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_7133291
_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         'C36 H56 B N5 O'
_chemical_formula_sum            'C36 H56 B N5 O'
_chemical_formula_weight         585.66
_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             2022-08-11
_audit_creation_method           'CIF-fill 1.3i (K.Radacki, 2005-22)'
_audit_update_record
;
2024-06-13 deposited with the CCDC.	2024-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                80.9440(10)
_cell_angle_beta                 74.9360(10)
_cell_angle_gamma                71.0580(10)
_cell_formula_units_Z            2
_cell_length_a                   10.16230(10)
_cell_length_b                   10.46690(10)
_cell_length_c                   17.7919(3)
_cell_measurement_reflns_used    24350
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.8460
_cell_measurement_theta_min      4.4620
_cell_volume                     1722.96(4)
_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 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 Arc150'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     83.00 136.00   0.50    0.10    --   85.25  20.00-112.02  106
  2  \w     87.00 137.00   0.50    0.10    --   85.25  23.00 -30.00  100
  3  \w     78.00 137.00   0.50    0.10    --   85.25  22.00   7.77  118
  4  \w    101.00 130.00   0.50    0.10    --   85.25  59.00  21.92   58
  5  \w     96.00 122.00   0.50    0.10    --   82.31  15.00 150.00   52
  6  \w     97.00 122.00   0.50    0.10    --   85.25  41.00 179.60   50
  7  \w     52.00  95.00   0.50    0.10    --   82.31  15.00 150.00   86
  8  \w     57.00 107.00   0.50    0.10    --   82.31  15.00  90.00  100
  9  \w     98.00 130.00   0.50    0.10    --   82.31  15.00 -90.00   64
 10  \w     87.00 132.00   0.50    0.10    --   82.31  15.00-150.00   90
 11  \w   -130.00 -92.00   0.50    0.10    --  -79.50 -41.00-173.79   76
 12  \w   -108.00 -75.00   0.50    0.10    --  -62.00 -52.00-112.66   66
 13  \w   -115.00 -86.00   0.50    0.10    --  -70.00 -53.00 -60.54   58
 14  \w   -122.00 -95.00   0.50    0.10    --  -79.50 -50.00-119.79   54
 15  \w   -121.00 -95.00   0.50    0.10    --  -79.50 -64.00 -29.51   52
 16  \w   -107.00 -82.00   0.50    0.10    --  -58.00 -49.00-147.70   50
 17  \w   -126.00 -95.00   0.50    0.10    --  -79.50 -49.00 -72.56   62
 18  \w   -118.00 -89.00   0.50    0.10    --  -70.00 -44.00  13.37   58
 19  \w   -101.00 -69.00   0.50    0.10    --  -54.00 -43.00  59.52   64
 20  \w   -117.00 -85.00   0.50    0.10    --  -70.00 -52.00 130.00   64
 21  \w   -122.00 -95.00   0.50    0.10    --  -79.50 -65.00 170.07   54
 22  \w    -93.00 -59.00   0.50    0.10    --  -46.00 -51.00 170.74   68
 23  \w    -88.00 -51.00   0.50    0.10    --  -79.50  99.00 127.15   74
 24  \w    -84.00 -11.00   0.50    0.10    --  -60.19 116.00 -57.00  146
 25  \w    -93.00 -21.00   0.50    0.10    --  -69.72 116.00 -57.00  144
 26  \w    -97.00 -31.00   0.50    0.10    --  -76.37 116.00 -57.00  132
 27  \w    -88.00 -45.00   0.50    0.10    --  -76.37 112.00-120.00   86
 28  \w   -128.00 -99.00   0.50    0.10    --  -79.50-120.00 -87.16   58
 29  \w     38.00  88.00   0.50    0.10    --   85.25-129.00 -37.13  100
 30  \w     38.00  97.00   0.50    0.10    --   85.25-131.00 -11.99  118
 31  \w     73.00  99.00   0.50    0.10    --   85.25-126.00 -49.80   52
 32  \w     37.00  69.00   0.50    0.10    --   85.25-126.00 -49.80   64
 33  \w     37.00  62.00   0.50    0.10    --   85.25-124.00-159.20   50
 34  \w     47.00  74.00   0.50    0.10    --   85.25-128.00-152.62   54
 35  \w     72.00 101.00   0.50    0.10    --   85.25-124.00-159.20   58
 36  \w     23.00  95.00   0.50    0.10    --   71.30-116.00-145.00  144
 37  \w     41.00  66.00   0.50    0.10    --   82.31-116.00-145.00   50
 38  \w     14.00  82.00   0.50    0.10    --   58.61-116.00-145.00  136
