Ultrathin two-dimensional (2D) manganese-based metal–organic framework nanosheets for selective photocatalytic oxidation of thioether
Zhu, Jing; Huo, Cuimeng; Chen, Jin; Ma, Xiaoxing; Zhu, Xiangjun; Li, Yan; Li, Guofang; Chen, Haitao; Duan, Xianying; Han, Fujiao; Kong, Hongjun; Zheng, Fuwei; Jiang, Aiyun; Dalton Transactions 53 (2024) 15688–15695; doi:10.1039/D4DT01251H

data_7716944
_publ_section_title
;
 Ultrathin two-dimensional (2D) manganese-based metal--organic framework
 nanosheets for selective photocatalytic oxidation of thioether
;
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              15688
_journal_page_last               15695
_journal_paper_doi               10.1039/D4DT01251H
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C64 H43 Mn2 N O20, 2(C0.918 H2.509 O0.285)'
_chemical_formula_sum            'C65.85 H48.06 Mn2 N O20.58'
_chemical_formula_weight         1292.47
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-08-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-08-27 deposited with the CCDC.	2024-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                71.856(3)
_cell_angle_beta                 69.878(3)
_cell_angle_gamma                75.205(2)
_cell_formula_units_Z            1
_cell_length_a                   12.3933(4)
_cell_length_b                   13.4724(4)
_cell_length_c                   14.8545(5)
_cell_measurement_reflns_used    9570
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      73.7090
_cell_measurement_theta_min      3.2980
_cell_volume                     2182.28(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.49a (Rigaku OD, 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    DMF/H2O/EtOH
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.965
_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    -76.00 -51.00   0.50    0.05    --  -39.95 129.00 158.00   50
  2  \w    -83.00 -58.00   0.50    0.05    --  -39.95 140.00 -28.00   50
  3  \w   -117.00 -92.00   0.50    0.05    --  -39.95-129.00  85.00   50
  4  \w    -98.00 -64.00   0.50    0.05    --  -39.95-140.00 -87.00   68
  5  \w     48.00 100.00   0.50    0.05    --   39.95-129.00  85.00  104
  6  \w     51.00  76.00   0.50    0.05    --   39.95-140.00 -87.00   50
  7  \w   -160.00 -93.00   0.50    0.20    --  -94.50-129.00  85.00  134
  8  \w    -99.00 -72.00   0.50    0.20    --  -94.50-140.00 -87.00   54
  9  \w    -93.00 -50.00   0.50    0.20    --  -94.50 140.00 -28.00   86
 10  \w     37.00 113.00   0.50    0.20    --  108.87-129.00  85.00  152
 11  \w    111.00 136.00   0.50    0.20    --  108.87 129.00 158.00   50
 12  \w     85.00 128.00   0.50    0.20    --  108.87 140.00 -28.00   86
 13  \w     71.00 123.00   0.50    0.20    --  108.87-140.00 -87.00  104
 14  \w    -13.00  44.00   0.50    0.05    --  -39.95  19.00  60.00  114
 15  \w    -27.00  25.00   0.50    0.05    --  -39.95  19.00 -60.00  104
 16  \w    -42.00 -13.00   0.50    0.05    --  -39.95  37.00-180.00   58
 17  \w     -3.00  38.00   0.50    0.05    --  -39.95  37.00-180.00   82
 18  \w    -26.00  43.00   0.50    0.05    --  -39.95  19.00 120.00  138
 19  \w      6.00 111.00   0.50    0.05    --   39.95  77.00 -30.00  210
 20  \w     71.00 122.00   0.50    0.05    --   39.95 178.00 -90.00  102
 21  \w    -50.00 -18.00   0.50    0.20    --  -94.50  45.00-150.00   64
 22  \w    -50.00 -15.00   0.50    0.20    --  -94.50  45.00 120.00   70
 23  \w   -107.00 -58.00   0.50    0.20    --  -94.50 -30.00 -90.00   98
 24  \w    -49.00 -15.00   0.50    0.20    --  -94.50  45.00 150.00   68
 25  \w   -177.00-120.00   0.50    0.20    --  -94.50 -30.00 -90.00  114
 26  \w    -50.00 -17.00   0.50    0.20    --  -94.50  45.00  30.00   66
 27  \w   -159.00-127.00   0.50    0.20    --  -94.50 -61.00 150.00   64
 28  \w   -105.00 -79.00   0.50    0.20    --  -94.50 -61.00 150.00   52
 29  \w     79.00 107.00   0.50    0.20    --  108.87-105.00 -16.84   56
 30  \w     79.00 111.00   0.50    0.20    --  108.87-125.00-180.00   64
 31  \w     80.00 177.00   0.50    0.20    --  108.87  61.00 150.00  194
 32  \w     98.00 176.00   0.50    0.20    --  108.87 125.00  30.00  156
 33  \w     34.00  60.00   0.50    0.20    --  108.87 -61.00 -60.00   52
 34  \w     98.00 176.00   0.50    0.20    --  108.87 125.00-180.00  156
 35  \w     55.00 106.00   0.50    0.20    --  108.87-125.00-150.00  102
 36  \w     44.00 110.00   0.50    0.20    --  108.87-125.00 -60.00  132
 37  \w     38.00  71.00   0.50    0.20    --  108.87 -61.00 -30.00   66
