Storage and release of two electrons from an electron-rich carbon-carbon bond: boron mediated reversible coupling of DMAP and 9-azajulolidine.
Cui, Yunshu; Xiang, Libo; Wang, Junyi; Li, Chunlei; Hao, Wei; Ye, Qing; Chemical communications (Cambridge, England) 56 (2020) 6794–6797; doi:10.1039/d0cc01575j

data_7126527
_publ_section_title
;
 Storage and release of two electrons from an electron-rich carbon-carbon
 bond: boron mediated reversible coupling of DMAP and 9-azajulolidine.
;
_journal_issue                   50
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6794
_journal_page_last               6797
_journal_paper_doi               10.1039/d0cc01575j
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C47 H54 B N4, 4(C H2 Cl2), Br'
_chemical_formula_sum            'C51 H62 B Br Cl8 N4'
_chemical_formula_weight         1105.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2020-02-27 deposited with the CCDC.	2020-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.512(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7601(16)
_cell_length_b                   13.8832(11)
_cell_length_c                   22.628(2)
_cell_measurement_reflns_used    9840
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.31
_cell_volume                     5444.4(8)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1064
_diffrn_reflns_av_unetI/netI     0.0679
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            75216
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.463
_diffrn_reflns_theta_min         2.315
_exptl_absorpt_coefficient_mu    1.185
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6085
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0840 before and 0.0648 after correction.
The Ratio of minimum to maximum transmission is 0.8163.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellowish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.083
_refine_diff_density_max         1.823
_refine_diff_density_min         -1.371
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         11207
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.1789
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7868
_reflns_number_total             11207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01575j2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7126523--7126527.cif.'
_cod_original_cell_volume        5444.3(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        ' C51 H62 B Br Cl8 N4'
_cod_database_code               7126527
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              70299