Pressure-induced postsynthetic cluster anion substitution in a MIL-53 topology scandium metal-organic framework.
Thom, Alexander J. R.; Turner, Gemma F.; Davis, Zachary H.; Ward, Martin R.; Pakamorė, Ignas; Hobday, Claire L.; Allan, David R.; Warren, Mark R.; Leung, Wai L. W.; Oswald, Iain D. H.; Morris, Russell E.; Moggach, Stephen A.; Ashbrook, Sharon E.; Forgan, Ross S.; Chemical science 14 (2023) 7716–7724; doi:10.1039/d3sc00904a

data_1569393
_publ_section_title
;
 Pressure-induced postsynthetic cluster anion substitution in a MIL-53
 topology scandium metal-organic framework.
;
_journal_issue                   28
_journal_name_full               'Chemical science'
_journal_page_first              7716
_journal_page_last               7724
_journal_paper_doi               10.1039/d3sc00904a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety
'Sc2 C33.9 H22.2 O10, 1.6(C3 H7 N O), 0.2(C H4 O)'
_chemical_formula_sum            'C36.1 H28.4 N1.2 O11.7 Sc2'
_chemical_formula_weight         756.12
_chemical_name_common            GUF-1
_space_group_crystal_system      orthorhombic
_space_group_IT_number           67
_space_group_name_Hall           '-C 2a 2'
_space_group_name_H-M_alt        'C m m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-04
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-01 deposited with the CCDC.	2023-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.3533(15)
_cell_length_b                   26.584(5)
_cell_length_c                   11.879(2)
_cell_measurement_pressure       230000
_cell_measurement_reflns_used    433
_cell_measurement_temperature    298
_cell_measurement_theta_max      17.4430
_cell_measurement_theta_min      2.2790
_cell_volume                     2322.1(8)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_pressure         230000
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.371
_diffrn_measured_fraction_theta_max 0.361
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -35.00  35.00   0.20    0.40 -90.00 -11.00   0.00    --   350
  2  \w   -133.00 -85.00   0.20    0.40    --  -11.00  70.00 -24.23  240
  3  \w   -141.00 -85.00   0.20    0.40    --  -11.00  70.00 155.77  280
  4  \w   -113.00 -82.00   0.20    0.40    --   12.00  70.00 155.77  155
  5  \w   -113.00 -82.00   0.20    0.40    --   12.00  70.00 -24.23  155
  6  \w   -101.00 -41.00   0.20    0.40    --   12.00 -70.00  24.23  300
  7  \w   -102.00 -41.00   0.20    0.40    --   12.00 -70.00-155.77  305
  8  \w    -97.00 -64.00   0.20    0.40    --  -11.00 -70.00-155.77  165
  9  \w    -97.00 -64.00   0.20    0.40    --  -11.00 -70.00  24.23  165
;
_diffrn_measurement_device       '4-circle diffractometer'
_diffrn_measurement_device_type  'I19-2, Diamond Light Source'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4589
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_Laue_measured_fraction_full 0.371
_diffrn_reflns_Laue_measured_fraction_max 0.361
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1401
_diffrn_reflns_point_group_measured_fraction_full 0.371
_diffrn_reflns_point_group_measured_fraction_max 0.361
_diffrn_reflns_theta_full        15.982
_diffrn_reflns_theta_max         16.678
_diffrn_reflns_theta_min         2.574
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.34
_exptl_absorpt_correction_T_max  0.7442
_exptl_absorpt_correction_T_min  0.5466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0815 before and 0.0636 after correction.
The Ratio of minimum to maximum transmission is 0.7345.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_description       block
_exptl_crystal_F_000             778
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         478
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1256
_refine_ls_R_factor_gt           0.1025
_refine_ls_shift/su_max          1.746
_refine_ls_shift/su_mean         0.261
_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          0.2710
_refine_ls_wR_factor_ref         0.2879
_reflns_Friedel_coverage         0.000
_reflns_number_gt                320
_reflns_number_total             478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00904a2.cif
_cod_data_source_block           230MPa
_cod_depositor_comments
'Adding full bibliography for 1569390--1569403.cif.'
_cod_original_cell_volume        2322.2(8)
_cod_original_sg_symbol_Hall     '-C 2b 2'
_cod_original_sg_symbol_H-M      'C m m e'
_cod_original_formula_sum        'Sc2 C36.1 H28.4 N1.2 O11.7'
_cod_database_code               1569393
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, H7 of C7, All O(H) groups
 At 1.2 times of:
  H2 of C9, H4 of C4, H3 of C3
2. Restrained distances
 O2-H2
 0.875 with sigma of 0.001
 C4-C3
 1.39 with sigma of 0.01
 C5-C4
 1.39 with sigma of 0.01
 C6-C5
 1.44 with sigma of 0.01
 C3-C2
 1.39 with sigma of 0.01
 C2-C1
 1.502 with sigma of 0.01
 O1-C1
 1.245 with sigma of 0.01
 C6-C4
 2.454 with sigma of 0.01
 C1-C3
 2.497 with sigma of 0.01
 O1-C2
 2.349 with sigma of 0.01
 C3-C5
 2.4 with sigma of 0.01
 C2-C4
 2.4 with sigma of 0.01
 O1_$1-O1
 2.213 with sigma of 0.01
 C3_$1-C3
 2.4 with sigma of 0.01
 C4-C4_$1
 2.4 with sigma of 0.01
 C4_$1-C2
 2.4 with sigma of 0.01
 C5-C3_$1
 2.4 with sigma of 0.01
 O4-C10
 1.35 with sigma of 0.01
 N1-C8 \\sim N1-C9
 with sigma of 0.02
3. Restrained planarity
 C7, O3, N1, C8, C9
 with sigma of 0.1
 C1, O1, O1_$1, C2, C5, C6, C6_$2
 with sigma of 0.01
 C2, C5, C3_$1, C3, C4_$1, C1, C6, C4
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C7 \\sim O3 \\sim N1 \\sim C8 \\sim C9: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uiso(O3) = Uiso(C7) = Uiso(N1) = Uiso(C8) = Uiso(C9)
Uanis(C2) = Uanis(C5) = Uanis(C3) = Uanis(C4)
Uanis(C6) = Uanis(O1) = Uanis(C1)
Uiso(O4) = Uiso(C10)
5. Rigid body (RIGU) restrains
 C7, O3, N1, C8, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C7(0.1) H7(0.1) O3(0.1) N1(0.2) C8(0.2) H8A(0.2) H8B(0.2) H8C(0.2)
 C9(0.1) H9A(0.1) H9B(0.1) H9C(0.1) O4(0.125) H4A(0.125) C10(0.125) H10A(0.125)
 H10B(0.125) H10C(0.125)
7.a Free rotating group:
 C7(O3,N1,C8,C9)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7)
7.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
7.d Idealised tetrahedral OH refined as rotating group:
 O4(H4A)
;
_shelx_res_checksum              9756
_olex2_submission_special_instructions 'No special instructions were received'