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_7012554
_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         'C38 H42 Li2 N4 O4'
_chemical_formula_sum            'C38 H42 Li2 N4 O4'
_chemical_formula_weight         632.64
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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             2002-08-01T11:48:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                77.010(2)
_cell_angle_beta                 85.387(2)
_cell_angle_gamma                66.242(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6917(4)
_cell_length_b                   11.8407(5)
_cell_length_c                   15.3648(9)
_cell_measurement_reflns_used    73598
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.283
_cell_measurement_theta_min      1.018
_cell_measurement_wavelength     0.71073
_cell_volume                     1734.63(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_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, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.991479E-1
_diffrn_orient_matrix_UB_12      -0.307285E-1
_diffrn_orient_matrix_UB_13      -0.154435E-1
_diffrn_orient_matrix_UB_21      -0.246849E-1
_diffrn_orient_matrix_UB_22      0.239624E-1
_diffrn_orient_matrix_UB_23      -0.649233E-1
_diffrn_orient_matrix_UB_31      -0.21379E-2
_diffrn_orient_matrix_UB_32      0.859786E-1
_diffrn_orient_matrix_UB_33      -0.28905E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21314
_diffrn_reflns_reduction_process
;
Scaled and merged with SORTAV
R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.19
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.9732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.195
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.038
_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     601
_refine_ls_number_reflns         7179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1183
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+0.1646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.135
_refine_ls_wR_factor_ref         0.1619
_reflns_number_gt                4221
_reflns_number_total             7179
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b212079h.txt
_cod_data_source_block           2g
_cod_database_code               7012554