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_7133294
_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      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-08-07
_audit_creation_method           'CIF-fill 1.4m (K.Radacki, 2005-23)'
_audit_update_record
;
2024-06-13 deposited with the CCDC.	2024-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                76.108(2)
_cell_angle_beta                 79.110(2)
_cell_angle_gamma                68.167(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8020(2)
_cell_length_b                   12.3555(3)
_cell_length_c                   13.8232(2)
_cell_measurement_reflns_used    26799
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.5790
_cell_measurement_theta_min      3.2850
_cell_volume                     1652.28(6)
_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 2018/2 (Sheldrick, 2018)''
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 HPA
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HyPix Arc150'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w    -97.00 -22.00   0.50    0.05    --  -69.54 126.00-120.00  150
  2  \w   -103.00 -68.00   0.50    0.05    --  -54.00 -50.00   0.64   70
  3  \w   -128.00 -93.00   0.50    0.05    --  -79.50 -50.00  17.24   70
  4  \w   -111.00 -76.00   0.50    0.05    --  -62.00 -49.00  73.28   70
  5  \w     42.00  92.00   0.50    0.05    --   84.34 -95.00 150.00  100
  6  \w   -116.00 -79.00   0.50    0.05    --  -66.00 -45.00 137.10   74
  7  \w     42.00  92.00   0.50    0.05    --   84.34 -95.00 -30.00  100
  8  \w   -130.00 -92.00   0.50    0.05    --  -79.50 -42.00  40.75   76
  9  \w     42.00  92.00   0.50    0.05    --   84.34 -95.00-180.00  100
 10  \w    -92.00 -31.00   0.50    0.05    --  -76.37 112.00  60.00  122
 11  \w     44.00 121.00   0.50    0.05    --   71.26  14.00  23.00  154
 12  \w   -126.00 -92.00   0.50    0.05    --  -79.50 -57.00  94.33   68
 13  \w   -122.00 -87.00   0.50    0.05    --  -74.00 -51.00 169.20   70
 14  \w     49.00 134.00   0.50    0.05    --   84.34  14.00  23.00  170
 15  \w    -74.00 -39.00   0.50    0.05    --  -26.00 -52.00 125.54   70
 16  \w   -128.00 -93.00   0.50    0.05    --  -79.50 -51.00 104.08   70
 17  \w   -124.00 -94.00   0.50    0.05    --  -79.50 -64.00 140.30   60
 18  \w   -126.00 -92.00   0.50    0.05    --  -79.50-123.00-161.62   68
 19  \w     44.00 109.00   0.50    0.05    --   58.45  14.00  23.00  130
 20  \w     34.00  60.00   0.50    0.05    --   22.00  58.00  20.94   52
 21  \w     31.00  60.00   0.50    0.05    --   18.00  55.00-136.82   58
 22  \w     30.00  56.00   0.50    0.05    --   18.00  60.00 -62.82   52
 23  \w     31.00  93.00   0.50    0.05    --   76.32-112.00 150.00  124
 24  \w    -92.00 -35.00   0.50    0.05    --  -79.50 102.00 -64.48  114
 25  \w   -120.00 -86.00   0.50    0.05    --  -74.00 -60.00 -15.89   68
 26  \w    -39.00  -3.00   0.50    0.05    --  -22.00 109.00  51.66   72
 27  \w   -120.00 -86.00   0.50    0.05    --  -74.00 -60.00 -50.35   68
 28  \w   -120.00 -86.00   0.50    0.05    --  -74.00 -59.00 -77.75   68
 29  \w   -120.00 -86.00   0.50    0.05    --  -74.00 -59.00-107.20   68
 30  \w   -120.00 -86.00   0.50    0.05    --  -74.00 -60.00   1.29   68
 31  \w    -86.00 -51.00   0.50    0.05    --  -38.00 -52.00-160.45   70
 32  \w   -121.00 -86.00   0.50    0.05    --  -74.00 -58.00  75.64   70
 33  \w    -95.00 -60.00   0.50    0.05    --  -46.00 -49.00 -39.64   70
 34  \w   -121.00 -86.00   0.50    0.05    --  -74.00 -55.00-130.79   70
 35  \w     44.00 126.00   0.50    0.05    --   76.32  14.00  23.00  164
 36  \w     48.00 121.00   0.50    0.05    --   84.34  15.00 -60.00  146
 37  \w   -107.00 -72.00   0.50    0.05    --  -58.00 -49.00 111.32   70
 38  \w   -126.00 -40.00   0.50    0.05    --  -76.37 -14.00-147.00  172
 39  \w     42.00  92.00   0.50    0.05    --   84.34 -95.00 120.00  100
