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_1569390
_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  C32.5 H19.5 O10,  2.84(C H4 O), 0.90(H2 O)'
_chemical_formula_sum            'C35.1 H35.5 O14.2 Sc2'
_chemical_formula_weight         723.19
_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             2022-10-24
_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                   7.3445(19)
_cell_length_b                   23.984(3)
_cell_length_c                   13.1770(13)
_cell_measurement_pressure       710000
_cell_measurement_reflns_used    1543
_cell_measurement_temperature    298
_cell_measurement_theta_max      15.2480
_cell_measurement_theta_min      2.0940
_cell_volume                     2321.1(7)
_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         710000
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.799
_diffrn_measured_fraction_theta_max 0.799
_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    -17.20 -10.00   0.20    0.40 -90.00 -11.00   0.00    --    36
  2  \w   -128.40-120.60   0.20    0.40    --  -11.00  70.00 -24.23   39
  3  \w   -129.60-120.40   0.20    0.40    --  -11.00  70.00 155.77   46
  4  \w   -107.80 -95.80   0.20    0.40    --   12.00  70.00 155.77   60
  5  \w   -105.40 -96.00   0.20    0.40    --   12.00  70.00 -24.23   47
  6  \w    -61.80 -50.60   0.20    0.40    --   12.00 -70.00  24.23   56
  7  \w    -58.40 -48.80   0.20    0.40    --   12.00 -70.00-155.77   48
  8  \w    -83.80 -72.00   0.20    0.40    --  -11.00 -70.00-155.77   59
  9  \w    -85.00 -72.80   0.20    0.40    --  -11.00 -70.00  24.23   61
;
_diffrn_measurement_device       '4-circle diffractometer'
_diffrn_measurement_device_type  'Diamond Light Source I19 EH2'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0556990000
_diffrn_orient_matrix_UB_12      0.0089095000
_diffrn_orient_matrix_UB_13      0.0113244000
_diffrn_orient_matrix_UB_21      0.0339820000
_diffrn_orient_matrix_UB_22      0.0169448000
_diffrn_orient_matrix_UB_23      0.0071678000
_diffrn_orient_matrix_UB_31      -0.0112799000
_diffrn_orient_matrix_UB_32      0.0064879000
_diffrn_orient_matrix_UB_33      -0.0344157000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_reflns_av_R_equivalents  0.1334
_diffrn_reflns_av_unetI/netI     0.0659
_diffrn_reflns_Laue_measured_fraction_full 0.799
_diffrn_reflns_Laue_measured_fraction_max 0.799
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            482
_diffrn_reflns_point_group_measured_fraction_full 0.799
_diffrn_reflns_point_group_measured_fraction_max 0.799
_diffrn_reflns_theta_full        13.374
_diffrn_reflns_theta_max         13.374
_diffrn_reflns_theta_min         2.411
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.34
_exptl_absorpt_correction_T_max  0.4245
_exptl_absorpt_correction_T_min  0.3115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
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    1.035
_exptl_crystal_description       block
_exptl_crystal_F_000             744.68
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.061
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         482
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      2.010
_refine_ls_R_factor_all          0.1523
_refine_ls_R_factor_gt           0.1371
_refine_ls_shift/su_max          0.862
_refine_ls_shift/su_mean         0.081
_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          0.4127
_refine_ls_wR_factor_ref         0.4424
_reflns_Friedel_coverage         0.000
_reflns_number_gt                395
_reflns_number_total             482
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00904a2.cif
_cod_data_source_block           710MPa
_cod_depositor_comments
'Adding full bibliography for 1569390--1569403.cif.'
_cod_original_sg_symbol_Hall     '-C 2b 2'
_cod_original_sg_symbol_H-M      'C m m e'
_cod_original_formula_sum        'Sc2 C35.1 H35.5 O14.2'
_cod_database_code               1569390
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.978
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H7A,H7B,H7C} of C7, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups, {H8A,H8B,H8C} of C8, All O(H) groups
2. Restrained distances
 O2-H2
 0.875 with sigma of 0.001
 O2-C7
 1.4 with sigma of 0.02
 C7-O2
 1.4 with sigma of 0.01
 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-C8
 1.35 with sigma of 0.01
 O3-C9
 1.4 with sigma of 0.01
 O3-H3A
 0.875 with sigma of 0.001
 H3A-C9
 1.806 with sigma of 0.001
 C9-H3A
 1.806 with sigma of 0.01
 O5-H5B
 0.875 with sigma of 0.001
 H5B-H5A
 1.35 with sigma of 0.001
 O5-H5A
 0.875 with sigma of 0.001
3. Restrained planarity
 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
Uanis(C2) = Uanis(C5) = Uanis(C3) = Uanis(C4)
Uanis(C6) = Uanis(O1) = Uanis(C1)
Uiso(O4) = Uiso(C8)
Uiso(O3) = Uiso(C9)
Uanis(O2) = Uanis(C7)
Uanis(C2) = Uanis(C6) = Uanis(C1) = Uanis(C5) = Uanis(C4) = Uanis(C3) =
Uanis(O1)
5. Others
 Fixed Sof: H2(0.1675) O4(0.22) H4A(0.11) C8(0.22) H8A(0.22) H8B(0.22)
 H8C(0.22) C7(0.0825) H7A(0.0825) H7B(0.165) H7C(0.165) O3(0.075) C9(0.075)
 H9A(0.075) H9B(0.075) H9C(0.075) H5A(0.3434) H5B(0.1717)
6.a Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
6.d Idealised tetrahedral OH refined as rotating group:
 O4(H4A)
;
_shelx_res_checksum              78782
_olex2_exptl_crystal_mounting_method
;
The crystal is loaded in a miniature Merrill-Bassett 
diamond anvil cell in a hydrostatic medium of MeOH
;
_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 34.783
_oxdiff_exptl_absorpt_empirical_full_min 0.339