Reactions of LiCHR2 and related lithium alkyls with α-H free nitriles and the crystal structures of eleven representative lithium 1,3-diazaallyls, 1-azaallyls and β-diketiminates
Hitchcock, Peter B.; Lappert, Michael F.; Layh, Marcus; Liu, Dian-Sheng; Sablong, Rafael; Shun, Tian; Journal of the Chemical Society, Dalton Transactions  (2000) 2301–; doi:10.1039/b002376k

data_7009623
_publ_section_title
;
 Reactions of LiCHR2 and related lithium alkyls with \a-H free nitriles
 and the crystal structures of eleven representative lithium
 1,3-diazaallyls, 1-azaallyls and \b-diketiminates
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2301
_journal_paper_doi               10.1039/b002376k
_journal_year                    2000
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C23 H36 Li1 N3 Si1'
_chemical_formula_structural     'C23 H36 LI N3 SI'
_chemical_formula_sum            'C23 H36 Li N3 Si'
_chemical_formula_weight         389.58
_chemical_name_common            '[Li(tmeda)(Me3SiNCPhCHPh)]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             2000-03-07T16:35:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 111.457(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0529(3)
_cell_length_b                   31.5904(10)
_cell_length_c                   8.2296(2)
_cell_measurement_reflns_used    13045
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      4.529
_cell_measurement_wavelength     0.71073
_cell_volume                     2432.38(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_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, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_sigmaI/netI    0.0784
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12641
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         4.54
_exptl_absorpt_coefficient_mu    0.108
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4262
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0686P)^2^+0.8883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1532
_reflns_number_gt                2841
_reflns_number_total             4262
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002376k.txt
_cod_data_source_block           mar1200
_cod_original_cell_volume        2432.38(12)
_cod_original_sg_symbol_Hall     '-P 2yab'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7009623