<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_1570797
_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         'C22 H29 Ag N2'
_chemical_formula_sum            'C22 H29 Ag N2'
_chemical_formula_weight         429.34
_chemical_name_systematic        (SIMes)AgMe
_chemical_properties_physical
'Air-sensitive,Moisture-sensitive,Heat-sensitive,Light-sensitive,Photo-sensitive,decomposes quickly'
_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.cc2fs02b
_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                 112.995(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.3928(6)
_cell_length_b                   14.3855(4)
_cell_length_c                   17.9551(6)
_cell_measurement_reflns_used    43596
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.3410
_cell_measurement_theta_min      3.9950
_cell_volume                     4135.5(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.980
_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    -78.00  -6.00   0.50    0.49    --  -49.52 107.00 -74.00  144
  2  \w     21.00  57.00   0.50    0.49    --   49.52-107.00-172.00   72
  3  \w    -72.00 -47.00   0.50    1.96    --  -85.75 107.00 -74.00   50
  4  \w   -145.00-120.00   0.50    1.96    --  -85.75-107.00-172.00   50
  5  \w     59.00  95.00   0.50    1.96    --  107.25-107.00-172.00   72
  6  \w    114.00 152.00   0.50    1.96    --  107.25 107.00 -74.00   76
  7  \w    -75.00 -38.00   0.50    0.49    --  -49.52 -57.00 150.00   74
  8  \w    -69.00 -43.00   0.50    0.49    --  -49.52 -57.00-180.00   52
  9  \w   -116.00 -55.00   0.50    0.49    --  -49.52 -57.00 120.00  122
 10  \w   -105.00 -48.00   0.50    0.49    --  -49.52 -38.00-150.00  114
 11  \w   -115.00 -74.00   0.50    0.49    --  -49.52-125.00  90.00   82
 12  \w   -120.00 -80.00   0.50    0.49    --  -49.52 -57.00-180.00   80
 13  \w     90.00 117.00   0.50    0.49    --   49.52  77.00-150.00   54
 14  \w    -18.00   7.00   0.50    0.49    --   49.52 -19.00 -60.00   50
 15  \w     32.00  58.00   0.50    0.49    --   49.52  77.00-150.00   52
 16  \w    -50.00 -14.00   0.50    1.96    --  -85.75  45.00-150.00   72
 17  \w    -95.00 -68.00   0.50    1.96    --  -85.75 -69.00 175.03   54
 18  \w    -91.00 -65.00   0.50    1.96    --  -85.75 -77.00-150.00   52
 19  \w    -95.00 -69.00   0.50    1.96    --  -85.75 -66.00-151.30   52
 20  \w   -114.00 -73.00   0.50    1.96    --  -85.75 -59.00 141.37   82
 21  \w    -48.00 -21.00   0.50    1.96    --  -85.75  45.00  30.00   54
 22  \w    -50.00 -24.00   0.50    1.96    --  -85.75  45.00-120.00   52
 23  \w    -90.00 -65.00   0.50    1.96    --  -85.75 -77.00-179.00   50
 24  \w    -92.00 -67.00   0.50    1.96    --  -85.75 -71.00 151.52   50
 25  \w    -92.00 -67.00   0.50    1.96    --  -85.75 -71.00-175.03   50
 26  \w   -158.00 -69.00   0.50    1.96    --  -85.75 -71.00 132.81  178
 27  \w    -97.00 -71.00   0.50    1.96    --  -85.75 -77.00-120.00   52
 28  \w    -94.00 -69.00   0.50    1.96    --  -85.75 -67.00 139.81   50
 29  \w    -99.00 -72.00   0.50    1.96    --  -85.75 -58.00-171.56   54
 30  \w    -98.00 -71.00   0.50    1.96    --  -85.75 -61.00 150.00   54
 31  \w   -148.00-121.00   0.50    1.96    --  -85.75 -71.00 151.52   54
 32  \w    -96.00 -71.00   0.50    1.96    --  -85.75 -61.00-180.00   50
 33  \w   -154.00-114.00   0.50    1.96    --  -85.75 -77.00-120.00   80
 34  \w     96.00 169.00   0.50    1.96    --  107.25  77.00-150.00  146
 35  \w     95.00 152.00   0.50    1.96    --  107.25  61.00 120.00  114
 36  \w    125.00 150.00   0.50    1.96    --  107.25  77.00  90.00   50
 37  \w     88.00 113.00   0.50    1.96    --  107.25  77.00  90.00   50
 38  \w    125.00 178.00   0.50    1.96    --  107.25  15.00 -60.00  106
 39  \w     35.00  98.00   0.50    1.96    --  107.25 -77.00  90.00  126
 40  \w    107.00 134.00   0.50    1.96    --  107.25  45.00-150.00   54
 41  \w    149.00 175.00   0.50    1.96    --  107.25  45.00-180.00   52
 42  \w     38.00  71.00   0.50    1.96    --  107.25 -61.00  90.00   66
