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_7126524
_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         'C86 H100 B2 N8'
_chemical_formula_sum            'C86 H100 B2 N8'
_chemical_formula_weight         1267.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-12-27
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2020-02-27 deposited with the CCDC.	2020-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.157(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.282(2)
_cell_length_b                   30.185(4)
_cell_length_c                   18.933(2)
_cell_measurement_reflns_used    9486
_cell_measurement_temperature    99.92
_cell_measurement_theta_max      24.70
_cell_measurement_theta_min      2.30
_cell_volume                     9210.8(19)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_structure_refinement  'XL n/a (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99.92
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1113
_diffrn_reflns_av_unetI/netI     0.0954
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            88147
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.774
_diffrn_reflns_theta_max         24.774
_diffrn_reflns_theta_min         2.296
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.053
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0831 before and 0.0602 after correction.
The Ratio of minimum to maximum transmission is 0.8722.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    0.914
_exptl_crystal_description       prism
_exptl_crystal_F_000             2728
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.154
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         15742
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1351
_refine_ls_R_factor_gt           0.0731
_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^)+(0.1138P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1981
_refine_ls_wR_factor_ref         0.2251
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8095
_reflns_number_total             15742
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01575j2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7126523--7126527.cif.'
_cod_original_cell_volume        9211(2)
_cod_database_code               7126524
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C019(H019), C18(H18), C21(H21), C30(H30), C33(H33), C60(H60), C69(H69),
 C72(H72)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C00P(H00P), C15(H15), C14(H14),
 C16(H16), C26(H26), C27(H27), C28(H28), C36(H36), C37(H37), C39(H39), C40(H40),
  C46(H46), C47(H47), C49(H49), C50(H50), C53(H53), C54(H54), C55(H55),
 C65(H65), C66(H66), C67(H67), C78(H78), C79(H79), C80(H80), C83(H83), C84(H84),
  C85(H85)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C),
 C48(H48A,H48B,H48C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C61(H61A,H61B,
 H61C), C62(H62A,H62B,H62C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C73(H73A,
 H73B,H73C), C74(H74A,H74B,H74C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              94927
_shelx_fab_checksum              89676
_olex2_submission_special_instructions 'No special instructions were received'