Guest exchange in a porous cucurbit[6]uril-based metal-organic rotaxane framework probed by NMR and X-ray crystallography.
Wu, Xue-Song; Wang, Xin-Long; Zhu, Fu-Long; Bao, Hong-Fei; Qin, Chao; Su, Zhong-Min; Chemical communications (Cambridge, England) 54 (2018) 5474–5477; doi:10.1039/c8cc02847h

data_7121606
_publ_section_title
;
 Guest exchange in a porous cucurbit[6]uril-based metal-organic rotaxane
 framework probed by NMR and X-ray crystallography.
;
_journal_issue                   43
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5474
_journal_page_last               5477
_journal_paper_doi               10.1039/c8cc02847h
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety
'0.25(C96 H64 Cl4 Cu8 N8 O32), 0.5(C36 H36 N24 O12), 2.5(C6)'
_chemical_formula_sum            'C57 H49 Cl Cu2 N14 O14'
_chemical_formula_weight         1316.63
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-09 deposited with the CCDC.
2018-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.261(11)
_cell_length_b                   29.33(2)
_cell_length_c                   14.304(9)
_cell_measurement_reflns_used    4894
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      50.000
_cell_measurement_theta_min      1.953
_cell_volume                     6822(8)
_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        'SAINT+ 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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27618
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        24.957
_diffrn_reflns_theta_max         24.957
_diffrn_reflns_theta_min         3.199
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.730
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.115
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         6141
_refine_ls_number_restraints     699
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0856P)^2^+19.4080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1604
_refine_ls_wR_factor_ref         0.1756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4894
_reflns_number_total             6141
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc02847h2.cif
_cod_data_source_block           Ph-MORF-1
_cod_depositor_comments
'Adding full bibliography for 7121605--7121606.cif.'
_cod_original_cell_volume        6821(8)
_cod_database_code               7121606
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.54
_shelx_estimated_absorpt_t_min   0.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 C36-C35
 1.38 with sigma of 0.01
 C36-C36_$1 = C36_$1-C35_$1 = C37_$1-C35_$1 = C37-C37_$1 = C37-C35 = C36-C35
 1.38 with sigma of 0.01
 C34-C31 = C34-C31_$1 = C33_$1-C31_$1 = C32-C33_$1 = C32-C33 = C33-C31
 1.38 with sigma of 0.01
 C37-C36 = C37_$1-C36_$1
 2.38 with sigma of 0.011
 C34-C33_$1 = C32-C31_$1 = C34-C33
 2.38 with sigma of 0.001
 C33-C31_$1 = C33_$1-C31
 2.78 with sigma of 0.001
 C38_$2-C38 = C40-C38 = C40-C39 = C39_$2-C39 = C40_$2-C39_$2 = C40_$2-C38_$2
 1.38 with sigma of 0.01
 C38_$2-C39
 2.75 with sigma of 0.01
 C40-C40_$2
 2.75 with sigma of 0.01
 C38_$2-C40
 2.38 with sigma of 0.01
 C40-C39_$2
 2.38 with sigma of 0.01
3. Restrained planarity
 C38_$2, C38, C40, C39, C39_$2, C40_$2
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.03
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C00Q \\sim C16 \\sim
C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim
C38 \\sim C39 \\sim C40 \\sim C26 \\sim C27 \\sim C29 \\sim C30 \\sim C25 \\sim
C28 \\sim C35 \\sim C36 \\sim C37 \\sim C31 \\sim C32 \\sim C33 \\sim C34:
within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.03
Uanis(C38) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C32) \\sim Ueq,
Uanis(C36) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.007 and
sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: H2(0.5) H13(0.5) H14(0.5) H15(0.5) C38(0.5) C39(0.5) C40(0.5)
 C26(0.5) C27(0.5) C29(0.5) C30(0.5) C25(0.5) C28(0.5) C35(0.5) C36(0.5)
 C37(0.5) C31(0.5) C32(0.25) C33(0.5) C34(0.25)
6.a Ternary CH refined with riding coordinates:
 C18(H18), C19(H19), C22(H22)
6.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C20(H20A,H20B), C23(H23A,H23B), C24(H24A,H24B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C11(H11)
6.d Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7), C26(C27,C29,C30,C25,C28)
;
_shelx_res_checksum              31865
_olex2_submission_special_instructions 'No special instructions were received'