 38  \w    102.00 147.00   0.50    0.20    --  108.87 125.00 -60.00   90
 39  \w     36.00  61.00   0.50    0.20    --  108.87-125.00-180.00   50
 40  \w     60.00  97.00   0.50    0.20    --  108.87 -94.00  90.00   74
 41  \w    133.00 173.00   0.50    0.20    --  108.87   0.00   0.00   80
 42  \w     29.00  64.00   0.50    0.20    --  108.87 -94.00 -60.00   70
 43  \w     74.00 100.00   0.50    0.20    --  108.87 -94.00 -60.00   52
 44  \w     82.00 172.00   0.50    0.20    --  108.87  30.00 120.00  180
 45  \w     58.00  84.00   0.50    0.20    --  108.87   0.00   0.00   52
 46  \w     24.00  53.00   0.50    0.20    --  108.87   0.00   0.00   58
 47  \w     34.00  66.00   0.50    0.20    --  108.87 -61.00-150.00   64
 48  \w     46.00  81.00   0.50    0.20    --  108.87 -77.00  90.00   70
 49  \w     35.00  63.00   0.50    0.20    --  108.87 -77.00 -30.00   56
 50  \w     80.00 105.00   0.50    0.20    --  108.87 -77.00-120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_unetI/netI     0.0897
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25387
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.054
_diffrn_reflns_theta_min         3.269
_exptl_absorpt_coefficient_mu    2.822
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.49a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.983
_exptl_crystal_description       block
_exptl_crystal_F_000             665
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         8564
_refine_ls_number_restraints     996
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0626
_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^)+(0.0855P)^2^+1.1003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1670
_refine_ls_wR_factor_ref         0.1797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6464
_reflns_number_total             8564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01251h2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments          'Adding full bibliography for 7716944.cif.'
_cod_database_code               7716944
_shelx_shelxl_version_number     2018/3
_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 C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 N1-C33 = N1-C32
 1.35 with sigma of 0.001
 C33-C31
 2.38 with sigma of 0.001
 O12-C1A
 1.42 with sigma of 0.02
 C1A-C1B
 1.51 with sigma of 0.02
 O12-C1B
 2.37 with sigma of 0.04
3. Rigid bond restraints
 O12, C1A, C1B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C1 \\sim C9 \\sim C27 \\sim C16 \\sim C7 \\sim C3 \\sim C4 \\sim C24 \\sim C5
\\sim C15 \\sim C23 \\sim C25 \\sim C6 \\sim C10 \\sim C2 \\sim C26 \\sim C22
\\sim C17 \\sim C8 \\sim C29 \\sim C28 \\sim C21 \\sim C18 \\sim C11 \\sim C30
\\sim C20 \\sim C19 \\sim C14 \\sim C12 \\sim C13 \\sim C33 \\sim C31 \\sim
C32: within 3.8A with sigma of 0.02 and sigma for terminal atoms of 0.01 within
3.8A
O12 \\sim C1A \\sim C1B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C1C: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim
Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O8)
\\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.02 and sigma for terminal
atoms of 0.01
Uanis(O11) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O12) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C1B) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O9A) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(C1C) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 O12, C1A, C1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=FVAR(1)
 Sof(O12)=Sof(H12A)=FVAR(2)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=FVAR(3)
 Fixed Sof: C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) N1(0.5) C31(0.5) H31(0.5)
 C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5) O10(0.5) H10A(0.5) H10B(0.5) O11(0.5)
 O9A(0.5) O9(0.5) H9A(0.5) H9B(0.5) C1C(0.5)
7.a Rotating group:
 O10(H10A,H10B), O9(H9A,H9B)
7.b Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB)
7.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C3(H3), C24(H24), C6(H6), C8(H8), C21(H21), C18(H18), C11(H11),
 C30(H30), C20(H20), C19(H19), C14(H14), C12(H12), C13(H13), C31(H31)
7.d Tetrahedral OH refined with riding coordinates:
 O2(H2), O4(H4)
7.e Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C32(H32A,H32B,H32C), C1B(H1BA,H1BB,H1BC)
7.f Idealised tetrahedral OH refined as rotating group:
 O12(H12A)
;
_shelx_res_checksum              72807
_shelx_hkl_checksum              66270
_shelx_fab_checksum              34175
_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
;