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_7703564
_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            'C48 H71 Ge N2 Na O6'
_chemical_formula_weight         867.64
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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            4
_cell_length_a                   12.205(3)
_cell_length_b                   19.4474(18)
_cell_length_c                   20.653(6)
_cell_measurement_reflns_used    3434
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.2400
_cell_measurement_theta_min      3.5560
_cell_volume                     4902.1(19)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur EOS'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17664
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.556
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       plate
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.510
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 2579 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         9511
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0393P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                7444
_reflns_number_total             9511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04652f2.cif
_cod_data_source_block           gebianna
_cod_depositor_comments
'Adding full bibliography for 7703563--7703565.cif.'
_cod_original_cell_volume        4902.1(18)
_cod_database_code               7703564
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.723
_shelx_estimated_absorpt_t_max   0.929
_shelx_res_checksum              45468