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_7133292
_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 H54 B N5'
_chemical_formula_sum            'C35 H54 B N5'
_chemical_formula_weight         555.64
_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_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                 92.4420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.32910(10)
_cell_length_b                   13.6009(2)
_cell_length_c                   18.6157(3)
_cell_measurement_reflns_used    33087
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.3760
_cell_measurement_theta_min      3.9590
_cell_volume                     3371.73(8)
_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 1.000
_diffrn_measured_fraction_theta_max 0.995
_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     17.00  65.00   0.50    6.00    --   58.61 -93.00 -63.00   96
   2  \w    -66.00 -18.00   0.50    6.00    --  -60.00  93.00  48.00   96
   3  \w    -75.00 -27.00   0.50    6.00    --  -69.42  93.00  48.00   96
   4  \w     29.00  77.00   0.50    6.00    --   71.30 -93.00 -63.00   96
   5  \w    -82.00 -34.00   0.50    6.00    --  -76.37  93.00  48.00   96
   6  \w     40.00  88.00   0.50    6.00    --   82.31 -93.00 -63.00   96
   7  \w     59.00  94.00   0.50    6.00    --   46.00  52.00 176.57   70
   8  \w     64.00  99.00   0.50    6.00    --   50.00  48.00 -74.12   70
   9  \w     63.00  98.00   0.50    6.00    --   50.00  52.00-167.95   70
  10  \w   -102.00 -67.00   0.50    6.00    --  -54.00 -52.00-158.45   70
  11  \w     16.00  66.00   0.50    6.00    --   58.61 -95.00 -60.00  100
  12  \w   -112.00 -75.00   0.50    6.00    --  -62.00 -45.00 105.08   74
  13  \w     76.00 116.00   0.50    6.00    --   64.96  37.00  65.52   80
  14  \w   -117.00 -83.00   0.50    6.00    --  -70.00 -55.00  32.31   68
  15  \w     29.00  79.00   0.50    6.00    --   71.30 -95.00 -30.00  100
  16  \w    -97.00 -28.00   0.50    6.00    --  -76.37 112.00 -30.00  138
  17  \w    -97.00 -28.00   0.50    6.00    --  -76.37 112.00-180.00  138
  18  \w   -124.00 -89.00   0.50    6.00    --  -78.00 -61.00 166.23   70
  19  \w   -123.00 -97.00   0.50    6.00    --  -79.50 -66.00-152.28   52
  20  \w   -125.00 -90.00   0.50    6.00    --  -79.50 -62.00  16.34   70
  21  \w   -127.00 -92.00   0.50    6.00    --  -79.50 -54.00  91.11   70
  22  \w   -125.00 -90.00   0.50    6.00    --  -79.50 -62.00-101.16   70
  23  \w   -126.00 -92.00   0.50    6.00    --  -79.50 -57.00 -22.14   68
  24  \w   -102.00 -32.00   0.50    6.00    --  -79.50 129.00  67.40  140
  25  \w   -100.00 -31.00   0.50    6.00    --  -79.50 122.00 -62.78  138
  26  \w   -130.00 -91.00   0.50    6.00    --  -79.50 -41.00 -65.37   78
  27  \w     34.00  97.00   0.50    6.00    --   82.31-112.00-120.00  126
  28  \w     34.00  97.00   0.50    6.00    --   82.31-112.00 -60.00  126
  29  \w     34.00  97.00   0.50    6.00    --   82.31-112.00 150.00  126
  30  \w     40.00  90.00   0.50    6.00    --   82.31 -95.00-150.00  100
  31  \w     40.00  90.00   0.50    6.00    --   82.31 -95.00-180.00  100
  32  \w     46.00 133.00   0.50    6.00    --   82.31  15.00 -90.00  174
  33  \w     34.00  97.00   0.50    6.00    --   82.31-112.00 120.00  126
  34  \w     40.00  95.00   0.50    6.00    --   85.25-104.00-155.86  110
  35  \w     91.00 132.00   0.50    6.00    --   85.25 138.00  11.08   82
  36  \w     92.00 132.00   0.50    6.00    --   85.25 135.00 121.91   80
  37  \w     44.00  89.00   0.50    6.00    --   85.25 -90.00 -89.00   90
  38  \w     46.00  84.00   0.50    6.00    --   85.25 -82.00-114.47   76
  39  \w     66.00 136.00   0.50    6.00    --   85.25  17.00-140.03  140
  40  \w     98.00 136.00   0.50    6.00    --   85.25  43.00-170.35   76
  41  \w     37.00  97.00   0.50    6.00    --   85.25-112.00 165.81  120
  42  \w     39.00 107.00   0.50    6.00    --   85.25-137.00  -6.43  136
  43  \w     96.00 138.00   0.50    6.00    --   85.25  31.00  48.55   84
  44  \w     40.00  94.00   0.50    6.00    --   85.25-103.00  43.14  108
  45  \w     91.00 132.00   0.50    6.00    --   85.25 136.00  35.72   82
