Impact of the proximity effect on uranyl coordination of conformationally variable weakly-bonded cucurbit[6]uril-bipyridinium pseudorotaxane
Li, Feize; Mei, Lei; Peng, Haiyue; Hu, Kongqiu; Chai, Zhifang; Liu, Ning; CrystEngComm 24 (2022) 1955–1965; doi:10.1039/D1CE01330K

data_7244323
_publ_section_title
;
 Impact of the proximity effect on uranyl coordination of conformationally
 variable weakly-bonded cucurbit[6]uril-bipyridinium pseudorotaxane
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_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1955
_journal_page_last               1965
_journal_paper_doi               10.1039/D1CE01330K
_journal_volume                  24
_journal_year                    2022
_chemical_absolute_configuration unk
_chemical_formula_moiety
'C19 H22 N3.733 O15.198 U2, C36 H36 N24 O12, 2(H2 O), 0.267(Br), 0.5[H2O]'
_chemical_formula_sum            'C55 H62 Br0.27 N27.74 O29.21 U2'
_chemical_formula_weight         2085.334
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_Int_Tables_number      9
_audit_creation_date             2021-10-18
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.10.14 svn.r9718050b for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2022-01-12 deposited with the CCDC.	2022-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.982(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3214(7)
_cell_length_b                   17.8962(7)
_cell_length_c                   22.4009(9)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    292.36
_cell_measurement_theta_max      33.32
_cell_measurement_theta_min      2.96
_cell_volume                     6710.8(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      292.36
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.9985
_diffrn_reflns_Laue_measured_fraction_max 0.9988
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            79808
_diffrn_reflns_point_group_measured_fraction_full 0.9953
_diffrn_reflns_point_group_measured_fraction_max 0.9957
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    5.097
_exptl_absorpt_correction_T_max  0.7470
_exptl_absorpt_correction_T_min  0.5375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1051 before and 0.0703 after correction.
The Ratio of minimum to maximum transmission is 0.7195.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.064
_exptl_crystal_description       block
_exptl_crystal_F_000             4052.2
_refine_diff_density_max         1.8214
_refine_diff_density_min         -1.0035
_refine_diff_density_rms         0.1315
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   0.048(3)
_refine_ls_d_res_high            0.7697
_refine_ls_d_res_low             6.9031
_refine_ls_goodness_of_fit_ref   1.0459
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    120
_refine_ls_number_parameters     1070
_refine_ls_number_reflns         15363
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.0444
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0160P)^2^+5.4322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0626
_reflns_Friedel_coverage         0.993
_reflns_limit_h_max              23
_reflns_limit_h_min              -23
_reflns_limit_k_max              23
_reflns_limit_k_min              -23
_reflns_limit_l_max              29
_reflns_limit_l_min              -29
_reflns_number_gt                12988
_reflns_number_total             15363
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1ce01330k2.cif
_cod_data_source_block           URCP1
_cod_depositor_comments
'Adding full bibliography for 7244318--7244323.cif.'
_cod_original_sg_symbol_Hall     ' C -2yc'
_cod_original_formula_sum        'Br0.27 C55 H62 N27.74 O29.21 U2 '
_cod_database_code               7244323
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C8-C7 \\sim C9B-C8 \\sim C9B-C10A \\sim C11-C10A \\sim C12-C11 \\sim C13-C12
 with sigma of 0.01
 O30-N1 \\sim O28-N1 \\sim O29-N1
 with sigma of 0.01
3. Restrained planarity
 N1, O28, O29, O30
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C9B) \\sim Ueq, Uanis(C9A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
Uanis(C9) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N1) = Uanis(Br1)
5. Rigid body (RIGU) restrains
 C9B, C9A, C10A, C11, C12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(Br1)=1-FVAR(1)
 Sof(N1)=Sof(O28)=Sof(O29)=Sof(O30)=FVAR(1)
 Fixed Sof: H12c(0.5) H12d(0.5) H12a(0.5) H12b(0.5) C9B(0.5) H9Ba(0.5)
 H9Bb(0.5) H8aa(0.5) H8ab(0.5) H8bc(0.5) H8bd(0.5) C11(0.5) H11a(0.5) H11b(0.5)
 C10A(0.5) H10a(0.5) H10b(0.5) C10(0.5) H10c(0.5) H10d(0.5) C9(0.5) H9a(0.5)
 H9b(0.5) C9A(0.5) H9Aa(0.5) H9Ab(0.5)
7.a Riding coordinates:
 O27(H27c,H27d)
7.b Free rotating group:
 O26(H26a,H26b)
7.c Ternary CH refined with riding coordinates:
 C32(H32), C43(H43), C40(H40), C35(H35), C37(H37), C34(H34), C41(H41),
 C36(H36), C38(H38), C39(H39), C33(H33), C42(H42)
7.d Secondary CH2 refined with riding coordinates:
 C52(H52a,H52b), C13(H13a,H13b), C50(H50a,H50b), C12(H12c,H12d), C12(H12a,
 H12b), C9B(H9Ba,H9Bb), C8(H8aa,H8ab), C8(H8bc,H8bd), C48(H48a,H48b), C25(H25a,
 H25b), C29(H29a,H29b), C31(H31a,H31b), C23(H23a,H23b), C21(H21a,H21b), C7(H7a,
 H7b), C27(H27a,H27b), C44(H44a,H44b), C54(H54a,H54b), C46(H46a,H46b), C11(H11a,
 H11b), C10A(H10a,H10b), C10(H10c,H10d), C9(H9a,H9b), C9A(H9Aa,H9Ab)
7.e Aromatic/amide H refined with riding coordinates:
 C4(H4), C15(H15), C16(H16), C17(H17), C6(H6), C14(H14), C5(H5), C3(H3)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 16 electrons were 
found in a volume of 32\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 0.5[H2O] per 
Formula Unit which account for 20 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'