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_7717902
_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         'C27 H56 B N3 Sn2'
_chemical_formula_sum            'C27 H56 B N3 Sn2'
_chemical_formula_weight         670.93
_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_Hall           'I 4bw -2c'
_space_group_name_H-M_alt        'I 41 c d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-08-26
_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            8
_cell_length_a                   16.74320(10)
_cell_length_b                   16.74320(10)
_cell_length_c                   21.92770(10)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.1190
_cell_measurement_theta_min      5.2650
_cell_volume                     6147.10(6)
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_computing_data_collection
;
 CrysAlisPro system (CCD 43.63a 64-bit (release 03-03-2023))
;
_computing_data_reduction        'CrysAlisPro 1.171.43.63a (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 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w   -128.00 -93.00   0.50    0.05    --  -79.50 -51.00-176.23   70
  2  \w   -115.00 -80.00   0.50    0.05    --  -66.00 -49.00-151.18   70
  3  \w   -102.00 -67.00   0.50    0.05    --  -54.00 -52.00  52.78   70
  4  \w    -99.00 -64.00   0.50    0.05    --  -50.00 -48.00  25.74   70
  5  \w   -107.00 -72.00   0.50    0.05    --  -58.00 -49.00 -75.56   70
  6  \w   -112.00 -75.00   0.50    0.05    --  -62.00 -46.00 -46.07   74
  7  \w   -103.00 -68.00   0.50    0.05    --  -54.00 -48.00 -13.59   70
  8  \w   -120.00 -83.00   0.50    0.05    --  -70.00 -45.00-110.96   74
  9  \w   -130.00 -92.00   0.50    0.05    --  -79.50 -42.00  20.12   76
 10  \w   -128.00 -93.00   0.50    0.05    --  -79.50 -52.00  62.26   70
 11  \w   -115.00 -80.00   0.50    0.05    --  -66.00 -47.00  76.54   70
 12  \w   -124.00 -86.00   0.50    0.05    --  -74.00 -41.00 112.33   76
 13  \w   -103.00 -68.00   0.50    0.05    --  -54.00 -49.00 166.58   70
 14  \w   -126.00 -93.00   0.50    0.05    --  -79.50-121.00 138.78   66
 15  \w    -97.00 -33.00   0.50    0.05    --  -79.50 115.00  67.10  128
 16  \w    -97.00 -22.00   0.50    0.05    --  -69.76 126.00  90.00  150
 17  \w    -97.00 -33.00   0.50    0.05    --  -79.50 115.00 -28.01  128
 18  \w    -97.00 -33.00   0.50    0.05    --  -79.50 115.00 -45.95  128
 19  \w    -92.00 -31.00   0.50    0.05    --  -76.35 112.00-150.00  122
 20  \w     46.00 133.00   0.50    0.05    --   82.28  15.00-120.00  174
 21  \w     91.00 117.00   0.50    0.05    --   82.28  15.00-180.00   52
 22  \w     59.00  85.00   0.50    0.05    --   82.28  15.00-180.00   52
 23  \w     84.00 132.00   0.50    0.05    --   82.28  15.00-150.00   96
 24  \w     53.00  79.00   0.50    0.05    --   82.28  15.00 -30.00   52
 25  \w     60.00 112.00   0.50    0.05    --   82.28  15.00   0.00  104
 26  \w     51.00 129.00   0.50    0.05    --   82.28  15.00  60.00  156
 27  \w     81.00 107.00   0.50    0.05    --   82.28  15.00  90.00   52
 28  \w     79.00 105.00   0.50    0.05    --   82.28  15.00 150.00   52
 29  \w     77.00 132.00   0.50    0.05    --   82.28  15.00 120.00  110
 30  \w     90.00 116.00   0.50    0.05    --   82.28  15.00 -60.00   52
 31  \w     95.00 133.00   0.50    0.05    --   82.28  15.00 -90.00   76
 32  \w     43.00  90.00   0.50    0.05    --   82.28 -95.00-180.00   94
 33  \w     39.00  67.00   0.50    0.05    --   82.28-112.00-150.00   56
 34  \w     37.00  93.00   0.50    0.05    --   82.28-112.00 -60.00  112
 35  \w     37.00  93.00   0.50    0.05    --   82.28-112.00 150.00  112
 36  \w     37.00  93.00   0.50    0.05    --   82.28-112.00 120.00  112
