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_7244320
_publ_section_title
;
 Impact of the proximity effect on uranyl coordination of conformationally
 variable weakly-bonded cucurbit[6]uril-bipyridinium pseudorotaxane
;
_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_formula_moiety
'C18 H25 N2 O20 S2 U2, C36 H36 N24 O12, 4(H2 O), 4(O)'
_chemical_formula_sum            'C54 H69 N26 O40 S2 U2'
_chemical_formula_weight         2262.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-08-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-01-12 deposited with the CCDC.	2022-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                105.650(2)
_cell_angle_beta                 95.320(2)
_cell_angle_gamma                113.732(2)
_cell_formula_units_Z            1
_cell_length_a                   12.4914(7)
_cell_length_b                   13.5836(7)
_cell_length_c                   13.6906(6)
_cell_measurement_reflns_used    7925
_cell_measurement_temperature    292.26
_cell_measurement_theta_max      32.21
_cell_measurement_theta_min      2.92
_cell_volume                     1993.62(18)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      292.26
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14537
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.923
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.220
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.5123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0930 before and 0.0570 after correction. The Ratio of minimum to maximum transmission is 0.6861. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_description       block
_exptl_crystal_F_000             1111
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.068
_refine_diff_density_min         -1.673
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         6611
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0797P)^2^+5.2082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5629
_reflns_number_total             6611
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01330k2.cif
_cod_data_source_block           URCP3
_cod_depositor_comments
'Adding full bibliography for 7244318--7244323.cif.'
_cod_database_code               7244320
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.364
_shelx_estimated_absorpt_t_min   0.283
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C9-C10
 1.45 with sigma of 0.02
 C8-C9
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim
Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.001
Uanis(O19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(O20) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.001
Uanis(O22) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C10(0.5) C9(0.5) H9(0.5) O19(0.5) O20(0.25) O21(0.25)
5.a Free rotating group:
 O17(H17A,H17B), O18(H18A,H18B)
5.b Rotating group:
 O4(H4A,H4B), O6(H6A,H6B)
5.c Ternary CH refined with riding coordinates:
 C19(H19), C21(H21), C20(H20), C17(H17), C22(H22), C18(H18), C9(H9)
5.d Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C23(H23A,H23B), C15(H15A,H15B), C11(H11A,H11B), C13(H13A,
 H13B), C27(H27A,H27B), C7(H7A,H7B), C8(H8A,H8B)
5.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C5(H5), C4(H4)
;
_shelx_res_checksum              37595
_olex2_submission_special_instructions 'No special instructions were received'