Structures and reactions of monomeric and dimeric lithium diazapentadienyl complexes with electrophiles: synthesis of α-C,C'-dialkyl-β-diimines, and dissolution-reversible synthesis of an α-alkoxylithium-β-diimine
Carey, David T.; Cope-Eatough, Elaine K.; Vilaplana-Mafé, Eva; Mair, Francis S.; Pritchard, Robin G.; Warren, John E.; Woods, Rebecca J.; Dalton Transactions  (2003) 1083–; doi:10.1039/b212079h

data_7012553
_publ_section_title
;
 Structures and reactions of monomeric and dimeric lithium
 diazapentadienyl complexes with electrophiles: synthesis of
 \a-C,C'-dialkyl-\b-diimines, and dissolution-reversible synthesis of
 an \a-alkoxylithium-\b-diimine
;
_journal_issue                   6
_journal_name_full               'Dalton Transactions'
_journal_page_first              1083
_journal_paper_doi               10.1039/b212079h
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C35 H53 Li1 N2 O3'
_chemical_formula_sum            'C35 H53 Li N2 O3'
_chemical_formula_weight         556.73
_space_group_IT_number           160
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      160
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2002-09-16T16:50:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   32.123(9)
_cell_length_b                   32.123(9)
_cell_length_c                   9.273(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7.6
_cell_measurement_wavelength     0.71073
_cell_volume                     8287(4)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5339
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.2
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  0.9876
_exptl_absorpt_correction_T_min  0.9815
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was   3
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.004
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.15
_refine_diff_density_min         -0.125
_refine_diff_density_rms         0.03
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(4)
_refine_ls_extinction_coef       0.00069(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         1817
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.055
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1434
_reflns_number_gt                1022
_reflns_number_total             1817
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b212079h.txt
_cod_data_source_block           2c
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               7012553