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_7134239
_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         'C56 H78 Al B N P, 2(C5 H12)'
_chemical_formula_sum            'C66 H102 Al B N P'
_chemical_formula_weight         978.332
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2024-10-10
_audit_creation_method
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_audit_update_record
;
2025-01-16 deposited with the CCDC.	2025-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                64.5271(9)
_cell_angle_beta                 81.4188(8)
_cell_angle_gamma                85.6856(8)
_cell_formula_units_Z            2
_cell_length_a                   12.62854(13)
_cell_length_b                   16.37572(14)
_cell_length_c                   16.40523(16)
_cell_measurement_reflns_used    50929
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.0470
_cell_measurement_theta_min      2.9730
_cell_volume                     3028.30(6)
_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    'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_structure_refinement
'olex2.refine 1.5-ac6-020 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.9933
_diffrn_measured_fraction_theta_max 0.9507
_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     37.00  93.00   0.50    0.05    --   82.26-112.00-120.00  112
  2  \w     41.00  93.00   0.50    0.05    --   85.25-102.00 -78.16  104
  3  \w     41.00  93.00   0.50    0.05    --   85.25-101.00 -27.91  104
  4  \w     40.00  90.00   0.50    0.05    --   82.26 -95.00 -30.00  100
  5  \w     43.00  92.00   0.50    0.05    --   85.25 -96.00  50.58   98
  6  \w     40.00  90.00   0.50    0.05    --   82.26 -95.00 120.00  100
  7  \w     40.00  90.00   0.50    0.05    --   82.26 -95.00-120.00  100
  8  \w     40.00  90.00   0.50    0.05    --   82.26 -95.00-180.00  100
  9  \w     40.00  90.00   0.50    0.05    --   82.26 -95.00-150.00  100
 10  \w     43.00  92.00   0.50    0.05    --   85.25 -94.00-115.81   98
 11  \w     52.00 122.00   0.50    0.05    --   71.26  17.00  27.00  140
 12  \w     39.00 109.00   0.50    0.05    --   58.45  17.00  27.00  140
 13  \w     63.00 133.00   0.50    0.05    --   82.26  17.00  27.00  140
 14  \w     98.00 136.00   0.50    0.05    --   85.25  43.00 110.91   76
 15  \w     76.00 116.00   0.50    0.05    --   64.85  36.00  67.34   80
 16  \w     56.00  91.00   0.50    0.05    --   42.00  49.00  43.85   70
 17  \w     30.00  56.00   0.50    0.05    --   18.00  60.00  80.12   52
 18  \w     34.00  60.00   0.50    0.05    --   22.00  59.00 112.65   52
 19  \w     34.00  60.00   0.50    0.05    --   22.00  57.00  34.41   52
 20  \w     34.00  60.00   0.50    0.05    --   22.00  59.00 -53.38   52
 21  \w     30.00  56.00   0.50    0.05    --   18.00  60.00 -97.73   52
 22  \w     30.00  56.00   0.50    0.05    --   18.00  60.00-177.55   52
 23  \w     34.00  60.00   0.50    0.05    --   22.00  58.00-140.21   52
 24  \w     59.00  94.00   0.50    0.05    --   46.00  52.00 121.83   70
 25  \w    -93.00 -35.00   0.50    0.05    --  -79.50 106.00 119.22  116
 26  \w   -102.00 -32.00   0.50    0.05    --  -79.50 130.00  93.54  140
 27  \w    -97.00 -33.00   0.50    0.05    --  -79.50 116.00 146.87  128
 28  \w    -97.00 -33.00   0.50    0.05    --  -79.50 115.00  53.43  128
 29  \w    -97.00 -32.00   0.50    0.05    --  -78.00 115.00  42.75  130
 30  \w    -97.00 -32.00   0.50    0.05    --  -78.00 114.00  17.43  130
 31  \w    -97.00 -32.00   0.50    0.05    --  -78.00 114.00 -17.08  130
 32  \w    -97.00 -22.00   0.50    0.05    --  -69.54 126.00-150.00  150
 33  \w    -92.00 -31.00   0.50    0.05    --  -76.37 112.00-120.00  122
 34  \w    -88.00 -14.00   0.50    0.05    --  -60.16 126.00 -90.00  148
 35  \w    -92.00 -31.00   0.50    0.05    --  -76.37 112.00 -30.00  122
 36  \w    -31.00  -4.00   0.50    0.05    --  -14.00 111.00  63.24   54
 37  \w    -92.00 -31.00   0.50    0.05    --  -76.37 112.00 150.00  122
 38  \w   -123.00 -97.00   0.50    0.05    --  -79.50 -66.00  78.41   52
