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_7133295
_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      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             2023-05-08
_audit_creation_method           'CIF-fill 1.4d (K.Radacki, 2005-23)'
_audit_update_record
;
2024-06-13 deposited with the CCDC.	2024-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.619(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6634(2)
_cell_length_b                   19.2539(2)
_cell_length_c                   18.6478(3)
_cell_measurement_reflns_used    13898
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.9120
_cell_measurement_theta_min      3.3330
_cell_volume                     3372.02(10)
_computing_cell_refinement       'CrysAlisPro 1.171.43.63a (Rigaku OD, 2023)'
_computing_data_collection
;
 CrysAlisPro system (CCD 42.72a 64-bit (release 07-10-2022))
;
_computing_data_reduction        'CrysAlisPro 1.171.43.63a (Rigaku OD, 2023)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     52.00 135.00   0.50    0.22    --   85.03  15.00-150.00  166
  2  \w     49.00 130.00   0.50    0.22    --   85.03  15.00 -60.00  162
  3  \w     87.00 128.00   0.50    0.22    --   85.03  15.00  60.00   82
  4  \w     65.00 118.00   0.50    0.22    --   85.03  15.00 150.00  106
  5  \w     17.00  55.00   0.50    0.22    --   58.77 -95.00 150.00   76
  6  \w     17.00  45.00   0.50    0.22    --   58.77 -95.00  60.00   56
  7  \w     44.00  69.00   0.50    0.22    --   85.03-112.00   0.00   50
  8  \w     33.00  93.00   0.50    0.22    --   77.28-112.00 -60.00  120
  9  \w     29.00  56.00   0.50    0.22    --   58.77 -95.00 -90.00   54
 10  \w     51.00  93.00   0.50    0.22    --   77.28-112.00-180.00   84
 11  \w     36.00  66.00   0.50    0.22    --   77.28 -95.00-180.00   60
 12  \w     16.00  56.00   0.50    0.22    --   58.77 -95.00-150.00   80
 13  \w     45.00  92.00   0.50    0.22    --   85.03 -95.00 -60.00   94
 14  \w     58.00  92.00   0.50    0.22    --   85.03 -95.00-150.00   68
 15  \w     16.00  51.00   0.50    0.22    --   58.77 -95.00 -30.00   70
 16  \w     67.00  92.00   0.50    0.22    --   85.03 -95.00-120.00   50
 17  \w     53.00  92.00   0.50    0.22    --   85.03 -95.00   0.00   78
 18  \w     65.00  90.00   0.50    0.22    --   85.03 -95.00 -30.00   50
 19  \w     49.00  91.00   0.50    0.22    --   85.03 -95.00  60.00   84
 20  \w     45.00  92.00   0.50    0.22    --   85.03 -95.00  90.00   94
 21  \w     55.00  89.00   0.50    0.22    --   85.03 -95.00 120.00   68
 22  \w     67.00  92.00   0.50    0.22    --   85.03 -95.00 150.00   50
 23  \w     67.00  92.00   0.50    0.22    --   85.03 -95.00 -90.00   50
 24  \w    -73.00 -24.00   0.50    0.22    --  -69.97 126.00 -60.00   98
 25  \w    -97.00 -33.00   0.50    0.22    --  -79.50 116.00-176.66  128
 26  \w    -97.00 -35.00   0.50    0.22    --  -79.50 115.00  -4.17  124
 27  \w    -53.00 -23.00   0.50    0.22    --  -69.97 126.00  30.00   60
 28  \w    -76.00 -33.00   0.50    0.22    --  -76.33 112.00  60.00   86
 29  \w    -70.00 -34.00   0.50    0.22    --  -79.50 118.00 148.81   72
 30  \w   -106.00 -42.00   0.50    0.22    --  -76.33 -15.00 -30.00  128
 31  \w    -87.00 -36.00   0.50    0.22    --  -69.97 -15.00  90.00  102
 32  \w   -125.00 -49.00   0.50    0.22    --  -76.33 -15.00 -90.00  152
 33  \w   -127.00 -87.00   0.50    0.22    --  -76.33 -15.00-120.00   80
 34  \w   -110.00 -71.00   0.50    0.22    --  -60.22 -15.00-180.00   78
;
_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      0.1234225000
_diffrn_orient_matrix_UB_12      -0.0414888000
_diffrn_orient_matrix_UB_13      -0.0184915000
_diffrn_orient_matrix_UB_21      -0.0288346000
_diffrn_orient_matrix_UB_22      0.0348489000
_diffrn_orient_matrix_UB_23      -0.0764600000
_diffrn_orient_matrix_UB_31      0.1040646000
_diffrn_orient_matrix_UB_32      0.0588665000
_diffrn_orient_matrix_UB_33      0.0322747000
_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  0.0346
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.129
_diffrn_reflns_theta_min         3.349
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.43.63a (Rigaku Oxford Diffraction, 2023) 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    1.154
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_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          0.120
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         6826
_refine_ls_number_restraints     480
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0611
_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^)+(0.0926P)^2^+1.8549P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1650
_refine_ls_wR_factor_ref         0.1752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5467
_reflns_number_total             6826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02923b2.cif
_cod_data_source_block           Compound6b
_cod_depositor_comments
'Adding full bibliography for 7133290--7133296.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7133295
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.897
_shelx_estimated_absorpt_t_max   0.969
_shelx_res_checksum              50405
_shelx_hkl_checksum              8699