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_7244319
_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         'C21 H16 N4 O18 U2, C36 H36 N24 O12, 4(H2 O)'
_chemical_formula_sum            'C57 H60 N28 O34 U2'
_chemical_formula_weight         2157.39
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-01-12 deposited with the CCDC.	2022-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                64.880(6)
_cell_angle_beta                 89.809(6)
_cell_angle_gamma                79.159(6)
_cell_formula_units_Z            1
_cell_length_a                   12.304(2)
_cell_length_b                   12.4966(18)
_cell_length_c                   13.125(2)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    292.28
_cell_measurement_theta_max      21.320
_cell_measurement_theta_min      3.013
_cell_volume                     1787.9(5)
_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      292.28
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0782
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            28458
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        21.354
_diffrn_reflns_theta_max         21.354
_diffrn_reflns_theta_min         3.013
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.640
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.4802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1036 before and 0.0776 after correction. The Ratio of minimum to maximum transmission is 0.6449. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_description       block
_exptl_crystal_F_000             1054
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         3990
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0241P)^2^+24.8341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1041
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3518
_reflns_number_total             3990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01330k2.cif
_cod_data_source_block           URCP2
_cod_depositor_comments
'Adding full bibliography for 7244318--7244323.cif.'
_cod_original_cell_volume        1787.8(5)
_cod_database_code               7244319
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.457
_shelx_estimated_absorpt_t_min   0.152
_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
 C34-C8
 1.4 with sigma of 0.02
 C10-C33
 2.2 with sigma of 0.02
 C33-C8
 1.55 with sigma of 0.02
 C30-C34
 2.2 with sigma of 0.02
 C10-C31
 1.55 with sigma of 0.02
 C30-C11
 1.55 with sigma of 0.02
 C34-C31
 1.55 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.001
Uanis(C33) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C30) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.001
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(C11) \\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O17) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.01
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: C30(0.55) H30(0.55) C11(0.35) H11(0.35) C31(0.25) H31A(0.25)
 H31B(0.25) C10(0.25) H10A(0.35) H10B(0.35) C33(0.55) H33A(0.4) H33B(0.4)
 C34(0.55) H34A(0.55) H34B(0.55)
5.a Free rotating group:
 O17(H17A,H17B), O11(H11A,H11B)
5.b Ternary CH refined with riding coordinates:
 C18(H18), C22(H22), C21(H21), C20(H20), C19(H19), C17(H17), C30(H30), C11(H11)
5.c Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C16(H16A,H16B), C13(H13A,H13B), C27(H27A,H27B), C23(H23A,
 H23B), C25(H25A,H25B), C31(H31A,H31B), C10(H10A,H10B), C33(H33A,H33B),
 C34(H34A,H34B)
5.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C4(H4), C5(H5), C6(H6)
;
_shelx_res_checksum              6351
_olex2_submission_special_instructions 'No special instructions were received'