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_1569403
_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 H18 O10, 1.2(C3 H7 NO)'
_chemical_formula_sum            'H24 N1.2 O10.6 Sc2'
_chemical_formula_weight         713.67
_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                   7.3054(5)
_cell_length_b                   26.5207(17)
_cell_length_c                   11.7550(9)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      3.37
_cell_volume                     2277.5(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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_temperature      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31343
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.323
_diffrn_reflns_theta_min         1.536
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.342
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1290 before and 0.0709 after correction.
The Ratio of minimum to maximum transmission is 0.9071.
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    1.041
_exptl_crystal_description       block
_exptl_crystal_F_000             731
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.881
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         1562
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0904
_refine_ls_shift/su_max          1.854
_refine_ls_shift/su_mean         0.206
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1612P)^2^+14.5173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2662
_refine_ls_wR_factor_ref         0.2682
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1486
_reflns_number_total             1562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00904a2.cif
_cod_data_source_block           Ambient
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '__audit_creation_date' was replaced with
'_audit_creation_date'.

Automatic conversion script
Id: cif_correct_tags 8170 2020-07-09 18:12:32Z antanas 

 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 H24 N1.2 O10.6'
_cod_database_code               1569403
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.950
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, H7 of C7
 At 1.2 times of:
  H4 of C4, H3 of C3, H2 of C9
2. Restrained distances
 O2-H2
 0.875 with sigma of 0.001
 N1-C8 \\sim N1-C9
 with sigma of 0.02
3. Restrained planarity
 C7, O3, N1, C8, C9
 with sigma of 0.1
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(C6) = Uanis(C5) = Uanis(C3) = Uanis(C4) = Uanis(O1) = Uanis(C2) =
Uanis(C1)
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(0.075) H7(0.075) O3(0.075) N1(0.15) C8(0.15) H8A(0.15)
 H8B(0.15) H8C(0.15) C9(0.075) H9A(0.075) H9B(0.075) H9C(0.075)
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)
;
_shelx_res_checksum              38816
_olex2_submission_special_instructions 'No special instructions were received'