Transition-metal-like coordination chemistry of dicoordinate borylenes with organic azides.
Witte, Robert; Kar, Sourav; Radacki, Krzysztof; Härterich, Marcel; Rang, Maximilian; Michel, Maximilian; Mihm, Cornelius; Czernetzki, Corinna; Brückner, Tobias; Beck, Eva; Lutz, Sarah; Dewhurst, Rian D.; Braunschweig, Holger; Chemical communications (Cambridge, England) 60 (2024) 8629–8632; doi:10.1039/d4cc02923b

data_7133293
_publ_section_title
;
 Transition-metal-like coordination chemistry of dicoordinate borylenes
 with organic azides.
;
_journal_issue                   65
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8629
_journal_page_last               8632
_journal_paper_doi               10.1039/d4cc02923b
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C35 H52 B Cl2 N5'
_chemical_formula_sum            'C35 H52 B Cl2 N5'
_chemical_formula_weight         624.52
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           'CIF-fill 1.2y (K.Radacki, 2005-22)'
_audit_update_record
;
2024-06-13 deposited with the CCDC.	2024-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.6140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.6475(4)
_cell_length_b                   15.5802(3)
_cell_length_c                   18.9468(2)
_cell_measurement_reflns_used    35500
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.8450
_cell_measurement_theta_min      3.4010
_cell_volume                     6966.74(19)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_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 (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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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     23.00  48.00   0.50    0.31    --   58.61-115.00 -14.00   50
   2  \w    -44.00 -18.00   0.50    0.31    --  -60.19 115.00  75.00   52
   3  \w    -63.00 -26.00   0.50    0.31    --  -69.72 115.00  75.00   74
   4  \w     41.00  94.00   0.50    0.31    --   71.30-115.00 -14.00  106
   5  \w    -97.00 -71.00   0.50    0.31    --  -76.37 115.00  75.00   52
   6  \w     41.00  66.00   0.50    0.31    --   82.31-115.00 -14.00   50
   7  \w    -94.00 -61.00   0.50    0.31    --  -46.00 -48.00 -40.36   66
   8  \w     60.00  92.00   0.50    0.31    --   46.00  52.00  45.22   64
   9  \w     32.00  66.00   0.50    0.31    --   58.61 -95.00-120.00   68
  10  \w   -110.00 -75.00   0.50    0.31    --  -62.00 -51.00 141.82   70
  11  \w   -108.00 -81.00   0.50    0.31    --  -62.00 -51.00  37.48   54
  12  \w   -114.00 -81.00   0.50    0.31    --  -66.00 -47.00 -81.30   66
  13  \w   -109.00 -83.00   0.50    0.31    --  -70.00 -55.00  69.15   52
  14  \w     43.00  79.00   0.50    0.31    --   71.30 -95.00  60.00   72
  15  \w   -127.00 -98.00   0.50    0.31    --  -79.50 -36.00-105.78   58
  16  \w   -120.00 -94.00   0.50    0.31    --  -79.50 -64.00-135.89   52
  17  \w   -126.00 -95.00   0.50    0.31    --  -79.50 -59.00  19.26   62
  18  \w     70.00  96.00   0.50    0.31    --   82.31-112.00  30.00   52
  19  \w     70.00  96.00   0.50    0.31    --   82.31-112.00  90.00   52
  20  \w     70.00  97.00   0.50    0.31    --   82.31-112.00  60.00   54
  21  \w     65.00  96.00   0.50    0.31    --   82.31-112.00   0.00   62
  22  \w     98.00 133.00   0.50    0.31    --   85.25  40.00 -68.35   70
  23  \w     65.00  97.00   0.50    0.31    --   85.25-117.00  11.34   64
  24  \w    104.00 129.00   0.50    0.31    --   85.25 113.00 173.56   50
  25  \w     65.00  94.00   0.50    0.31    --   85.25-107.00 108.24   58
  26  \w     42.00  96.00   0.50    0.31    --   85.25-130.00  -1.09  108
  27  \w     50.00  75.00   0.50    0.31    --   85.25-100.00 125.77   50
  28  \w     51.00  87.00   0.50    0.31    --   85.25 -90.00   4.21   72
  29  \w     46.00  72.00   0.50    0.31    --   85.25 -74.00 -98.51   52
  30  \w     38.00  64.00   0.50    0.31    --   85.25-118.00-131.13   52
  31  \w     97.00 137.00   0.50    0.31    --   85.25  33.00 150.26   80
  32  \w    103.00 128.00   0.50    0.31    --   85.25 114.00  74.88   50
  33  \w     54.00  88.00   0.50    0.31    --   85.25-110.00  62.83   68
  34  \w    104.00 134.00   0.50    0.31    --   85.25 114.00 125.70   60
  35  \w    103.00 129.00   0.50    0.31    --   85.25  52.00-137.34   52
  36  \w    102.00 129.00   0.50    0.31    --   85.25  49.00 159.08   54
  37  \w     65.00  91.00   0.50    0.31    --   85.25-127.00 -59.57   52
  38  \w     98.00 132.00   0.50    0.31    --   85.25  45.00  57.84   68
  39  \w     65.00 100.00   0.50    0.31    --   85.25-122.00-160.96   70
  40  \w     45.00  71.00   0.50    0.31    --   85.25-102.00 -51.73   52
  41  \w     98.00 125.00   0.50    0.31    --   85.25  44.00  70.79   54
  42  \w     40.00  85.00   0.50    0.31    --   85.25-130.00-178.40   90
  43  \w     62.00  88.00   0.50    0.31    --   85.25-123.00 154.50   52
  44  \w     99.00 124.00   0.50    0.31    --   85.25  49.00 -26.69   50
  45  \w     97.00 124.00   0.50    0.31    --   85.25  58.00  23.33   54
  46  \w     98.00 132.00   0.50    0.31    --   85.25  44.00 -98.69   68
  47  \w     48.00  89.00   0.50    0.31    --   85.25-101.00-111.50   82
  48  \w     43.00  94.00   0.50    0.31    --   85.25-112.00-159.35  102
  49  \w     97.00 122.00   0.50    0.31    --   85.25  56.00-109.60   50

;
_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_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22478
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.070
_diffrn_reflns_theta_min         3.399
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R X-ray Source'
_exptl_absorpt_coefficient_mu    1.902
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021) Empirical 
absorption correction using spherical harmonics, implemented in SCALE3 
ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     800
_refine_ls_number_reflns         22478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0890P)^2^+2.3373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1530
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19772
_reflns_number_total             22478
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
 Component 2 rotated by -179.9928\% around [1.00 0.00 -0.05] (reciprocal) or [1.00 -0.00 0.00] (direct)
;
_cod_data_source_file            d4cc02923b2.cif
_cod_data_source_block           Compound6c
_cod_depositor_comments
'Adding full bibliography for 7133290--7133296.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7133293
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              5995
_shelx_hkl_checksum              6573