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_7133106
_publ_section_title
;
 Mechanical bonding of rigid MORFs using a tetratopic rotaxane.
;
_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 H60 Co2 N6 O19'
_chemical_formula_sum            'C68 H60 Co2 N6 O19'
_chemical_formula_weight         1383.08
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-03-14 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7950(9)
_cell_length_b                   33.970(2)
_cell_length_c                   13.8988(8)
_cell_measurement_reflns_used    9328
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.544
_cell_measurement_theta_min      2.248
_cell_volume                     7929.6(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 0.999
_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  0.0600
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            164104
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.314
_diffrn_reflns_theta_min         1.902
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.483
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6599
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       prism
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.600
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         10028
_refine_ls_number_restraints     182
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0726
_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^)+(0.1170P)^2^+17.3598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2003
_refine_ls_wR_factor_ref         0.2519
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6755
_reflns_number_total             10028
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02065k2.cif
_cod_data_source_block           as_iv__0msp
_cod_depositor_comments
'Adding full bibliography for 7133105--7133106.cif.'
_cod_database_code               7133106
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.935
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C32A-C31A = C34A-C33A
 1.37 with sigma of 0.02
 C32A-C33A
 1.38 with sigma of 0.02
 C32B-C31B = C29-C34B = C34B-C33B
 1.37 with sigma of 0.02
 C31A-C30A
 1.36 with sigma of 0.02
 C32B-C33B
 1.38 with sigma of 0.02
 C31B-C30B = C30B-C29
 1.36 with sigma of 0.02
 C32B-C34B
 2.38 with sigma of 0.04
 C31B-C29
 2.36 with sigma of 0.04
 C32A-C30A = C30A-C34A
 2.37 with sigma of 0.04
 C32A-C34A
 2.38 with sigma of 0.04
 C32B-C30B = C30B-C34B = C29-C33B
 2.37 with sigma of 0.04
 C32A-C31A \\sim C31A-C30A \\sim C34A-C33A \\sim C33A-C32A
 with sigma of 0.02
 C32A-C34A \\sim C32A-C30A \\sim C34A-C30A \\sim C33A-C31A
 with sigma of 0.04
 C32B-C31B \\sim C31B-C30B \\sim C30B-C29 \\sim C29-C34B \\sim C34B-C33B \\sim
C33B-C32B
 with sigma of 0.02
 C32B-C34B \\sim C32B-C30B \\sim C34B-C30B \\sim C29-C31B \\sim C29-C33B \\sim
C33B-C31B
 with sigma of 0.04
3. Restrained planarity
 C30A, C31A, C32A, C33A, C34A
 with sigma of 0.1
 C29, C30B, C31B, C32B, C33B, C34B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C29 \\sim C30B \\sim C31B \\sim C32B \\sim C33B \\sim C34B: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C30A \\sim C31A \\sim C32A \\sim C33A \\sim C34A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Uanis(C30B) = Uanis(C30A)
5. Rigid body (RIGU) restrains
 C30A, C31A, C32A, C33A, C34A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C29, C30B, C31B, C32B, C33B, C34B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C30B, C31B, C32B, C33B, C34B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O6B)=Sof(C30B)=Sof(H30B)=Sof(C31B)=Sof(H31B)=Sof(C32B)=Sof(H32B)=
 Sof(C33B)=Sof(H33B)=Sof(C34B)=Sof(H34B)=1-FVAR(1)
 Sof(O6A)=Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=
 Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)=FVAR(1)
 Fixed Sof: H10A(0.5) H10B(0.5)
7.a Rotating group:
 O9(H9A,H9B), O10(H10A,H10B)
7.b Secondary CH2 refined with riding coordinates:
 C9(H9C,H9D), C11(H11A,H11B), C25(H25A,H25B), C28(H28A,H28B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C13(H13), C14(H14), C16(H16), C17(H17), C20(H20),
 C21(H21), C23(H23), C24(H24), C27(H27), C30A(H30A), C30B(H30B), C31A(H31A),
 C31B(H31B), C32A(H32A), C32B(H32B), C33A(H33A), C33B(H33B), C34A(H34A),
 C34B(H34B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              1106
_shelx_hkl_checksum              48314
_shelx_fab_checksum              81745
_olex2_submission_special_instructions 'No special instructions were received'