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_7717901
_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_absolute_configuration unk
_chemical_formula_moiety         'C21 H38 B N3'
_chemical_formula_sum            'C21 H38 B N3'
_chemical_formula_weight         343.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-09-03
_audit_creation_method           'CIF-fill 1.5e (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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5782(5)
_cell_length_b                   13.3262(4)
_cell_length_c                   8.4378(2)
_cell_measurement_reflns_used    8974
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.9900
_cell_measurement_theta_min      4.0850
_cell_volume                     2089.00(10)
_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 1.000
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w    -65.00 -33.00   0.50    0.43    --  -69.75 126.00 150.00   64
  2  \w    -94.00 -53.00   0.50    0.43    --  -69.75 126.00  30.00   82
  3  \w    -63.00 -27.00   0.50    0.43    --  -69.75 126.00 -30.00   72
  4  \w    -99.00 -41.00   0.50    0.43    --  -78.50 121.00   0.78  116
  5  \w    -60.00 -35.00   0.50    0.43    --  -78.50 122.00  42.67   50
  6  \w    -97.00 -68.00   0.50    0.43    --  -78.50 120.00 146.19   58
  7  \w    -61.00 -36.00   0.50    0.43    --  -78.50 119.00 176.83   50
  8  \w    -97.00 -71.00   0.50    0.43    --  -78.50 119.00 176.83   52
  9  \w    -66.00 -31.00   0.50    0.43    --  -69.75 126.00 -90.00   70
 10  \w   -100.00 -74.00   0.50    0.43    --  -78.50 125.00-162.30   52
 11  \w    -93.00 -62.00   0.50    0.43    --  -69.75 126.00-120.00   62
 12  \w    -95.00 -43.00   0.50    0.43    --  -78.50 114.00-132.63  104
 13  \w    -96.00 -49.00   0.50    0.43    --  -78.50 116.00 -94.13   94
 14  \w    -88.00 -34.00   0.50    0.43    --  -75.18 112.00-180.00  108
 15  \w    -97.00 -42.00   0.50    0.43    --  -78.50 119.00 -70.62  110
 16  \w    -96.00 -55.00   0.50    0.43    --  -78.50 116.00  55.32   82
 17  \w    -62.00 -37.00   0.50    0.43    --  -75.18 112.00  90.00   50
 18  \w    -66.00 -40.00   0.50    0.43    --  -78.50 116.00 121.88   52
 19  \w    -62.00 -37.00   0.50    0.43    --  -75.18 112.00 150.00   50
 20  \w   -107.00 -31.00   0.50    0.43    --  -60.27 -15.00  30.00  152
 21  \w   -117.00 -56.00   0.50    0.43    --  -69.75 -15.00 120.00  122
 22  \w    -96.00 -36.00   0.50    0.43    --  -60.27 -15.00 120.00  120
 23  \w   -103.00 -37.00   0.50    0.43    --  -69.75 -15.00   0.00  132
 24  \w    -65.00 -32.00   0.50    0.43    --  -60.27 -15.00-120.00   66
 25  \w   -103.00 -71.00   0.50    0.43    --  -60.27 -15.00-120.00   64
 26  \w    -99.00 -73.00   0.50    0.43    --  -69.75 -15.00-150.00   52
 27  \w   -111.00 -64.00   0.50    0.43    --  -75.18 -15.00-180.00   94
 28  \w   -111.00 -82.00   0.50    0.43    --  -75.18 -15.00-120.00   58
 29  \w   -122.00 -47.00   0.50    0.43    --  -75.18 -15.00 -30.00  150
 30  \w   -120.00 -52.00   0.50    0.43    --  -75.18 -15.00  90.00  136
 31  \w     62.00 101.00   0.50    0.43    --   76.88  15.00  30.00   78
 32  \w     50.00  98.00   0.50    0.43    --   80.80-117.00 167.61   96
 33  \w     43.00  97.00   0.50    0.43    --   80.80-116.00  35.42  108
 34  \w     23.00  58.00   0.50    0.43    --   58.93-126.00 -30.00   70
;
_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      0.0162339000
_diffrn_orient_matrix_UB_12      0.1102265000
_diffrn_orient_matrix_UB_13      -0.0422106000
_diffrn_orient_matrix_UB_21      -0.0498080000
_diffrn_orient_matrix_UB_22      -0.0080002000
_diffrn_orient_matrix_UB_23      -0.1451567000
_diffrn_orient_matrix_UB_31      -0.0643273000
_diffrn_orient_matrix_UB_32      0.0340092000
_diffrn_orient_matrix_UB_33      0.1021659000
_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  0.0366
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            24160
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.263
_diffrn_reflns_theta_min         4.083
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.756
_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    1.092
_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          0.210
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.118
_refine_diff_density_min         -0.158
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details
;
 Flack x determined using 1460 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, 
 Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3968
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0434P)^2^+0.2225P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0817
_reflns_Friedel_coverage         0.808
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.908
_reflns_number_gt                3659
_reflns_number_total             3968
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00069f2.cif
_cod_data_source_block           5a
_cod_depositor_comments
'Adding full bibliography for 7717899--7717905.cif.'
_cod_database_code               7717901
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.907
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              32648