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_7244322
_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
'C38 H50 N4 O27 S2 U3, 2(C36 H36 N24 O12), Cl'
_chemical_formula_sum            'C110 H122 Cl N52 O51 S2 U3'
_chemical_formula_weight         3802.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.1168(13)
_cell_length_b                   24.6194(15)
_cell_length_c                   24.9596(10)
_cell_measurement_reflns_used    9613
_cell_measurement_temperature    302.0
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.40
_cell_volume                     14205.1(13)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      302.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1398
_diffrn_reflns_av_unetI/netI     0.1210
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            97620
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.036
_diffrn_reflns_theta_max         25.036
_diffrn_reflns_theta_min         1.854
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.567
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.6621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0949 before and 0.0797 after correction.
The Ratio of minimum to maximum transmission is 0.8893.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_description       needle
_exptl_crystal_F_000             7516
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.021
_refine_diff_density_max         7.670
_refine_diff_density_min         -3.092
_refine_diff_density_rms         0.283
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.458(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1976
_refine_ls_number_reflns         25075
_refine_ls_number_restraints     2217
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.1428
_refine_ls_R_factor_gt           0.0881
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1733P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2335
_refine_ls_wR_factor_ref         0.2746
_reflns_Friedel_coverage         0.859
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                15164
_reflns_number_total             25075
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01330k2.cif
_cod_data_source_block           URCP4
_cod_depositor_comments
'Adding full bibliography for 7244318--7244323.cif.'
_cod_database_code               7244322
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.254
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.542(14)
 0.458(14)
2. 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
3. Restrained distances
 C37-N44
 1.5 with sigma of 0.02
 C34-C40
 1.4 with sigma of 0.02
 N44-C37
 1.45 with sigma of 0.02
 C39-C7
 1.45 with sigma of 0.02
 C26-C18
 1.4 with sigma of 0.02
 C4-N88
 1.45 with sigma of 0.02
 N70-C52
 1.45 with sigma of 0.02
 C2-N5
 1.45 with sigma of 0.02
 C02Q-N78
 1.45 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C63) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
5. 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
6.a Rotating group:
 O6(H6A,H6B), O7(H7A,H7B), O4(H4A,H4B)
6.b Ternary CH refined with riding coordinates:
 C01N(H01N), C02D(H02E), C02R(H02R), C034(H034), C03T(H03T), C048(H048),
 C05U(H05U), C06C(H06C), C07E(H07E), C8(H8), C17(H17), C11(H11), C37(H37),
 C43(H43), C10(H10), C52(H52), C29(H29), C57(H57), C56(H56), C68(H68), C15(H15),
  C16(H16), C35(H35), C12(H12)
6.c Secondary CH2 refined with riding coordinates:
 C026(H02A,H02B), C02A(H02C,H02D), C02H(H02F,H02G), C02I(H02H,H02I), C02Q(H02J,
 H02K), C03R(H03B,H03C), C03V(H03D,H03E), C047(H04A,H04B), C04D(H04C,H04D),
 C04K(H04E,H04F), C051(H05A,H05B), C05H(H05C,H05D), C05L(H05G,H05H), C05N(H05E,
 H05F), C05R(H05I,H05J), C08G(H08A,H08B), C45(H45A,H45B), C3(H3A,H3B), C66(H66A,
 H66B), C31(H31A,H31B), C2(H2A,H2B), C38(H38A,H38B), C42(H42A,H42B), C58(H58A,
 H58B), C74(H74A,H74B), C60(H60A,H60B), C49(H49A,H49B), C55(H55A,H55B),
 C72(H72A,H72B), C40(H40A,H40B), C33(H33A,H33B), C34(H34A,H34B), C44(H44A,H44B),
  C30(H30A,H30B), C26(H26A,H26B), C4(H4C,H4D), C18(H18A,H18B), C23(H23A,H23B)
6.d Aromatic/amide H refined with riding coordinates:
 C01B(H01B), C03A(H03A), C1(H1), C41(H41), C50(H50), C59(H59), C77(H77),
 C79(H79), C24(H24), C22(H22), C20(H20), C25(H25), C51(H51), C47(H47), C61(H61),
  C53(H53)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              49774
_shelx_fab_checksum              36613
_olex2_submission_special_instructions 'No special instructions were received'