 40  \w   -123.00 -87.00   0.50    0.05    --  -74.00 -46.00 108.13   72
 41  \w   -130.00 -92.00   0.50    0.05    --  -79.50 -42.00-164.42   76
 42  \w   -127.00 -92.00   0.50    0.05    --  -79.50 -53.00 -41.89   70
 43  \w   -122.00 -87.00   0.50    0.05    --  -74.00 -54.00 -98.76   70
 44  \w    -97.00 -22.00   0.50    0.05    --  -69.54 126.00-180.00  150
 45  \w    -92.00 -31.00   0.50    0.05    --  -76.37 112.00-150.00  122
 46  \w   -130.00 -92.00   0.50    0.05    --  -79.50 -42.00-151.94   76
 47  \w   -122.00 -87.00   0.50    0.05    --  -74.00 -54.00  34.89   70
 48  \w   -126.00 -86.00   0.50    0.05    --  -79.50-135.00  41.60   80
 49  \w   -115.00 -80.00   0.50    0.05    --  -66.00 -47.00-177.86   70
 50  \w    -92.00 -31.00   0.50    0.05    --  -76.37 112.00 150.00  122
 51  \w     42.00  92.00   0.50    0.05    --   84.34 -95.00-120.00  100
 52  \w     42.00  92.00   0.50    0.05    --   84.34 -95.00 -90.00  100
 53  \w     42.00  92.00   0.50    0.05    --   84.34 -95.00-150.00  100
 54  \w     42.00  92.00   0.50    0.05    --   84.34 -95.00  90.00  100
 55  \w   -110.00 -37.00   0.50    0.05    --  -60.16 -14.00-147.00  146
 56  \w   -128.00 -93.00   0.50    0.05    --  -79.50 -51.00-177.66   70
 57  \w    -92.00 -31.00   0.50    0.05    --  -76.37 112.00   0.00  122
 58  \w   -119.00 -37.00   0.50    0.05    --  -69.54 -14.00-147.00  164
 59  \w     42.00  92.00   0.50    0.05    --   84.34 -95.00  30.00  100
 60  \w    -97.00 -22.00   0.50    0.05    --  -69.54 126.00 -60.00  150
 61  \w     52.00  87.00   0.50    0.05    --   38.00  51.00 -33.79   70
 62  \w     39.00  93.00   0.50    0.05    --   84.34-112.00  30.00  108
 63  \w     42.00  92.00   0.50    0.05    --   84.34 -95.00  60.00  100
 64  \w     30.00  60.00   0.50    0.05    --   18.00  59.00 100.12   60
 65  \w     34.00  60.00   0.50    0.05    --   22.00  59.00  55.58   52
 66  \w    -92.00 -31.00   0.50    0.05    --  -76.37 112.00  30.00  122
 67  \w   -120.00 -83.00   0.50    0.05    --  -70.00 -45.00  42.45   74
 68  \w    -92.00 -31.00   0.50    0.05    --  -76.37 112.00  90.00  122
 69  \w   -126.00 -93.00   0.50    0.05    --  -79.50-120.00 113.48   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
;
 CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      -0.1508518000
_diffrn_orient_matrix_UB_12      0.0643458000
_diffrn_orient_matrix_UB_13      -0.0097329000
_diffrn_orient_matrix_UB_21      -0.0202195000
_diffrn_orient_matrix_UB_22      -0.1206214000
_diffrn_orient_matrix_UB_23      0.0182161000
_diffrn_orient_matrix_UB_31      -0.0270479000
_diffrn_orient_matrix_UB_32      -0.0010461000
_diffrn_orient_matrix_UB_33      0.1136529000
_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  0.0413
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            43345
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.728
_diffrn_reflns_theta_min         3.314
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.41.112a (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            red
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_preparation
;
 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          0.210
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.260
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         6539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0836P)^2^+0.9088P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1604
_refine_ls_wR_factor_ref         0.1659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5583
_reflns_number_total             6539
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02923b2.cif
_cod_data_source_block           Compound6a
_cod_depositor_comments
'Adding full bibliography for 7133290--7133296.cif.'
_cod_database_code               7133294
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.903
_shelx_estimated_absorpt_t_max   0.952
_shelx_res_checksum              97436
_shelx_hkl_checksum              60146