<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_1570799
_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 H51 Ag N2 O4 Si'
_chemical_formula_sum            'C33 H51 Ag N2 O4 Si'
_chemical_formula_weight         675.72
_chemical_name_common            (IMes)AgTBOS
_chemical_name_systematic        (IMes)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.cc2frzy4
_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                 104.952(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1581(2)
_cell_length_b                   16.6129(2)
_cell_length_c                   19.1762(3)
_cell_measurement_reflns_used    44533
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      38.8380
_cell_measurement_theta_min      2.2310
_cell_volume                     3434.31(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f   -339.92  20.08   0.80    5.00  18.74  -1.76 -59.25    --   450
  2  \w    -77.80  22.20   0.80   10.00    --  -42.55  84.14  86.32  125
  3  \w    -85.45  18.55   0.80    5.00    --   -1.76 -59.25-123.92  130
  4  \w    -85.45  18.55   0.80    5.00    --   -1.76 -59.25 -51.92  130
  5  \w    -85.45  18.55   0.80    5.00    --   -1.76 -59.25  20.08  130
  6  \w    -85.45  18.55   0.80    5.00    --   -1.76 -59.25 164.08  130
  7  \w    -85.45  18.55   0.80    5.00    --   -1.76 -59.25  92.08  130
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0054690000
_diffrn_orient_matrix_UB_12      0.0291165000
_diffrn_orient_matrix_UB_13      -0.0277107000
_diffrn_orient_matrix_UB_21      -0.0084293000
_diffrn_orient_matrix_UB_22      -0.0311995000
_diffrn_orient_matrix_UB_23      -0.0260695000
_diffrn_orient_matrix_UB_31      -0.0650074000
_diffrn_orient_matrix_UB_32      0.0015952000
_diffrn_orient_matrix_UB_33      -0.0042891000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            143474
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.575
_diffrn_reflns_theta_min         1.646
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    1.307
_exptl_crystal_description       cube
_exptl_crystal_F_000             1424
_exptl_crystal_preparation       'Prepared from IMesAgCl and NaTBOS'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.126
_refine_diff_density_min         -1.798
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         9629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0469P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0900
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7836
_reflns_number_total             9629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04067d2.cif
_cod_data_source_block           mo_ch_107_autored
_cod_depositor_comments
'Adding full bibliography for 1570794--1570800.cif.'
_cod_database_code               1570799
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.880
_shelx_estimated_absorpt_t_min   0.880
_reflns_odcompleteness_completeness 69.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     47.62
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C009(H009), C00A(H00A), C00U(H00), C00X(H2), C010(H010), C012(H012)
2.b Idealised Me refined as rotating group:
 C00G(H00B,H00C,H00D), C00H(H00E,H00F,H00G), C00I(H00H,H00I,H00J), C00J(H00K,
 H00L,H00M), C00O(H00N,H00O,H00P), C00P(H00Q,H00R,H00S), C00Q(H00T,H00U,H00V),
 C00R(H00W,H00X,H00Y), C00T(H00Z,H,HA), C00W(H1,HB,HC), C00Y(H3,HD,HE), C00Z(H4,
 HF,HG), C011(H01A,H01B,H01C), C014(H01D,H01E,H01F), C015(H01G,H01H,H01I)
;
_shelx_res_checksum              93791
_olex2_exptl_crystal_mounting_method 'XRD Oil and Kapton'
_olex2_submission_original_sample_id CH107
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.151
_oxdiff_exptl_absorpt_empirical_full_min 0.916