<sup>109</sup>Ag NMR chemical shift as a descriptor for Brønsted acidity from molecules to materials.
Hansen, Colin; Docherty, Scott R.; Cao, Weicheng; Yakimov, Alexander V.; Copéret, Christophe; Chemical science 15 (2024) 3028–3032; doi:10.1039/d3sc04067d

data_1570798
_publ_section_title
;
 <sup>109</sup>Ag NMR chemical shift as a descriptor for Br&#xf8;nsted
 acidity from molecules to materials.
;
_journal_issue                   8
_journal_name_full               'Chemical science'
_journal_page_first              3028
_journal_page_last               3032
_journal_paper_doi               10.1039/d3sc04067d
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C33 H53 Ag N2 O4 Si'
_chemical_formula_sum            'C33 H53 Ag N2 O4 Si'
_chemical_formula_weight         677.73
_chemical_name_common            (SIMes)AgOTBOS
_chemical_name_systematic        (SIMes)Ag(OSi(OtBu)3)
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Light-sensitive,Photo-sensitive
_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   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2fs03c
_audit_creation_date             2023-04-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-19 deposited with the CCDC.	2024-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.487(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1099(2)
_cell_length_b                   16.5691(2)
_cell_length_c                   19.2966(3)
_cell_measurement_reflns_used    57122
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.9880
_cell_measurement_theta_min      2.2960
_cell_volume                     3439.20(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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   -114.00 -66.00   0.50    0.18    --  -49.52-140.00 -49.00   96
  2  \w   -120.00 -95.00   0.50    0.18    --  -49.52-131.00 124.00   50
  3  \w    -83.00 -58.00   0.50    0.18    --  -49.52 140.00  10.00   50
  4  \w    -73.00 -47.00   0.50    0.18    --  -49.52 131.00-163.00   52
  5  \w     58.00  98.00   0.50    0.18    --   49.52-131.00 124.00   80
  6  \w     45.00 100.00   0.50    0.18    --   49.52-140.00 -49.00  110
  7  \w   -140.00-115.00   0.50    0.73    --  -90.00-131.00 124.00   50
  8  \w   -134.00-109.00   0.50    0.73    --  -90.00-140.00 -49.00   50
  9  \w    -79.00 -54.00   0.50    0.73    --  -90.00 131.00-163.00   50
 10  \w    105.00 130.00   0.50    0.73    --  111.50 140.00  10.00   50
 11  \w    129.00 155.00   0.50    0.73    --  111.50 131.00-163.00   52
 12  \w     77.00 116.00   0.50    0.73    --  111.50-131.00 124.00   78
 13  \w     95.00 123.00   0.50    0.73    --  111.50-140.00 -49.00   56
 14  \w    -25.00  24.00   0.50    0.18    --  -49.52  19.00  90.00   98
 15  \w   -121.00 -77.00   0.50    0.18    --  -49.52-125.00-180.00   88
 16  \w    -21.00  20.00   0.50    0.18    --  -49.52  19.00 120.00   82
 17  \w    -24.00   1.00   0.50    0.18    --  -49.52  19.00  60.00   50
 18  \w   -121.00 -73.00   0.50    0.18    --  -49.52-125.00  60.00   96
 19  \w    -27.00   8.00   0.50    0.18    --  -49.52  19.00-180.00   70
 20  \w     53.00 108.00   0.50    0.18    --   49.52  77.00 -90.00  110
 21  \w    -22.00  26.00   0.50    0.18    --   49.52 -19.00 -90.00   96
 22  \w     -5.00  23.00   0.50    0.18    --   49.52 -19.00  90.00   56
 23  \w    130.00 176.00   0.50    0.73    --  111.50  30.00-150.00   92
 24  \w     91.00 132.00   0.50    0.73    --  111.50 -88.00  34.20   82
 25  \w     41.00  77.00   0.50    0.73    --  111.50 -88.00  34.20   72
 26  \w     69.00 104.00   0.50    0.73    --  111.50-125.00 -90.00   70
 27  \w     42.00  71.00   0.50    0.73    --  111.50 -61.00-150.00   58
 28  \w     41.00  70.00   0.50    0.73    --  111.50 -61.00-180.00   58
 29  \w     42.00  69.00   0.50    0.73    --  111.50 -61.00 150.00   54
 30  \w    104.00 130.00   0.50    0.73    --  111.50  15.00  60.00   52
 31  \w     44.00  70.00   0.50    0.73    --  111.50 -61.00  30.00   52
 32  \w     91.00 178.00   0.50    0.73    --  111.50  77.00  90.00  174
 33  \w     42.00 104.00   0.50    0.73    --  111.50 -95.00-180.00  124
 34  \w     43.00 105.00   0.50    0.73    --  111.50 -95.00   0.00  124
 35  \w    140.00 177.00   0.50    0.73    --  111.50 125.00-150.00   74
 36  \w     45.00  92.00   0.50    0.73    --  111.50 -77.00 120.00   94
 37  \w     50.00  77.00   0.50    0.73    --  111.50 -77.00  30.00   54
 38  \w     43.00 106.00   0.50    0.73    --  111.50 -99.00 -28.58  126
 39  \w    108.00 167.00   0.50    0.73    --  111.50  45.00 -60.00  118
 40  \w    142.00 169.00   0.50    0.73    --  111.50  61.00-120.00   54
 41  \w     97.00 122.00   0.50    0.73    --  111.50-138.00-171.65   50
 42  \w    105.00 133.00   0.50    0.73    --  111.50  30.00-120.00   56
 43  \w     96.00 133.00   0.50    0.73    --  111.50  77.00-120.00   74
 44  \w    113.00 178.00   0.50    0.73    --  111.50  45.00  60.00  130
