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_7129948
_publ_section_title
;
 2D and 3D metal-organic frameworks constructed with a mechanically
 rigidified [3]rotaxane ligand.
;
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d2cc01198k
_journal_year                    2022
_chemical_formula_moiety
'0.25(C100 H68 N8 O40 Zn8), 2(C18 H36 O6), C2 H8 N'
_chemical_formula_sum            'C63 H97 N3 O22 Zn2'
_chemical_formula_weight         1379.17
_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
_audit_creation_date             2022-02-16
_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                 109.282(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   40.094(2)
_cell_length_b                   13.0784(10)
_cell_length_c                   18.2044(11)
_cell_measurement_reflns_used    6525
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      56.950
_cell_measurement_theta_min      3.112
_cell_volume                     9010.3(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0994
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47713
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        50.497
_diffrn_reflns_theta_max         50.497
_diffrn_reflns_theta_min         3.110
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_T_max  0.0400
_exptl_absorpt_correction_T_min  0.0022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.017
_exptl_crystal_description       block
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         7052
_refine_ls_number_restraints     443
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.1890
_refine_ls_R_factor_gt           0.1083
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2765
_refine_ls_wR_factor_ref         0.3550
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2522
_reflns_number_total             7052
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01198k2.cif
_cod_data_source_block           b20123104a15251_0m
_cod_database_code               7129948
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.920
_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,
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C28-C23
 1.52 with sigma of 0.02
 C35-C34
 2.5 with sigma of 0.02
 N2-C34 = N2-C35 = N3-C36 = N3-C37
 1.42 with sigma of 0.02
 C35-C34 = C36-C37
 2.5 with sigma of 0.04
 C33-C20 \\sim C20-C18 \\sim C33-C25 \\sim C25-C18
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C21 \\sim C20 \\sim C33 \\sim C29 \\sim C17 \\sim O10 \\sim C22: within 4A with
sigma of 0.02 and sigma for terminal atoms of 0.04
C34 \\sim N2 \\sim C35 \\sim C31 \\sim C33 \\sim C29 \\sim C30 \\sim Zn1 \\sim
O11 \\sim C37 \\sim C25: within 2A with sigma of 0.015 and sigma for terminal
atoms of 0.015
4. Rigid body (RIGU) restrains
 O11, C31, C23, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.006
 O8, C13
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.009 and sigma for 1-3 distances of 0.015
 C17, C25, C33, C18
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.003
5. Others
 Fixed Sof: C18(0.5) H18A(0.5) H18B(0.5) C19(0.5) H19A(0.5) H19B(0.5)
 H20C(0.5) H20D(0.5) H20A(0.5) H20B(0.5) C22(0.5) H22A(0.5) H22B(0.5) H24C(0.5)
 H24D(0.5) H24A(0.5) H24B(0.5) H25C(0.5) H25D(0.5) H25A(0.5) H25B(0.5)
 H26C(0.5) H26D(0.5) H26A(0.5) H26B(0.5) C32(0.5) H32A(0.5) H32B(0.5) C33(0.5)
 H33A(0.5) H33B(0.5) C38(0.5) H38A(0.5) H38B(0.5) N2(0.25) H2A(0.25) H2B(0.25)
 C34(0.25) H34A(0.25) H34B(0.25) H34C(0.25) C35(0.25) H35A(0.25) H35B(0.25)
 H35C(0.25) N3(0.25) H3A(0.25) H3B(0.25) C36(0.25) H36A(0.25) H36B(0.25)
 H36C(0.25) C37(0.25) H37A(0.25) H37B(0.25) H37C(0.25)
6.a Riding coordinates:
 N1(H1), N2(H2A,H2B), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), N3(H3A,H3B),
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C)
6.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,
 H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20C,H20D),
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24C,H24D),
  C24(H24A,H24B), C25(H25C,H25D), C25(H25A,H25B), C26(H26C,H26D), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
 C32(H32A,H32B), C33(H33A,H33B), C38(H38A,H38B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C9(H9), C12(H12), C31(H31)
6.d Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7)
;
_olex2_submission_special_instructions 'No special instructions were received'