Avenue to novel <i>o</i>-carboranyl boron compounds - reactivity study of <i>o</i>-carborane-fused aminoborirane towards organic azides.
Wang, Junyi; Xiang, Libo; Liu, Xiaocui; Matler, Alexander; Lin, Zhenyang; Ye, Qing; Chemical science 15 (2024) 4839–4845; doi:10.1039/d4sc00489b

data_1571059
_publ_section_title
;
 Avenue to novel <i>o</i>-carboranyl boron compounds - reactivity study of
 <i>o</i>-carborane-fused aminoborirane towards organic azides.
;
_journal_issue                   13
_journal_name_full               'Chemical science'
_journal_page_first              4839
_journal_page_last               4845
_journal_paper_doi               10.1039/d4sc00489b
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C14 H31 B11 Cl2 N4 Si2'
_chemical_formula_sum            'C14 H31 B11 Cl2 N4 Si2'
_chemical_formula_weight         501.42
_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             2023-11-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-19 deposited with the CCDC.	2024-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                85.5810(10)
_cell_angle_beta                 72.4300(10)
_cell_angle_gamma                72.3450(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0990(2)
_cell_length_b                   10.65880(10)
_cell_length_c                   13.6478(2)
_cell_measurement_reflns_used    20145
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.6940
_cell_measurement_theta_min      3.3760
_cell_volume                     1334.42(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)''
_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 0.994
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     98.00 132.00   0.50    0.05    --   85.25  38.00 -87.07   68
  2  \w    100.00 126.00   0.50    0.05    --   85.25  47.00 -34.16   52
  3  \w     68.00 126.00   0.50    0.05    --   82.26  15.00 -90.00  116
  4  \w    108.00 133.00   0.50    0.05    --   82.26  15.00-180.00   50
  5  \w     61.00 121.00   0.50    0.05    --   85.25  14.00   0.56  120
  6  \w     89.00 128.00   0.50    0.05    --   82.26  15.00  30.00   78
  7  \w     83.00 134.00   0.50    0.05    --   85.25  22.00 156.31  102
  8  \w     87.00 124.00   0.50    0.05    --   82.26  15.00 120.00   74
  9  \w     51.00 111.00   0.50    0.05    --   82.26  15.00  90.00  120
 10  \w     49.00  74.00   0.50    0.05    --   85.25-118.00 159.98   50
 11  \w     32.00  98.00   0.50    0.05    --   78.00-117.00  -9.19  132
 12  \w     36.00  98.00   0.50    0.05    --   82.26-117.00 -35.00  124
 13  \w     67.00  93.00   0.50    0.05    --   82.26-112.00-150.00   52
 14  \w     37.00  62.00   0.50    0.05    --   82.26-112.00 -60.00   50
 15  \w     50.00  76.00   0.50    0.05    --   82.26-112.00-180.00   52
 16  \w     14.00  80.00   0.50    0.05    --   58.45-117.00 -35.00  132
 17  \w     37.00  62.00   0.50    0.05    --   82.26-112.00-120.00   50
 18  \w     25.00  93.00   0.50    0.05    --   71.26-117.00 -35.00  136
 19  \w     41.00  92.00   0.50    0.05    --   85.25-106.00 -11.43  102
 20  \w     43.00  69.00   0.50    0.05    --   82.26-112.00 -30.00   52
 21  \w     46.00  92.00   0.50    0.05    --   85.25 -97.00-160.81   92
 22  \w     37.00  71.00   0.50    0.05    --   82.26-112.00  30.00   68
 23  \w     42.00  88.00   0.50    0.05    --   82.26 -95.00   0.00   92
 24  \w     47.00  85.00   0.50    0.05    --   82.26 -95.00  60.00   76
 25  \w     43.00  92.00   0.50    0.05    --   85.25 -96.00 123.97   98
 26  \w     47.00  90.00   0.50    0.05    --   82.26 -95.00 150.00   86
 27  \w     42.00  93.00   0.50    0.05    --   82.26-112.00 120.00  102
 28  \w     40.00  73.00   0.50    0.05    --   85.25-107.00  93.24   66
 29  \w     44.00  89.00   0.50    0.05    --   82.26 -95.00  30.00   90
