Ag<sup>1+</sup> incorporation <i>via</i> a Zr<sup>4+</sup>-anchored metalloligand: fine-tuning catalytic Ag sites in Zr/Ag bimetallic clusters for enhanced eCO<sub>2</sub>RR-to-CO activity.
Li, Liang-Jun; Mu, Wen-Lei; Tian, Yi-Qi; Yu, Wei-Dong; Li, Lan-Yan; Yan, Jun; Liu, Chao; Chemical science 15 (2024) 7643–7650; doi:10.1039/d3sc07005k

data_1571294
_publ_section_title
;
 Ag<sup>1+</sup> incorporation <i>via</i> a Zr<sup>4+</sup>-anchored
 metalloligand: fine-tuning catalytic Ag sites in Zr/Ag bimetallic
 clusters for enhanced eCO<sub>2</sub>RR-to-CO activity.
;
_journal_issue                   20
_journal_name_full               'Chemical science'
_journal_page_first              7643
_journal_page_last               7650
_journal_paper_doi               10.1039/d3sc07005k
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety
'C181 H191 Ag7 O25 S16 Zr2, C6 H16 N, C6 H15 N, 2(C2 H3 N), 2[C6H16N], 7[CH3CN]'
_chemical_formula_sum            'C197 H228 Ag7 N4 O25 S16 Zr2'
_chemical_formula_weight         4502.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-25 deposited with the CCDC.	2024-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.6186(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.50529(11)
_cell_length_b                   36.9188(2)
_cell_length_c                   32.66914(16)
_cell_measurement_reflns_used    83034
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.7220
_cell_measurement_theta_min      1.8380
_cell_volume                     23259.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_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      150
_diffrn_detector                 'Image Plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.933
_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    -79.00   1.00   0.50    0.40    --  -47.45 105.00-149.00  160
  2  \w    -39.00 -14.00   0.50    1.62    --  -86.25  37.00-180.00   50
  3  \w    -42.00 -13.00   0.50    1.62    --  -86.25  37.00-120.00   58
  4  \w    -20.00  27.00   0.50    0.40    --  -47.45  19.00 -30.00   94
  5  \w    -41.00 -13.00   0.50    1.62    --  -86.25  37.00 -30.00   56
  6  \w    -49.00 -13.00   0.50    1.62    --  -86.25  77.00 -30.00   72
  7  \w    -50.00 -15.00   0.50    1.62    --  -86.25  57.00  60.00   70
  8  \w    -41.00 -14.00   0.50    1.62    --  -86.25  37.00  60.00   54
  9  \w    -26.00  26.00   0.50    0.40    --  -47.45  19.00 120.00  104
 10  \w    -42.00 -16.00   0.50    1.62    --  -86.25  37.00 150.00   52
 11  \w   -100.00 -60.00   0.50    1.62    --  -86.25  77.00 -30.00   80
 12  \w    -81.00 -15.00   0.50    1.62    --  -86.25 105.00-149.00  132
 13  \w    -24.00  26.00   0.50    0.40    --   47.45 -19.00-120.00  100
 14  \w     31.00  57.00   0.50    1.62    --   98.15 -57.00 -60.00   52
 15  \w     27.00  66.00   0.50    1.62    --   98.15 -57.00 -90.00   78
 16  \w     37.00  62.00   0.50    1.62    --   98.15 -57.00 -30.00   50
 17  \w     34.00  66.00   0.50    1.62    --   98.15 -57.00   0.00   64
 18  \w     25.00  50.00   0.50    0.40    --   47.45-105.00 110.00   50
 19  \w     44.00 109.00   0.50    1.62    --   98.15-105.00 110.00  130
 20  \w     29.00  56.00   0.50    1.62    --   98.15 -57.00 150.00   54
 21  \w     29.00  66.00   0.50    1.62    --   98.15 -57.00 120.00   74
 22  \w    102.00 143.00   0.50    1.62    --   98.15 105.00-149.00   82
 23  \w     35.00  62.00   0.50    1.62    --   98.15 -57.00-180.00   54
 24  \w     60.00 104.00   0.50    1.62    --   98.15-125.00-150.00   88
 25  \w   -109.00 -70.00   0.50    0.40    --  -47.45-125.00-180.00   78
 26  \w   -120.00 -76.00   0.50    0.40    --  -47.45-125.00 -90.00   88
 27  \w   -120.00 -95.00   0.50    1.62    --  -86.25-105.00 110.00   50
 28  \w   -112.00 -63.00   0.50    1.62    --  -86.25 -77.00 120.00   98
 29  \w   -155.00-139.50   0.50    1.62    --  -86.25 -77.00 120.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0076731000
_diffrn_orient_matrix_UB_12      -0.0379649000
_diffrn_orient_matrix_UB_13      -0.0197090000
_diffrn_orient_matrix_UB_21      0.0368472000
_diffrn_orient_matrix_UB_22      0.0132944000
_diffrn_orient_matrix_UB_23      -0.0357689000
_diffrn_orient_matrix_UB_31      0.0704647000