 39  \w   -126.00 -91.00   0.50    0.05    --  -79.50 -58.00 120.34   70
 40  \w   -124.00 -92.00   0.50    0.05    --  -79.50 -63.00 -23.95   64
 41  \w   -124.00 -92.00   0.50    0.05    --  -79.50 -63.00  -8.15   64
 42  \w   -102.00 -67.00   0.50    0.05    --  -54.00 -52.00 -61.77   70
 43  \w   -102.00 -67.00   0.50    0.05    --  -54.00 -52.00 -44.56   70
 44  \w   -126.00 -92.00   0.50    0.05    --  -79.50 -57.00-105.36   68
 45  \w   -120.00 -86.00   0.50    0.05    --  -74.00 -59.00-126.63   68
 46  \w   -124.00 -92.00   0.50    0.05    --  -79.50 -63.00-154.69   64
 47  \w   -102.00 -67.00   0.50    0.05    --  -54.00 -52.00-151.84   70
 48  \w   -120.00 -83.00   0.50    0.05    --  -70.00 -45.00  79.31   74
 49  \w   -128.00 -93.00   0.50    0.05    --  -79.50 -49.00 157.14   70
 50  \w   -107.00 -72.00   0.50    0.05    --  -58.00 -48.00 122.30   70
 51  \w    -96.00 -58.00   0.50    0.05    --  -46.00 -43.00 144.60   76
 52  \w   -132.00 -81.00   0.50    0.05    --  -79.50 -24.00  -9.13  102
 53  \w   -111.00 -41.00   0.50    0.05    --  -60.16 -17.00-141.00  140
 54  \w   -120.00 -50.00   0.50    0.05    --  -69.54 -17.00-141.00  140
 55  \w   -127.00 -57.00   0.50    0.05    --  -76.37 -17.00-141.00  140
 56  \w   -126.00 -85.00   0.50    0.05    --  -79.50-137.00 -25.22   82
 57  \w   -126.00 -92.00   0.50    0.05    --  -79.50-123.00  79.58   68
 58  \w   -126.00 -92.00   0.50    0.05    --  -79.50-123.00 -11.54   68
 59  \w   -126.00 -93.00   0.50    0.05    --  -79.50-120.00  54.04   66
 60  \w   -126.00 -93.00   0.50    0.05    --  -79.50-121.00 -71.50   66
 61  \w   -126.00 -93.00   0.50    0.05    --  -79.50-120.00-103.12   66
 62  \w   -126.00 -92.00   0.50    0.05    --  -79.50-123.00-132.17   68
 63  \w   -126.00 -93.00   0.50    0.05    --  -79.50-121.00-164.08   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0920612000
_diffrn_orient_matrix_UB_12      -0.0126980000
_diffrn_orient_matrix_UB_13      -0.0667427000
_diffrn_orient_matrix_UB_21      -0.0782665000
_diffrn_orient_matrix_UB_22      0.0194698000
_diffrn_orient_matrix_UB_23      -0.0699907000
_diffrn_orient_matrix_UB_31      0.0249394000
_diffrn_orient_matrix_UB_32      0.1015886000
_diffrn_orient_matrix_UB_33      -0.0406447000
_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  0.0205
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_Laue_measured_fraction_full 0.9933
_diffrn_reflns_Laue_measured_fraction_max 0.9507
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            71227
_diffrn_reflns_point_group_measured_fraction_full 0.9933
_diffrn_reflns_point_group_measured_fraction_max 0.9507
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         75.22
_diffrn_reflns_theta_min         2.99
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.470
_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            colourless
_exptl_crystal_density_diffrn    1.073
_exptl_crystal_description       block
_exptl_crystal_F_000             1079.667
_exptl_crystal_size_max          0.452
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.128
_refine_diff_density_max         0.5756
_refine_diff_density_min         -0.4515
_refine_diff_density_rms         0.0384
_refine_ls_d_res_high            0.7973
_refine_ls_d_res_low             14.7827
_refine_ls_goodness_of_fit_ref   1.0521
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    146
_refine_ls_number_parameters     969
_refine_ls_number_reflns         11882
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.0508
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.0036
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+0.9724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0935
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              20
_reflns_limit_k_min              -17
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                11095
_reflns_number_total             11882
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5cc00308c3.cif
_cod_data_source_block           TiWe36_a_cmpd4
_cod_depositor_comments
'Adding full bibliography for 7134237--7134239.cif.'