 30  \w     16.00  66.00   0.50    0.05    --   58.45 -95.00  30.00  100
 31  \w     44.00  69.00   0.50    0.05    --   82.26 -95.00  90.00   50
 32  \w     40.00  65.00   0.50    0.05    --   82.26 -95.00 -60.00   50
 33  \w     45.00  90.00   0.50    0.05    --   82.26 -95.00-120.00   90
 34  \w     40.00  90.00   0.50    0.05    --   82.26 -95.00-180.00  100
 35  \w     62.00  90.00   0.50    0.05    --   82.26 -95.00-150.00   56
 36  \w     55.00  82.00   0.50    0.05    --   85.25 -86.00 -77.25   54
 37  \w    -97.00 -32.00   0.50    0.05    --  -78.00 114.00  30.25  130
 38  \w    -91.00 -24.00   0.50    0.05    --  -69.85 117.00  51.00  134
 39  \w   -108.00 -34.00   0.50    0.05    --  -79.50 140.00 142.03  148
 40  \w    -99.00 -33.00   0.50    0.05    --  -79.50 124.00  99.12  132
 41  \w    -82.00 -14.00   0.50    0.05    --  -60.36 117.00  51.00  136
 42  \w    -98.00 -30.00   0.50    0.05    --  -76.37 117.00  51.00  136
 43  \w    -97.00 -33.00   0.50    0.05    --  -79.50 118.00-148.61  128
 44  \w   -124.00 -92.00   0.50    0.05    --  -79.50 -63.00 -33.38   64
 45  \w   -127.00 -92.00   0.50    0.05    --  -79.50 -53.00-101.91   70
 46  \w   -128.00 -93.00   0.50    0.05    --  -79.50 -52.00-137.40   70
 47  \w   -122.00 -87.00   0.50    0.05    --  -74.00 -52.00 -63.77   70
 48  \w   -128.00 -93.00   0.50    0.05    --  -79.50 -52.00  21.48   70
 49  \w   -128.00 -93.00   0.50    0.05    --  -79.50 -50.00  -5.26   70
 50  \w   -125.00 -91.00   0.50    0.05    --  -79.50 -60.00  52.84   68
 51  \w    -86.00 -51.00   0.50    0.05    --  -38.00 -51.00 166.02   70
 52  \w   -128.00 -93.00   0.50    0.05    --  -79.50 -51.00 176.49   70
 53  \w   -117.00 -84.00   0.50    0.05    --  -70.00 -57.00 166.08   66
 54  \w   -129.00 -92.00   0.50    0.05    --  -79.50 -45.00 132.47   74
 55  \w   -111.00 -76.00   0.50    0.05    --  -62.00 -47.00  52.56   70
 56  \w    -91.00 -56.00   0.50    0.05    --  -42.00 -49.00-147.84   70
;
_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      -0.0240283000
_diffrn_orient_matrix_UB_12      -0.0242625000
_diffrn_orient_matrix_UB_13      0.1159555000
_diffrn_orient_matrix_UB_21      -0.1641861000
_diffrn_orient_matrix_UB_22      0.0290733000
_diffrn_orient_matrix_UB_23      0.0159829000
_diffrn_orient_matrix_UB_31      0.0224144000
_diffrn_orient_matrix_UB_32      -0.1468948000
_diffrn_orient_matrix_UB_33      -0.0179423000
_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  0.0322
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27112
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.220
_diffrn_reflns_theta_min         3.397
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    3.125
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.42.102a (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 colourless'
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_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          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5344
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+0.5297P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5039
_reflns_number_total             5344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc00489b2.cif
_cod_data_source_block           AlMa123_LiXi_a
_cod_depositor_comments
'Adding full bibliography for 1571058--1571061.cif.'
_cod_database_code               1571059
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.766
_shelx_estimated_absorpt_t_min   0.687
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
1.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
1.c Boron cage BH refined with riding coordinates:
 B1(H1), B3(H3A), B4(H4A), B5(H5A), B6(H6A), B7(H7), B8(H8), B9(H9), B10(H10),
 B11(H11)
;
_shelx_res_checksum              66906
_olex2_submission_special_instructions 'No special instructions were received'