 45  \w     61.00 111.00   0.50    0.73    --  111.50-125.00 -60.00  100
 46  \w     54.00  98.00   0.50    0.73    --  111.50 -77.00-120.00   88
 47  \w     97.00 135.00   0.50    0.73    --  111.50  61.00-180.00   76
 48  \w    104.00 132.00   0.50    0.73    --  111.50  30.00  60.00   56
 49  \w     64.00 109.00   0.50    0.73    --  111.50-125.00 -30.00   90
 50  \w     41.00  91.00   0.50    0.73    --  111.50 -77.00-180.00  100
 51  \w     49.00  75.00   0.50    0.73    --  111.50 -95.00 -60.00   52
 52  \w     42.00  91.00   0.50    0.73    --  111.50 -77.00 150.00   98
 53  \w     41.00  66.00   0.50    0.73    --  111.50 -61.00  60.00   50
 54  \w     46.00  71.00   0.50    0.73    --  111.50 -77.00-150.00   50
 55  \w     43.00  68.00   0.50    0.73    --  111.50 -77.00 -60.00   50
 56  \w     78.00 103.00   0.50    0.73    --  111.50 -77.00 -60.00   50
 57  \w     51.00  77.00   0.50    0.73    --  111.50 -77.00   0.00   52
 58  \w     83.00 108.00   0.50    0.73    --  111.50-125.00-120.00   50
 59  \w    105.00 145.00   0.50    0.73    --  111.50  15.00-180.00   80
 60  \w    138.00 166.00   0.50    0.73    --  111.50  15.00 -30.00   56
 61  \w    101.00 149.00   0.50    0.73    --  111.50 125.00  30.00   96
 62  \w    104.00 144.00   0.50    0.73    --  111.50  30.00   0.00   80
 63  \w     73.00 105.00   0.50    0.73    --  111.50 -95.00 -90.00   64
 64  \w     47.00  73.00   0.50    0.73    --  111.50 -95.00  30.00   52
 65  \w    120.00 164.00   0.50    0.73    --  111.50  30.00-180.00   88
 66  \w    120.00 157.00   0.50    0.73    --  111.50  30.00 -90.00   74
 67  \w    122.00 170.00   0.50    0.73    --  111.50  30.00 150.00   96
 68  \w     89.00 125.00   0.50    0.73    --  111.50 -87.00 -82.90   72
 69  \w     97.00 133.00   0.50    0.73    --  111.50  61.00 -60.00   72
 70  \w     98.00 125.00   0.50    0.73    --  111.50 125.00  90.00   54
 71  \w    141.00 166.00   0.50    0.73    --  111.50 125.00  90.00   50
 72  \w    103.00 129.00   0.50    0.73    --  111.50 125.00 120.00   52
 73  \w    131.00 156.00   0.50    0.73    --  111.50 125.00 150.00   50
 74  \w    111.00 148.00   0.50    0.73    --  111.50  30.00 -60.00   74
 75  \w    142.00 177.00   0.50    0.73    --  111.50  77.00-120.00   70
 76  \w    144.00 173.00   0.50    0.73    --  111.50  77.00 -90.00   58
 77  \w    153.00 178.00   0.50    0.73    --  111.50  77.00 -30.00   50
 78  \w     63.00  88.00   0.50    0.73    --  111.50 -86.00  94.78   50
 79  \w    108.00 134.00   0.50    0.73    --  111.50 -86.00  94.78   52
 80  \w    104.00 135.00   0.50    0.73    --  111.50  30.00 120.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0334751000
_diffrn_orient_matrix_UB_12      0.0875498000
_diffrn_orient_matrix_UB_13      -0.0243165000
_diffrn_orient_matrix_UB_21      -0.1027143000
_diffrn_orient_matrix_UB_22      -0.0313039000
_diffrn_orient_matrix_UB_23      -0.0635193000
_diffrn_orient_matrix_UB_31      -0.0941128000
_diffrn_orient_matrix_UB_32      0.0030659000
_diffrn_orient_matrix_UB_33      0.0465081000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            71442
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.795
_diffrn_reflns_theta_min         3.565
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.319
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_preparation       'Prepared from SIMesAgCl and NaTBOS'
_exptl_crystal_recrystallization_method 'Crystallized from cold Toluene'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.00050(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         7488
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0476P)^2^+2.8877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7428
_reflns_number_total             7488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04067d2.cif
_cod_data_source_block           exp_1203_auto
_cod_depositor_comments
'Adding full bibliography for 1570794--1570800.cif.'
_cod_database_code               1570798
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ag N C H O Si'
_shelx_estimated_absorpt_t_max   0.416
_shelx_estimated_absorpt_t_min   0.416
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C3(H3a,H3b)
2.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C20(H20), C27(H27), C29(H29)
2.c Idealised Me refined as rotating group:
 C15(H15a,H15b,H15c), C7(H7a,H7b,H7c), C11(H11a,H11b,H11c), C23(H23a,H23b,
 H23c), C22(H22a,H22b,H22c), C24(H24a,H24b,H24c), C9(H9a,H9b,H9c), C13(H13a,
 H13b,H13c), C5(H5a,H5b,H5c), C10(H10a,H10b,H10c), C6(H6a,H6b,H6c), C14(H14a,
 H14b,H14c), C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C31(H31a,H31b,H31c)
;
_shelx_res_checksum              16576
_olex2_exptl_crystal_mounting_method 'XRD oil and Kapton'
_olex2_submission_original_sample_id CH122
_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 1.788
_oxdiff_exptl_absorpt_empirical_full_min 0.680