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_7717905
_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         'C25 H52 B N3 O2 Sn2'
_chemical_formula_sum            'C25 H52 B N3 O2 Sn2'
_chemical_formula_weight         674.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-02-28
_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                 98.1740(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.04570(10)
_cell_length_b                   16.51580(10)
_cell_length_c                   18.33080(10)
_cell_measurement_reflns_used    13193
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.5070
_cell_measurement_theta_min      3.6120
_cell_volume                     3010.42(4)
_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 1.000
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w   -111.00 -43.00   0.50    0.05    --  -76.38 -15.00-120.00  136
  2  \w    -62.00 -30.00   0.50    0.05    --  -60.28 126.00-150.00   64
  3  \w    -51.00 -25.00   0.50    0.05    --  -60.28 126.00-120.00   52
  4  \w    -77.00 -35.00   0.50    0.05    --  -76.38 112.00-120.00   84
  5  \w    -54.00 -23.00   0.50    0.05    --  -69.77 126.00 -60.00   62
  6  \w   -124.00 -40.00   0.50    0.05    --  -76.38 -15.00 150.00  168
  7  \w     51.00 135.00   0.50    0.05    --   84.40  15.00 120.00  168
  8  \w     81.00 109.00   0.50    0.05    --   58.64  15.00  60.00   56
  9  \w     42.00  73.00   0.50    0.05    --   58.64  15.00 150.00   62
 10  \w     40.00  66.00   0.50    0.05    --   58.64  15.00  60.00   52
 11  \w     49.00 114.00   0.50    0.05    --   84.40  15.00-150.00  130
 12  \w     34.00  59.00   0.50    0.05    --   76.43 -95.00   0.00   50
 13  \w     40.00  65.00   0.50    0.05    --   84.40-112.00 -90.00   50
 14  \w     39.00  64.00   0.50    0.05    --   84.40-112.00-120.00   50
 15  \w     42.00  92.00   0.50    0.05    --   84.40-112.00  30.00  100
 16  \w     36.00  62.00   0.50    0.05    --   76.43 -95.00  60.00   52
 17  \w     18.00  45.00   0.50    0.05    --   58.64 -95.00  60.00   54
 18  \w     42.00  84.00   0.50    0.05    --   76.43 -95.00  90.00   84
 19  \w     56.00  83.00   0.50    0.05    --   76.43 -95.00 150.00   54
;
_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      0.0953151000
_diffrn_orient_matrix_UB_12      -0.0295823000
_diffrn_orient_matrix_UB_13      -0.0532023000
_diffrn_orient_matrix_UB_21      0.0859238000
_diffrn_orient_matrix_UB_22      -0.0444766000
_diffrn_orient_matrix_UB_23      0.0640567000
_diffrn_orient_matrix_UB_31      -0.0867166000
_diffrn_orient_matrix_UB_32      -0.0764839000
_diffrn_orient_matrix_UB_33      -0.0167369000
_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  0.0249
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18685
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.753
_diffrn_reflns_theta_min         3.619
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    13.374
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.766
_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            colourless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_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          0.170
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5902
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0221
_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^)+(0.0245P)^2^+2.7816P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0553
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5653
_reflns_number_total             5902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00069f2.cif
_cod_data_source_block           3b
_cod_depositor_comments
'Adding full bibliography for 7717899--7717905.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7717905
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.210
_shelx_estimated_absorpt_t_max   0.297
_shelx_res_checksum              89763