  46  \w     40.00  94.00   0.50    6.00    --   85.25-102.00-109.17  108
  47  \w     91.00 132.00   0.50    6.00    --   85.25 138.00 -86.65   82
  48  \w     43.00  92.00   0.50    6.00    --   85.25 -94.00 150.81   98
  49  \w    102.00 134.00   0.50    6.00    --   85.25 116.00 -91.35   64
  50  \w     38.00  95.00   0.50    6.00    --   85.25-109.00   4.23  114
  51  \w     38.00 103.00   0.50    6.00    --   85.25-133.00 140.84  130
  52  \w    102.00 133.00   0.50    6.00    --   85.25  52.00  63.56   62
  53  \w     69.00  97.00   0.50    6.00    --   85.25-112.00  37.40   56
  54  \w     40.00  66.00   0.50    6.00    --   85.25-112.00  37.40   52
  55  \w     46.00  93.00   0.50    6.00    --   85.25 -98.00  45.94   94
  56  \w     65.00  96.00   0.50    6.00    --   85.25-119.00 -66.58   62
  57  \w     57.00  94.00   0.50    6.00    --   85.25-102.00 -23.63   74
  58  \w     47.00  90.00   0.50    6.00    --   85.25 -94.00 171.05   86
  59  \w     48.00  97.00   0.50    6.00    --   85.25-115.00 -25.84   98
  60  \w    103.00 131.00   0.50    6.00    --   85.25 116.00  59.79   56
  61  \w     52.00  78.00   0.50    6.00    --   85.25-126.00 116.90   52
  62  \w     75.00 134.00   0.50    6.00    --   85.25  11.00  81.17  118
  63  \w    102.00 128.00   0.50    6.00    --   85.25  41.00-109.83   52
  64  \w     93.00 128.00   0.50    6.00    --   85.25  27.00 151.27   70
  65  \w     46.00  89.00   0.50    6.00    --   85.25 -91.00 108.23   86
  66  \w    103.00 129.00   0.50    6.00    --   85.25  32.00  75.39   52
  67  \w     52.00  97.00   0.50    6.00    --   85.25-111.00  14.81   90
  68  \w     49.00  75.00   0.50    6.00    --   85.25-119.00-178.18   52
  69  \w     39.00  64.00   0.50    6.00    --   85.25-106.00-158.76   50
  70  \w     51.00  77.00   0.50    6.00    --   85.25-101.00 104.94   52
  71  \w     38.00  76.00   0.50    6.00    --   85.25-127.00  38.70   76
  72  \w     42.00  71.00   0.50    6.00    --   85.25-138.00-173.29   58
  73  \w     51.00  84.00   0.50    6.00    --   85.25 -91.00  67.20   66
  74  \w     39.00  74.00   0.50    6.00    --   85.25-136.00  93.65   70
  75  \w     41.00  68.00   0.50    6.00    --   85.25-119.00 143.63   54
  76  \w     38.00  64.00   0.50    6.00    --   85.25-128.00  16.45   52
  77  \w     49.00  94.00   0.50    6.00    --   85.25 -99.00  68.86   90
  78  \w     46.00  72.00   0.50    6.00    --   85.25 -75.00-165.06   52
  79  \w    100.00 133.00   0.50    6.00    --   85.25  42.00 -79.92   66
  80  \w     97.00 130.00   0.50    6.00    --   85.25  56.00 -40.97   66

;
_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     0.0174
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15582
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.148
_diffrn_reflns_theta_min         4.000
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R X-ray Source'
_exptl_absorpt_coefficient_mu    0.485
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76777
_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            colourless
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_description       needle
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.449
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         15582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.1078
_refine_ls_R_factor_gt           0.0787
_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^)+(0.1593P)^2^+0.0426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2319
_refine_ls_wR_factor_ref         0.2601
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9811
_reflns_number_total             15582
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
 Component 2 rotated by 147.9911\% around [0.71 0.52 0.48] (reciprocal) or [0.79 0.55 0.29] (direct)
;
_cod_data_source_file            d4cc02923b2.cif
_cod_data_source_block           Compound7a
_cod_depositor_comments
'Adding full bibliography for 7133290--7133296.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7133292
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              65473
_shelx_hkl_checksum              98408