#------------------------------------------------------------------------------
#$Date: 2023-09-05 22:06:16 +0300 (Tue, 05 Sep 2023) $
#$Revision: 286031 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/93/1569396.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1569396
loop_
_publ_author_name
'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.'
_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 C34 H22.2 O10, 3.60(C H4 O), 1.90(H2 O)'
_chemical_formula_sum            'C37.6 H40.4 O15.5 Sc2'
_chemical_formula_weight         830.23
_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                   7.0143(12)
_cell_length_b                   21.941(7)
_cell_length_c                   13.6972(19)
_cell_measurement_pressure       4980000
_cell_measurement_reflns_used    955
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.6960
_cell_measurement_theta_min      1.6180
_cell_volume                     2108.0(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         4980000
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.824
_diffrn_measured_fraction_theta_max 0.824
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  35.00   0.20    0.40 -90.00 -11.00   0.00    --   350
  2  ω   -133.00 -85.00   0.20    0.40    --  -11.00  70.00 -24.23  240
  3  ω   -141.00 -85.00   0.20    0.40    --  -11.00  70.00 155.77  280
  4  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 155.77  155
  5  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 -24.23  155
  6  ω   -101.00 -41.00   0.20    0.40    --   12.00 -70.00  24.23  300
  7  ω   -102.00 -41.00   0.20    0.40    --   12.00 -70.00-155.77  305
  8  ω    -97.00 -64.00   0.20    0.40    --  -11.00 -70.00-155.77  165
  9  ω    -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       'ω and φ scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0265006000
_diffrn_orient_matrix_UB_12      -0.0180634000
_diffrn_orient_matrix_UB_13      0.0149443000
_diffrn_orient_matrix_UB_21      -0.0596838000
_diffrn_orient_matrix_UB_22      -0.0106974000
_diffrn_orient_matrix_UB_23      -0.0059546000
_diffrn_orient_matrix_UB_31      0.0237791000
_diffrn_orient_matrix_UB_32      -0.0066493000
_diffrn_orient_matrix_UB_33      -0.0316759000
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4589
_diffrn_reflns_av_R_equivalents  0.3538
_diffrn_reflns_av_unetI/netI     0.1084
_diffrn_reflns_Laue_measured_fraction_full 0.824
_diffrn_reflns_Laue_measured_fraction_max 0.824
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3488
_diffrn_reflns_point_group_measured_fraction_full 0.824
_diffrn_reflns_point_group_measured_fraction_max 0.824
_diffrn_reflns_theta_full        11.671
_diffrn_reflns_theta_max         11.671
_diffrn_reflns_theta_min         1.626
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.39
_exptl_absorpt_correction_T_max  0.7436
_exptl_absorpt_correction_T_min  0.3897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1113 before and 0.0759 after correction.
The Ratio of minimum to maximum transmission is 0.5241.
The λ/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    1.308
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.216
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         309
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_gt           0.1109
_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/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3232
_refine_ls_wR_factor_ref         0.3328
_reflns_Friedel_coverage         0.000
_reflns_number_gt                221
_reflns_number_total             309
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc00904a2.cif
_cod_data_source_block           4980MPa
_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 C37.6 H40.4 O15.5'
_cod_database_code               1569396
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.983
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,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
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)
Uanis(O2) = Uanis(C7)
Uanis(C2) = Uanis(C6) = Uanis(C1) = Uanis(C5) = Uanis(C4) = Uanis(C3) =
Uanis(O1)
5. Others
 Fixed Sof: H2(0.005) C7(0.245) H7A(0.245) H7B(0.49) H7C(0.49)
6.a Me refined with riding coordinates:
 C7(H7A,H7B,H7C)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
;
_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
;
_platon_squeeze_void_probe_radius 1.20
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'-x, y+1/2, -z'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z'
'-x+1/2, y+1, -z'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z'
'x, -y-1/2, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z'
'x+1/2, -y, z'
'-x+1/2, y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sc1 Sc 0.250000 0.250000 0.500000 0.080(4) Uani 1 4 d S T P B .
O2 O 0.500000 0.250000 0.4245(7) 0.082(7) Uani 1 4 d DS T P . .
O1 O 0.3418(7) 0.3164(4) 0.5949(5) 0.122(5) Uani 1 1 d D . . . .
C2 C 0.500000 0.3716(4) 0.7167(6) 0.122(5) Uani 1 2 d DS T P . .
C6 C 0.500000 0.4840(3) 0.9652(7) 0.122(5) Uani 1 2 d DS T P . .
C1 C 0.500000 0.3315(4) 0.6281(6) 0.122(5) Uani 1 2 d DS T P B .
C5 C 0.500000 0.4455(3) 0.8802(6) 0.122(5) Uani 1 2 d DS T P . .
C3 C 0.6713(7) 0.3900(3) 0.7573(6) 0.122(5) Uani 1 1 d D . . . .
H3 H 0.785995 0.377498 0.729623 0.147 Uiso 1 1 calc R U . . .
C4 C 0.6715(7) 0.4272(3) 0.8397(5) 0.122(5) Uani 1 1 d D . . . .
H4 H 0.786160 0.439593 0.867382 0.147 Uiso 1 1 calc R U . . .
H2 H 0.500000 0.250000 0.3606(7) 0.147 Uiso 0.02 4 d DS U P A 1
C7 C 0.500000 0.250000 0.3209(9) 0.082(7) Uani 0.98 4 d DS T P B 2
H7A H 0.370963 0.250000 0.297554 0.099 Uiso 0.49 2 calc R U P B 2
H7B H 0.564519 0.285725 0.297554 0.099 Uiso 0.49 1 calc R U P B 2
H7C H 0.564518 0.214275 0.297554 0.099 Uiso 0.49 1 calc R U P B 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0007 0.0006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0001 0.0023 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sc Sc 0.1054 0.1588 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Sc1 Sc1 Sc1 180.0 2_655 2 ?
