CAAC-stabilised 9,10-diboraanthracene: an electronically and structurally flexible platform for small-molecule activation and metal complexation.
Dietz, Maximilian; Arrowsmith, Merle; Braunschweig, Holger; Dalton transactions (Cambridge, England : 2003) 53 (2024) 449–453; doi:10.1039/d3dt03787h

data_7714662
_publ_section_title
;
 CAAC-stabilised 9,10-diboraanthracene: an electronically and structurally
 flexible platform for small-molecule activation and metal complexation.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              449
_journal_page_last               453
_journal_paper_doi               10.1039/d3dt03787h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C52 H72 B2 N2'
_chemical_formula_sum            'C52 H72 B2 N2'
_chemical_formula_weight         746.73
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-10-27
_audit_creation_method           'CIF-fill 1.3n (K.Radacki, 2005-22)'
_audit_update_record
;
2023-11-09 deposited with the CCDC.	2023-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.89720(10)
_cell_length_b                   15.60870(10)
_cell_length_c                   41.3288(3)
_cell_measurement_reflns_used    23015
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.8010
_cell_measurement_theta_min      3.1510
_cell_volume                     8964.93(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.68a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.68a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.68a (Rigaku OD, 2022)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_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 0.993
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w    -95.00 -60.80   0.60    3.00    --  -46.00 -48.00-103.67   57
  2  \w     16.00  64.60   0.60    3.00    --   58.30 -95.00  30.00   81
  3  \w   -117.00 -84.00   0.60    3.00    --  -70.00 -56.00-154.09   55
  4  \w   -120.00 -87.00   0.60    3.00    --  -74.00 -59.00  85.19   55
  5  \w    -92.00 -32.00   0.60    3.00    --  -76.30 112.00 120.00  100
  6  \w   -126.00 -93.00   0.60    3.00    --  -79.50-120.00-104.32   55
  7  \w   -125.00 -92.00   0.60    3.00    --  -79.50 -60.00 -86.42   55
  8  \w   -125.00 -92.00   0.60    3.00    --  -79.50 -60.00-118.59   55
  9  \w     98.00 134.60   0.60    3.00    --   85.25  42.00 -74.20   61
 10  \w     39.00  96.60   0.60    3.00    --   85.25-117.00 -94.01   96
 11  \w     41.00  92.00   0.60    3.00    --   85.25-103.00  36.64   85
 12  \w    104.00 131.00   0.60    3.00    --   85.25 113.00-169.65   45
 13  \w     97.00 130.00   0.60    3.00    --   85.25  61.00-123.05   55
 14  \w     38.00 101.00   0.60    3.00    --   85.25-128.00-118.40  105
 15  \w     45.00  87.00   0.60    3.00    --   85.25 -88.00  77.72   70
 16  \w     44.00  71.00   0.60    3.00    --   85.25 -73.00-110.38   45
 17  \w     99.00 132.60   0.60    3.00    --   85.25  51.00 132.93   56
 18  \w     98.00 134.60   0.60    3.00    --   85.25  43.00 113.77   61
 19  \w     96.00 135.60   0.60    3.00    --   85.25  35.00   7.12   66
 20  \w     96.00 132.00   0.60    3.00    --   85.25 127.00  62.11   60
 21  \w     43.00  91.00   0.60    3.00    --   85.25 -95.00 116.42   80
 22  \w     41.00  92.00   0.60    3.00    --   85.25-102.00   4.50   85
 23  \w     46.00  85.00   0.60    3.00    --   85.25 -83.00 149.58   65
 24  \w    105.00 129.60   0.60    3.00    --   85.25 111.00  57.17   41
 25  \w   -121.00 -91.60   0.60    3.00    --  -70.00 -38.00  27.04   49
;
_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      -0.0227612000
_diffrn_orient_matrix_UB_12      -0.0964804000
_diffrn_orient_matrix_UB_13      -0.0019424000
_diffrn_orient_matrix_UB_21      0.0606659000
_diffrn_orient_matrix_UB_22      -0.0069245000
_diffrn_orient_matrix_UB_23      -0.0310946000
_diffrn_orient_matrix_UB_31      0.0899269000
_diffrn_orient_matrix_UB_32      -0.0196265000
_diffrn_orient_matrix_UB_33      0.0204745000
_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  0.0690
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            67929
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        17.684
_diffrn_reflns_theta_max         70.075
_diffrn_reflns_theta_min         3.833
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.900
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.42.68a (Rigaku Oxford Diffraction, 2022) 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 light colourless'
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_description       block
_exptl_crystal_F_000             3264
_exptl_crystal_preparation
;
 Crystalls were grown from saturated solution. 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_recrystallization_method
'Re-crystallisation from solvent: benzene/pentane'
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         8508
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+3.0805P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1287
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6808
_reflns_number_total             8508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03787h2.cif
_cod_data_source_block           MaDi263_MaDi_a_(DBA)H2
_cod_depositor_comments
'Adding full bibliography for 7714662--7714667.cif.'
_cod_database_code               7714662
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.947
_shelx_estimated_absorpt_t_max   0.986
_shelx_res_checksum              94548