Multiple deprotonation of primary aromatic diamines by LiAlH4.
Less, Robert J.; Allen, Lucy K.; Steiner, Alexander; Wright, Dominic S.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 4141–4147; doi:10.1039/c4dt03802a

data_7033661
_publ_section_title
;
 Multiple deprotonation of primary aromatic diamines by LiAlH4.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4141
_journal_page_last               4147
_journal_paper_doi               10.1039/c4dt03802a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C20 H16 Al N4 1-, C12 H32 Li N4 1+'
_chemical_formula_sum            'C32 H48 Al Li N8'
_chemical_formula_weight         578.70
_chemical_name_systematic
; 
 ? 
;
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-12-08 deposited with the CCDC.
2015-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   21.4696(13)
_cell_length_b                   21.4696(13)
_cell_length_c                   29.3995(17)
_cell_measurement_reflns_used    5514
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      79.77
_cell_measurement_theta_min      6.613
_cell_volume                     13551.5(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            9270
_diffrn_reflns_theta_full        56.02
_diffrn_reflns_theta_max         56.02
_diffrn_reflns_theta_min         7.94
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4992
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/TMEDA'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.162
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2194
_refine_ls_number_restraints     209
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1388
_refine_ls_R_factor_gt           0.1034
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1500P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2653
_refine_ls_wR_factor_ref         0.2892
_reflns_number_gt                1531
_reflns_number_total             2194
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt03802a2.cif
_cod_data_source_block           dw1436afddd
_cod_depositor_comments
'Adding full bibliography for 7033660--7033662.cif.'
_cod_original_sg_symbol_H-M      Fddd
_cod_database_code               7033661