 43  \w     38.00  63.00   0.50    1.96    --  107.25 -61.00-120.00   50
 44  \w    102.00 142.00   0.50    1.96    --  107.25  45.00-180.00   80
 45  \w     38.00  64.00   0.50    1.96    --  107.25 -77.00-180.00   52
 46  \w     36.00  69.00   0.50    1.96    --  107.25 -61.00-180.00   66
 47  \w    133.00 178.00   0.50    1.96    --  107.25  77.00 120.00   90
 48  \w     87.00 113.00   0.50    1.96    --  107.25  77.00 120.00   52
 49  \w    148.00 178.00   0.50    1.96    --  107.25  15.00  30.00   60
 50  \w    150.00 178.00   0.50    1.96    --  107.25  15.00 -30.00   56
 51  \w     38.00  79.00   0.50    1.96    --  107.25 -77.00 -30.00   82
 52  \w    135.00 176.00   0.50    1.96    --  107.25  30.00-120.00   82
 53  \w    118.00 145.00   0.50    1.96    --  107.25  15.00  30.00   54
 54  \w    110.00 135.00   0.50    1.96    --  107.25  15.00 -30.00   50
 55  \w     99.00 124.00   0.50    1.96    --  107.25  61.00-180.00   50
 56  \w    107.00 139.00   0.50    1.96    --  107.25  61.00-150.00   64
 57  \w    141.00 178.00   0.50    1.96    --  107.25  30.00-180.00   74
 58  \w    103.00 129.00   0.50    1.96    --  107.25  30.00-180.00   52
 59  \w     43.00  69.00   0.50    1.96    --  107.25 -61.00 120.00   52
 60  \w     38.00  71.00   0.50    1.96    --  107.25 -61.00   0.00   66
 61  \w     45.00  70.00   0.50    1.96    --  107.25 -61.00  30.00   50
;
_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      -0.0828843000
_diffrn_orient_matrix_UB_12      0.0492764000
_diffrn_orient_matrix_UB_13      -0.0495537000
_diffrn_orient_matrix_UB_21      0.0211460000
_diffrn_orient_matrix_UB_22      -0.0042878000
_diffrn_orient_matrix_UB_23      -0.0756365000
_diffrn_orient_matrix_UB_31      -0.0440488000
_diffrn_orient_matrix_UB_32      -0.0950070000
_diffrn_orient_matrix_UB_33      -0.0224731000
_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  0.0356
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            64187
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.050
_diffrn_reflns_theta_min         3.000
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.843
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64985
_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    1.379
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_preparation       'Prepared from SIMesAgCl and MeMgBr'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.712
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.00039(3)
_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   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         8667
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0486P)^2^+4.4846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0884
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8335
_reflns_number_total             8667
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04067d2.cif
_cod_data_source_block           exp_1272_auto
_cod_depositor_comments
'Adding full bibliography for 1570794--1570800.cif.'
_cod_database_code               1570797
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N H Ag'
_shelx_estimated_absorpt_t_max   0.508
_shelx_estimated_absorpt_t_min   0.303
_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:
 C24(H24A,H24B), C2(H2A,H2B), C3(H3A,H3B), C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C18(H18), C29(H29), C31(H31), C7(H7), C40(H40), C9(H9), C38(H38)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C34(H34A,H34B,H34C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C26(H26A,H26B,H26C), C21(H21A,H21B,H21C), C4(H4A,H4B,H4C), C11(H11A,
 H11B,H11C), C33(H33A,H33B,H33C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C35(H35A,H35B,H35C), C13(H13A,H13B,H13C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              50301
_olex2_exptl_crystal_mounting_method 'XRD oil and Kapton'
_olex2_submission_original_sample_id CH128
_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 1.410
_oxdiff_exptl_absorpt_empirical_full_min 0.726