 37  \w     42.00  93.00   0.50    0.05    --   82.28-112.00  90.00  102
 38  \w     37.00  93.00   0.50    0.05    --   82.28-112.00  60.00  112
 39  \w     38.00  93.00   0.50    0.05    --   82.28-112.00  30.00  110
 40  \w     44.00  83.00   0.50    0.05    --   82.28-112.00   0.00   78
 41  \w     37.00  71.00   0.50    0.05    --   82.28-112.00 -30.00   68
 42  \w     58.00  85.00   0.50    0.05    --   82.28-112.00 -90.00   54
 43  \w     42.00  93.00   0.50    0.05    --   85.25-101.00 -62.36  102
 44  \w     40.00  65.00   0.50    0.05    --   85.25-112.00-117.68   50
 45  \w     46.00  72.00   0.50    0.05    --   85.25-108.00-118.64   52
 46  \w     39.00  90.00   0.50    0.05    --   82.28-112.00-180.00  102
 47  \w     66.00  92.00   0.50    0.05    --   85.25-100.00-132.58   52
 48  \w     43.00  78.00   0.50    0.05    --   85.25-109.00-135.49   70
 49  \w     42.00  91.00   0.50    0.05    --   85.25 -97.00-106.40   98
 50  \w     40.00  90.00   0.50    0.05    --   82.28 -95.00   0.00  100
 51  \w     40.00  89.00   0.50    0.05    --   82.28 -95.00 -30.00   98
 52  \w     41.00  67.00   0.50    0.05    --   82.28 -95.00  30.00   52
 53  \w     48.00  88.00   0.50    0.05    --   82.28 -95.00  90.00   80
 54  \w     43.00  92.00   0.50    0.05    --   85.25-100.00 152.10   98
 55  \w     43.00  70.00   0.50    0.05    --   82.28 -95.00 120.00   54
 56  \w     48.00  90.00   0.50    0.05    --   82.28 -95.00  60.00   84
 57  \w     40.00  89.00   0.50    0.05    --   82.28 -95.00 -90.00   98
;
_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      -0.0736226000
_diffrn_orient_matrix_UB_12      -0.0513870000
_diffrn_orient_matrix_UB_13      0.0153309000
_diffrn_orient_matrix_UB_21      -0.0445911000
_diffrn_orient_matrix_UB_22      0.0751664000
_diffrn_orient_matrix_UB_23      0.0220074000
_diffrn_orient_matrix_UB_31      -0.0324845000
_diffrn_orient_matrix_UB_32      0.0132769000
_diffrn_orient_matrix_UB_33      -0.0649413000
_diffrn_radiation_monochromator  'multi-layer mirror'
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_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_unetI/netI     0.0264
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_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            58495
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.299
_diffrn_reflns_theta_min         5.284
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    13.043
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.43.63a (Rigaku Oxford Diffraction, 2023) Empirical 
 absorption correction using spherical harmonics, implemented in SCALE3 
 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_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          0.370
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.872
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Flack x determined using 1197 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, 
 Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2928
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0791P)^2^+1.4765P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.807
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_reflns_Friedel_fraction_max     0.847
_reflns_number_gt                2843
_reflns_number_total             2928
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00069f2.cif
_cod_data_source_block           3a
_cod_depositor_comments
'Adding full bibliography for 7717899--7717905.cif.'
_cod_original_cell_volume        6147.10(8)
_cod_database_code               7717902
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.086
_shelx_estimated_absorpt_t_max   0.304
_shelx_res_checksum              78376