Cyclic Alkyl(amino)iminates (CAAIs) as Strong 2σ,4π-Electron Donor Ligands for the Stabilisation of Boranes and Diboranes(4): A Synthetic and Computational Study
Huynh, Silvia; Arrowsmith, Merle; Meier, Lukas; Dietz, Maximilian; Härterich, Marcel; Michel, Maximilian; Gärtner, Annalena; Braunschweig, Holger; Dalton Transactions  (2023) –; doi:10.1039/D3DT00298E

data_7712432
_publ_section_title
;
 Cyclic Alkyl(amino)iminates (CAAIs) as Strong 2\s,4\p-Electron Donor
 Ligands for the Stabilisation of Boranes and Diboranes(4): A Synthetic
 and Computational Study
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00298E
_journal_year                    2023
_chemical_formula_moiety         'C41 H62 B N5 S'
_chemical_formula_sum            'C41 H62 B N5 S'
_chemical_formula_weight         667.82
_chemical_name_systematic        (CAAI)2BNCS
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           'CIF-fill 1.2y (K.Radacki, 2005-22)'
_audit_update_record
;
2023-01-19 deposited with the CCDC.	2023-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.1630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.53740(10)
_cell_length_b                   19.8419(2)
_cell_length_c                   21.4198(2)
_cell_measurement_reflns_used    20311
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.5510
_cell_measurement_theta_min      3.0290
_cell_volume                     4021.85(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 HPA
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HyPix Arc150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     94.00 121.00   0.50    0.40    --   77.50  41.00 146.25   54
   2  \w     92.00 117.00   0.50    0.40    --   77.50  49.00  36.07   50
   3  \w     78.00 104.00   0.50    0.40    --   70.00  74.00  39.96   52
   4  \w     94.00 121.00   0.50    0.40    --   77.50  40.00 -40.70   54
   5  \w     92.00 117.00   0.50    0.40    --   77.50  46.00-171.41   50
   6  \w     94.00 121.00   0.50    0.40    --   77.50  39.00-137.85   54
   7  \w     88.00 117.00   0.50    0.40    --   77.50  26.00 -93.36   58
   8  \w     39.00 108.00   0.50    0.40    --   73.52   0.00  90.00  138
   9  \w   -117.00 -90.00   0.50    0.40    --  -74.00 -39.00   1.92   54
  10  \w   -106.00 -80.00   0.50    0.40    --  -74.00 -77.00 -18.57   52
  11  \w   -105.00 -79.00   0.50    0.40    --  -74.00 -79.00 -89.45   52
  12  \w   -105.00 -79.00   0.50    0.40    --  -74.00 -79.00  71.58   52
  13  \w    -70.00 -44.00   0.50    0.40    --  -38.00 -77.00 113.09   52
  14  \w    -88.00 -62.00   0.50    0.40    --  -50.00 -63.00 156.16   52
  15  \w   -104.00 -78.00   0.50    0.40    --  -66.00 -62.00 133.21   52
  16  \w   -113.00 -87.00   0.50    0.40    --  -74.00 -59.00 119.91   52
  17  \w   -104.00 -78.00   0.50    0.40    --  -66.00 -62.00  96.88   52
  18  \w   -108.00 -82.00   0.50    0.40    --  -70.00 -61.00  62.54   52
  19  \w   -117.00 -89.00   0.50    0.40    --  -74.00 -43.00  72.56   56
  20  \w   -113.00 -86.00   0.50    0.40    --  -70.00 -41.00 -33.12   54
  21  \w   -116.00 -89.00   0.50    0.40    --  -74.00 -49.00 -44.44   54
  22  \w   -109.00 -83.00   0.50    0.40    --  -70.00 -60.00 -79.39   52
  23  \w   -116.00 -89.00   0.50    0.40    --  -74.00 -49.00-111.73   54
  24  \w   -113.00 -86.00   0.50    0.40    --  -70.00 -40.00-149.59   54
  25  \w    -61.00 -35.00   0.50    0.40    --  -74.00  61.00-156.57   52
  26  \w    -62.00 -36.00   0.50    0.40    --  -74.00  64.00 -33.30   52
  27  \w    -95.00 -29.00   0.50    0.40    --  -69.45 126.00  60.00  132
  28  \w    -83.00 -38.00   0.50    0.40    --  -74.00 100.00  32.48   90
  29  \w     54.00 105.00   0.50    0.40    --   77.50-129.00 172.64  102
  30  \w     37.00 103.00   0.50    0.40    --   77.50-126.00 167.14  132
  31  \w     37.00  98.00   0.50    0.40    --   77.50-116.00  34.18  122
  32  \w     68.00  97.00   0.50    0.40    --   77.50-114.00 132.02   58
  33  \w     28.00  94.00   0.50    0.40    --   68.94-126.00 -90.00  132
  34  \w     73.00  99.00   0.50    0.40    --   77.50-117.00-128.26   52
  35  \w     37.00 103.00   0.50    0.40    --   77.50-126.00-157.17  132

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42988
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.072
_diffrn_reflns_theta_min         3.047
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R X-ray Source'
_exptl_absorpt_coefficient_mu    0.955
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.470
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.96a (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            'clear colourless'
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.383
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         7646
_refine_ls_number_restraints     199
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0500P)^2^+1.5729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1059
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6699
_reflns_number_total             7646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00298e2.cif
_cod_data_source_block           MaDi202_SiHu_a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7712432
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.713
_shelx_estimated_absorpt_t_max   0.954
_shelx_res_checksum              93331
_shelx_hkl_checksum              31997