O2 Sc1 Sc1 30.5(2) . 2_655 ?
O2 Sc1 Sc1 149.5(2) . 2 ?
O2 Sc1 Sc1 30.5(2) 13_556 2 ?
O2 Sc1 Sc1 149.5(2) 13_556 2_655 ?
O2 Sc1 O2 180.0 . 13_556 ?
O2 Sc1 O1 87.1(2) 13_556 . ?
O2 Sc1 O1 92.9(2) . . ?
O2 Sc1 O1 87.1(2) 13_556 11_565 ?
O2 Sc1 O1 87.1(2) . 13_556 ?
O2 Sc1 O1 92.9(2) 13_556 13_556 ?
O2 Sc1 O1 92.9(2) 13_556 7_546 ?
O2 Sc1 O1 87.1(2) . 7_546 ?
O2 Sc1 O1 92.9(2) . 11_565 ?
O1 Sc1 Sc1 71.75(15) 11_565 2_655 ?
O1 Sc1 Sc1 71.75(15) . 2_655 ?
O1 Sc1 Sc1 108.25(15) 13_556 2_655 ?
O1 Sc1 Sc1 71.75(15) 7_546 2 ?
O1 Sc1 Sc1 71.75(15) 13_556 2 ?
O1 Sc1 Sc1 108.25(15) 11_565 2 ?
O1 Sc1 Sc1 108.25(15) . 2 ?
O1 Sc1 Sc1 108.25(15) 7_546 2_655 ?
O1 Sc1 O1 180.0(3) 11_565 7_546 ?
O1 Sc1 O1 90.3(5) 13_556 7_546 ?
O1 Sc1 O1 89.7(5) 13_556 11_565 ?
O1 Sc1 O1 90.3(5) 11_565 . ?
O1 Sc1 O1 180.0 13_556 . ?
O1 Sc1 O1 89.7(5) 7_546 . ?
Sc1 O2 Sc1 118.9(5) 2_655 . ?
Sc1 O2 H2 120.5(2) . . ?
Sc1 O2 H2 120.5(3) 2_655 . ?
C7 O2 Sc1 120.5(2) . . ?
C1 O1 Sc1 134.3(6) . . ?
C3 C2 C1 119.7(3) . . ?
C3 C2 C1 119.7(3) 12_655 . ?
C3 C2 C3 120.5(6) . 12_655 ?
C6 C6 C5 179.7(6) 4_567 . ?
O1 C1 O1 126.2(9) . 12_655 ?
O1 C1 C2 116.9(5) . . ?
O1 C1 C2 116.9(5) 12_655 . ?
C4 C5 C6 119.7(3) . . ?
C4 C5 C6 119.7(3) 12_655 . ?
C4 C5 C4 120.6(7) 12_655 . ?
C2 C3 H3 120.1 . . ?
C2 C3 C4 119.8(4) . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 119.6(5) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
O2 C7 H7A 109.5 . . ?
O2 C7 H7A 109.474(5) . 2_655 ?
O2 C7 H7B 109.474(5) . 2_655 ?
O2 C7 H7B 109.5 . . ?
O2 C7 H7B 109.474(5) . 12_655 ?
O2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sc1 Sc1 3.5071(6) 2_655 ?
Sc1 Sc1 3.5071(6) 2 ?
Sc1 O2 2.036(5) 13_556 ?
Sc1 O2 2.036(5) . ?
Sc1 O1 2.056(8) 7_546 ?
Sc1 O1 2.056(8) . ?
Sc1 O1 2.056(8) 13_556 ?
Sc1 O1 2.056(8) 11_565 ?
O2 H2 0.8750(11) . ?
O2 C7 1.419(9) . ?
O1 C1 1.244(5) . ?
C2 C1 1.498(8) . ?
C2 C3 1.384(5) 12_655 ?
C2 C3 1.384(5) . ?
C6 C6 1.18(2) 4_567 ?
C6 C5 1.438(8) . ?
C5 C4 1.385(5) 12_655 ?
C5 C4 1.385(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.393(7) . ?
C4 H4 0.9300 . ?
C7 H7A 0.9600 2_655 ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 12_655 ?
C7 H7B 0.9600 . ?
C7 H7B 0.9600 2_655 ?
C7 H7C 0.9600 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Sc1 O1 C1 O1 16.4(4) . . . 12_655 ?
Sc1 O1 C1 C2 -163.6(5) . . . . ?
C2 C3 C4 C5 -0.1(2) . . . . ?
C6 C5 C4 C3 -179.89(19) . . . . ?
C1 C2 C3 C4 -179.90(18) . . . . ?
C3 C2 C1 O1 0.00(13) 12_655 . . . ?
C3 C2 C1 O1 -179.98(8) 12_655 . . 12_655 ?
C3 C2 C1 O1 179.98(8) . . . . ?
C3 C2 C1 O1 0.00(13) . . . 12_655 ?
C3 C2 C3 C4 0.1(2) 12_655 . . . ?
C4 C5 C4 C3 0.2(3) 12_655 . . . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.044 0.250 0.000 229 91 ' '
2 -0.044 0.750 0.000 229 91 ' '
3 -0.054 0.500 0.500 216 77 ' '
4 -0.054 1.000 0.500 216 77 ' '
