Three layered cucurbit[6]uril-based metal-organic rotaxane networks functionalized by sulfonic groups for proton conduction
Li, Ying; Xu, Yan-Jun; Fan, Ming-Yue; Feng, Zhen-Jie; Li, Jun-Jun; Wu, Xue-Song; Sun, Jing; Wang, Xinlong; Su, Zhong-Min; Dalton Transactions  (2022) –; doi:10.1039/D2DT01283A

data_7710721
_publ_section_title
;
 Three layered cucurbit[6]uril-based metal-organic rotaxane networks
 functionalized by sulfonic groups for proton conduction
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01283A
_journal_year                    2022
_chemical_formula_moiety         'C17 H21 Cu N2 O9 S, C18 H18 N12 O6, 4(H2 O)'
_chemical_formula_sum            'C35 H47 Cu N14 O19 S'
_chemical_formula_weight         1063.46
_chemical_name_systematic        CUST-712
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-07-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-07-13 deposited with the CCDC.	2022-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.559(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5994(18)
_cell_length_b                   16.5057(19)
_cell_length_c                   17.149(2)
_cell_measurement_reflns_used    3669
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      22.20
_cell_measurement_theta_min      2.16
_cell_volume                     4160.7(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0485
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23782
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.102
_diffrn_reflns_theta_max         25.102
_diffrn_reflns_theta_min         1.529
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.676
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       block
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         7352
_refine_ls_number_restraints     163
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0541P)^2^+2.7634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1243
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5332
_reflns_number_total             7352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01283a2.cif
_cod_data_source_block           2
_cod_database_code               7710721
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.877
_shelx_estimated_absorpt_t_min   0.855
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H37A,H37B} of C37, {H35B,H35A} of C35, {H36A,H36B} of C36,
   {H1AA,H1AB} of C1A, {H38A,H38B} of C38, {H34C,H34D} of C34A, {H25A,H25B} of
  C25, {H29A,H29B} of C29, {H31A,H31B} of C31, {H23A,H23B} of C23, {H20A,H20B}
  of C20, {H30A,H30B} of C30, {H32A,H32B} of C32, {H34A,H34B} of C34B, All C(H,
  H,H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups, {H1BA,H1BB} of C1B
2. Restrained distances
 C1A-C1B
 1.568 with sigma of 0.001
 C1B-H1BB
 0.97 with sigma of 0.001
 C1B-H1BA
 0.97 with sigma of 0.001
 C1A-H1BA
 2.11 with sigma of 0.001
 C1A-H1BB
 2.11 with sigma of 0.001
 C38-H34B
 1.2453 with sigma of 0.0001
 C1B-C1A \\sim C37-C1A
 with sigma of 0.001
 C34A-C28 \\sim C28-C1B_$1 \\sim C38-C28 \\sim C34B-C28
 with sigma of 0.001
 C36-C34B_$1 \\sim C36-C35
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C34B \\sim C34A \\sim C37 \\sim C1A \\sim C1B \\sim C35 \\sim C36 \\sim C38:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C34A) \\sim Ueq, Uanis(C1B) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C36) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C34B) \\sim Ueq, Uanis(C38) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 C34A, C28, C37, C1A, C1B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C34B, C38, C37, C35, C36, C1B, C1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H28C(0.5) H28D(0.5) H28A(0.5) H28B(0.5) C34B(0.25) H34A(0.25)
 H34B(0.25) C34A(0.25) H34C(0.25) H34D(0.25) C37(0.25) H37A(0.25) H37B(0.25)
 C1A(0.25) H1AA(0.25) H1AB(0.25) C1B(0.25) H1BA(0.25) H1BB(0.25) C35(0.25)
 H35B(0.25) H35A(0.25) C36(0.25) H36A(0.25) H36B(0.25) C38(0.25) H38A(0.25)
 H38B(0.25)
6.a Riding coordinates:
 C34B(H34A,H34B), C35(H35B,H35A), C36(H36A,H36B)
6.b Free rotating group:
 O13(H13A,H13B), O17(H17A,H17B), O18(H18A,H18B), O19(H19A,H19B)
6.c Rotating group:
 O2(H2A,H2B), O11(H11A,H11B)
6.d Ternary CH refined with riding coordinates:
 C16(H16), C17(H17), C19(H19), C21(H21), C22(H22), C24(H24)
6.e Secondary CH2 refined with riding coordinates:
 N12(H12A,H12B), C20(H20A,H20B), C23(H23A,H23B), C25(H25A,H25B), C28(H28C,
 H28D), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
 C32(H32A,H32B), C34A(H34C,H34D), C37(H37A,H37B), C1A(H1AA,H1AB), C38(H38A,H38B)
6.f Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C9(H9), C12(H12), C15(H15), C27(H27), C33(H33)
;
_shelx_res_checksum              84260
_shelx_hkl_checksum              31859
_olex2_submission_special_instructions 'No special instructions were received'