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_7244321
_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
'C296 H328 N112 O148 S8 U12, 20(H2 O), 8(O), 4(C36 H36 N24 O12)'
_chemical_formula_sum            'C440 H512 N208 O224 S8 U12'
_chemical_formula_weight         15411.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-01-12
_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                90
_cell_angle_beta                 103.095(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   23.0996(13)
_cell_length_b                   18.4319(11)
_cell_length_c                   33.9541(19)
_cell_measurement_reflns_used    9688
_cell_measurement_temperature    143.01
_cell_measurement_theta_max      68.38
_cell_measurement_theta_min      2.94
_cell_volume                     14080.7(14)
_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)'
_diffrn_ambient_temperature      143.01
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8 Venture Photon II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            190705
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.532
_diffrn_reflns_theta_min         2.672
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.850
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.3779
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_description       block
_exptl_crystal_F_000             7632
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.258
_exptl_crystal_size_min          0.116
_refine_diff_density_max         5.107
_refine_diff_density_min         -3.494
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2045
_refine_ls_number_reflns         25654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+89.0799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1159
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23361
_reflns_number_total             25654
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01330k2.cif
_cod_data_source_block           URCP5
_cod_depositor_comments
'Adding full bibliography for 7244318--7244323.cif.'
_cod_database_code               7244321
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.366
_shelx_estimated_absorpt_t_min   0.114
_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. Others
 Fixed Sof: O53(0.75) O56(0.75) H56A(0.75) H56B(0.75) O54(0.75) H54A(0.75)
 H54B(0.75) O55(0.5) H55C(0.5) H55D(0.5) O58(0.25)
3.a Free rotating group:
 O51(H51C,H51D), O49(H49C,H49D), O50(H50A,H50B), O56(H56A,H56B), O54(H54A,
 H54B), O55(H55C,H55D)
3.b Rotating group:
 O17(H17A,H17B)
3.c Ternary CH refined with riding coordinates:
 C32(H32), C33(H33), C42(H42), C41(H41), C39(H39), C40(H40), C38(H38),
 C43(H43), C35(H35), C34(H34), C36(H36), C37(H37), C93(H93), C89(H89), C96(H96),
  C94(H94), C90(H90), C95(H95), C91(H91), C92(H92), C97(H97), C88(H88),
 C87(H87), C98(H98)
3.d Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C45(H45A,H45B), C66(H66A,H66B), C67(H67A,H67B), C64(H64A,
 H64B), C65(H65A,H65B), C63(H63A,H63B), C10(H10A,H10B), C31(H31A,H31B),
 C68(H68A,H68B), C7(H7A,H7B), C47(H47A,H47B), C9(H9A,H9B), C27(H27A,H27B),
 C62(H62A,H62B), C13(H13A,H13B), C53(H53A,H53B), C21(H21A,H21B), C51(H51A,H51B),
  C8(H8A,H8B), C55(H55A,H55B), C12(H12A,H12B), C11(H11A,H11B), C23(H23A,H23B),
 C49(H49A,H49B), C29(H29A,H29B), C85(H85A,H85B), C83(H83A,H83B), C103(H10C,
 H10D), C81(H81A,H81B), C75(H75A,H75B), C79(H79A,H79B), C107(H10E,H10F),
 C105(H10G,H10H), C109(H10I,H10J), C101(H10K,H10L), C99(H99A,H99B), C77(H77A,
 H77B)
3.e Aromatic/amide H refined with riding coordinates:
 C69(H69), C3(H3), C59(H59), C14(H14), C6(H6), C15(H15), C18(H18), C58(H58),
 C17(H17), C72(H72), C4(H4), C70(H70), C60(H60), C5(H5), C61(H61), C71(H71)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              91844
_shelx_fab_checksum              97422
_olex2_submission_special_instructions 'No special instructions were received'