Atomic-level engineering of single Ag1+ site distribution on titanium–oxo cluster surfaces to boost CO2 electroreduction
Meng, Ru-Xin; Zhao, Lan-Cheng; Luo, Li-Pan; Tian, Yi-Qi; Shao, Yong-Liang; Tang, Qing; Wang, Likai; Yan, Jun; Liu, Chao; Chemical Science 16 (2025) 6845–6852; doi:10.1039/D4SC07186G

data_1573747
_publ_section_title
;
 Atomic-level engineering of single Ag1+ site distribution on
 titanium--oxo cluster surfaces to boost CO2 electroreduction
;
_journal_issue                   16
_journal_name_full               'Chemical Science'
_journal_page_first              6845
_journal_page_last               6852
_journal_paper_doi               10.1039/D4SC07186G
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C200 H221.83 Na O36 S20 Ti8'
_chemical_formula_sum            'C200 H221.72 Na O36 S20 Ti8'
_chemical_formula_weight         4248.87
_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     dual
_audit_creation_date             2024-04-19
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-19 deposited with the CCDC.	2025-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.7590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.1669(3)
_cell_length_b                   21.7916(2)
_cell_length_c                   35.9210(6)
_cell_measurement_reflns_used    29685
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      75.1710
_cell_measurement_theta_min      2.4460
_cell_volume                     25950.0(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.951
_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   -122.00 -42.00   0.50    8.00    --  -45.27 -30.00 -14.00  160
  2  \w     66.00  96.00   0.50    8.00    --   45.27  30.00 146.00   60
  3  \w    -21.00   5.00   0.50    8.00    --   45.27 -30.00 -14.00   52
  4  \w     37.00  64.00   0.50    8.00    --   45.27  30.00 146.00   54
  5  \w   -176.00 -81.00   0.50   20.00    -- -100.00 -30.00 -14.00  190
  6  \w     90.00 116.00   0.50   20.00    --  109.64  30.00 146.00   52
  7  \w    -94.00 -23.00   0.50    8.00    --  -45.27 125.00-120.00  142
  8  \w    -38.00  27.00   0.50    8.00    --  -45.27  30.00 146.00  130
  9  \w    -27.00  23.00   0.50    8.00    --   45.27 -19.00-180.00  100
 10  \w    -12.00  24.00   0.50    8.00    --   45.27 -19.00-120.00   72
 11  \w    -53.00 -26.00   0.50   20.00    -- -100.00  45.00 -90.00   54
 12  \w    -54.00 -29.00   0.50   20.00    -- -100.00  45.00 -30.00   50
 13  \w    -52.00 -25.00   0.50   20.00    -- -100.00  45.00-120.00   54
 14  \w    -53.00 -27.00   0.50   20.00    -- -100.00  45.00 150.00   52
 15  \w    -54.00 -26.00   0.50   20.00    -- -100.00  45.00-150.00   56
 16  \w    -74.00 -34.00   0.50   20.00    -- -100.00  61.00 120.00   80
 17  \w    -51.00 -26.00   0.50   20.00    -- -100.00  45.00  30.00   50
 18  \w    -53.00 -27.00   0.50   20.00    -- -100.00  45.00 -60.00   52
 19  \w    -67.00 -28.00   0.50   20.00    -- -100.00  61.00 -30.00   78
 20  \w    -53.00 -27.00   0.50   20.00    -- -100.00  45.00  90.00   52
 21  \w    -51.00 -26.00   0.50   20.00    -- -100.00  45.00-180.00   50
 22  \w    -65.00 -32.00   0.50   20.00    -- -100.00  61.00-150.00   66
 23  \w    -57.00 -30.00   0.50   20.00    -- -100.00  61.00  60.00   54
 24  \w     39.00  67.00   0.50   20.00    --  109.64 -61.00-120.00   56
 25  \w     76.00 102.00   0.50   20.00    --  109.64 -77.00-120.00   52
 26  \w     43.00  69.00   0.50   20.00    --  109.64 -77.00-120.00   52
 27  \w     44.00 103.00   0.50   20.00    --  109.64 -77.00  60.00  118
 28  \w     40.00  67.00   0.50   20.00    --  109.64 -61.00-180.00   54
 29  \w     41.00  66.00   0.50   20.00    --  109.64 -61.00 -90.00   50
 30  \w     43.00  68.00   0.50   20.00    --  109.64 -61.00  90.00   50
 31  \w     40.00 102.00   0.50   20.00    --  109.64-125.00 -90.00  124
 32  \w     41.00  68.00   0.50   20.00    --  109.64 -61.00  60.00   54