_diffrn_orient_matrix_UB_32      -0.0110640000
_diffrn_orient_matrix_UB_33      0.0246509000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0891
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            174967
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.980
_diffrn_reflns_theta_min         1.817
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.114
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear greenish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       block
_exptl_crystal_F_000             9212
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.374
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2681
_refine_ls_number_reflns         43385
_refine_ls_number_restraints     939
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0973P)^2^+61.2701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1835
_refine_ls_wR_factor_ref         0.1947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                34839
_reflns_number_total             43385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc07005k2.cif
_cod_data_source_block           Zr2Ag7
_cod_depositor_comments
'Adding full bibliography for 1571291--1571294.cif.'
_cod_database_code               1571294
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHONZrSAg
_shelx_estimated_absorpt_t_max   0.224
_shelx_estimated_absorpt_t_min   0.125
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C98-C100
 2.2 with sigma of 0.01
 H01B-H04G
 2.2 with sigma of 0.01
 C58-C25
 1.5 with sigma of 0.01
 C053-C42 \\sim C053-C38
 with sigma of 0.02
 C053-C41 \\sim C053-C62
 with sigma of 0.02
 C053-C63 \\sim C053-C64
 with sigma of 0.02
 C04N-C59 \\sim C04N-C20
 with sigma of 0.02
 C04N-C21 \\sim C04N-C60
 with sigma of 0.02
 C04N-C61 \\sim C04N-C22
 with sigma of 0.02
 C28-C12 \\sim C28-C66
 with sigma of 0.02
 C28-C13 \\sim C28-C67
 with sigma of 0.02
 C28-C11 \\sim C28-C65
 with sigma of 0.02
 C04D-C68 \\sim C04D-C8
 with sigma of 0.02
 C04D-C69 \\sim C04D-C9
 with sigma of 0.02
 C04D-C70 \\sim C04D-C10
 with sigma of 0.02
 C03G-C73 \\sim C03G-C53
 with sigma of 0.02
 C03G-C71 \\sim C03G-C29
 with sigma of 0.02
 C03G-C72 \\sim C03G-C32
 with sigma of 0.02
 C04M-C74 \\sim C04M-C36
 with sigma of 0.02
 C04M-C76 \\sim C04M-C27
 with sigma of 0.02
 C04M-C75 \\sim C04M-C26
 with sigma of 0.02
 C05B-C78 \\sim C05B-C34
 with sigma of 0.02
 C05B-C80 \\sim C05B-C52
 with sigma of 0.02
 C05B-C81 \\sim C05B-C48
 with sigma of 0.02
 C86-C15 \\sim C86-C85
 with sigma of 0.02
 C86-C16 \\sim C86-C84
 with sigma of 0.02
 C86-C83 \\sim C86-C14
 with sigma of 0.02
 C90-C87 \\sim C90-C91
 with sigma of 0.02
 C90-C82 \\sim C90-C89
 with sigma of 0.02
 C90-C54 \\sim C90-C88
 with sigma of 0.02
 C97-C92 \\sim C97-C93
 with sigma of 0.02
 C97-C94 \\sim C97-C95
 with sigma of 0.02
 C97-C39 \\sim C97-C96
 with sigma of 0.02
 C101-C46 \\sim C101-C100
 with sigma of 0.02
 C101-C55 \\sim C101-C98
 with sigma of 0.02
 C101-C37 \\sim C101-C99
 with sigma of 0.02
 C7-C102 \\sim C7-C56
 with sigma of 0.02
 C7-C3 \\sim C7-C4
 with sigma of 0.02
 C7-C5 \\sim C7-C6
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C50 \\sim C24 \\sim C57 \\sim C23 \\sim C58 \\sim C25 \\sim N7: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C22 \\sim C59 \\sim C20 \\sim C21 \\sim C60 \\sim C61: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C41 \\sim C62 \\sim C42 \\sim C63 \\sim C38 \\sim C64: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C11 \\sim C65 \\sim C12 \\sim C66 \\sim C13 \\sim C67: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C68 \\sim C8 \\sim C69 \\sim C9 \\sim C70 \\sim C10: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C53 \\sim C71 \\sim C29 \\sim C72 \\sim C32 \\sim C73: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C76 \\sim C27 \\sim C74 \\sim C36 \\sim C75 \\sim C26: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C48 \\sim C78 \\sim C34 \\sim C80 \\sim C52 \\sim C81: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C83 \\sim C14 \\sim C16 \\sim C84 \\sim C15 \\sim C85 \\sim C86: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C88 \\sim C87 \\sim C82 \\sim C89 \\sim C54 \\sim C90 \\sim C91: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C92 \\sim C93 \\sim C94 \\sim C95 \\sim C39 \\sim C96 \\sim C97: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C55 \\sim C98 \\sim C37 \\sim C99 \\sim C46 \\sim C100 \\sim C101: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C102 \\sim C56 \\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
