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_7713101
_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         'C29 H50 Ag N3 Si2'
_chemical_formula_sum            'C29 H50 Ag N3 Si2'
_chemical_formula_weight         604.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
;
2022-11-08 deposited with the CCDC.	2023-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.751(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2489(8)
_cell_length_b                   12.2700(5)
_cell_length_c                   12.8905(6)
_cell_measurement_reflns_used    14198
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      32.6620
_cell_measurement_theta_min      3.4870
_cell_volume                     3082.4(2)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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     -6.00  55.00   0.50    2.10    --   25.27  57.00  60.00  122
  2  \w     42.00 108.00   0.50    2.10    --   25.27 178.00-150.00  132
  3  \w     42.00 108.00   0.50    2.10    --   25.27 178.00-120.00  132
  4  \w     42.00 108.00   0.50    2.10    --   25.27 178.00 -90.00  132
  5  \w    -59.00  48.00   0.50    2.10    --   25.27 -38.00  60.00  214
  6  \w      0.00  81.00   0.50    2.10    --   25.27-108.00 -74.00  162
  7  \w     39.00 108.00   0.50    2.10    --   25.27-178.00-180.00  138
  8  \w    -23.00  25.00   0.50    2.10    --  -24.95 -99.00 120.00   96
  9  \w   -117.00 -63.00   0.50    2.10    --  -24.95-178.00  90.00  108
 10  \w    -80.00 -21.00   0.50    2.10    --  -24.95 108.00  23.00  118
;
_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      -0.0096697000
_diffrn_orient_matrix_UB_12      -0.0507499000
_diffrn_orient_matrix_UB_13      0.0178538000
_diffrn_orient_matrix_UB_21      -0.0011057000
_diffrn_orient_matrix_UB_22      0.0243635000
_diffrn_orient_matrix_UB_23      0.0493982000
_diffrn_orient_matrix_UB_31      -0.0350570000
_diffrn_orient_matrix_UB_32      0.0132020000
_diffrn_orient_matrix_UB_33      -0.0225673000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19847
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.275
_diffrn_reflns_theta_min         3.321
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.753
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.438
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       needle
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.526
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.109
_refine_diff_density_max         1.426
_refine_diff_density_min         -1.362
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0804P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3500
_reflns_number_total             3815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01042b2.cif
_cod_data_source_block           cg-01-35_auto
_cod_database_code               7713101
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C29 H50 Ag1 N3 Si2'
_diffrn_oxdiff_digest_frames
;
01451d7f672f1176663307a4f840003c7901354cb38
;
_diffrn_oxdiff_digest_hkl
;
01f76458f723928ad1e1bc00bb52ae8c92d66f
;
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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 Ternary CH refined with riding coordinates:
 C5(H5), C7(H7), C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C12(H12A,
 H12B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2)
2.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              3335
_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 2.154
_oxdiff_exptl_absorpt_empirical_full_min 0.512