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_7134237
_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         '2(C48 H70 Al B N P), C5 H12'
_chemical_formula_sum            'C101 H152 Al2 B2 N2 P2'
_chemical_formula_weight         1531.76
_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             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                88.332(2)
_cell_angle_beta                 80.801(2)
_cell_angle_gamma                84.137(2)
_cell_formula_units_Z            1
_cell_length_a                   10.6564(2)
_cell_length_b                   10.7517(2)
_cell_length_c                   20.7177(5)
_cell_measurement_reflns_used    23543
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.6060
_cell_measurement_theta_min      4.1160
_cell_volume                     2330.74(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.30a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.30a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.30a (Rigaku OD, 2021)'
_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 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 0.992
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w   -125.00 -91.00   0.50    0.42    --  -79.50 -61.00 -77.59   68
  2  \w   -125.00 -91.00   0.50    0.42    --  -79.50 -60.00 -18.02   68
  3  \w   -127.00 -92.00   0.50    0.42    --  -79.50 -55.00  73.44   70
  4  \w   -129.00 -93.00   0.50    0.42    --  -79.50 -48.00  36.98   72
  5  \w   -128.00 -93.00   0.50    0.42    --  -79.50 -49.00-150.75   70
  6  \w   -110.00 -31.00   0.50    0.42    --  -60.07 -15.00  90.00  158
  7  \w   -127.00 -92.00   0.50    0.42    --  -79.50 -55.00 142.06   70
  8  \w   -103.00 -68.00   0.50    0.42    --  -54.00 -50.00 125.06   70
  9  \w   -101.00 -61.00   0.50    0.42    --  -50.00 -39.00  66.67   80
 10  \w    -54.00 -26.00   0.50    0.42    --  -14.00 -59.00 119.22   56
 11  \w    -82.00 -47.00   0.50    0.42    --  -34.00 -52.00 -15.75   70
 12  \w    -95.00 -60.00   0.50    0.42    --  -46.00 -48.00  24.48   70
 13  \w    -98.00 -63.00   0.50    0.42    --  -50.00 -51.00 -43.62   70
 14  \w   -100.00 -63.00   0.50    0.42    --  -50.00 -45.00 -91.53   74
 15  \w    -95.00 -60.00   0.50    0.42    --  -46.00 -48.00-152.21   70
 16  \w    -54.00 -26.00   0.50    0.42    --  -14.00 -58.00-157.01   56
 17  \w     46.00 133.00   0.50    0.42    --   82.23  15.00 -60.00  174
 18  \w     97.00 136.00   0.50    0.42    --   85.25  40.00-152.81   78
 19  \w     46.00 133.00   0.50    0.42    --   82.23  15.00-180.00  174
 20  \w     46.00 133.00   0.50    0.42    --   82.23  15.00  30.00  174
 21  \w     98.00 136.00   0.50    0.42    --   85.25  43.00 -30.07   76
 22  \w     98.00 135.00   0.50    0.42    --   85.25  45.00 171.67   74
 23  \w     46.00 133.00   0.50    0.42    --   82.23  15.00  90.00  174
 24  \w     20.00  86.00   0.50    0.42    --   58.47-126.00-120.00  132
 25  \w     40.00  90.00   0.50    0.42    --   82.23 -95.00-120.00  100
 26  \w     41.00  93.00   0.50    0.42    --   85.25-102.00 -27.67  104
 27  \w     40.00  90.00   0.50    0.42    --   82.23 -95.00 -90.00  100
 28  \w     40.00  90.00   0.50    0.42    --   82.23 -95.00  30.00  100
 29  \w     40.00  90.00   0.50    0.42    --   82.23 -95.00  60.00  100
 30  \w     40.00  90.00   0.50    0.42    --   82.23 -95.00 120.00  100
 31  \w     40.00  90.00   0.50    0.42    --   82.23 -95.00   0.00  100
 32  \w     40.00  90.00   0.50    0.42    --   82.23 -95.00-180.00  100
 33  \w     40.00  90.00   0.50    0.42    --   82.23 -95.00-150.00  100
 34  \w     40.00  90.00   0.50    0.42    --   82.23 -95.00 -60.00  100
 35  \w     16.00  66.00   0.50    0.42    --   58.47 -95.00  90.00  100
 36  \w    105.00 131.00   0.50    0.42    --   85.25 110.00 157.69   52
 37  \w     40.00  90.00   0.50    0.42    --   82.23 -95.00 150.00  100
 38  \w     40.00  90.00   0.50    0.42    --   82.23 -95.00  90.00  100
 39  \w   -102.00 -32.00   0.50    0.42    --  -79.50 131.00 122.70  140
 40  \w    -97.00 -33.00   0.50    0.42    --  -79.50 116.00 138.32  128
 41  \w    -97.00 -33.00   0.50    0.42    --  -79.50 115.00 122.13  128
 42  \w    -97.00 -32.00   0.50    0.42    --  -78.00 114.00-100.07  130
 43  \w    -97.00 -33.00   0.50    0.42    --  -79.50 116.00-164.22  128
 44  \w    -97.00 -33.00   0.50    0.42    --  -79.50 115.00 -14.89  128
 45  \w    -97.00 -33.00   0.50    0.42    --  -79.50 115.00   3.91  128
 46  \w    -97.00 -33.00   0.50    0.42    --  -79.50 116.00  66.97  128
 47  \w   -126.00 -96.00   0.50    0.42    --  -79.50-116.00 176.26   60
 48  \w   -125.00 -97.00   0.50    0.42    --  -79.50-113.00 -22.30   56
;
_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      -0.0224203000
_diffrn_orient_matrix_UB_12      -0.0830309000
_diffrn_orient_matrix_UB_13      0.0618151000
_diffrn_orient_matrix_UB_21      -0.1399220000
_diffrn_orient_matrix_UB_22      -0.0051166000
_diffrn_orient_matrix_UB_23      -0.0093382000
_diffrn_orient_matrix_UB_31      0.0397279000
_diffrn_orient_matrix_UB_32      -0.1176031000
_diffrn_orient_matrix_UB_33      -0.0420362000
_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  0.0278
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46152
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.165
_diffrn_reflns_theta_min         4.134
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.659
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.42.30a (Rigaku Oxford Diffraction, 2021) 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    1.091
_exptl_crystal_description       block
_exptl_crystal_F_000             838
_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          0.260
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         9235
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0505P)^2^+0.9076P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8334
_reflns_number_total             9235
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00308c3.cif
_cod_data_source_block           LeWu008_TiWe_refine2_a_cmpd2
_cod_depositor_comments
'Adding full bibliography for 7134237--7134239.cif.'
_cod_database_code               7134237
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.793
_shelx_estimated_absorpt_t_max   0.937
_shelx_res_checksum              97565
_shelx_hkl_checksum              64434