Rapid and high-throughput synthesis of diverse MOFs with centrifuge tube grinding strategy
Wang, Hao-Cheng; Liu, Xiao; Ma, Jian-Gong; Cheng, Peng; Green Chemistry 26 (2024) 7312–7319; doi:10.1039/D4GC00865K

data_7248647
_publ_section_title
;
 Rapid and high-throughput synthesis of diverse MOFs with centrifuge tube
 grinding strategy
;
_journal_issue                   12
_journal_name_full               'Green Chemistry'
_journal_page_first              7312
_journal_page_last               7319
_journal_paper_doi               10.1039/D4GC00865K
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C48 H66 Hf6 O33, 3(C4 H6 O2), C4 H10 O'
_chemical_formula_sum            'C64 H94 Hf6 O40'
_chemical_formula_weight         2574.33
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-01-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-02-25 deposited with the CCDC.	2024-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.3140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0824(2)
_cell_length_b                   17.9419(2)
_cell_length_c                   30.7631(4)
_cell_measurement_reflns_used    41781
_cell_measurement_temperature    148.0(3)
_cell_measurement_theta_max      29.1350
_cell_measurement_theta_min      3.2930
_cell_volume                     9371.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      148.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.909
_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     -7.00  91.00   1.00   15.00    --   18.63  37.00   0.00   98
  2  \w     35.00  64.00   1.00   15.00    --   18.63 178.00 -60.00   29
  3  \w    -90.00  10.00   1.00   15.00    --  -19.56 -77.00  30.00  100
  4  \w    -50.00  42.00   1.00   15.00    --  -19.56  77.00   0.00   92
  5  \w    -41.00  48.00   1.00   15.00    --  -19.56  57.00 -90.00   89
  6  \w    -79.00  -5.00   1.00   15.00    --  -19.56 128.00 111.72   74
  7  \w    -96.00 -34.00   1.00   15.00    --  -19.56 178.00   0.00   62
  8  \w    -85.00   2.00   1.00   15.00    --  -19.56 -57.00 112.00   87
  9  \w    -90.00  10.00   1.00   15.00    --  -19.56 -77.00-120.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0199590000
_diffrn_orient_matrix_UB_12      -0.0188021000
_diffrn_orient_matrix_UB_13      -0.0158297000
_diffrn_orient_matrix_UB_21      -0.0280019000
_diffrn_orient_matrix_UB_22      -0.0292868000
_diffrn_orient_matrix_UB_23      -0.0006864000
_diffrn_orient_matrix_UB_31      -0.0237072000
_diffrn_orient_matrix_UB_32      0.0187262000
_diffrn_orient_matrix_UB_33      -0.0169545000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            137865
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.308
_diffrn_reflns_theta_min         2.849
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.697
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.825
_exptl_crystal_description       block
_exptl_crystal_F_000             4920
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.312
_exptl_crystal_size_min          0.298
_refine_diff_density_max         2.409
_refine_diff_density_min         -1.670
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1012
_refine_ls_number_reflns         23334
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+215.6274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1286
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18325
_reflns_number_total             23334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4gc00865k2.cif
_cod_data_source_block           p201212e_sq
_cod_depositor_comments          'Adding full bibliography for 7248647.cif.'
_cod_database_code               7248647
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         HfCHON
_shelx_estimated_absorpt_t_max   0.240
_shelx_estimated_absorpt_t_min   0.206
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  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
 C13-C1
 1.54 with sigma of 0.02
 C02D-C01S
 1.54 with sigma of 0.02
 C027-C01S
 1.4 with sigma of 0.02
 C3-O2
 1.43 with sigma of 0.02
 O016-C3
 1.3 with sigma of 0.02
 C3-O016
 1.43 with sigma of 0.02
 C2-C1
 1.54 with sigma of 0.02
 C1-C13
 1.34 with sigma of 0.02
 C15-C02I
 1.54 with sigma of 0.02
 C20-C15
 1.34 with sigma of 0.02
 C11-C19
 1.54 with sigma of 0.02
 H015-O17
 1.85 with sigma of 0.02
 C19-C21
 1.54 with sigma of 0.02
 H2-O00Y
 1.88 with sigma of 0.02
 C16-C18
 1.34 with sigma of 0.02
 C16-C10
 1.54 with sigma of 0.02
 H00F-H015
 2.1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C16) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
: with sigma of 0 and sigma for terminal atoms of 0
Uanis(C14) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C3) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O2) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C19) \\sim Ueq: with sigma of 0 and sigma for terminal atoms of 0
Uanis(C18) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(Hf01) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C20) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O012) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4.a Rotating group:
 O014(H01A,H01B)
4.b Ternary CH refined with riding coordinates:
 O00B(H00B), O00C(H00C), O00E(H00E), O00F(H00F)
4.c Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C11(H11A,H11B), C19(H19A,H19B)
4.d X=CH2 refined with riding coordinates:
 C01R(H01F,H01G), C01V(H01H,H01I), C01Y(H01J,H01K), C01Z(H01L,H01M), C027(H02G,
 H02H), C028(H02I,H02J), C02E(H02Q,H02R), C02F(H02S,H02T), C02G(H02U,H02V),
 C02K(H02Z,HB), C02L(H02,HC), C14(H14A,H14B), C20(H20A,H20B), C18(H18A,H18B),
 C13(H13A,H13B)
4.e Idealised Me refined as rotating group:
 C01O(H01C,H01D,H01E), C020(H02A,H02B,H02C), C022(H02D,H02E,H02F), C029(H02K,
 H02L,H02M), C02D(H02N,H02O,H02P), C02H(H02W,H02X,H02Y), C02I(H1,H,HA), C4(H4A,
 H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C21(H21A,H21B,H21C), C2(H2A,H2B,H2C)
4.f Idealised tetrahedral OH refined as rotating group:
 O015(H015), O019(H019), O01A(H01N), O2(H2)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              51326
_shelx_fab_checksum              94639
_platon_squeeze_void_probe_radius 1.20
_olex2_date_sample_data_collection 2020-12-13
_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 1.931
_oxdiff_exptl_absorpt_empirical_full_min 0.636