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_7703565
_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            'C79 H88 B2 K2 N4 O2'
_chemical_formula_weight         1225.35
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.394(3)
_cell_length_b                   33.394(3)
_cell_length_c                   12.3370(9)
_cell_measurement_reflns_used    4116
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.81
_cell_measurement_theta_min      2.44
_cell_volume                     13758(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Smart Apex (CCD)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            38965
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         0.862
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  0.9663
_exptl_absorpt_correction_T_min  0.8578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/2'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       prism
_exptl_crystal_F_000             5232
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     819
_refine_ls_number_reflns         12049
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0658
_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^)+(0.1088P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1604
_refine_ls_wR_factor_ref         0.1753
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                8868
_reflns_number_total             12049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04652f2.cif
_cod_data_source_block           bianbok
_cod_depositor_comments
'Adding full bibliography for 7703563--7703565.cif.'
_cod_database_code               7703565
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.937
_shelx_estimated_absorpt_t_max   0.964
_shelx_res_checksum              91598