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_7717903
_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         'C19 H34 B N3 O2'
_chemical_formula_sum            'C19 H34 B N3 O2'
_chemical_formula_weight         347.30
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-03-27
_audit_creation_method           'CIF-fill 1.4t (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                   6.38220(10)
_cell_length_b                   8.04120(10)
_cell_length_c                   39.2727(6)
_cell_measurement_reflns_used    12929
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.2800
_cell_measurement_theta_min      4.4590
_cell_volume                     2015.50(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.111a (Rigaku OD, 2024)'
_computing_data_collection
;
 CrysAlisPro system (CCD 43.112a 64-bit (release 01-03-2024))
;
_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 0.988
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w    -92.00 -65.00   0.25    0.13    --  -76.38 112.00-120.00  108
  2  \w    -62.00 -33.00   0.25    0.13    --  -76.38 112.00-120.00  116
  3  \w    -85.00 -50.00   0.25    0.13    --  -76.38 -15.00  60.00  140
  4  \w   -127.00-100.00   0.25    0.13    --  -76.38 -15.00  60.00  108
  5  \w   -109.00 -32.00   0.25    0.13    --  -60.28 -15.00 120.00  308
  6  \w     46.00 125.00   0.25    0.13    --   76.43  15.00   0.00  316
  7  \w     71.00 135.00   0.25    0.13    --   84.40  15.00 -60.00  256
  8  \w     50.00 131.00   0.25    0.13    --   84.40  15.00-120.00  324
  9  \w    103.00 128.00   0.25    0.13    --   84.40  15.00   0.00  100
 10  \w     48.00 127.00   0.25    0.13    --   84.40  15.00 150.00  316
 11  \w     40.00 113.00   0.25    0.13    --   76.43  15.00  90.00  292
 12  \w     65.00  90.00   0.25    0.13    --   84.40 -95.00 -60.00  100
 13  \w     42.00  93.00   0.25    0.13    --   76.43-112.00-150.00  204
 14  \w     46.00  72.00   0.25    0.13    --   58.64-126.00 -90.00  104
 15  \w     21.00  46.00   0.25    0.13    --   58.64-126.00 -60.00  100
 16  \w     25.00  59.00   0.25    0.13    --   58.64-126.00  60.00  136
 17  \w     47.00  93.00   0.25    0.13    --   76.43-112.00  60.00  184
 18  \w     26.00  52.00   0.25    0.13    --   58.64-126.00  90.00  104
 19  \w     16.00  49.00   0.25    0.13    --   58.64 -95.00 120.00  132
 20  \w     30.00  56.00   0.25    0.13    --   58.64 -95.00  60.00  104
 21  \w     19.00  45.00   0.25    0.13    --   58.64 -95.00   0.00  104
 22  \w     16.00  42.00   0.25    0.13    --   58.64 -95.00 -30.00  104
 23  \w     22.00  48.00   0.25    0.13    --   58.64 -95.00-180.00  104
 24  \w     19.00  48.00   0.25    0.13    --   58.64 -95.00 -90.00  116
 25  \w     67.00  92.00   0.25    0.13    --   84.40 -95.00-180.00  100
 26  \w     41.00  75.00   0.25    0.13    --   76.43 -95.00 -30.00  136
 27  \w     66.00  92.00   0.25    0.13    --   84.40 -95.00 -90.00  104
 28  \w     65.00  91.00   0.25    0.13    --   84.40 -95.00 -30.00  104
 29  \w     55.00  91.00   0.25    0.13    --   84.40 -95.00  60.00  144
 30  \w     38.00  82.00   0.25    0.13    --   76.43 -95.00  90.00  176
 31  \w     34.00  69.00   0.25    0.13    --   76.43 -95.00 150.00  140
 32  \w     42.00  92.00   0.25    0.13    --   84.40 -95.00 120.00  200
 33  \w     67.00  92.00   0.25    0.13    --   84.40 -95.00  90.00  100
 34  \w     51.00  92.00   0.25    0.13    --   84.40 -95.00   0.00  164
 35  \w     43.00  92.00   0.25    0.13    --   84.40 -95.00-120.00  196
 36  \w     43.00  90.00   0.25    0.13    --   84.40 -95.00-150.00  188
;
_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      -0.1756257000
_diffrn_orient_matrix_UB_12      0.1073202000
_diffrn_orient_matrix_UB_13      -0.0154951000
_diffrn_orient_matrix_UB_21      -0.1350248000
_diffrn_orient_matrix_UB_22      -0.0290633000
_diffrn_orient_matrix_UB_23      0.0319729000
_diffrn_orient_matrix_UB_31      0.0956896000
_diffrn_orient_matrix_UB_32      0.1560273000
_diffrn_orient_matrix_UB_33      0.0166508000
_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  0.0446
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            24242
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.891
_diffrn_reflns_theta_min         4.503
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.805
_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    1.145
_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          0.190
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.185
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 'Refined as an inversion twin.'
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0528P)^2^+0.1260P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0931
_reflns_Friedel_coverage         0.647
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.910
_reflns_number_gt                3504
_reflns_number_total             3934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00069f2.cif
_cod_data_source_block           4b
_cod_depositor_comments
'Adding full bibliography for 7717899--7717905.cif.'
_cod_database_code               7717903
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.899
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              38781