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_7129947
_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         '2(C16 H18 N O4), 2(C18 H36 O6)'
_chemical_formula_sum            'C68 H108 N2 O20'
_chemical_formula_weight         1273.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-12-29
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2022-02-26 deposited with the CCDC.	2022-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                78.268(2)
_cell_angle_beta                 81.410(2)
_cell_angle_gamma                77.789(2)
_cell_formula_units_Z            2
_cell_length_a                   13.1611(2)
_cell_length_b                   14.9762(3)
_cell_length_c                   19.1811(4)
_cell_measurement_reflns_used    13356
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      75.9460
_cell_measurement_theta_min      4.1580
_cell_volume                     3595.51(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -73.00  37.00   1.00    1.00    --  -41.77  19.00   0.00  110
  2  \w   -116.00 -31.00   1.00    1.00    --  -41.77 -38.00-180.00   85
  3  \w    -81.00 -19.00   1.00    1.00    --  -41.77 125.00  90.00   62
  4  \w    -26.00  58.00   1.00    1.00    --   41.77 -57.00  30.00   84
  5  \w     45.00  98.00   1.00    1.00    --   41.77-125.00 -30.00   53
  6  \w     27.00  52.00   1.00    1.00    --   41.77-125.00  60.00   25
  7  \w    111.00 158.00   1.00    4.00    --  112.00  61.00 150.00   47
  8  \w     39.00 117.00   1.00    4.00    --  112.00-125.00 150.00   78
  9  \w     39.00 137.00   1.00    4.00    --  112.00 -45.00  90.00   98
 10  \w     56.00 101.00   1.00    4.00    --  112.00 -94.00-180.00   45
 11  \w    103.00 177.00   1.00    4.00    --  112.00  61.00-150.00   74
 12  \w    101.00 160.00   1.00    4.00    --  112.00  45.00 -60.00   59
 13  \w     95.00 165.00   1.00    4.00    --  112.00 125.00 150.00   70
 14  \w     88.00 153.00   1.00    4.00    --  112.00  45.00 -90.00   65
 15  \w     39.00 116.00   1.00    4.00    --  112.00-125.00  30.00   77
 16  \w     89.00 118.00   1.00    4.00    --  112.00-125.00 -90.00   29
 17  \w     41.00 139.00   1.00    4.00    --  112.00 -61.00-150.00   98
 18  \w    128.00 172.00   1.00    4.00    --  112.00 125.00-180.00   44
 19  \w    -32.00  -6.00   1.00    6.00    --  -41.89  38.00-180.00   26
 20  \w    153.00 178.00   1.00   24.00    --  112.00  61.00   0.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0258420000
_diffrn_orient_matrix_UB_12      -0.0354942000
_diffrn_orient_matrix_UB_13      0.0777205000
_diffrn_orient_matrix_UB_21      0.0008334000
_diffrn_orient_matrix_UB_22      -0.1001746000
_diffrn_orient_matrix_UB_23      -0.0087186000
_diffrn_orient_matrix_UB_31      0.1177038000
_diffrn_orient_matrix_UB_32      -0.0119858000
_diffrn_orient_matrix_UB_33      -0.0263949000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26589
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.134
_diffrn_reflns_theta_min         3.457
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75195
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       block
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         14572
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0846
_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^)+(0.1444P)^2^+2.4524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2435
_refine_ls_wR_factor_ref         0.2576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12176
_reflns_number_total             14572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01198k2.cif
_cod_data_source_block           exp_846
_cod_original_cell_volume        3595.52(12)
_cod_database_code               7129947
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_usercomment     BDM
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.872
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Restrained distances
 O008-C01A \\sim O0-C0AA
 with sigma of 0.02
 C00N-C01A \\sim C00N-C0AA
 with sigma of 0.02
 O00U-C01A \\sim O00V-C0AA
 with sigma of 0.02
 O00U-C02E \\sim O00V-C1AA
 with sigma of 0.02
 C029-C02E \\sim C0-C1AA
 with sigma of 0.02
 O008-C00N \\sim O0-C00N
 with sigma of 0.04
 O008-O00U \\sim O0-O00V
 with sigma of 0.04
 C00N-O00U \\sim C00N-O00V
 with sigma of 0.04
 O00U-C029 \\sim O00V-C0
 with sigma of 0.04
 C01A-C02E \\sim C0AA-C1AA
 with sigma of 0.04
2. Rigid bond restraints
 O008, O0
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(O008) = Uanis(O0)
4. Rigid body (RIGU) restrains
 C023, C01Z, O013
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O00H, C021
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C00Z, N00G, C01E
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C00Z, N1, C01E
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O008, O0
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(H1BA)=Sof(HC)=Sof(C0AA)=Sof(O0)=Sof(O00V)=Sof(C1AA)=Sof(H1AB)=Sof(H1AC)=
 Sof(C0)=Sof(H0A)=Sof(H0B)=Sof(H0C)=Sof(N1)=Sof(H1)=1-FVAR(1)
 Sof(O008)=Sof(N00G)=Sof(H00G)=Sof(O00U)=Sof(C01A)=Sof(HA)=Sof(HB)=Sof(C029)=
 Sof(H02)=Sof(HQ)=Sof(HR)=Sof(C02E)=Sof(H9AA)=Sof(HV)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C00S(H00A,H00B), C016(H7AA,H), C017(H01A,H01B), C018(H01C,H01D), C01C(H01E,
 H01F), C01D(H01G,H01H), C01E(HA,HB), C01E(H1BA,HC), C01F(H01,HD), C01H(H0AA,
 HE), C01I(H1AA,HF), C01J(H01I,H01J), C01L(H01K,H01L), C01M(H01M,H01N),
 C01N(H2AA,HI), C01O(H01O,H01P), C01P(H01Q,H01R), C01Q(H3AA,HJ), C01R(H4AA,HK),
 C01S(H01S,H01T), C01T(H5AA,HL), C01U(H01U,H01V), C01V(H01W,H01X), C01W(H01Y,
 HM), C01X(H01Z,HN), C01Y(H3BA,HO), C01Z(H6AA,HP), C020(H02A,H02B), C021(H02I,
 H02J), C022(H02C,H02D), C023(H02K,H02L), C024(H02E,H02F), C025(H02M,H02N),
 C026(H02O,H02P), C027(H02Q,H02R), C028(H02S,H02T), C02A(H4BA,HS), C02B(H02U,
 H02V), C02C(H02G,H02H), C02E(H9AA,HV), C02F(H02W,H02X), C02G(H02Y,HW),
 C02I(H02Z,HZ), C1AA(H1AB,H1AC)
6.b Aromatic/amide H refined with riding coordinates:
 N009(H009), N00G(H00G), C00K(H00K), C00Q(H00Q), C00R(H00R), C00T(H00T),
 C00V(H00V), C00Y(H00Y), C010(H010), C011(H011), C01B(H0BA), C01G(H2BA), N1(H1)
6.c Idealised Me refined as rotating group:
 C01K(H8AA,HG,HH), C029(H02,HQ,HR), C02D(H5BA,HT,HU), C02H(H6BA,HX,HY), C0(H0A,
 H0B,H0C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.320
_oxdiff_exptl_absorpt_empirical_full_min 0.557