Alkali metal reduction of 1,3,2-diazaborol and 1,3,2-diazagermol derivatives based on 1,2-bis[(2,6-diisopropylphenyl)imino]acenaphthene.
Lukina, Daria A.; Skatova, Alexandra A.; Lukoyanov, Anton N.; Kozlova, Ekaterina A.; Fedushkin, Igor L.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2941–2946; doi:10.1039/c9dt04652f

data_7703563
_publ_section_title
;
 Alkali metal reduction of 1,3,2-diazaborol and 1,3,2-diazagermol
 derivatives based on 1,2-bis[(2,6-diisopropylphenyl)imino]acenaphthene.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2941
_journal_page_last               2946
_journal_paper_doi               10.1039/c9dt04652f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C96.75 H127 B2 Br2 Li4 N4 O4'
_chemical_formula_weight         1619.22
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-10-04 deposited with the CCDC.	2020-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                101.192(2)
_cell_angle_beta                 102.617(2)
_cell_angle_gamma                91.829(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2924(4)
_cell_length_b                   14.4434(3)
_cell_length_c                   24.8139(7)
_cell_measurement_reflns_used    10288
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.1560
_cell_measurement_theta_min      3.3300
_cell_volume                     4546.7(2)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'SHELXTL  (Sheldrick, 2003)'
_computing_publication_material  'SHELXTL  (Sheldrick, 2003)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_unetI/netI     0.0737
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            73871
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.038
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.942
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SCALE3 ABSPACK, CrysAlisPro, Agilent Technologies (2012) 
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       prism
_exptl_crystal_F_000             1719
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.435
_exptl_crystal_size_min          0.330
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1209
_refine_ls_number_reflns         17853
_refine_ls_number_restraints     278
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0684P)^2^+0.8144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1285
_refine_ls_wR_factor_ref         0.1456
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11573
_reflns_number_total             17853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04652f2.cif
_cod_data_source_block           bbian3
_cod_depositor_comments
'Adding full bibliography for 7703563--7703565.cif.'
_cod_database_code               7703563
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.558
_shelx_estimated_absorpt_t_max   0.746
_shelx_res_checksum              40427