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_7714666
_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         'C55 H70 B2 Cr N2 O3, C4 H8 O'
_chemical_formula_sum            'C59 H78 B2 Cr N2 O4'
_chemical_formula_weight         952.85
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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             2023-10-31
_audit_creation_method           'CIF-fill 1.4o (K.Radacki, 2005-23)'
_audit_update_record
;
2023-11-09 deposited with the CCDC.	2023-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.8830(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.25260(10)
_cell_length_b                   22.8684(2)
_cell_length_c                   19.7806(2)
_cell_measurement_reflns_used    45353
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.2000
_cell_measurement_theta_min      2.9290
_cell_volume                     5078.44(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.89a (Rigaku OD, 2023)'
_computing_data_collection
;
 CrysAlisPro system (CCD 42.102a 64-bit (release 15-09-2023))
;
_computing_data_reduction        'CrysAlisPro 1.171.43.89a (Rigaku OD, 2023)'
_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 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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     39.00  79.00   0.50    0.10    --   85.25-135.00 102.90   80
  2  \w     32.00  98.00   0.50    0.10    --   78.00-115.00 111.67  132
  3  \w     41.00 108.00   0.50    0.10    --   85.25-140.00-123.09  134
  4  \w     20.00  86.00   0.50    0.10    --   58.45-126.00-180.00  132
  5  \w     37.00  93.00   0.50    0.10    --   82.26-112.00-120.00  112
  6  \w     37.00  93.00   0.50    0.10    --   82.26-112.00 -60.00  112
  7  \w     37.00  93.00   0.50    0.10    --   82.26-112.00  30.00  112
  8  \w     37.00  93.00   0.50    0.10    --   82.26-112.00  60.00  112
  9  \w     40.00  92.00   0.50    0.10    --   82.26-112.00 120.00  104
 10  \w     63.00  92.00   0.50    0.10    --   85.25 -99.00  58.47   58
 11  \w     47.00  74.00   0.50    0.10    --   85.25 -96.00 -55.07   54
 12  \w     57.00  86.00   0.50    0.10    --   85.25 -96.00-111.34   58
 13  \w     16.00  66.00   0.50    0.10    --   58.45 -95.00-120.00  100
 14  \w     40.00  90.00   0.50    0.10    --   82.26 -95.00-120.00  100
 15  \w     16.00  66.00   0.50    0.10    --   58.45 -95.00 -60.00  100
 16  \w     64.00  90.00   0.50    0.10    --   82.26 -95.00 -30.00   52
 17  \w     56.00  92.00   0.50    0.10    --   85.25 -94.00  22.10   72
 18  \w     40.00  90.00   0.50    0.10    --   82.26 -95.00  90.00  100
 19  \w     47.00  91.00   0.50    0.10    --   85.25 -93.00 130.55   88
 20  \w     40.00  90.00   0.50    0.10    --   82.26 -95.00 120.00  100
 21  \w    103.00 131.00   0.50    0.10    --   85.25 114.00-144.95   56
 22  \w     94.00 130.00   0.50    0.10    --   85.25 132.00-133.44   72
 23  \w     99.00 131.00   0.50    0.10    --   85.25 124.00 127.03   64
 24  \w    102.00 130.00   0.50    0.10    --   85.25 118.00 155.62   56
 25  \w     98.00 132.00   0.50    0.10    --   85.25  57.00-135.95   68
 26  \w    100.00 127.00   0.50    0.10    --   85.25  49.00-157.79   54
 27  \w     46.00 133.00   0.50    0.10    --   82.26  15.00-150.00  174
 28  \w    104.00 130.00   0.50    0.10    --   85.25  54.00 -39.79   52
 29  \w     98.00 133.00   0.50    0.10    --   85.25  42.00  96.27   70
 30  \w    -97.00 -32.00   0.50    0.10    --  -78.00 114.00 -13.12  130
 31  \w   -102.00 -32.00   0.50    0.10    --  -79.50 131.00   1.26  140
 32  \w   -108.00 -33.00   0.50    0.10    --  -79.50 139.00-125.17  150
