
_chemical_formula_weight         2124.60
_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             2017-10-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.9392(11)
_cell_length_b                   23.9392(11)
_cell_length_c                   15.6881(8)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.28
_cell_measurement_theta_min      2.30
_cell_volume                     8990.6(7)
_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 0.997
_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  0.2142
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            111268
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        23.299
_diffrn_reflns_theta_max         23.299
_diffrn_reflns_theta_min         2.140
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0796 before and 0.0695 after correction.
The Ratio of minimum to maximum transmission is 0.9099.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.785
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.170
_refine_diff_density_min         -1.068
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.020(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.398
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         3572
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.459
_refine_ls_R_factor_all          0.1310
_refine_ls_R_factor_gt           0.1084
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3373
_refine_ls_wR_factor_ref         0.3533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2582
_reflns_number_total             3572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b09496_si_010.cif
_cod_data_source_block           pcn700_po_sq
_cod_original_cell_volume        8990.6(9)
_cod_database_code               4131727
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.956
_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
 C9-C10
 1.44 with sigma of 0.02
 C5-C5_$1 = C14-C13
 1.5 with sigma of 0.02
 C15_$2-C15_$3
 1.4 with sigma of 0.01
 O3-C1 = O4-C1 = O6-C9
 1.27 with sigma of 0.02
 C11-C10 \\sim C12-C11 \\sim C13-C12 \\sim C15-C14 \\sim C2-C3 \\sim C3-C4
\\sim C4-C5 \\sim C5-C6 \\sim C6-C7
 \\sim C7-C2
 with sigma of 0.01
 C3-C8 \\sim C5-C8
 with sigma of 0.015
3. Restrained planarity
 C1, C2, C3, C4, C8, C5, C6, C7
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C8) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7)
\\sim Ueq: with sigma of 0.015 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uiso(C15) = Uiso(C14) = Uiso(C13) = Uiso(C12) = Uiso(C11) = Uiso(C10) = Uiso(C9)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C11(H11), C12(H12)
5.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              24516
_shelx_hkl_checksum              60373
_shelx_fab_checksum              54082
_olex2_submission_special_instructions 'No special instructions were received'