 33  \w     72.00 105.00   0.50   20.00    --  109.64-125.00-120.00   66
 34  \w     39.00 103.00   0.50   20.00    --  109.64 -77.00   0.00  128
 35  \w     42.00  69.00   0.50   20.00    --  109.64-125.00-120.00   54
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0109058000
_diffrn_orient_matrix_UB_12      0.0112681000
_diffrn_orient_matrix_UB_13      -0.0414213000
_diffrn_orient_matrix_UB_21      0.0426944000
_diffrn_orient_matrix_UB_22      0.0254656000
_diffrn_orient_matrix_UB_23      -0.0058845000
_diffrn_orient_matrix_UB_31      0.0147868000
_diffrn_orient_matrix_UB_32      -0.0649775000
_diffrn_orient_matrix_UB_33      -0.0094918000
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0860
_diffrn_reflns_av_unetI/netI     0.0712
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            198731
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.589
_diffrn_reflns_theta_min         2.372
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    3.959
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82031
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_description       block
_exptl_crystal_F_000             8867
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.896
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2764
_refine_ls_number_reflns         51889
_refine_ls_number_restraints     958
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1465
_refine_ls_R_factor_gt           0.0980
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1862P)^2^+7.3358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2910
_refine_ls_wR_factor_ref         0.3272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27120
_reflns_number_total             51889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07186g2.cif
_cod_data_source_block           Ti8L5
_cod_depositor_comments
'Adding full bibliography for 1573744--1573747.cif.'
_cod_database_code               1573747
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.383
_shelx_estimated_absorpt_t_min   0.242
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H) groups, All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C27-C26
 1.5 with sigma of 0.01
 C71-C67
 2.2 with sigma of 0.01
 C90-C88
 2.2 with sigma of 0.01
 C69-C67
 2.2 with sigma of 0.01
 C84-C82
 2.4 with sigma of 0.01
 C72-C66
 1.5 with sigma of 0.01
 C72-C67
 1.5 with sigma of 0.01
 C27-C13
 1.5 with sigma of 0.01
 C46-C56
 2.2 with sigma of 0.01
 C20-C76
 2.2 with sigma of 0.01
 C32-C29
 2.2 with sigma of 0.01
 C24-C87
 2.2 with sigma of 0.01
 C61-C18
 2.2 with sigma of 0.01
 C12-C24 \\sim C12-C61
 with sigma of 0.02
 C12-C87 \\sim C12-C64
 with sigma of 0.02
 C12-C62 \\sim C12-C18
 with sigma of 0.02
 C27-C22 \\sim C27-C21
 with sigma of 0.02
 C27-C13 \\sim C27-C26
 with sigma of 0.02
 C27-C23 \\sim C27-C25
 with sigma of 0.02
 C33-C10 \\sim C33-C29
 with sigma of 0.02
 C33-C28 \\sim C33-C30
 with sigma of 0.02
 C33-C31 \\sim C33-C32
 with sigma of 0.02
 C40-C38 \\sim C40-C39
 with sigma of 0.02
 C40-C37 \\sim C40-C34
 with sigma of 0.02
 C40-C35 \\sim C40-C36
 with sigma of 0.02
 C42-C48 \\sim C46-C48
 with sigma of 0.02
 C48-C43 \\sim C48-C56
 with sigma of 0.02
 C48-C41 \\sim C48-C47
 with sigma of 0.02
 C8-C17 \\sim C8-C15
 with sigma of 0.02
 C8-C14 \\sim C8-C76
 with sigma of 0.02
 C8-C19 \\sim C8-C20
 with sigma of 0.02
 C53-C50 \\sim C53-C54
 with sigma of 0.02
 C53-C51 \\sim C53-C52
 with sigma of 0.02
 C53-C11 \\sim C53-C49
 with sigma of 0.02
 C9-C60 \\sim C9-C63
 with sigma of 0.02
 C9-C55 \\sim C9-C57
 with sigma of 0.02
 C9-C58 \\sim C9-C59
 with sigma of 0.02
 C72-C70 \\sim C72-C71
 with sigma of 0.02
 C72-C68 \\sim C72-C69
 with sigma of 0.02
 C72-C66 \\sim C72-C67
 with sigma of 0.02
 C81-C79 \\sim C81-C80
 with sigma of 0.02
 C81-C74 \\sim C81-C78
 with sigma of 0.02
 C81-C75 \\sim C81-C73
