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_7710720
_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, 3(H2 O), H O'
_chemical_formula_sum            'C35 H67 Cu N14 O29 S'
_chemical_formula_weight         1243.62
_chemical_name_systematic        CUST-711
_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                 102.123(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0560(15)
_cell_length_b                   19.1390(18)
_cell_length_c                   18.0435(17)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    295.21
_cell_measurement_theta_max      63.408
_cell_measurement_theta_min      3.353
_cell_volume                     5421.0(9)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'APEX3 Ver. 2016.5-0 (Bruker-AXS, 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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      295.21
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51584
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        63.679
_diffrn_reflns_theta_max         63.678
_diffrn_reflns_theta_min         3.353
_exptl_absorpt_coefficient_mu    1.835
_exptl_absorpt_correction_T_max  0.693
_exptl_absorpt_correction_T_min  0.676
_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    1.524
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         8862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0688P)^2^+4.7971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1377
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6789
_reflns_number_total             8862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01283a2.cif
_cod_data_source_block           1
_cod_database_code               7710720
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.710
_shelx_estimated_absorpt_t_min   0.667
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Riding coordinates:
 N14(H14C)
2.b Free rotating group:
 O16(H16A,H16B), O17(H17A), O18(H18A,H18B), O19(H19)
2.c Rotating group:
 O4(H4A,H4B), O14(H14A,H14B)
2.d Ternary CH refined with riding coordinates:
 C17(H17), C18(H18), C20(H20), C25(H25), C26(H26), C27(H27)
2.e Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C21(H21A,H21B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,
 H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B)
2.f Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C7(H7), C9(H9), C13(H13), C23(H23), C24(H24)
;
_shelx_res_checksum              65035
_shelx_hkl_checksum              85056
_shelx_fab_checksum              7499
_olex2_submission_special_instructions 'No special instructions were received'