Catalytic exploration of NHC-Ag(I)HMDS complexes for the hydroboration and hydrosilylation of carbonyl compounds.
Giarrusso, Claudia P.; Zeil, Daniel V.; Blair, Victoria L.; Dalton Transactions  (2023) –; doi:10.1039/D3DT01042B

data_7713100
_publ_section_title
;
 Catalytic exploration of NHC-Ag(I)HMDS complexes for the hydroboration
 and hydrosilylation of carbonyl compounds.
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01042B
_journal_year                    2023
_chemical_formula_moiety         'C33 H54 Ag N3 Si2'
_chemical_formula_sum            'C33 H54 Ag N3 Si2'
_chemical_formula_weight         656.84
_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     direct
_audit_creation_date             2022-05-25
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-11-07 deposited with the CCDC.	2023-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.1928(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.90827(13)
_cell_length_b                   13.42943(13)
_cell_length_c                   21.6307(2)
_cell_measurement_reflns_used    20318
_cell_measurement_temperature    122.99(11)
_cell_measurement_theta_max      79.7280
_cell_measurement_theta_min      3.6090
_cell_volume                     3635.24(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.99(11)
_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 0.971
_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    -70.00  21.00   0.50    0.60    --  -50.61  76.00  82.00  182
  2  \w   -121.00 -31.00   0.50    0.60    --  -50.61 -76.00 -43.00  180
  3  \w    -20.00  70.00   0.50    0.60    --   50.61 -76.00 -43.00  180
  4  \w     32.00 122.00   0.50    0.60    --   50.61  76.00  82.00  180
  5  \w   -109.00 -18.00   0.50    2.40    --  -90.00  76.00  82.00  182
  6  \w   -161.00 -71.00   0.50    2.40    --  -90.00 -76.00 -43.00  180
  7  \w     92.00 178.00   0.50    2.40    --  111.50  76.00  82.00  172
  8  \w     49.00 112.00   0.50    2.40    --  111.50 -76.00 -43.00  126
  9  \w   -120.00 -81.00   0.50    0.60    --  -50.61-125.00-180.00   78
 10  \w   -121.00 -75.00   0.50    0.60    --  -50.61-125.00 120.00   92
 11  \w    -68.00 -37.00   0.50    2.40    --  -90.00  30.00 -60.00   62
 12  \w     41.00  66.00   0.50    2.40    --  111.50 -30.00 -30.00   50
 13  \w     41.00  66.00   0.50    2.40    --  111.50 -45.00-120.00   50
 14  \w     40.00  65.00   0.50    2.40    --  111.50 -30.00 120.00   50
 15  \w     43.00  75.00   0.50    2.40    --  111.50 -45.00-150.00   64
 16  \w     40.00  65.00   0.50    2.40    --  111.50 -30.00 150.00   50
 17  \w     43.00  95.00   0.50    2.40    --  111.50 -94.00 120.00  104
 18  \w     41.00  73.00   0.50    2.40    --  111.50 -45.00 -60.00   64
 19  \w     41.00  66.00   0.50    2.40    --  111.50 -45.00 150.00   50
 20  \w    110.00 177.00   0.50    2.40    --  111.50  61.00   0.00  134
 21  \w     42.00  69.00   0.50    2.40    --  111.50 -45.00 -30.00   54
 22  \w     44.00  76.00   0.50    2.40    --  111.50 -45.00  30.00   64
 23  \w     40.00  66.00   0.50    2.40    --  111.50 -30.00   0.00   52
 24  \w     50.00  76.00   0.50    2.40    --  111.50 -45.00-180.00   52
 25  \w     40.00  65.00   0.50    2.40    --  111.50 -30.00-150.00   50
 26  \w     41.00  67.00   0.50    2.40    --  111.50-125.00  90.00   52
 27  \w     73.00 111.00   0.50    2.40    --  111.50-125.00  90.00   76
 28  \w     70.00 125.00   0.50    2.40    --  111.50 -77.00  90.00  110
 29  \w     63.00 118.00   0.50    2.40    --  111.50   0.00  60.00  110
 30  \w     41.00  68.00   0.50    2.40    --  111.50 -45.00  90.00   54
;
_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      0.0755336000
_diffrn_orient_matrix_UB_12      0.0902637000
_diffrn_orient_matrix_UB_13      0.0072053000
_diffrn_orient_matrix_UB_21      -0.0340456000
_diffrn_orient_matrix_UB_22      0.0321444000
_diffrn_orient_matrix_UB_23      0.0605825000
_diffrn_orient_matrix_UB_31      0.0909360000
_diffrn_orient_matrix_UB_32      -0.0629799000
_diffrn_orient_matrix_UB_33      0.0410685000
_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  0.0681
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            38136
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.301
_diffrn_reflns_theta_min         3.642
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.244
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.021
_refine_diff_density_max         1.533
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         7733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0733P)^2^+1.7326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1201
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6724
_reflns_number_total             7733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01042b2.cif
_cod_data_source_block           cg-01-77
_cod_database_code               7713100
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 Ag1 N1 Si1'
_chemical_oxdiff_usercomment     Dipp
_diffrn_oxdiff_digest_frames
;
0188cb173b55ea7fcdbd980d01366506b602904eb9f
;
_diffrn_oxdiff_digest_hkl
;
01a9036af772e9099cc7347b4ccc763e6d446e
;
_reflns_odcompleteness_completeness 99.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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 Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C25(H25), C22(H22)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C20(H20), C18(H18), C6(H6), C7(H7), C2(H2), C19(H19), C3(H3)
2.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C27(H27A,H27B,H27C), C26(H26A,
 H26B,H26C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C11(H11A,H11B,H11C),
 C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              82036
_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 2.646
_oxdiff_exptl_absorpt_empirical_full_min 0.503