A BNAlP-heterocycle.
Wellnitz, Tim; Wüst, Leonie; Braunschweig, Holger; Hering-Junghans, Christian; Chemical communications (Cambridge, England) 61 (2025) 4014–4017; doi:10.1039/d5cc00308c

data_7134238
_publ_section_title
;
 A BNAlP-heterocycle.
;
_journal_issue                   20
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4014
_journal_page_last               4017
_journal_paper_doi               10.1039/d5cc00308c
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C52 H74 Al B N P, C6 H6'
_chemical_formula_sum            'C58 H80 Al B N P'
_chemical_formula_weight         859.99
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-09-27
_audit_creation_method           'CIF-fill 1.5e (K.Radacki, 2005-23)'
_audit_update_record
;
2025-01-16 deposited with the CCDC.	2025-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                73.2850(10)
_cell_angle_beta                 82.1070(10)
_cell_angle_gamma                75.4270(10)
_cell_formula_units_Z            2
_cell_length_a                   10.18840(10)
_cell_length_b                   13.07660(10)
_cell_length_c                   21.5233(2)
_cell_measurement_reflns_used    25060
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.3260
_cell_measurement_theta_min      3.6070
_cell_volume                     2651.49(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.100a (Rigaku OD, 2023)'
_computing_data_collection
;
 CrysAlisPro system (CCD 42.94a 64-bit (release 21-06-2023))
;
_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 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 0.993
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     34.00  60.00   0.50    0.18    --   22.00  59.00-108.88   52
  2  \w     30.00  56.00   0.50    0.18    --   18.00  60.00  26.98   52
  3  \w     34.00  60.00   0.50    0.18    --   22.00  59.00  63.38   52
  4  \w     46.00 133.00   0.50    0.18    --   82.26  15.00  90.00  174
  5  \w     98.00 133.00   0.50    0.18    --   85.25  53.00 -17.22   70
  6  \w     46.00 133.00   0.50    0.18    --   82.26  15.00 -60.00  174
  7  \w     46.00 133.00   0.50    0.18    --   82.26  15.00 -90.00  174
  8  \w     38.00 109.00   0.50    0.18    --   58.45  15.00-150.00  142
  9  \w    -95.00 -60.00   0.50    0.18    --  -46.00 -49.00 -15.45   70
 10  \w   -124.00 -94.00   0.50    0.18    --  -79.50 -64.00-129.37   60
 11  \w   -124.00 -89.00   0.50    0.18    --  -78.00 -61.00 -87.32   70
 12  \w   -120.00 -86.00   0.50    0.18    --  -74.00 -59.00 -75.53   68
 13  \w    -95.00 -60.00   0.50    0.18    --  -46.00 -50.00  71.65   70
 14  \w    -94.00 -59.00   0.50    0.18    --  -46.00 -51.00 150.31   70
 15  \w   -125.00 -91.00   0.50    0.18    --  -79.50 -60.00 137.23   68
 16  \w   -121.00 -86.00   0.50    0.18    --  -74.00 -57.00 174.45   70
 17  \w   -121.00 -86.00   0.50    0.18    --  -74.00 -58.00 109.13   70
 18  \w   -117.00 -84.00   0.50    0.18    --  -70.00 -57.00  92.10   66
 19  \w   -121.00 -86.00   0.50    0.18    --  -74.00 -58.00  58.10   70
 20  \w   -121.00 -86.00   0.50    0.18    --  -74.00 -56.00  38.09   70
 21  \w   -121.00 -86.00   0.50    0.18    --  -74.00 -56.00 -51.43   70
 22  \w   -118.00 -83.00   0.50    0.18    --  -70.00 -54.00 -69.45   70
 23  \w   -102.00 -67.00   0.50    0.18    --  -54.00 -52.00-116.89   70
 24  \w   -127.00 -92.00   0.50    0.18    --  -79.50 -53.00-112.55   70
 25  \w   -114.00 -79.00   0.50    0.18    --  -66.00 -52.00 -50.46   70
 26  \w   -103.00 -67.00   0.50    0.18    --  -54.00 -46.00-164.24   72
 27  \w   -111.00 -76.00   0.50    0.18    --  -62.00 -49.00 -37.55   70
 28  \w   -124.00 -87.00   0.50    0.18    --  -74.00 -44.00 -13.88   74
 29  \w   -129.00 -93.00   0.50    0.18    --  -79.50 -48.00  12.90   72
 30  \w   -122.00 -87.00   0.50    0.18    --  -74.00 -52.00 145.17   70
 31  \w   -124.00 -86.00   0.50    0.18    --  -74.00 -43.00 176.46   76
 32  \w   -106.00 -71.00   0.50    0.18    --  -58.00 -52.00 110.87   70
 33  \w   -124.00 -87.00   0.50    0.18    --  -74.00 -44.00  61.31   74
