2D and 3D metal-organic frameworks constructed with a mechanically rigidified [3]rotaxane ligand.
Li, Xia; Xie, Jialin; Du, Zhenglin; Yu, Ruiyang; Jia, Jianhua; Chen, Zhong; Zhu, Kelong; Chemical communications (Cambridge, England)  (2022) –; doi:10.1039/d2cc01198k

data_7129946
_publ_section_title
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 2D and 3D metal-organic frameworks constructed with a mechanically
 rigidified [3]rotaxane ligand.
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_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d2cc01198k
_journal_year                    2022
_chemical_formula_moiety         '0.5(C88 H72 N12 O16 Zn4), 2(C18 H36 O6)'
_chemical_formula_sum            'C80 H108 N6 O20 Zn2'
_chemical_formula_weight         1604.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-11-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-02-26 deposited with the CCDC.	2022-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.536(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.5555(8)
_cell_length_b                   14.5616(8)
_cell_length_c                   19.0686(10)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.648
_cell_measurement_theta_min      3.325
_cell_volume                     4033.9(4)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 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      100.0
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker D8 VENTURE Metaljet PHOTON II'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26671
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        53.064
_diffrn_reflns_theta_max         53.064
_diffrn_reflns_theta_min         4.172
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  0.7505
_exptl_absorpt_correction_T_min  0.6435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0674 before and 0.0508 after correction.
The Ratio of minimum to maximum transmission is 0.8574.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       block
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.280
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         6877
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.357
_refine_ls_R_factor_all          0.1308
_refine_ls_R_factor_gt           0.1022
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2897
_refine_ls_wR_factor_ref         0.3228
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4754
_reflns_number_total             6877
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01198k2.cif
_cod_data_source_block           b190919a0823_0m
_cod_database_code               7129946
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.906
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
2. Restrained distances
 C34-C28
 1.53 with sigma of 0.02
 C32-H32B = C38-C32
 1.53 with sigma of 0.02
 C39-C38
 1.53 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C30 \\sim C33: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02
O9 \\sim C40: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O9, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N3, C16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C34, C28, O7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C37, C36
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O11, C35, C40
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C22, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C30, C39, C38, C32
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C25, C33
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(H35C)=Sof(H35D)=Sof(O11)=1-FVAR(1)
 Sof(O10)=Sof(H35A)=Sof(H35B)=FVAR(1)
 Sof(H37C)=Sof(H37D)=Sof(C41)=Sof(H41A)=Sof(H41B)=1-FVAR(2)
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H37A)=Sof(H37B)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C22(H22A,H22B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B),
  C35(H35C,H35D), C36(H36A,H36B), C37(H37A,H37B), C37(H37C,H37D), C38(H38A,
 H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B)
6.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23)
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_olex2_submission_special_instructions 'No special instructions were received'