 with sigma of 0.02
 C85-C16 \\sim C84-C16
 with sigma of 0.02
 C83-C16 \\sim C82-C16
 with sigma of 0.02
 C16-C45 \\sim C16-C44
 with sigma of 0.02
 C91-H91A \\sim C77-H91A
 with sigma of 0.02
 C91-H91B \\sim C77-H91B
 with sigma of 0.02
 C91-H91C \\sim C77-H91C
 with sigma of 0.02
 C91-C92 \\sim C77-C92
 with sigma of 0.02
 C92-C86 \\sim C92-C88
 with sigma of 0.02
 C92-C89 \\sim C92-C90
 with sigma of 0.02
 C86-H86A \\sim C88-H86A
 with sigma of 0.02
 C86-H86B \\sim C88-H86B
 with sigma of 0.02
 C86-H86C \\sim C88-H86C
 with sigma of 0.02
 C89-H89A \\sim C90-H89A
 with sigma of 0.02
 C89-H89B \\sim C90-H89B
 with sigma of 0.02
 C89-H89C \\sim C90-H89C
 with sigma of 0.02
 C7-C1 \\sim C7-C2
 with sigma of 0.02
 C7-C5 \\sim C7-C6
 with sigma of 0.02
 C7-C3 \\sim C7-C4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C77 \\sim C86 \\sim C88 \\sim C89 \\sim C90 \\sim C91 \\sim C92: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
C85 \\sim C44 \\sim C45 \\sim C82 \\sim C83 \\sim C84 \\sim C16: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C12 \\sim C24 \\sim C62 \\sim C87 \\sim C61 \\sim C64 \\sim C18: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C27 \\sim C13 \\sim C22 \\sim C23 \\sim C21 \\sim C25 \\sim C26: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C33 \\sim C10 \\sim C28 \\sim C31 \\sim C29 \\sim C30 \\sim C32: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C40 \\sim C35 \\sim C37 \\sim C38 \\sim C34 \\sim C36 \\sim C39: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C48 \\sim C41 \\sim C42 \\sim C43 \\sim C46 \\sim C47 \\sim C56: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C53 \\sim C11 \\sim C50 \\sim C51 \\sim C49 \\sim C52 \\sim C54: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C8 \\sim C14 \\sim C17 \\sim C19 \\sim C15 \\sim C76 \\sim C20: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C9 \\sim C55 \\sim C58 \\sim C60 \\sim C57 \\sim C59 \\sim C63: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C72 \\sim C66 \\sim C68 \\sim C70 \\sim C67 \\sim C69 \\sim C71: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C81 \\sim C75 \\sim C74 \\sim C79 \\sim C73 \\sim C78 \\sim C80: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C89 \\sim C91 \\sim C86 \\sim C92: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(C15) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C78)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=1-FVAR(1)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=
 Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(H87C)=FVAR(1)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=1-FVAR(2)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(2)
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=1-FVAR(3)
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(3)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=1-FVAR(4)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=FVAR(4)
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=1-FVAR(5)
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(5)
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H76C)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=1-FVAR(6)
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(6)
 Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=
 Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=1-FVAR(7)
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=
 Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=FVAR(7)
 Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=
 Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=1-FVAR(8)
 Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=FVAR(8)
 Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=
 Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=1-FVAR(9)
 Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=
 Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=FVAR(9)
 Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H78C)=
 Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=1-FVAR(10)
 Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=
 Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=FVAR(10)
 Sof(H91A)=Sof(H91B)=Sof(H91C)=Sof(H86A)=Sof(H86B)=Sof(H86C)=Sof(H89A)=
 Sof(H89B)=Sof(H89C)=FVAR(11)
 Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(H84C)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=1-FVAR(12)
 Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(H85C)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(H83C)=
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=FVAR(12)
 Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(H88C)=
 Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(H90C)=1-FVAR(13)
 Sof(C91)=Sof(C86)=Sof(C89)=FVAR(13)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C6)=
 Sof(H6A)=Sof(H6B)=Sof(H6C)=1-FVAR(14)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(14)
 Fixed Sof: Na1(0.5) Na01(0.5)
5.a Riding coordinates:
 C05A(H05A,H05B,H05C), C05G(H05E,H05F,H05G), C05I(H05H,H05I,H05J), C05Q(H05K,
 H05L,H05M), C05R(H05N,H05P,H05Q), C05T(H05R,H05S,H05T), C05W(H05U,H05V,H05W),
 C05X(H05X,H05Y,H), C05Y(H05Z,HA,HB), C05Z(H05,HC,HD), C06B(H06A,H06B,H06C),
 C85(H85A,H85B,H85C), C06D(H06D,H06E,H06F), C06E(H06G,H06H,H06I), C06G(H06J,
 H06K,H06L), C1(H1A,H1B,H1C), C83(H83A,H83B,H83C), C91(H91A,H91B,H91C), C5(H5A,
 H5B,H5C), C86(H86A,H86B,H86C), C062(H06M,H06N,H06O), C063(H06P,H06Q,H06R),
 C066(H06S,H06T,H06U), C067(H06V,H06W,H06X), C068(H06Y,HE,HF), C069(H06Z,HG),
 C070(H07A,H07B,H07C), C3(H3A,H3B,H3C), C89(H89A,H89B,H89C), C45(H45A,H45B,
 H45C), C75(H75A,H75B,H75C), C74(H74A,H74B,H74C), C79(H79A,H79B,H79C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C),
 C62(H62A,H62B,H62C), C87(H87A,H87B,H87C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C35(H35A,H35B,H35C), C37(H37A,
 H37B,H37C), C38(H38A,H38B,H38C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C55(H55A,H55B,
 H55C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C14(H14A,H14B,H14C), C17(H17A,
 H17B,H17C), C19(H19A,H19B,H19C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C),
 C70(H70A,H70B,H70C), C73(H73A,H73B,H73C), C78(H78A,H78B,H78C), C80(H80A,H80B,
 H80C), C15(H15A,H15B,H15C), C76(H76A,H76B,H76C), C61(H61A,H61B,H61C), C64(H64A,
 H64B,H64C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C),
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C39(H39A,
 H39B,H39C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C),
 C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C59(H59A,H59B,H59C), C63(H63A,H63B,H63C), C69(H69A,H69B,H69C), C71(H71A,
 H71B,H71C), C84(H84A,H84B,H84C), C82(H82A,H82B,H82C), C44(H44A,H44B,H44C),
 C88(H88A,H88B,H88C), C90(H90A,H90B,H90C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C),
 C6(H6A,H6B,H6C)
5.b Aromatic/amide H refined with riding coordinates:
 C02F(H02F), C02N(H02N), C02Q(H02Q), C02T(H02T), C03I(H03I), C03K(H03K),
 C03L(H03L), C03M(H03M), C03N(H03N), C03S(H03S), C03W(H03W), C04A(H04A),
 C04B(H04B), C04C(H04C), C04F(H04F), C04G(H04G), C04H(H04H), C04J(H04J),
 C04L(H04L), C04M(H04M), C04O(H04O), C04V(H04V), C04X(H04X), C04Y(H04Y),
 C04Z(H04Z), C05B(H05D), C05O(H05O), C035(H035), C036(H036), C037(H037),
 C038(H038), C041(H041), C044(H044), C045(H045), C047(H047), C049(H049),
 C050(H050), C053(H053), C056(H056), C65(H65)
5.c Idealised Me refined as rotating group:
 C67(H67A,H67B,H67C), C77(H77A,H77B,H77C)
5.d Idealised tetrahedral OH refined as rotating group:
 O01P(H01P), O01Q(H01Q)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              32883
_shelx_hkl_checksum              89282
_shelx_fab_checksum              31601
_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 2.218
_oxdiff_exptl_absorpt_empirical_full_min 0.456