Formation of an air-stable diborane <i>via</i> a stepwise BH<sub>3</sub> addition of pyrido[1,2-<i>a</i>]isoindole with H<sub>2</sub> evolution.
Dong, Jiaqi; Zhang, Lutao; Tan, Dehui; Wu, Jianfeng; Wang, Nan; Mellerup, Soren K.; Wang, Suning; Yang, Deng-Tao; Chemical communications (Cambridge, England) 57 (2021) 9882–9885; doi:10.1039/d1cc04228a

data_7128945
_publ_section_title
;
 Formation of an air-stable diborane <i>via</i> a stepwise BH<sub>3</sub>
 addition of pyrido[1,2-<i>a</i>]isoindole with H<sub>2</sub> evolution.
;
_journal_issue                   77
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9882
_journal_page_last               9885
_journal_paper_doi               10.1039/d1cc04228a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C12 H13 B2 N'
_chemical_formula_sum            'C12 H13 B2 N'
_chemical_formula_weight         192.85
_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
_audit_creation_date             2020-11-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-08-03 deposited with the CCDC.	2021-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                69.122(5)
_cell_angle_beta                 89.652(6)
_cell_angle_gamma                83.064(6)
_cell_formula_units_Z            2
_cell_length_a                   6.995(5)
_cell_length_b                   8.942(6)
_cell_length_c                   9.230(6)
_cell_measurement_reflns_used    558
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      2.73
_cell_volume                     535.1(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      179.98
_diffrn_measured_fraction_theta_full 0.814
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 0.814
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2289
_diffrn_reflns_point_group_measured_fraction_full 0.814
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.992
_diffrn_reflns_theta_min         2.732
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.995
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             204
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.118
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         1574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0581P)^2^+0.1377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1351
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1080
_reflns_number_total             1574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04228a2.cif
_cod_data_source_block           dy9b
_cod_depositor_comments          'Adding full bibliography for 7128945.cif.'
_cod_database_code               7128945
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.987
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Uiso: H1A(0.05) H1B(0.05) H1C(0.05) H2A(0.05) H2B(0.05)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'