Uanis(C13) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq,
Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C68)
\\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C87) \\sim Ueq,
Uanis(C54) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C63) \\sim Ueq,
Uanis(C41) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C61)
\\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C46) \\sim Ueq,
Uanis(C75) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C78)
\\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C5) \\sim Ueq,
Uanis(C39) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C51)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C83) \\sim Ueq,
Uanis(C25) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C74) \\sim Ueq,
Uanis(C47) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C42, C41, C63
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C38, C62, C64
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C59, C21, C61
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20, C60, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12, C13, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C66, C67, C65
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C68, C69, C70
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8, C9, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C73, C71, C72
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C53, C29, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C74, C76, C75
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C36, C27, C26
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C78, C80, C81
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34, C52, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15, C16, C83
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C85, C84, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C87, C82, C54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C91, C89, C88
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C92, C94, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C93, C95, C96
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C46, C55, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C100, C98, C99
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C102, C3, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C56, C4, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=1-FVAR(1)
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=
 Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=FVAR(1)
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=1-FVAR(2)
 Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=
 Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=FVAR(2)
 Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=
 Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=1-FVAR(3)
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(3)
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10D)=Sof(H10E)=Sof(H10F)=
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=1-FVAR(4)
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=
 Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=FVAR(4)
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=1-FVAR(5)
 Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=
 Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=FVAR(5)
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=1-FVAR(6)
 Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H76C)=
 Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=FVAR(6)
 Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=1-FVAR(7)
 Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H78C)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=
 Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=FVAR(7)
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(H85C)=
 Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(H84C)=1-FVAR(8)
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(H83C)=FVAR(8)
 Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(H88C)=Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(H91C)=
 Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(H89C)=1-FVAR(9)
 Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(H87C)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=
 Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=FVAR(9)
 Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(H95C)=Sof(C96)=Sof(H96A)=Sof(H96B)=Sof(H96C)=
 Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(H93C)=1-FVAR(10)
 Sof(C92)=Sof(H92A)=Sof(H92B)=Sof(H92C)=Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(H94C)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(10)
 Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(H98C)=Sof(C99)=Sof(H99A)=Sof(H99B)=Sof(H99C)=
 Sof(C100)=Sof(H10G)=Sof(H10H)=Sof(H10I)=1-FVAR(11)
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(11)
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=1-FVAR(12)
 Sof(C102)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(12)
6.a Riding coordinates:
 C63(H63A,H63B,H63C), C13(H13A,H13B,H13C), C11(H11A,H11B,H11C), C33(H33A,H33B,
 H33C), C23(H23A,H23B,H23C), C64(H64A,H64B,H64C), C62(H62A,H62B,H62C), C38(H38A,
 H38B,H38C)
6.b Ternary CH refined with riding coordinates:
 N02Z(H02Z)
6.c Secondary CH2 refined with riding coordinates:
 C04P(H04C,H04D), C04U(H04E,H04I), C05A(H05J,H05K), C24(H24A,H24B), C57(H57A,
 H57B), C58(H58A,H58B)
6.d Aromatic/amide H refined with riding coordinates:
 C01K(H01K), C01M(H01M), C01Q(H01Q), C01R(H01R), C01S(H01S), C01W(H01W),
 C021(H021), C023(H023), C02G(H02G), C02H(H02H), C02J(H02J), C02M(H02M),
 C02O(H02O), C02P(H02P), C02T(H02T), C02U(H02U), C02W(H02W), C02X(H02X),
 C032(H032), C036(H036), C03A(H03A), C03D(H03D), C03I(H03I), C03T(H03T),
 C03U(H03U), C03Y(H03Y), C03Z(H03Z), C043(H043), C044(H044), C048(H048),
 C04A(H04A), C04B(H04B), C04F(H04F), C04G(H04G), C04H(H04H), C04J(H04J),
 C04K(H04K), C04S(H04S), C04V(H04V), C04W(H04W), C04X(H04X), C04Z(H04Z),
 C050(H050), C054(H054)
6.e Tetrahedral OH refined with riding coordinates:
 O019(H019), O01B(H01B)
6.f Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C55(H55A,H55B,H55C), C058(H05G,H05H,H05I), C059(H05A,
 H05B,H05C), C05D(H05L,H05M,H05N), C05E(H05D,H05E,H05F), C50(H50A,H50B,H50C),
 C51(H51A,H51B,H51C), C92(H92A,H92B,H92C), C37(H37A,H37B,H37C), C102(H10A,H10B,
 H10C), C3(H3A,H3B,H3C), C15(H15A,H15B,H15C), C05N(H05O,H05P,H05Q), C94(H94A,
 H94B,H94C), C5(H5A,H5B,H5C), C59(H59A,H59B,H59C), C74(H74A,H74B,H74C),
 C49(H49A,H49B,H49C), C68(H68A,H68B,H68C), C87(H87A,H87B,H87C), C40(H40A,H40B,
 H40C), C16(H16A,H16B,H16C), C42(H42A,H42B,H42C), C30(H30A,H30B,H30C),
 C061(H06A,H06B,H06C), C69(H69A,H69B,H69C), C73(H73A,H73B,H73C), C19(H19A,H19B,
 H19C), C70(H70A,H70B,H70C), C44(H44A,H44B,H44C), C71(H71A,H71B,H71C), C21(H21A,
 H21B,H21C), C82(H82A,H82B,H82C), C72(H72A,H72B,H72C), C39(H39A,H39B,H39C),
 C17(H17A,H17B,H17C), C76(H76A,H76B,H76C), C83(H83A,H83B,H83C), C43(H43A,H43B,
 H43C), C18(H18A,H18B,H18C), C78(H78A,H78B,H78C), C12(H12A,H12B,H12C), C61(H61A,
 H61B,H61C), C80(H80A,H80B,H80C), C75(H75A,H75B,H75C), C81(H81A,H81B,H81C),
 C45(H45A,H45B,H45C), C41(H41A,H41B,H41C), C54(H54A,H54B,H54C), C25(H25A,H25B,
 H25C), C22(H22A,H22B,H22C), C20(H20A,H20B,H20C), C60(H60A,H60B,H60C), C67(H67A,
 H67B,H67C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C9(H9A,H9B,H9C),
 C10(H10D,H10E,H10F), C8(H8A,H8B,H8C), C53(H53A,H53B,H53C), C29(H29A,H29B,H29C),
  C32(H32A,H32B,H32C), C27(H27A,H27B,H27C), C36(H36A,H36B,H36C), C26(H26A,H26B,
 H26C), C52(H52A,H52B,H52C), C48(H48A,H48B,H48C), C34(H34A,H34B,H34C), C14(H14A,
 H14B,H14C), C85(H85A,H85B,H85C), C84(H84A,H84B,H84C), C88(H88A,H88B,H88C),
 C91(H91A,H91B,H91C), C89(H89A,H89B,H89C), C95(H95A,H95B,H95C), C96(H96A,H96B,
 H96C), C93(H93A,H93B,H93C), C98(H98A,H98B,H98C), C99(H99A,H99B,H99C),
 C100(H10G,H10H,H10I), C56(H56A,H56B,H56C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C)
6.g Idealised tetrahedral OH refined as rotating group:
 O04O(H04O)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              8108
_shelx_fab_checksum              10273
_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 2.173
_oxdiff_exptl_absorpt_empirical_full_min 0.469