Structural transformation of metal oxo species within UiO-66 type metal–organic frameworks
Wasson, Megan C.; Xie, Haomiao; Wang, Xingjie; Duncan, Joshua S.; Farha, Omar K.; CrystEngComm  (2022) –; doi:10.1039/D2CE00650B

data_7245131
_publ_section_title
;
 Structural transformation of metal oxo species within UiO-66 type
 metal--organic frameworks
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00650B
_journal_year                    2022
_chemical_formula_moiety         'C72 H60 Ce5 N4 O34'
_chemical_formula_sum            'C72 H60 Ce5 N4 O34'
_chemical_formula_weight         2225.84
_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             2022-04-18
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2022-04-18 deposited with the CCDC.	2022-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                89.9738(15)
_cell_angle_beta                 86.8717(14)
_cell_angle_gamma                89.3377(13)
_cell_formula_units_Z            2
_cell_length_a                   13.9994(2)
_cell_length_b                   15.2612(3)
_cell_length_c                   17.7824(3)
_cell_measurement_reflns_used    28735
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      79.1000
_cell_measurement_theta_min      3.9210
_cell_volume                     3793.25(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.903
_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    -90.00 -48.00   0.50    2.50    --  -47.42 137.00 -56.00   84
  2  \w     34.00 102.00   0.50    2.50    --   47.42-137.00-120.00  136
  3  \w     69.00  95.00   0.50    2.50    --   47.42 132.00 126.00   52
  4  \w     68.00  93.00   0.50    2.50    --   47.42 137.00 -56.00   50
  5  \w    -99.00 -74.00   0.50   10.00    -- -106.00 132.00 126.00   50
  6  \w   -101.00 -76.00   0.50   10.00    -- -106.00 137.00 -56.00   50
  7  \w     90.00 121.00   0.50   10.00    --  113.25-137.00-120.00   62
  8  \w     95.00 134.00   0.50   10.00    --  113.25 132.00 126.00   78
  9  \w     92.00 117.00   0.50   10.00    --  113.25-132.00  56.00   50
 10  \w     67.00 155.00   0.50   10.00    --  113.25 137.00 -56.00  176
 11  \w   -115.00 -79.00   0.50    2.50    --  -47.42   0.00 -60.00   72
 12  \w   -115.00 -77.00   0.50    2.50    --  -47.42   0.00  90.00   76
 13  \w    -27.00  17.00   0.50    2.50    --   47.42 -19.00 -30.00   88
 14  \w    -27.00  13.00   0.50    2.50    --   47.42 -19.00 -60.00   80
 15  \w    -21.00  16.00   0.50    2.50    --   47.42 -19.00-120.00   74
 16  \w    -74.00 -34.00   0.50   10.00    -- -106.00  61.00 150.00   80
 17  \w    -66.00 -36.00   0.50   10.00    -- -106.00 103.00  77.07   60
 18  \w   -106.00 -70.00   0.50   10.00    -- -106.00 103.00  77.07   72
 19  \w   -134.00 -84.00   0.50   10.00    -- -106.00 -77.00 -30.00  100
 20  \w    101.00 178.00   0.50   10.00    --  113.25  30.00 -60.00  154
 21  \w     50.00 136.00   0.50   10.00    --  113.25 -77.00  30.00  172
 22  \w    152.00 178.00   0.50   10.00    --  113.25  30.00 120.00   52
 23  \w    107.00 133.00   0.50   10.00    --  113.25  30.00 120.00   52
 24  \w    101.00 176.00   0.50   10.00    --  113.25  30.00  60.00  150
 25  \w     42.00  69.00   0.50   10.00    --  113.25 -61.00-180.00   54
 26  \w     70.00 106.00   0.50   10.00    --  113.25 -94.00 120.00   72
 27  \w     42.00 102.00   0.50   10.00    --  113.25 -94.00  30.00  120
 28  \w     43.00  68.00   0.50   10.00    --  113.25 -61.00 -90.00   50
 29  \w     10.00  35.00   0.50    2.50    --    0.78   4.00 -70.00   50
 30  \w    -71.00 -34.00   0.50    2.50    --    0.78  -4.00 113.00   74
 31  \w    -12.00  14.00   0.50    2.50    --    0.78 -99.00-150.00   52
 32  \w    -23.00  26.00   0.50    2.50    --    0.78 -99.00  60.00   98
 33  \w   -128.00-102.00   0.50   10.00    --  -78.30 -57.00 150.00   52
 34  \w    -42.00 -17.00   0.50   10.00    --  -78.30  37.00   0.00   50
 35  \w    -95.00 -35.00   0.50   10.00    --  -78.30  77.00 -60.00  120
 36  \w   -101.00 -69.00   0.50   10.00    --  -78.30 -57.00 150.00   64
 37  \w    -66.00 -10.00   0.50   10.00    --  -78.30  57.00 -60.00  112
 38  \w    -42.00 -17.00   0.50   10.00    --  -78.30  37.00 -60.00   50
 39  \w    -42.00 -16.00   0.50   10.00    --  -78.30  37.00-150.00   52
 40  \w    -64.00 -27.00   0.50   10.00    --  -78.30  77.00-120.00   74