 34  \w   -125.00 -84.00   0.50    0.18    --  -79.50-139.00-141.62   82
 35  \w   -127.00 -90.00   0.50    0.18    --  -79.50-126.00-119.27   74
 36  \w   -127.00 -89.00   0.50    0.18    --  -79.50-129.00  19.28   76
 37  \w   -126.00 -95.00   0.50    0.18    --  -79.50-117.00-141.21   62
 38  \w   -125.00 -94.00   0.50    0.18    --  -79.50-119.00 -14.08   62
 39  \w   -126.00 -92.00   0.50    0.18    --  -79.50-122.00  88.48   68
 40  \w   -126.00 -92.00   0.50    0.18    --  -79.50-123.00 144.24   68
 41  \w   -126.00 -93.00   0.50    0.18    --  -79.50-120.00 169.99   66
 42  \w    -92.00 -31.00   0.50    0.18    --  -76.37 112.00 120.00  122
 43  \w   -100.00 -62.00   0.50    0.18    --  -79.50 126.00 107.98   76
 44  \w    -45.00 -18.00   0.50    0.18    --  -14.00 132.00  18.18   54
 45  \w    -92.00 -31.00   0.50    0.18    --  -76.37 112.00 150.00  122
 46  \w    -92.00 -31.00   0.50    0.18    --  -76.37 112.00  30.00  122
 47  \w    -92.00 -31.00   0.50    0.18    --  -76.37 112.00  60.00  122
 48  \w    -97.00 -32.00   0.50    0.18    --  -78.00 114.00 -79.22  130
 49  \w    -97.00 -22.00   0.50    0.18    --  -69.54 126.00-180.00  150
 50  \w    -92.00 -31.00   0.50    0.18    --  -76.37 112.00-120.00  122
 51  \w     40.00  90.00   0.50    0.18    --   82.26 -95.00 -90.00  100
 52  \w     42.00  93.00   0.50    0.18    --   85.25 -98.00-170.60  102
 53  \w     39.00 108.00   0.50    0.18    --   85.25-139.00  98.84  138
 54  \w     39.00  98.00   0.50    0.18    --   85.25-119.00 112.03  118
 55  \w     37.00  93.00   0.50    0.18    --   82.26-112.00 150.00  112
 56  \w     42.00  93.00   0.50    0.18    --   85.25 -97.00 112.06  102
 57  \w     29.00  79.00   0.50    0.18    --   71.26 -95.00  30.00  100
 58  \w     40.00  90.00   0.50    0.18    --   82.26 -95.00  60.00  100
 59  \w     40.00  90.00   0.50    0.18    --   82.26 -95.00  30.00  100
 60  \w     40.00  90.00   0.50    0.18    --   82.26 -95.00   0.00  100
 61  \w     40.00  90.00   0.50    0.18    --   82.26 -95.00 -60.00  100
 62  \w     43.00  92.00   0.50    0.18    --   85.25 -95.00-118.06   98
 63  \w     40.00  90.00   0.50    0.18    --   82.26 -95.00-150.00  100
;
_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      0.0867548000
_diffrn_orient_matrix_UB_12      -0.0936806000
_diffrn_orient_matrix_UB_13      0.0493122000
_diffrn_orient_matrix_UB_21      0.0033648000
_diffrn_orient_matrix_UB_22      0.0803467000
_diffrn_orient_matrix_UB_23      0.0396111000
_diffrn_orient_matrix_UB_31      -0.1303518000
_diffrn_orient_matrix_UB_32      -0.0263712000
_diffrn_orient_matrix_UB_33      0.0401497000
_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  0.0345
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.993
_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       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            62117
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.280
_diffrn_reflns_theta_min         3.621
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.874
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.856
_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    1.077
_exptl_crystal_description       plate
_exptl_crystal_F_000             936
_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          0.140
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         10460
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0616
_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^)+(0.0833P)^2^+2.1038P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.1711
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8929
_reflns_number_total             10460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00308c3.cif
_cod_data_source_block           TiWe26_a_cmpd3
_cod_depositor_comments
'Adding full bibliography for 7134237--7134239.cif.'
_cod_original_cell_volume        2651.49(5)
_cod_database_code               7134238
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.887
_shelx_estimated_absorpt_t_max   0.966
_shelx_res_checksum              99682
_shelx_hkl_checksum              22396