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_7033660
_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
"'C68 H96 Al4 Li4 N12 O8, 0.5 (C4 H8 O),   0.5 (C6 11 H25)'"
_chemical_formula_sum            'C73 H107 Al4 Li4 N12 O8.5'
_chemical_formula_weight         1424.39
_chemical_name_systematic
; 
 ? 
;
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 101.022(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8568(5)
_cell_length_b                   25.4155(9)
_cell_length_c                   20.1493(8)
_cell_measurement_reflns_used    259874
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      23.82
_cell_measurement_theta_min      1.00
_cell_volume                     7970.6(5)
_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 0.973
_diffrn_measured_fraction_theta_max 0.973
_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           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32127
_diffrn_reflns_theta_full        23.80
_diffrn_reflns_theta_max         23.80
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.867
_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    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3044
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/hexane'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     926
_refine_ls_number_reflns         11879
_refine_ls_number_restraints     1553
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+11.0116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
_refine_ls_wR_factor_ref         0.1814
_reflns_number_gt                7865
_reflns_number_total             11879
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt03802a2.cif
_cod_data_source_block           dw1355
_cod_depositor_comments
'Adding full bibliography for 7033660--7033662.cif.'
_cod_original_cell_volume        7970.5(5)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C73 H107 Al4 Li4 N12 O8.50'
_cod_database_code               7033660