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_7710722
_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         'C16 H17 Cu N2 O8 S, C18 H18 N12 O6'
_chemical_formula_sum            'C34 H47 Cu N14 O20 S'
_chemical_formula_weight         1067.45
_chemical_name_systematic        CUST-713
_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
_audit_creation_date             2022-07-09
_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                 108.310(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8654(5)
_cell_length_b                   15.1748(5)
_cell_length_c                   20.4442(7)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    297.2
_cell_measurement_theta_max      63.95
_cell_measurement_theta_min      3.24
_cell_volume                     4378.3(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      297.2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33680
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        63.961
_diffrn_reflns_theta_max         63.961
_diffrn_reflns_theta_min         3.242
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.013
_exptl_absorpt_correction_T_max  0.669
_exptl_absorpt_correction_T_min  0.648
_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    1.619
_exptl_crystal_description       block
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         7226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0692P)^2^+3.6608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1405
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5487
_reflns_number_total             7226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01283a2.cif
_cod_data_source_block           3
_cod_database_code               7710722
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.689
_shelx_estimated_absorpt_t_min   0.644
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O8(H8A,H8B)
2.b Ternary CH refined with riding coordinates:
 C19(H19), C20(H20), C25(H25), C27(H27), C29(H29), C31(H31)
2.c Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), C9(H9A,H9B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B),
 C26(H26A,H26B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B)
2.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C8(H8), C13(H13), C15(H15), C21(H21)
;
_shelx_res_checksum              12053
_shelx_hkl_checksum              45066
_shelx_fab_checksum              81394
_olex2_submission_special_instructions 'No special instructions were received'