N–H / P–H bond activation of ammonia, amines and phosphines at a transient borylene
Weber, Marco; Kar, Sourav; Joos, Pia; Dewhurst, Rian David; Braunschweig, Holger; Chemical Science  (2026) –; doi:10.1039/D6SC00526H

data_1576631
_publ_section_title
;
 N-H/P-H bond activation of ammonia, amines and phosphines at a transient
 borylene.
;
_journal_issue                   16
_journal_name_full               'Chemical science'
_journal_page_first              8189
_journal_page_last               8196
_journal_paper_doi               10.1039/d6sc00526h
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         'C62 H98 B2 N4'
_chemical_formula_sum            'C62 H98 B2 N4'
_chemical_formula_weight         921.06
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-05-29
_audit_creation_method           'CIF-fill 1.5c (K.Radacki, 2005-23)'
_audit_update_record
;
2026-01-07 deposited with the CCDC.	2026-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.3730(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.18720(10)
_cell_length_b                   38.0186(3)
_cell_length_c                   16.41330(10)
_cell_measurement_reflns_used    33001
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.6860
_cell_measurement_theta_min      2.9430
_cell_volume                     5697.48(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 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 0.993
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     39.00  64.00   0.50    0.73    --   73.62-126.00  14.00   50
  2  \w     25.00  85.00   0.50    0.73    --   60.18-126.00  14.00  120
  3  \w     40.00  70.00   0.50    0.73    --   80.28 -95.00 120.00   60
  4  \w     76.00 101.00   0.50    0.73    --   80.28-126.00  14.00   50
  5  \w     39.00  65.00   0.50    0.73    --   80.28-126.00  14.00   52
  6  \w     46.00  90.00   0.50    0.73    --   83.50 -97.00-113.84   88
  7  \w     37.00  63.00   0.50    0.73    --   80.28-112.00-120.00   52
  8  \w     54.00 128.00   0.50    0.73    --   80.28  15.00 -30.00  148
  9  \w     58.00  83.00   0.50    0.73    --   42.00  52.00 111.80   50
 10  \w    -52.00 -24.00   0.50    0.73    --  -61.62 126.00  90.00   56
 11  \w    -91.00 -65.00   0.50    0.73    --  -71.68 126.00  90.00   52
 12  \w    -89.00 -64.00   0.50    0.73    --  -76.32 126.00  90.00   50
 13  \w    -60.00 -35.00   0.50    0.73    --  -79.50 119.00 159.88   50
 14  \w    -62.00 -32.00   0.50    0.73    --  -71.68 126.00  90.00   60
 15  \w    -96.00 -70.00   0.50    0.73    --  -79.50 119.00 159.88   52
 16  \w    -97.00 -36.00   0.50    0.73    --  -79.50 117.00  93.96  122
 17  \w    -84.00 -36.00   0.50    0.73    --  -79.50 125.00  53.35   96
 18  \w    -97.00 -71.00   0.50    0.73    --  -79.50 114.00  78.29   52
 19  \w    -97.00 -67.00   0.50    0.73    --  -79.50 115.00  27.18   60
 20  \w    -97.00 -43.00   0.50    0.73    --  -79.50 114.00   2.27  108
 21  \w    -76.00 -50.00   0.50    0.73    --  -79.50 114.00 -20.72   52
 22  \w    -71.00 -45.00   0.50    0.73    --  -79.50 121.00 -52.49   52
 23  \w    -97.00 -36.00   0.50    0.73    --  -79.50 114.00 -63.18  122
 24  \w    -98.00 -72.00   0.50    0.73    --  -79.50 121.00 -52.49   52
 25  \w    -97.00 -66.00   0.50    0.73    --  -79.50 114.00 -24.76   62
 26  \w    -89.00 -38.00   0.50    0.73    --  -79.50 102.00 -18.77  102
 27  \w   -115.00 -86.00   0.50    0.73    --  -70.00 -56.00 -49.00   58
 28  \w   -113.00 -82.00   0.50    0.73    --  -66.00 -48.00  -0.86   62
 29  \w   -102.00 -73.00   0.50    0.73    --  -58.00 -52.00  27.29   58
 30  \w   -127.00 -97.00   0.50    0.73    --  -79.50 -47.00 102.77   60
 31  \w    -99.00 -73.00   0.50    0.73    --  -58.00 -52.00  93.25   52
 32  \w   -108.00 -80.00   0.50    0.73    --  -62.00 -47.00  66.30   56
 33  \w   -100.00 -70.00   0.50    0.73    --  -54.00 -42.00-165.90   60
 34  \w   -126.00 -94.00   0.50    0.73    --  -79.50 -42.00-149.03   64
 35  \w   -123.00 -98.00   0.50    0.73    --  -79.50 -40.00-171.63   50
 36  \w   -120.00 -92.00   0.50    0.73    --  -79.50-123.00-157.91   56
 37  \w   -124.00 -97.00   0.50    0.73    --  -79.50-126.00 148.11   54
;
_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      0.0933382000
_diffrn_orient_matrix_UB_12      0.0250401000
_diffrn_orient_matrix_UB_13      -0.0466341000
_diffrn_orient_matrix_UB_21      -0.0622512000
_diffrn_orient_matrix_UB_22      0.0317251000
_diffrn_orient_matrix_UB_23      0.0431433000
_diffrn_orient_matrix_UB_31      0.1260149000
_diffrn_orient_matrix_UB_32      -0.0028644000
_diffrn_orient_matrix_UB_33      0.0699009000
_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  0.0419
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            59721
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.098
_diffrn_reflns_theta_min         2.948
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.450
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72091
_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    1.074
_exptl_crystal_description       plate
_exptl_crystal_F_000             2032
_exptl_crystal_preparation
;
 Crystals were grown at -30 \%C from saturated solution in pentane. 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          0.630
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1272
_refine_ls_number_reflns         11282
_refine_ls_number_restraints     2934
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0676P)^2^+1.2890P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1268
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10123
_reflns_number_total             11282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6sc00526h2.cif
_cod_data_source_block           MaWe096_a
_cod_depositor_comments
'Adding full bibliography for 1576631--1576636.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1576631
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.765
_shelx_estimated_absorpt_t_max   0.923
_shelx_res_checksum              52662