Expression of hyperconjugative stereoelectronic interactions in borazines.
Wakchaure, Vivek Chandrakant; Dosso, Jacopo; Crosta, Martina; Kählig, Hanspeter; Ward, Benjamin D.; Bonifazi, Davide; Chemical communications (Cambridge, England) 61 (2025) 1200–1203; doi:10.1039/d4cc05188b

data_7134032
_publ_section_title
;
 Expression of hyperconjugative stereoelectronic interactions in
 borazines.
;
_journal_issue                   6
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1200
_journal_page_last               1203
_journal_paper_doi               10.1039/d4cc05188b
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C36 H48 B3 N3'
_chemical_formula_sum            'C36 H48 B3 N3'
_chemical_formula_weight         555.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-05-06 deposited with the CCDC.	2024-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8518(8)
_cell_length_b                   12.9244(10)
_cell_length_c                   21.2118(19)
_cell_measurement_reflns_used    12452
_cell_measurement_temperature    293
_cell_measurement_theta_max      20.35
_cell_measurement_theta_min      2.27
_cell_volume                     3249.2(4)
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)'
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1050
_diffrn_reflns_av_unetI/netI     0.0791
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31179
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.332
_diffrn_source                   'Axo Mo'
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.9950
_exptl_absorpt_correction_T_min  0.3695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_recrystallization_method 'Slow evaporation CH2Cl2'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 1233 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   4.8(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         5613
_refine_ls_number_restraints     775
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0857P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1370
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_full    0.963
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                3128
_reflns_number_total             5613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05188b2.cif
_cod_data_source_block           bvw129
_cod_depositor_comments
'Adding full bibliography for 7134031--7134032.cif.'
_cod_database_code               7134032
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.981
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: H7B(0.5) H7A(0.5) C11(0.5) H11A(0.5) H11B(0.5) C8(0.5) H8A(0.5)
 H8B(0.5) C9(0.5) H9A(0.5) H9B(0.5) C10(0.5) H10A(0.5) H10B(0.5) C12(0.5)
 H12A(0.5) H12B(0.5) C37(0.5) H37A(0.5) H37B(0.5) C38(0.5) H38A(0.5) H38B(0.5)
 C39(0.5) H39A(0.5) H39B(0.5) C40(0.5) H40A(0.5) H40B(0.5) C41(0.5) H41A(0.5)
 H41B(0.5)
5.a Ternary CH refined with riding coordinates:
 C31(H31), C7(H7B), C7(H7A), C19(H19)
5.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C23(H23A,H23B), C36(H36A,H36B), C34(H34A,H34B), C35(H35A,
 H35B), C21(H21A,H21B), C33(H33A,H33B), C20(H20A,H20B), C24(H24A,H24B),
 C11(H11A,H11B), C22(H22A,H22B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B),
 C12(H12A,H12B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
  C41(H41A,H41B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C28(H28), C14(H14), C26(H26), C3(H3), C27(H27), C5(H5),
 C18(H18), C4(H4), C17(H17), C30(H30), C29(H29), C15(H15), C16(H16)
;
_shelx_res_checksum              60487
_shelx_hkl_checksum              63116
_olex2_submission_special_instructions 'No special instructions were received'