 39  \w     48.00  93.00   0.50    0.10    --   82.31-112.00-120.00   90
 40  \w     72.00  97.00   0.50    0.10    --   82.31-112.00 -90.00   50
 41  \w     44.00  85.00   0.50    0.10    --   85.25-122.00  -4.21   82
 42  \w     71.00  97.00   0.50    0.10    --   82.31-112.00   0.00   52
 43  \w     72.00  97.00   0.50    0.10    --   82.31-112.00  60.00   50
 44  \w     38.00  66.00   0.50    0.10    --   85.25-121.00 117.10   56
 45  \w     39.00  94.00   0.50    0.10    --   85.25-121.00 139.11  110
 46  \w     48.00  97.00   0.50    0.10    --   82.31-112.00 120.00   98
 47  \w     72.00  97.00   0.50    0.10    --   82.31-112.00 150.00   50
 48  \w     34.00  68.00   0.50    0.10    --   82.31-112.00  60.00   68
 49  \w     40.00  68.00   0.50    0.10    --   82.31-112.00 150.00   56
 50  \w     41.00  95.00   0.50    0.10    --   85.25-107.00  75.39  108
 51  \w     41.00  75.00   0.50    0.10    --   85.25-102.00  90.37   68
 52  \w     50.00  76.00   0.50    0.10    --   82.31-112.00  30.00   52
 53  \w     61.00  97.00   0.50    0.10    --   82.31-112.00 -30.00   72
 54  \w     41.00  92.00   0.50    0.10    --   85.25-101.00   5.74  102
 55  \w     40.00  66.00   0.50    0.10    --   82.31 -95.00  30.00   52
 56  \w     43.00  95.00   0.50    0.10    --   85.25-104.00-106.61  104
 57  \w     72.00  97.00   0.50    0.10    --   82.31-112.00-150.00   50
 58  \w     68.00  93.00   0.50    0.10    --   85.25 -98.00-167.85   50
 59  \w     40.00  65.00   0.50    0.10    --   82.31 -95.00-150.00   50
 60  \w     40.00  65.00   0.50    0.10    --   82.31 -95.00 -90.00   50
 61  \w     31.00  72.00   0.50    0.10    --   71.30 -95.00  60.00   82
 62  \w     43.00  80.00   0.50    0.10    --   82.31 -95.00 150.00   74
 63  \w     46.00  84.00   0.50    0.10    --   85.25 -82.00 145.57   76
 64  \w     48.00  74.00   0.50    0.10    --   85.25 -78.00 -52.35   52
 65  \w    107.00 133.00   0.50    0.10    --   85.25 124.00-102.01   52
 66  \w     93.00 123.00   0.50    0.10    --   85.25 136.00-142.51   60
;
_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      -0.1318293000
_diffrn_orient_matrix_UB_12      -0.0511726000
_diffrn_orient_matrix_UB_13      0.0179303000
_diffrn_orient_matrix_UB_21      0.0055270000
_diffrn_orient_matrix_UB_22      -0.0265676000
_diffrn_orient_matrix_UB_23      0.0869503000
_diffrn_orient_matrix_UB_31      -0.0981342000
_diffrn_orient_matrix_UB_32      0.1450726000
_diffrn_orient_matrix_UB_33      0.0145078000
_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  0.0662
_diffrn_reflns_av_unetI/netI     0.0086
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13828
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.073
_diffrn_reflns_theta_min         2.580
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57179
_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            orange
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_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          0.378
_exptl_crystal_size_mid          0.247
_exptl_crystal_size_min          0.149
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         13828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0665
_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^)+(0.1295P)^2^+0.2646P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2020
_refine_ls_wR_factor_ref         0.2075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12140
_reflns_number_total             13828
_reflns_threshold_expression     'I > 2\s(I)'
_twin_dimensionality             triperiodic
_twin_formation_mechanism        gt
_twin_morphology                 polysynthetic
_cod_data_source_file            d4cc02923b2.cif
_cod_data_source_block           Compound7b
_cod_depositor_comments
'Adding full bibliography for 7133290--7133296.cif.'
_cod_database_code               7133291
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              36657
_shelx_hkl_checksum              22505