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_1576635
_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         'C35 H55 B N2, C30 H44 B Cl N'
_chemical_formula_sum            'C65 H99 B2 Cl N3'
_chemical_formula_weight         979.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-07-04
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.7397(2)
_cell_length_b                   19.4055(2)
_cell_length_c                   34.7313(4)
_cell_measurement_reflns_used    28864
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.0180
_cell_measurement_theta_min      3.3330
_cell_volume                     11956.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.128a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.128a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.128a (Rigaku OD, 2024)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     64.00  91.00   0.50    2.31    --   75.05-125.00  60.00   54
  2  \w     34.00  61.00   0.50    2.31    --   75.05-125.00  60.00   54
  3  \w     39.00  69.00   0.50    2.31    --   60.09-125.00  30.00   60
  4  \w     44.00  79.00   0.50    2.31    --   73.60-125.00-150.00   70
  5  \w   -120.00 -61.00   0.50    2.31    --  -75.12 -15.00-180.00  118
  6  \w   -111.00 -70.00   0.50    2.31    --  -75.12 -15.00-120.00   82
  7  \w    -59.00 -29.00   0.50    2.31    --  -61.72 125.00-180.00   60
  8  \w    -92.00 -34.00   0.50    2.31    --  -71.97 125.00-150.00  116
  9  \w    -90.00 -62.00   0.50    2.31    --  -71.97 125.00 -60.00   56
 10  \w    -57.00 -32.00   0.50    2.31    --  -71.97 125.00 -60.00   50
 11  \w    -75.00 -21.00   0.50    2.31    --  -61.72 125.00  30.00  108
 12  \w    -71.00 -22.00   0.50    2.31    --  -61.72 125.00 120.00   98
 13  \w   -111.00 -59.00   0.50    2.31    --  -75.12 -15.00 120.00  104
;
_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      0.0612937000
_diffrn_orient_matrix_UB_12      0.0546973000
_diffrn_orient_matrix_UB_13      0.0075059000
_diffrn_orient_matrix_UB_21      0.0289956000
_diffrn_orient_matrix_UB_22      -0.0424154000
_diffrn_orient_matrix_UB_23      0.0344866000
_diffrn_orient_matrix_UB_31      0.0543485000
_diffrn_orient_matrix_UB_32      -0.0388949000
_diffrn_orient_matrix_UB_33      -0.0268396000
_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  0.0307
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            48828
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.329
_diffrn_reflns_theta_min         3.562
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.853
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.43.128a (Rigaku Oxford Diffraction, 2024) Empirical 
 absorption correction using spherical harmonics, implemented in SCALE3 
 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_description       block
_exptl_crystal_F_000             4296
_exptl_crystal_preparation
;
 Crystals were grown at 25 \%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          0.230
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         11358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0671P)^2^+6.4444P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1373
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10032
_reflns_number_total             11358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6sc00526h2.cif
_cod_data_source_block           MaWe103_MaWe_a
_cod_depositor_comments
'Adding full bibliography for 1576631--1576636.cif.'
_cod_database_code               1576635
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.828
_shelx_estimated_absorpt_t_max   0.920
_shelx_res_checksum              29157