Controlling the secondary assembly of porous anionic uranyl-organic polyhedra through organic cationic templates.
Zeng, Li-Wen; Hu, Kong-Qiu; Huang, Zhi-Wei; Mei, Lei; Kong, Xiang-He; Liu, Kang; Zhang, Xiao-Lin; Zhang, Zhi-Hui; Chai, Zhi-Fang; Shi, Wei-Qun; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4499–4503; doi:10.1039/d1dt00289a

data_7706842
_publ_section_title
;
 Controlling the secondary assembly of porous anionic uranyl-organic
 polyhedra through organic cationic templates.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4499
_journal_page_last               4503
_journal_paper_doi               10.1039/d1dt00289a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C84 H112 N24 O32 U4, 2(C7.532 H15 N2), 0.936(C), 6(C3 H7 N O)'
_chemical_formula_sum            'C118 H184 N34 O38 U4'
_chemical_formula_weight         3639.10
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc26k0jb
_audit_creation_date             2021-03-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2021-03-05 deposited with the CCDC.	2021-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.1058(4)
_cell_length_b                   18.1058(4)
_cell_length_c                   27.6190(6)
_cell_measurement_reflns_used    9813
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      68.28
_cell_measurement_theta_min      2.92
_cell_volume                     9054.1(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            25736
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.419
_diffrn_reflns_theta_min         4.710
_exptl_absorpt_coefficient_mu    10.518
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.3728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1594 before and 0.0759 after correction.
The Ratio of minimum to maximum transmission is 0.4950.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       block
_exptl_crystal_F_000             3604
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.090
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.159
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.647(10)
_refine_ls_extinction_coef       0.000209(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         8188
_refine_ls_number_restraints     505
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0695P)^2^+17.3363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.931
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                7970
_reflns_number_total             8188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00289a2.cif
_cod_data_source_block           cu_zxl_20170909_114_hu6a_0m_sq
_cod_depositor_comments
'Adding full bibliography for 7706841--7706842.cif.'
_cod_original_cell_volume        9054.1(4)
_cod_database_code               7706842
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.353(10)
 0.647(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C22-N7
 1.55 with sigma of 0.01
 C29-C37 = C37-C35
 1.54 with sigma of 0.01
 C29-C34 = C34-C36
 1.54 with sigma of 0.01
 C29-C25
 1.54 with sigma of 0.01
 C27-C23
 1.4 with sigma of 0.01
 H3-H5B
 2.2 with sigma of 0.01
 H3-H18A
 2.2 with sigma of 0.01
4. Restrained planarity
 C28, C26, N10, C33, O9
 with sigma of 0.1
 C32, C31, C30, O12, O14
 with sigma of 0.1
 N7, C23, C27, N8, C24
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
C27 \\sim N8 \\sim C24 \\sim N7 \\sim C23 \\sim C22: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O9) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O14) \\sim Ueq,
Uanis(C29) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(O12)=1-FVAR(1)
 Sof(O14)=FVAR(1)
 Sof(C36)=Sof(C34)=0.5*(1-FVAR(3))
 Sof(C37)=Sof(C35)=0.5*FVAR(3)
 Fixed Sof: H37A(0.5) H37B(0.5) H35A(0.5) H35B(0.5) H35C(0.5) C33(0.5)
 H33(0.5) C29(0.5) H34(0.5) H29(0.5) C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5)
 C27(0.5) H27(0.5) C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5) C25(0.5) H25A(0.5)
 H25B(0.5) C24(0.5) H24(0.5) C23(0.5) H23(0.5) H22A(0.5) H22B(0.5) H22C(0.5)
 N7(0.5) N8(0.5) O9(0.5) N10(0.5)
8.a Ternary CH refined with riding coordinates:
 C2(H2), C9(H9), C15(H15)
8.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C37(H37A,H37B), C29(H34,H29), C25(H25A,H25B), C4(H4A,H4B),
 C6(H6A,H6B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B), C11(H11A,H11B), C12(H12A,
 H12B), C13(H13A,H13B), C14(H14A,H14B), C17(H17A,H17B), C18(H18A,H18B)
8.c Me refined with riding coordinates:
 C22(H22A,H22B,H22C)
8.d Aromatic/amide H refined with riding coordinates:
 C33(H33), C30(H30), C27(H27), C24(H24), C23(H23), N3(H3)
8.e Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C28(H28A,H28B,
 H28C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              53134
_shelx_hkl_checksum              9602
_shelx_fab_checksum              75384
_platon_squeeze_special_details
;
A solvent mask was calculated and 196 electrons were 
found in a volume of 881\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 2[C3H7NO] and 
2[NC2H8]+ cations per Formula Unit.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'