 33  \w   -125.00 -91.00   0.50    0.10    --  -79.50 -61.00  53.56   68
 34  \w   -124.00 -94.00   0.50    0.10    --  -79.50 -64.00  45.83   60
 35  \w   -125.00 -91.00   0.50    0.10    --  -79.50 -60.00  44.43   68
 36  \w   -125.00 -91.00   0.50    0.10    --  -79.50 -60.00  21.99   68
 37  \w   -124.00 -94.00   0.50    0.10    --  -79.50 -64.00  24.42   60
 38  \w   -117.00 -85.00   0.50    0.10    --  -70.00 -58.00  35.18   64
 39  \w   -126.00 -91.00   0.50    0.10    --  -79.50 -58.00  25.91   70
 40  \w   -126.00 -91.00   0.50    0.10    --  -79.50 -58.00  31.51   70
 41  \w   -126.00 -91.00   0.50    0.10    --  -79.50 -59.00  60.02   70
 42  \w   -124.00 -94.00   0.50    0.10    --  -79.50 -64.00 111.62   60
 43  \w   -124.00 -92.00   0.50    0.10    --  -79.50 -63.00  88.08   64
 44  \w    -99.00 -64.00   0.50    0.10    --  -50.00 -48.00 104.38   70
 45  \w    -99.00 -64.00   0.50    0.10    --  -50.00 -48.00 170.98   70
 46  \w   -129.00 -93.00   0.50    0.10    --  -79.50 -47.00 116.21   72
 47  \w   -122.00 -87.00   0.50    0.10    --  -74.00 -54.00  51.63   70
 48  \w   -102.00 -67.00   0.50    0.10    --  -54.00 -52.00 -60.73   70
 49  \w   -115.00 -80.00   0.50    0.10    --  -66.00 -47.00 -83.13   70
 50  \w   -122.00 -87.00   0.50    0.10    --  -74.00 -54.00-106.42   70
 51  \w   -130.00 -91.00   0.50    0.10    --  -79.50 -39.00-124.68   78
 52  \w   -132.00 -87.00   0.50    0.10    --  -79.50 -28.00 -41.20   90
 53  \w   -126.00 -93.00   0.50    0.10    --  -79.50-120.00 -35.12   66
 54  \w   -126.00 -93.00   0.50    0.10    --  -79.50-120.00 -72.08   66
 55  \w   -126.00 -92.00   0.50    0.10    --  -79.50-123.00 -96.01   68
 56  \w   -126.00 -93.00   0.50    0.10    --  -79.50-120.00  15.72   66
 57  \w   -126.00 -88.00   0.50    0.10    --  -79.50-130.00  31.23   76
 58  \w   -126.00 -88.00   0.50    0.10    --  -79.50-131.00 124.14   76
;
_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      -0.1100478000
_diffrn_orient_matrix_UB_12      -0.0392683000
_diffrn_orient_matrix_UB_13      -0.0144490000
_diffrn_orient_matrix_UB_21      0.0539079000
_diffrn_orient_matrix_UB_22      -0.0457771000
_diffrn_orient_matrix_UB_23      0.0503202000
_diffrn_orient_matrix_UB_31      -0.0617646000
_diffrn_orient_matrix_UB_32      0.0300107000
_diffrn_orient_matrix_UB_33      0.0578996000
_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  0.0432
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            98753
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.074
_diffrn_reflns_theta_min         2.958
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    2.229
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.490
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.43.89a (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 brown'
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_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_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofurane'
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         9635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0594P)^2^+1.7497P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9016
_reflns_number_total             9635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03787h2.cif
_cod_data_source_block           MaDi329_MaDi_a_(DBA)Cr(CO)3
_cod_depositor_comments
'Adding full bibliography for 7714662--7714667.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7714666
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.509
_shelx_estimated_absorpt_t_max   0.825
_shelx_res_checksum              40282