Mechanical bonding of rigid MORFs using a tetratopic rotaxane.
Saura-Sanmartin, Adrian; Cutillas-Font, Guillermo; Martinez-Cuezva, Alberto; Alajarin, Mateo; Esteban-Betegón, Fátima; Pena-Sánchez, Pilar; Gándara, Felipe; Berna, Jose; Chemical communications (Cambridge, England) 60 (2024) 6431–6434; doi:10.1039/d4cc02065k

data_7133105
_publ_section_title
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 Mechanical bonding of rigid MORFs using a tetratopic rotaxane.
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_journal_issue                   50
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6431
_journal_page_last               6434
_journal_paper_doi               10.1039/d4cc02065k
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C68 H58 Cu2 N6 O16'
_chemical_formula_sum            'C68 H58 Cu2 N6 O16'
_chemical_formula_weight         1342.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
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2024-03-14 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.426(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.307(2)
_cell_length_b                   14.1238(11)
_cell_length_c                   16.6531(12)
_cell_measurement_reflns_used    9272
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.235
_cell_measurement_theta_min      2.391
_cell_volume                     7535.0(9)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON II CMOS'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0984
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            176547
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.555
_diffrn_reflns_theta_min         2.051
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0847 before and 0.0679 after correction.
The Ratio of minimum to maximum transmission is 0.9303.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       lath
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.122
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         11539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0736
_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^)+(0.0853P)^2^+21.0339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1768
_refine_ls_wR_factor_ref         0.1894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8370
_reflns_number_total             11539
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02065k2.cif
_cod_data_source_block           as_iii_140_0msp_a
_cod_depositor_comments
'Adding full bibliography for 7133105--7133106.cif.'
_cod_original_cell_volume        7535.1(10)
_cod_database_code               7133105
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.890
_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,H) groups
2.a Rotating group:
 O8(H8A,H8B)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C25(H25A,H25B), C28(H28A,H28B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C3(H3), C5(H5), C7(H7), C13(H13), C14(H14), C16(H16),
 C17(H17), C20(H20), C21(H21), C23(H23), C24(H24), C27(H27), C30(H30), C31(H31),
  C32(H32), C33(H33), C34(H34)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              16468
_shelx_hkl_checksum              5402
_shelx_fab_checksum              27874
_olex2_submission_special_instructions 'No special instructions were received'