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_7712428
_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         'C44 H74 B2 N6'
_chemical_formula_sum            'C44 H74 B2 N6'
_chemical_formula_weight         708.71
_chemical_name_systematic        (CAAI)2B2(NMe2)2
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-08-26
_audit_creation_method           'CIF-fill 1.3i (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                 100.6440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.63470(10)
_cell_length_b                   16.5638(3)
_cell_length_c                   25.4585(3)
_cell_measurement_reflns_used    13426
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.5560
_cell_measurement_theta_min      3.5610
_cell_volume                     4407.38(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.73a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.73a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.73a (Rigaku OD, 2020)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 HPA
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HyPix 6000'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w    -21.00  26.00   0.50    0.31    --  -47.45  19.00-120.00   94
  2  \w     34.00  97.00   0.50    0.31    --   47.45-129.00 -47.00  126
  3  \w     35.00 120.00   0.50    1.26    --  107.75-129.00 -47.00  170
  4  \w     84.00 116.00   0.50    1.26    --  107.75-125.00  30.00   64
  5  \w     56.00  96.00   0.50    1.26    --  107.75 -77.00 150.00   80
  6  \w     40.00 128.00   0.50    1.26    --  107.75-140.00 139.00  176
  7  \w     40.00 104.00   0.50    0.31    --   47.45-140.00 139.00  128
  8  \w     42.00  71.00   0.50    1.26    --  107.75 -61.00   0.00   58
  9  \w     39.00  71.00   0.50    1.26    --  107.75 -61.00 -60.00   64
 10  \w     80.00 107.00   0.50    1.26    --  107.75 -94.00 -90.00   54
 11  \w     53.00  83.00   0.50    1.26    --  107.75-125.00-180.00   60
 12  \w     44.00 107.00   0.50    1.26    --  107.75-125.00 -90.00  126
 13  \w     38.00  71.00   0.50    1.26    --  107.75 -61.00-180.00   66
 14  \w    127.00 172.00   0.50    1.26    --  107.75  15.00-150.00   90
 15  \w    132.00 158.00   0.50    1.26    --  107.75  15.00 -60.00   52
 16  \w     96.00 168.00   0.50    1.26    --  107.75  30.00   0.00  144
 17  \w     97.00 160.00   0.50    1.26    --  107.75  45.00 120.00  126
 18  \w     92.00 173.00   0.50    1.26    --  107.75 125.00   0.00  162
 19  \w     82.00 178.00   0.50    1.26    --  107.75 140.00-161.00  192
 20  \w     37.00 108.00   0.50    1.26    --  107.75 -94.00 150.00  142
 21  \w     36.00 112.00   0.50    1.26    --  107.75-125.00 150.00  152
 22  \w   -102.00 -18.00   0.50    1.26    --  -86.25 140.00-161.00  168
 23  \w   -103.00 -18.00   0.50    0.31    --  -47.45 140.00-161.00  170
 24  \w   -120.00 -68.00   0.50    0.31    --  -47.45-129.00 -47.00  104
 25  \w   -120.00 -70.00   0.50    0.31    --  -47.45-125.00  60.00  100
 26  \w   -120.00 -60.00   0.50    0.31    --  -47.45-140.00 139.00  120
 27  \w   -101.00 -74.00   0.50    0.31    --  -47.45-125.00-180.00   54
 28  \w   -138.00-113.00   0.50    1.26    --  -86.25-129.00 -47.00   50
 29  \w   -119.00 -71.00   0.50    0.31    --  -47.45-125.00   0.00   96
 30  \w   -120.00 -70.00   0.50    0.31    --  -47.45-125.00  90.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
;
 CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      0.0104521000
_diffrn_orient_matrix_UB_12      -0.0911290000
_diffrn_orient_matrix_UB_13      -0.0106189000
_diffrn_orient_matrix_UB_21      0.0236104000
_diffrn_orient_matrix_UB_22      0.0183548000
_diffrn_orient_matrix_UB_23      -0.0567276000
_diffrn_orient_matrix_UB_31      0.1450238000
_diffrn_orient_matrix_UB_32      0.0035278000
_diffrn_orient_matrix_UB_33      0.0215073000
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            22148
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.463
_diffrn_reflns_theta_min         3.533
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet X-ray Source'
_exptl_absorpt_coefficient_mu    0.465
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.41.73a (Rigaku Oxford Diffraction, 2020) Empirical 
 absorption correction using spherical harmonics, implemented in SCALE3 
 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_preparation
;
 Crystalls were grown from saturated solution. For data collection the 
 crystal was immersed in a film of perfluoropolyether oil, mounted on a 
 polyimide loop and transferred to stream of cold nitrogen (Oxford Cryostream 
 800).
;
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4554
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0684P)^2^+4.9557P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1487
_refine_ls_wR_factor_ref         0.1509
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4174
_reflns_number_total             4554
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00298e2.cif
_cod_data_source_block           MaHa042_SiHu_a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7712428
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.850
_shelx_estimated_absorpt_t_max   0.917
_shelx_res_checksum              42796
_shelx_hkl_checksum              71336