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_7717899
_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         'C16 H34 B N3 O2 Si2'
_chemical_formula_sum            'C16 H34 B N3 O2 Si2'
_chemical_formula_weight         367.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-02-02
_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                91.745(3)
_cell_angle_beta                 91.755(2)
_cell_angle_gamma                94.665(3)
_cell_formula_units_Z            2
_cell_length_a                   6.2636(2)
_cell_length_b                   9.1707(3)
_cell_length_c                   18.6096(6)
_cell_measurement_reflns_used    5759
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.9490
_cell_measurement_theta_min      4.7340
_cell_volume                     1064.34(6)
_computing_cell_refinement       'CrysAlisPro 1.171.43.100a (Rigaku OD, 2023)'
_computing_data_collection
;
 CrysAlisPro system (CCD 43.104a 64-bit (release 22-12-2023))
;
_computing_data_reduction        'CrysAlisPro 1.171.43.100a (Rigaku OD, 2023)'
_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 0.990
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     17.00  54.00   0.50    0.18    --   58.73-105.00-160.00   74
  2  \w    -40.00 -15.00   0.50    0.18    --  -60.32 105.00 -60.00   50
  3  \w    -73.00 -47.00   0.50    0.18    --  -69.87 105.00 -60.00   52
  4  \w     32.00  57.00   0.50    0.18    --   71.45-105.00-160.00   50
  5  \w    -72.00 -31.00   0.50    0.18    --  -76.34 105.00 -60.00   82
  6  \w     44.00  90.00   0.50    0.18    --   76.37-105.00-160.00   92
  7  \w     62.00  87.00   0.50    0.18    --   84.32-105.00-160.00   50
  8  \w     39.00  64.00   0.50    0.18    --   58.73 -95.00   0.00   50
  9  \w     23.00  60.00   0.50    0.18    --   58.73-126.00 120.00   74
 10  \w     16.00  53.00   0.50    0.18    --   58.73 -95.00-120.00   74
 11  \w     20.00  47.00   0.50    0.18    --   58.73 -95.00  90.00   54
 12  \w     16.00  56.00   0.50    0.18    --   58.73 -95.00  30.00   80
 13  \w   -114.00 -87.00   0.50    0.18    --  -69.87 -15.00 150.00   54
 14  \w   -100.00 -50.00   0.50    0.18    --  -69.87 -15.00  60.00  100
 15  \w    -69.00 -34.00   0.50    0.18    --  -69.87 -15.00 150.00   70
 16  \w     24.00  57.00   0.50    0.18    --   71.45-126.00 -30.00   66
 17  \w     30.00  56.00   0.50    0.18    --   71.45 -95.00 120.00   52
 18  \w    -69.00 -35.00   0.50    0.18    --  -76.34 112.00-180.00   68
 19  \w   -125.00 -45.00   0.50    0.18    --  -76.34 -15.00  90.00  160
 20  \w   -126.00 -41.00   0.50    0.18    --  -76.34 -15.00   0.00  170
 21  \w    -78.00 -50.00   0.50    0.18    --  -76.34 112.00 120.00   56
 22  \w     35.00  63.00   0.50    0.18    --   76.37 -95.00 -90.00   56
 23  \w     32.00  63.00   0.50    0.18    --   76.37-112.00 -30.00   62
 24  \w     34.00  59.00   0.50    0.18    --   76.37 -95.00  30.00   50
 25  \w     35.00  60.00   0.50    0.18    --   76.37 -95.00-150.00   50
 26  \w     37.00  62.00   0.50    0.18    --   76.37 -95.00  60.00   50
 27  \w     37.00  62.00   0.50    0.18    --   76.37 -95.00 120.00   50
 28  \w    -97.00 -52.00   0.50    0.18    --  -79.50 117.00  21.58   90
 29  \w    -97.00 -71.00   0.50    0.18    --  -79.50 115.00  88.70   52
 30  \w    -67.00 -42.00   0.50    0.18    --  -79.50 115.00  88.70   50
 31  \w     64.00  90.00   0.50    0.18    --   84.32 -95.00 -30.00   52
 32  \w     64.00  90.00   0.50    0.18    --   84.32 -95.00 -60.00   52
 33  \w     61.00  91.00   0.50    0.18    --   84.32 -95.00 -90.00   60
 34  \w     45.00  92.00   0.50    0.18    --   84.32 -95.00   0.00   94
 35  \w     60.00  91.00   0.50    0.18    --   84.32 -95.00-120.00   62
 36  \w     66.00  91.00   0.50    0.18    --   84.32 -95.00  90.00   50
 37  \w     51.00 133.00   0.50    0.18    --   84.32  15.00  30.00  164
 38  \w     48.00 133.00   0.50    0.18    --   84.32  15.00 -60.00  170
;
_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      0.0402196000
_diffrn_orient_matrix_UB_12      0.1602530000
_diffrn_orient_matrix_UB_13      0.0276218000
_diffrn_orient_matrix_UB_21      -0.0733005000
_diffrn_orient_matrix_UB_22      -0.0449440000
_diffrn_orient_matrix_UB_23      0.0750213000
_diffrn_orient_matrix_UB_31      0.2323213000
_diffrn_orient_matrix_UB_32      -0.0271661000
_diffrn_orient_matrix_UB_33      0.0218143000
_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  0.0321
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12195
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.427
_diffrn_reflns_theta_min         4.757
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    1.610
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.43.100a (Rigaku Oxford Diffraction, 2023) 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            'clear pale colourless'
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_description       plate
_exptl_crystal_F_000             400
_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          0.140
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         4103
_refine_ls_number_restraints     348
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0736P)^2^+0.3252P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1407
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3225
_reflns_number_total             4103
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00069f2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7717899--7717905.cif.'
_cod_database_code               7717899
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.806
_shelx_estimated_absorpt_t_max   0.910
_shelx_res_checksum              38787