<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_1570796
_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         'C30 H37 Ag N2'
_chemical_formula_sum            'C30 H37 Ag N2'
_chemical_formula_weight         533.48
_chemical_name_systematic        (SIMes)AgMes
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Light-sensitive,Photo-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2fs019
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.7456(3)
_cell_length_b                   16.8545(4)
_cell_length_c                   19.8172(5)
_cell_measurement_reflns_used    18121
_cell_measurement_temperature    100.1(3)
_cell_measurement_theta_max      79.8310
_cell_measurement_theta_min      4.3770
_cell_volume                     5259.2(2)
_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      100.1(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_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     96.00 178.00   0.50    2.40    --  111.50 125.00  90.00  164
  2  \w     99.00 175.00   0.50    2.40    --  111.50  61.00-170.00  152
  3  \w    123.00 160.00   0.50    2.40    --  111.50  30.00-180.00   74
  4  \w     69.00  96.00   0.50    2.40    --  111.50 -77.00 -30.00   54
  5  \w     49.00 102.00   0.50    2.40    --  111.50 -77.00   0.00  106
  6  \w     41.00  66.00   0.50    2.40    --  111.50 -61.00 -30.00   50
  7  \w     43.00  69.00   0.50    2.40    --  111.50 -61.00   0.00   52
  8  \w     42.00  70.00   0.50    2.40    --  111.50 -61.00  51.00   56
  9  \w     41.00  66.00   0.50    2.40    --  111.50 -61.00 120.00   50
 10  \w    -19.00   7.00   0.50    0.60    --   49.52 -61.00  51.00   52
 11  \w     41.00  66.00   0.50    2.40    --  111.50 -61.00-150.00   50
 12  \w     43.00  71.00   0.50    2.40    --  111.50 -61.00-180.00   56
 13  \w     63.00  98.00   0.50    2.40    --  111.50-125.00 -30.00   70
 14  \w    -62.00  21.00   0.50    0.60    --  -49.52  61.00-170.00  166
 15  \w    -63.00 -37.00   0.50    2.40    --  -90.00  61.00-170.00   52
 16  \w    -50.00 -24.00   0.50    2.40    --  -90.00  45.00  30.00   52
 17  \w   -143.00-118.00   0.50    2.40    --  -90.00 -61.00  51.00   50
 18  \w   -102.00 -77.00   0.50    0.60    --  -49.52 -61.00  51.00   50
 19  \w   -120.00 -83.00   0.50    0.60    --  -49.52-125.00-120.00   74
 20  \w   -120.00 -74.00   0.50    0.60    --  -49.52-125.00-180.00   92
;
_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      -0.0365134000
_diffrn_orient_matrix_UB_12      0.0780711000
_diffrn_orient_matrix_UB_13      0.0281270000
_diffrn_orient_matrix_UB_21      -0.0762971000
_diffrn_orient_matrix_UB_22      -0.0070962000
_diffrn_orient_matrix_UB_23      -0.0482816000
_diffrn_orient_matrix_UB_31      -0.0491075000
_diffrn_orient_matrix_UB_32      -0.0470045000
_diffrn_orient_matrix_UB_33      0.0540847000
_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  0.0273
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            27606
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.202
_diffrn_reflns_theta_min         4.444
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.277
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60850
_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    1.348
_exptl_crystal_description       block
_exptl_crystal_F_000             2224
_exptl_crystal_preparation       'Prepared from SMesAgCl and Mes2Mg'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.792
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.00017(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   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5617
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+6.4436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5370
_reflns_number_total             5617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04067d2.cif
_cod_data_source_block           exp_1221_auto
_cod_depositor_comments
'Adding full bibliography for 1570794--1570800.cif.'
_cod_database_code               1570796
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Ag'
_shelx_estimated_absorpt_t_max   0.744
_shelx_estimated_absorpt_t_min   0.573
_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:
 C6(H6), C8(H8), C17(H17), C15(H15), C26(H26), C24(H24)
2.c Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C20(H20a,H20b,H20c), C11(H11a,H11b,H11c), C10(H10a,H10b,
 H10c), C29(H29a,H29b,H29c), C21(H21a,H21b,H21c), C19(H19a,H19b,H19c), C30(H30a,
 H30b,H30c), C28(H28a,H28b,H28c)
;
_shelx_res_checksum              55252
_olex2_exptl_crystal_mounting_method 'XRD Oil and Kapton'
_olex2_submission_original_sample_id CH120
_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 1.489
_oxdiff_exptl_absorpt_empirical_full_min 0.788