 41  \w    -64.00 -36.00   0.50   10.00    --  -78.30  57.00  30.00   56
 42  \w    111.00 152.00   0.50   10.00    --   79.86   0.00-120.00   82
 43  \w      7.00  36.00   0.50   10.00    --   79.86 -37.00-150.00   58
 44  \w     12.00  38.00   0.50   10.00    --   79.86 -37.00  60.00   52
 45  \w    111.00 142.00   0.50   10.00    --   79.86   0.00-150.00   62
 46  \w      9.00  35.00   0.50   10.00    --   79.86 -37.00 -30.00   52
 47  \w      8.00  38.00   0.50   10.00    --   79.86 -37.00   0.00   60
 48  \w   -116.00 -91.00   0.50   10.00    --  -78.30  -4.00 113.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1101715000
_diffrn_orient_matrix_UB_12      0.0016230000
_diffrn_orient_matrix_UB_13      -0.0041188000
_diffrn_orient_matrix_UB_21      0.0030588000
_diffrn_orient_matrix_UB_22      -0.1009230000
_diffrn_orient_matrix_UB_23      -0.0016975000
_diffrn_orient_matrix_UB_31      0.0007255000
_diffrn_orient_matrix_UB_32      0.0018838000
_diffrn_orient_matrix_UB_33      -0.0866512000
_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  0.0526
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45422
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.674
_diffrn_reflns_theta_min         3.819
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    23.518
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.949
_exptl_crystal_description       plate
_exptl_crystal_F_000             2164
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         7.856
_refine_diff_density_min         -5.860
_refine_diff_density_rms         0.476
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1032
_refine_ls_number_reflns         14925
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.1231
_refine_ls_R_factor_gt           0.1205
_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^)+(0.0711P)^2^+623.2277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3275
_refine_ls_wR_factor_ref         0.3285
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14035
_reflns_number_total             14925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00650b2.cif
_cod_data_source_block           NU-351
_cod_original_cell_volume        3793.24(11)
_cod_database_code               7245131
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ce C O'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
C12 \\sim O14 \\sim O13: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C12 \\sim O13 \\sim C6 \\sim C7 \\sim C11: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C15 \\sim O16 \\sim O17 \\sim C9: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C24 \\sim C25 \\sim C28 \\sim C29 \\sim C27 \\sim C26 \\sim C33: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C94) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O96) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C45) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C12) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(O16)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C30) \\sim Ueq, Uanis(O31) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C30) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(O22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C21) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O93) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O13) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C69) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C33) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C94) = Uanis(C30)
Uanis(O31) = Uanis(O96)
2.a Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B), C50(H50A,H50B)
2.b Aromatic/amide H refined with riding coordinates:
 C44(H44), C56(H56), C20(H20), C7(H7), C38(H38), C49(H49), C8(H8), C55(H55),
 C37(H37), C68(H68), C11(H11), C28(H28), C62(H62), C43(H43), C19(H19), C86(H86),
  C10(H10), C29(H29), C89(H89), C67(H67), C25(H25), C108(H108), C90(H90),
 C26(H26), C98(H98), C87(H87), C103(H103), C77(H77), C74(H74), C78(H78),
 C75(H75), C113(H113)
2.c Idealised Me refined as rotating group:
 C106(H10A,H10B,H10C), C105(H10D,H10E,H10F), C111(H11A,H11B,H11C), C110(H11D,
 H11E,H11F), C101(H10G,H10H,H10I), C100(H10J,H10K,H10L), C116(H11G,H11H,H11I),
 C115(H11J,H11K,H11L)
;
_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 2.387
_oxdiff_exptl_absorpt_empirical_full_min 0.385