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_7717904
_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         'C22 H50 B2 N4 Sn2'
_chemical_formula_sum            'C22 H50 B2 N4 Sn2'
_chemical_formula_weight         629.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-01-16
_audit_creation_method           'CIF-fill 1.4r (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                 97.6470(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8317(2)
_cell_length_b                   11.31540(10)
_cell_length_c                   19.0710(2)
_cell_measurement_reflns_used    12890
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.1660
_cell_measurement_theta_min      4.6590
_cell_volume                     2958.28(6)
_computing_cell_refinement       'CrysAlisPro 1.171.43.100a (Rigaku OD, 2023)'
_computing_data_collection
;
 CrysAlisPro system (CCD 43.90a 64-bit (release 15-09-2023))
;
_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 1.000
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     57.00  92.00   0.50    0.05    --   84.34 -95.00 -30.00   70
  2  \w     18.00  44.00   0.50    0.05    --   58.74 -95.00-120.00   52
  3  \w     39.00  64.00   0.50    0.05    --   84.34-112.00 -30.00   50
  4  \w    -91.00 -37.00   0.50    0.05    --  -76.39 112.00 -90.00  108
  5  \w     48.00 135.00   0.50    0.05    --   84.34  15.00 -30.00  174
  6  \w     16.00  44.00   0.50    0.05    --   58.74 -95.00-150.00   56
  7  \w   -125.00 -41.00   0.50    0.05    --  -76.39 -15.00  30.00  168
  8  \w     16.00  42.00   0.50    0.05    --   58.74 -95.00  90.00   52
  9  \w     23.00  66.00   0.50    0.05    --   58.74-126.00 150.00   86
 10  \w     77.00 108.00   0.50    0.05    --   58.74  15.00   0.00   62
 11  \w     48.00  74.00   0.50    0.05    --   58.74  15.00   0.00   52
 12  \w     67.00  92.00   0.50    0.05    --   84.34 -95.00 120.00   50
 13  \w     42.00  67.00   0.50    0.05    --   84.34 -95.00 150.00   50
 14  \w     46.00  92.00   0.50    0.05    --   84.34 -95.00  60.00   92
 15  \w     48.00 133.00   0.50    0.05    --   84.34  15.00  60.00  170
 16  \w    -71.00 -38.00   0.50    0.05    --  -76.39 112.00 120.00   66
 17  \w    -65.00 -40.00   0.50    0.05    --  -76.39 112.00-150.00   50
 18  \w   -117.00 -80.00   0.50    0.05    --  -76.39 -15.00-180.00   74
 19  \w    -97.00 -35.00   0.50    0.05    --  -79.50 117.00  -0.16  124
 20  \w     40.00  93.00   0.50    0.05    --   76.33-112.00 120.00  106
 21  \w     66.00  91.00   0.50    0.05    --   84.34 -95.00 -60.00   50
 22  \w   -111.00 -47.00   0.50    0.05    --  -76.39 -15.00 120.00  128
 23  \w    -68.00 -42.00   0.50    0.05    --  -69.84 -15.00  90.00   52
 24  \w   -119.00 -70.00   0.50    0.05    --  -69.84 -15.00  90.00   98
 25  \w    -74.00 -45.00   0.50    0.05    --  -76.39 -15.00-180.00   58
 26  \w     42.00  88.00   0.50    0.05    --   84.34 -95.00-120.00   92
 27  \w     56.00  91.00   0.50    0.05    --   84.34 -95.00   0.00   70
 28  \w     16.00  43.00   0.50    0.05    --   58.74 -95.00  30.00   54
 29  \w     56.00  90.00   0.50    0.05    --   84.34 -95.00-180.00   68
 30  \w     37.00  83.00   0.50    0.05    --   76.33 -95.00-150.00   92
 31  \w     52.00  92.00   0.50    0.05    --   84.34 -95.00 -90.00   80
 32  \w     34.00  60.00   0.50    0.05    --   71.46 -95.00  30.00   52
 33  \w     66.00  91.00   0.50    0.05    --   84.34 -95.00  90.00   50
 34  \w     24.00  70.00   0.50    0.05    --   71.46-126.00  30.00   92
 35  \w     66.00  91.00   0.50    0.05    --   84.34 -95.00-150.00   50
;
_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      -0.0962131000
_diffrn_orient_matrix_UB_12      0.0599613000
_diffrn_orient_matrix_UB_13      0.0126398000
_diffrn_orient_matrix_UB_21      0.0500535000
_diffrn_orient_matrix_UB_22      0.0494226000
_diffrn_orient_matrix_UB_23      0.0709488000
_diffrn_orient_matrix_UB_31      0.0294205000
_diffrn_orient_matrix_UB_32      0.1117888000
_diffrn_orient_matrix_UB_33      -0.0380768000
_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  0.0789
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16207
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.830
_diffrn_reflns_theta_min         4.679
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    13.519
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.571
_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            yellow
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_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          0.300
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.517
_refine_diff_density_min         -1.236
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0682P)^2^+6.0259P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2901
_reflns_number_total             2965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00069f2.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 7717899--7717905.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7717904
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.107
_shelx_estimated_absorpt_t_max   0.376
_shelx_res_checksum              69803