Efficient synthesis of an unsupported aryl substituted iminoborane chain (HNArBH)<sub>2</sub>NAr (Ar = [1,1'-biphenyl]-2-yl).
Stauder, Rita; Ströbele, Markus; Bettinger, Holger F.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16467–16469; doi:10.1039/d4dt02280g

data_7717132
_publ_section_title
;
 Efficient synthesis of an unsupported aryl substituted iminoborane chain
 (HNArBH)<sub>2</sub>NAr (Ar = [1,1'-biphenyl]-2-yl).
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16467
_journal_page_last               16469
_journal_paper_doi               10.1039/d4dt02280g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C36 H31 B2 N3'
_chemical_formula_sum            'C36 H31 B2 N3'
_chemical_formula_weight         527.316
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-14
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-11-14 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.964(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.5173(12)
_cell_length_b                   9.9015(4)
_cell_length_c                   26.2782(13)
_cell_measurement_reflns_used    4912
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      74.7430
_cell_measurement_theta_min      4.0130
_cell_volume                     5751.3(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement
'olex2.refine 1.5-ac5-024 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9940
_diffrn_measured_fraction_theta_max 0.9448
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -76.00 -42.00   0.50   16.29    --  -43.85 123.00 -61.00   68
  2  \w    -39.00 -13.00   0.50   16.29    --  -43.85 123.00 -61.00   52
  3  \w     42.00  89.00   0.50   16.29    --   43.85-123.00-142.00   94
  4  \w   -154.00 -94.00   0.50   30.15    --  -96.00-123.00-142.00  120
  5  \w    -73.00 -48.00   0.50   30.15    --  -96.00 123.00 -61.00   50
  6  \w    121.00 146.00   0.50   30.15    --  107.76 123.00 -61.00   50
  7  \w    -80.00 -54.00   0.50   16.29    --  -43.85 140.00-180.00   52
  8  \w    -27.00  32.00   0.50   16.29    --  -43.85  19.00-120.00  118
  9  \w    -19.00  35.00   0.50   16.29    --  -43.85  19.00 120.00  108
 10  \w    -25.00  34.00   0.50   16.29    --  -43.85  19.00  60.00  118
 11  \w    -27.00  34.00   0.50   16.29    --  -43.85  19.00   0.00  122
 12  \w   -145.00-114.00   0.50   30.15    --  -96.00 -77.00-120.00   62
 13  \w    -47.00 -21.00   0.50   30.15    --  -96.00  45.00  90.00   52
 14  \w    -49.00 -21.00   0.50   30.15    --  -96.00  45.00 -60.00   56
 15  \w    -51.00 -25.00   0.50   30.15    --  -96.00  45.00-120.00   52
 16  \w    -48.00 -22.00   0.50   30.15    --  -96.00  45.00 150.00   52
 17  \w    -50.00 -21.00   0.50   30.15    --  -96.00  45.00 120.00   58
 18  \w   -170.00 -92.00   0.50   30.15    --  -96.00 -61.00  60.00  156
 19  \w     37.00  99.00   0.50   30.15    --  107.76 -94.00 -60.00  124
 20  \w     40.00  70.00   0.50   30.15    --  107.76 -61.00-150.00   60
 21  \w    124.00 149.00   0.50   30.15    --  107.76  77.00-150.00   50
 22  \w     65.00  91.00   0.50   30.15    --  107.76 -94.00 -30.00   52
 23  \w     35.00  99.00   0.50   30.15    --  107.76 -94.00-180.00  128
 24  \w     48.00  99.00   0.50   30.15    --  107.76 -94.00-120.00  102
 25  \w     53.00  96.00   0.50   30.15    --  107.76 -94.00 -90.00   86
 26  \w    110.00 176.00   0.50   30.15    --  107.76  61.00 -60.00  132
 27  \w    112.00 155.00   0.50   30.15    --  107.76 125.00  60.00   86
 28  \w     35.00  84.00   0.50   30.15    --  107.76-123.00-142.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0604053000
_diffrn_orient_matrix_UB_12      -0.0307495000
_diffrn_orient_matrix_UB_13      -0.0452631000
_diffrn_orient_matrix_UB_21      0.0150251000
_diffrn_orient_matrix_UB_22      -0.1519564000
_diffrn_orient_matrix_UB_23      0.0053010000
_diffrn_orient_matrix_UB_31      -0.0312748000
_diffrn_orient_matrix_UB_32      -0.0136048000
_diffrn_orient_matrix_UB_33      0.0425905000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.9940
_diffrn_reflns_Laue_measured_fraction_max 0.9448
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42123
_diffrn_reflns_point_group_measured_fraction_full 0.9940
_diffrn_reflns_point_group_measured_fraction_max 0.9448
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         75.70
_diffrn_reflns_theta_min         4.00
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.945
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.70a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       plate
_exptl_crystal_F_000             2230.465
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.2826
_refine_diff_density_min         -0.1919
_refine_diff_density_rms         0.0461
_refine_ls_d_res_high            0.7956
_refine_ls_d_res_low             11.0520
_refine_ls_goodness_of_fit_ref   1.0298
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1297
_refine_ls_number_reflns         11296
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.0295
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+0.1693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0812
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -29
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              -17
_reflns_number_gt                8660
_reflns_number_total             11296
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02280g2.cif
_cod_data_source_block           RS1
_cod_depositor_comments          'Adding full bibliography for 7717132.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7717132
_chemical_oxdiff_formula         'C72 H62 N6 B4'
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(H3b) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 3.957
_oxdiff_exptl_absorpt_empirical_full_min 0.321