_cod_original_cell_volume        3028.31(5)
_cod_database_code               7134239
_chemical_oxdiff_formula         C66H98BNAlP
_chemical_oxdiff_usercomment     TW194
_cell_oxdiff_angle_alpha         64.5271(9)
_cell_oxdiff_angle_beta          81.4188(8)
_cell_oxdiff_angle_gamma         85.6856(8)
_cell_oxdiff_length_a            12.62854(13)
_cell_oxdiff_length_b            16.37572(14)
_cell_oxdiff_length_c            16.40523(16)
_cell_oxdiff_measurement_reflns_used 50929
_cell_oxdiff_volume              3028.31(5)
_reflns_odcompleteness_completeness 99.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, H2 of C2
 At 1.2 times of:
  H4 of C4, H6 of C6, H8 of C8, H5 of C5, H7 of C7, H51 of C51, {H3A,H3B} of
  C3, H54 of C54, {H2A,H2B} of C2, {H4A,H4B} of C4, {H2A,H2B} of C2, {H3A,H3B}
  of C3, {H4A,H4B} of C4, {H4A,H4B} of C4, {H2A,H2B} of C2, {H3A,H3B} of C3,
  {H4A,H4B} of C4, {H2A,H2B} of C2, {H3A,H3B} of C3, H31 of C31, H35 of C35,
  H45 of C45, H41 of C41, H29 of C29, H36 of C36, H43 of C43, H30 of C30, H42
  of C42, H37 of C37, H48 of C48
 At 1.4 times of:
  {H1,H1AA} of C1
2. Restrained distances
 C1_12-C2_12 = C2_12-C3_12 = C3_12-C4_12 = C4_12-C5_12
 C1_13-C2_13 = C2_13-C3_13 = C3_13-C4_13 = C4_13-C5_13
 C1_121-C2_121 = C2_121-C3_121 = C3_121-C4_121 = C4_121-C5_121
 C1_131-C2_131 = C2_131-C3_131 = C3_131-C4_131 = C4_131-C5_131
 1.531 with sigma of 0.002
 C1_12-C3_12 = C3_12-C5_12 = C2_12-C4_12
 C1_13-C3_13 = C3_13-C5_13 = C2_13-C4_13
 C1_121-C3_121 = C3_121-C5_121 = C2_121-C4_121
 C1_131-C3_131 = C3_131-C5_131 = C2_131-C4_131
 2.552 with sigma of 0.003
3. Uiso/Uaniso restraints and constraints
: within 2A with sigma of 0.008 and sigma for terminal atoms of 0.016 within 2A
: with sigma of 0.006 and sigma for terminal atoms of 0.012
4. Rigid body (RIGU) restrains
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=
 Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=
 Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=
 Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=1-FVAR(2)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=
 Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B),
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
6.b Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C1(H1A,
 H1B,H1C), C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C5(H5A,H5B,H5C)
;
_olex2_refine_details
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA 5.0
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         R2SCAN
   BASIS SET:      def2-TZVP
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2024-10-09_20-26-04
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.246
_oxdiff_exptl_absorpt_empirical_full_min 0.847