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_7712422
_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         'C29 H42 B Br N2'
_chemical_formula_sum            'C29 H42 B Br N2'
_chemical_formula_weight         509.36
_chemical_name_systematic        (CAAI)BBrMes
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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     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                90.0
_cell_angle_beta                 106.480(3)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   10.0184(3)
_cell_length_b                   16.7493(4)
_cell_length_c                   17.4941(5)
_cell_measurement_reflns_used    11546
_cell_measurement_temperature    99.98(12)
_cell_measurement_theta_max      29.6570
_cell_measurement_theta_min      2.3960
_cell_volume                     2814.94(14)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(12)
_diffrn_detector                 HPA
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HyPix 6000'
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.8045
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w    -21.00  29.00   0.50    8.93    --    5.18 -84.00 117.00  100
  2  \w    -37.00 -12.00   0.50    8.93    --   -5.96 -84.00 117.00   50
  3  \w    -32.00  17.00   0.50    8.93    --   -5.96  84.00-122.00   98
  4  \w    -69.00   4.00   0.50    8.93    --    5.18 -19.00  60.00  146
  5  \w    -24.00  28.00   0.50    8.93    --   -5.96 -99.00 -30.00  104
  6  \w     -2.00  23.00   0.50    8.93    --   -5.96 -99.00  60.00   50
  7  \w    -16.00  24.00   0.50    8.93    --   -5.96 -99.00 -60.00   80
;
_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      -0.0267217000
_diffrn_orient_matrix_UB_12      0.0374130000
_diffrn_orient_matrix_UB_13      -0.0164804000
_diffrn_orient_matrix_UB_21      -0.0506363000
_diffrn_orient_matrix_UB_22      -0.0014792000
_diffrn_orient_matrix_UB_23      0.0212224000
_diffrn_orient_matrix_UB_31      0.0466315000
_diffrn_orient_matrix_UB_32      0.0198256000
_diffrn_orient_matrix_UB_33      0.0326260000
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.805
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30343
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.805
_diffrn_reflns_theta_full        26.3154
_diffrn_reflns_theta_max         31.1029
_diffrn_reflns_theta_min         2.1199
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet X-ray Source'
_exptl_absorpt_coefficient_mu    1.479
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85806
_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    1.202
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_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          0.289
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.063
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         7292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0275P)^2^+2.1027P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6037
_reflns_number_total             7292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00298e2.cif
_cod_data_source_block           MaHa052_SiHu_Mo_a
_cod_original_cell_volume        2814.92(15)
_cod_database_code               7712422
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              69533
_shelx_hkl_checksum              87117