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_7706841
_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 H108 N24 O32 U4, 16[C3H7NO], 4[NC2H8]'
_chemical_formula_sum            'C140 H252 N44 O48 U4'
_chemical_formula_weight         4271.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc26k0h9
_audit_creation_date             2021-03-02
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.02.10 svn.rb'16c95d35' for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2021-03-05 deposited with the CCDC.	2021-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.334(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.7224(11)
_cell_length_b                   27.2567(13)
_cell_length_c                   28.5054(14)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      67.44
_cell_measurement_theta_min      2.77
_cell_volume                     17178.5(15)
_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 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      170.00
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0583
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25628
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        39.995
_diffrn_reflns_theta_max         39.995
_diffrn_reflns_theta_min         2.773
_exptl_absorpt_coefficient_mu    11.246
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1190 before and 0.0895 after correction.
The Ratio of minimum to maximum transmission is 0.6614.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            buff
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       flakiness
_exptl_crystal_F_000             8608
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.529
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.233(13)
_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     1286
_refine_ls_number_reflns         10154
_refine_ls_number_restraints     3359
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0777P)^2^+94.6974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1281
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.952
_reflns_number_gt                9215
_reflns_number_total             10154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00289a2.cif
_cod_data_source_block           cu_20161116_22_hu43_0m_sq
_cod_depositor_comments
'Adding full bibliography for 7706841--7706842.cif.'
_cod_database_code               7706841
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.729
_shelx_estimated_absorpt_t_min   0.258
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.767(13)
 0.233(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C25-C26
 1.4 with sigma of 0.01
 N21-C79
 1.45 with sigma of 0.01
 C41-C39 = C57-N14 = C57-C56 = C4-N8 = C4-C16
 1.6 with sigma of 0.01
 U2-O25 = U2-O26
 1.76 with sigma of 0.01
 U1-O2 = U1-O2
 1.76 with sigma of 0.01
 U4-O18 = U4-O18
 1.76 with sigma of 0.01
 U3-O10 = U3-O9
 1.76 with sigma of 0.01
4. Rigid bond restraints
 U2, O25
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 U4, O17
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 U4, O18
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C8 \\sim C7 \\sim C6 \\sim C5 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C16 \\sim C15 \\sim C14 \\sim C18
\\sim C17 \\sim C19 \\sim C20 \\sim C21 \\sim C78 \\sim C76 \\sim C77 \\sim C85
\\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30
\\sim C35 \\sim C34 \\sim C33 \\sim C32 \\sim C31 \\sim C36 \\sim C37 \\sim C39
\\sim C38 \\sim C41 \\sim C40 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53
\\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61
\\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C69 \\sim C68
\\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim C79 \\sim C80
\\sim C81 \\sim C82 \\sim C83 \\sim C84 \\sim C48 \\sim C47 \\sim C46 \\sim C45
\\sim C44 \\sim C43 \\sim C42: within 3.8A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 3.8A
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O8 \\sim O7 \\sim O6 \\sim O5 \\sim O9
\\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O16 \\sim O15 \\sim O14 \\sim O18
\\sim O17 \\sim O19 \\sim O20 \\sim O21 \\sim O34 \\sim O23 \\sim O24 \\sim O25
\\sim O26 \\sim O27 \\sim O28 \\sim O29 \\sim O30 \\sim O32 \\sim O31: within
3.8A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 3.8A
Uanis(N21) \\sim Ueq, Uanis(N25) \\sim Ueq, Uanis(N24) \\sim Ueq, Uanis(C85)
\\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(N18) \\sim Ueq, Uanis(C78) \\sim Ueq,
Uanis(C62) \\sim Ueq, Uanis(C77) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N22) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C39) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O20)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(N22) \\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.a Ternary CH refined with riding coordinates:
 C11(H11), C17(H17), C23(H23), C26(H26), C34(H34), C41(H41), C54(H54),
 C61(H61), C69(H69), C71(H71), C83(H83), C44(H44)
7.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B),
 C16(H16A,H16B), C15(H15A,H15B), C14(H14A,H14B), C19(H19A,H19B), C20(H20A,H20B),
  C21(H21A,H21B), C78(H78A,H78B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C35(H35A,H35B), C33(H33A,H33B), C32(H32A,H32B),
 C31(H31A,H31B), C37(H37A,H37B), C39(H39A,H39B), C38(H38A,H38B), C40(H40A,H40B),
  C52(H52A,H52B), C53(H53A,H53B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,
 H58B), C59(H59A,H59B), C60(H60A,H60B), C62(H62A,H62B), C64(H64A,H64B),
 C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C72(H72A,H72B), C73(H73A,H73B),
  C74(H74A,H74B), C75(H75A,H75B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,
 H81B), C82(H82A,H82B), C48(H48A,H48B), C47(H47A,H47B), C46(H46A,H46B),
 C45(H45A,H45B)
7.c Fitted hexagon refined as free rotating group:
 N22(C76,N24,C77,N25,C85)
;
_shelx_res_checksum              19719
_shelx_hkl_checksum              34976
_shelx_fab_checksum              26530
_platon_squeeze_special_details
;
A solvent mask was calculated and 2943 electrons were 
found in a volume of 8866\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 16[C3H7NO] and 
4[NC2H8]+ cations per Formula Unit which account for 2992
electrons per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'