Hetero Diels-Alder reactions of isolable <i>N</i>-borylenamines.
Liang, Pei; Wei, Junhui; Wei, Yongliang; Wang, Xue; Liu, Fei; Wang, Tongdao; Chemical communications (Cambridge, England) 60 (2024) 5964–5967; doi:10.1039/d4cc01645a

data_7133053
_publ_section_title
;
 Hetero Diels-Alder reactions of isolable <i>N</i>-borylenamines.
;
_journal_issue                   46
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5964
_journal_page_last               5967
_journal_paper_doi               10.1039/d4cc01645a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C33 H11 B F15 N'
_chemical_formula_sum            'C33 H11 B F15 N'
_chemical_formula_weight         717.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
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_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-13
_audit_creation_method
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Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-05-07 deposited with the CCDC.	2024-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                100.952(9)
_cell_angle_beta                 99.276(8)
_cell_angle_gamma                103.819(8)
_cell_formula_units_Z            2
_cell_length_a                   10.152(3)
_cell_length_b                   10.204(3)
_cell_length_c                   14.905(4)
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_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD area detector'
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_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.0724
_diffrn_reflns_Laue_measured_fraction_full 0.996
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_diffrn_reflns_limit_h_max       13
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_diffrn_reflns_limit_k_min       -13
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_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29331
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.966
_diffrn_reflns_theta_min         2.281
_diffrn_source                   'sealed X-ray tube'
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_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.165
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_exptl_absorpt_correction_T_min  0.6736
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
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_exptl_crystal_description       block
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_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0498P)^2^+0.2302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1245
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4753
_reflns_number_total             7436
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01645a2.cif
_cod_data_source_block           mo_22may01lp1_0m
_cod_depositor_comments
'Adding full bibliography for 7133047--7133054.cif.'
_cod_original_cell_volume        1437.0(7)
_cod_database_code               7133053
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.966
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C15(H15), C3(H3), C14(H14), C12(H12), C11(H11), C4(H4), C13(H13),
 C5(H5)
;
_shelx_res_checksum              51785
_shelx_hkl_checksum              95337
_olex2_submission_special_instructions 'No special instructions were received'