<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_1570800
_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         'C27 H44 Ag N3 Si2'
_chemical_formula_sum            'C27 H44 Ag N3 Si2'
_chemical_formula_weight         574.70
_chemical_name_common            (SIMes)AgHMDS
_chemical_name_systematic        (SIMes)Ag(N(SiMe3)2)
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Light-sensitive,Photo-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2fs008
_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            16
_cell_length_a                   20.852(4)
_cell_length_b                   44.031(12)
_cell_length_c                   13.785(4)
_cell_measurement_reflns_used    9217
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      35.36
_cell_measurement_theta_min      2.91
_cell_volume                     12656(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            100378
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.250
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.730
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1686 before and 0.0810 after correction.
The Ratio of minimum to maximum transmission is 0.8607.
The \l/2 correction factor is Not present.
;
_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    1.206
_exptl_crystal_description       needle
_exptl_crystal_F_000             4832
_exptl_crystal_preparation       'Prepared from SIMesAgCl and LiHMDS'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: HMDSO'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 2211 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.009(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         5586
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0186P)^2^+27.3169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0642
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5148
_reflns_number_total             5586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04067d2.cif
_cod_data_source_block           ch-123-simesghmds
_cod_depositor_comments
'Adding full bibliography for 1570794--1570800.cif.'
_cod_database_code               1570800
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.898
_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:
 C3(H3A,H3B), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C21(H21), C14(H14), C12(H12)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C6(H6A,H6B,H6C), C25(H25A,H25B,H25C), C27(H27A,H27B,
 H27C), C5(H5A,H5B,H5C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C26(H26A,
 H26B,H26C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              17939
_olex2_exptl_crystal_mounting_method 'XRD oil and Kapton'
_olex2_submission_original_sample_id CH123
_olex2_submission_special_instructions 'No special instructions were received'