Remote C-H bond cooperation strategy enabled silver catalyzed borrowing hydrogen reactions.
Chen, Zhe; Ouyang, Laofeng; Wang, Ning; Li, Weikang; Ke, Zhuofeng; Chemical science 16 (2024) 163–170; doi:10.1039/d4sc05486e

data_1573254
_publ_section_title
;
 Remote C-H bond cooperation strategy enabled silver catalyzed borrowing
 hydrogen reactions.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              163
_journal_page_last               170
_journal_paper_doi               10.1039/d4sc05486e
_journal_volume                  16
_journal_year                    2024
_chemical_formula_moiety         'C9 H12 Ag N4, F6 P, C2 H3 N'
_chemical_formula_sum            'C11 H15 Ag F6 N5 P'
_chemical_formula_weight         470.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-25 deposited with the CCDC.	2024-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                97.817(3)
_cell_angle_beta                 98.360(3)
_cell_angle_gamma                109.228(4)
_cell_formula_units_Z            2
_cell_length_a                   8.9329(4)
_cell_length_b                   9.2591(3)
_cell_length_c                   11.0005(4)
_cell_measurement_reflns_used    4598
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      75.9650
_cell_measurement_theta_min      4.1150
_cell_volume                     833.34(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.965
_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   -112.00 -17.00   1.00    1.00    --  -41.94 -57.00   0.00   95
  2  \w    -62.00  27.00   1.00    1.00    --  -41.94  57.00 -90.00   89
  3  \w   -112.00 -16.00   1.00    1.00    --  -41.94 -57.00 120.00   96
  4  \w     20.00  72.00   1.00    1.00    --   41.94 -99.00  60.00   52
  5  \w     59.00  84.00   1.00    1.00    --   41.94-125.00 -60.00   25
  6  \w     65.00 119.00   1.00    1.48    --  111.00 178.00 150.00   54
  7  \w     36.00 133.00   1.00    1.48    --  111.00 -30.00  30.00   97
  8  \w     87.00 150.00   1.00    1.48    --  111.00  30.00  30.00   63
  9  \w     81.00 109.00   1.00    1.48    --  111.00-111.00-120.00   28
 10  \w     41.00  96.00   1.00    1.48    --  111.00 -30.00-150.00   55
 11  \w     84.00 122.00   1.00    1.48    --  111.00 -61.00 -30.00   38
 12  \w     46.00 119.00   1.00    1.48    --  111.00 -61.00 150.00   73
 13  \w     43.00 133.00   1.00    1.48    --  111.00 -30.00 120.00   90
 14  \w     82.00 109.00   1.00    1.48    --  111.00-111.00  90.00   27
 15  \w    150.00 175.00   1.00    1.48    --  111.00 111.00  60.00   25
 16  \w     79.00 109.00   1.00    1.48    --  111.00-111.00 -30.00   30
 17  \w    115.00 140.00   1.00    1.48    --  111.00 111.00  60.00   25
 18  \w     50.00  76.00   1.00    1.48    --  111.00-111.00-180.00   26
 19  \w     78.00 109.00   1.00    1.48    --  111.00-111.00-180.00   31
 20  \w     52.00  91.00   1.00    1.48    --  111.00 -94.00 120.00   39
 21  \w    110.00 135.00   1.00    1.48    --  111.00 111.00 120.00   25
 22  \w     90.00 143.00   1.00    1.48    --  111.00 178.00 120.00   53
 23  \w    107.00 170.00   1.00    1.48    --  111.00 111.00  90.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0288066000
_diffrn_orient_matrix_UB_12      0.0934003000
_diffrn_orient_matrix_UB_13      0.1336549000
_diffrn_orient_matrix_UB_21      0.1582337000
_diffrn_orient_matrix_UB_22      0.1175003000
_diffrn_orient_matrix_UB_23      -0.0200531000
_diffrn_orient_matrix_UB_31      -0.0945016000
_diffrn_orient_matrix_UB_32      0.0988580000
_diffrn_orient_matrix_UB_33      -0.0507747000
_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  0.0551
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6153
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.068
_diffrn_reflns_theta_min         4.143
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.263
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.00076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.92a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_description       plate
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.003
_refine_diff_density_max         1.256
_refine_diff_density_min         -1.173
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0599
_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^)+(0.1020P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1471
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3182
_reflns_number_total             3372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05486e2.cif
_cod_data_source_block           a23112204a0724
_cod_depositor_comments
'Adding full bibliography for 1573254--1573255.cif.'
_cod_database_code               1573254
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C11H17AgF6N5P
_chemical_oxdiff_usercomment     327
_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:
 C00B(H00A,H00B)
2.b Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00J(H00J), C00K(H00K), C00N(H00N)
2.c Idealised Me refined as rotating group:
 C00H(H00C,H00D,H00E), C00I(H00L,H00M,H00O), C00L(H00G,H00H,H00I)
;
_shelx_res_checksum              12650
_shelx_hkl_checksum              13193
_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 700.704
_oxdiff_exptl_absorpt_empirical_full_min 0.507