Synthesis of base-free boriranes and their conversion to borirenes using strong reductant.
Dotzauer, Simon; Kar, Sourav; Swoboda, Theresa; Weidemann, Christoph; Häfner, Andreas; Dewhurst, Rian D.; Braunschweig, Holger; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3857–3862; doi:10.1039/d5dt00069f

data_7717900
_publ_section_title
;
 Synthesis of base-free boriranes and their conversion to borirenes using
 strong reductant.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3857
_journal_page_last               3862
_journal_paper_doi               10.1039/d5dt00069f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C21 H38 B N3'
_chemical_formula_sum            'C21 H38 B N3'
_chemical_formula_weight         343.35
_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             2024-08-19
_audit_creation_method           'CIF-fill 1.5d (K.Radacki, 2005-23)'
_audit_update_record
;
2024-10-29 deposited with the CCDC.	2025-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.649(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2086(3)
_cell_length_b                   11.1581(2)
_cell_length_c                   16.0725(3)
_cell_measurement_reflns_used    14225
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.3000
_cell_measurement_theta_min      4.0560
_cell_volume                     2108.31(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.111a (Rigaku OD, 2024)'
_computing_data_collection
;
 CrysAlisPro system (CCD 43.128a 64-bit (release 20-06-2024))
;
_computing_data_reduction        'CrysAlisPro 1.171.43.111a (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 0.998
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     57.00 123.00   0.50    0.14    --   76.88  15.00-120.00  132
  2  \w     62.00 105.00   0.50    0.14    --   76.88  15.00 -60.00   86
  3  \w     44.00 107.00   0.50    0.14    --   76.88  15.00   0.00  126
  4  \w     51.00  97.00   0.50    0.14    --   80.80-121.00 173.92   92
  5  \w     49.00  99.00   0.50    0.14    --   80.80-122.00 125.64  100
  6  \w     48.00  91.00   0.50    0.14    --   80.80-105.00  38.28   86
  7  \w     67.00  97.00   0.50    0.14    --   80.80-116.00 -84.83   60
  8  \w    -61.00 -35.00   0.50    0.14    --  -60.27 -15.00  30.00   52
  9  \w   -105.00 -38.00   0.50    0.14    --  -60.27 -15.00 -30.00  134
 10  \w   -103.00 -54.00   0.50    0.14    --  -69.75 -15.00 -90.00   98
 11  \w   -100.00 -48.00   0.50    0.14    --  -60.27 -15.00-150.00  104
 12  \w    -74.00 -48.00   0.50    0.14    --  -75.18 -15.00 -30.00   52
 13  \w   -121.00 -77.00   0.50    0.14    --  -75.18 -15.00 -30.00   88
 14  \w   -102.00 -74.00   0.50    0.14    --  -60.27 -15.00  30.00   56
 15  \w   -119.00 -44.00   0.50    0.14    --  -75.18 -15.00  60.00  150
 16  \w   -105.00 -50.00   0.50    0.14    --  -60.27 -15.00 120.00  110
 17  \w    -89.00 -43.00   0.50    0.14    --  -75.18 112.00 150.00   92
 18  \w    -61.00 -23.00   0.50    0.14    --  -60.27 126.00  90.00   76
 19  \w    -51.00 -26.00   0.50    0.14    --  -69.75 126.00  30.00   50
 20  \w    -66.00 -40.00   0.50    0.14    --  -78.50 122.00 -46.94   52
 21  \w    -56.00 -27.00   0.50    0.14    --  -69.75 126.00 -60.00   58
 22  \w    -67.00 -26.00   0.50    0.14    --  -69.75 126.00-180.00   82
 23  \w   -100.00 -46.00   0.50    0.14    --  -78.50 126.00-125.86  108
 24  \w    -97.00 -53.00   0.50    0.14    --  -78.50 118.00 -61.51   88
 25  \w    -91.00 -65.00   0.50    0.14    --  -69.75 126.00 -60.00   52
 26  \w    -74.00 -37.00   0.50    0.14    --  -75.18 112.00-150.00   74
 27  \w    -99.00 -40.00   0.50    0.14    --  -78.50 121.00  12.52  118
 28  \w    -67.00 -41.00   0.50    0.14    --  -75.18 112.00   0.00   52
 29  \w    -67.00 -34.00   0.50    0.14    --  -75.18 112.00 -90.00   66
 30  \w    -63.00 -36.00   0.50    0.14    --  -75.18 112.00  60.00   54
 31  \w    -96.00 -49.00   0.50    0.14    --  -78.50 116.00 130.06   94
 32  \w    -98.00 -41.00   0.50    0.14    --  -78.50 121.00 150.66  114
;
_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      0.0786276000
_diffrn_orient_matrix_UB_12      -0.0771121000
_diffrn_orient_matrix_UB_13      0.0710793000
_diffrn_orient_matrix_UB_21      -0.0725547000
_diffrn_orient_matrix_UB_22      -0.1113795000
_diffrn_orient_matrix_UB_23      -0.0346356000
_diffrn_orient_matrix_UB_31      0.0755815000
_diffrn_orient_matrix_UB_32      -0.0267475000
_diffrn_orient_matrix_UB_33      -0.0605404000
_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  0.0290
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23808
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.285
_diffrn_reflns_theta_min         4.063
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.43.111a (Rigaku Oxford Diffraction, 2024) 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            colourless
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_description       plate
_exptl_crystal_F_000             760
_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          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0510P)^2^+0.6916P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3457
_reflns_number_total             4080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00069f2.cif
_cod_data_source_block           4a
_cod_depositor_comments
'Adding full bibliography for 7717899--7717905.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7717900
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.942
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              19438