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_7009621
_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_formula_sum            'C29 H45 Li N2 O2 Si2'
_chemical_formula_weight         516.79
_chemical_name_common            '[Li(thf)2(Me3SiNCPhCHPhNSiMe3)]'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL
_cell_angle_alpha                86.25(3)
_cell_angle_beta                 80.98(4)
_cell_angle_gamma                76.52(3)
_cell_formula_units_Z            6
_cell_length_a                   10.189(5)
_cell_length_b                   21.686(5)
_cell_length_c                   22.163(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     4701(3)
_computing_data_collection       'Enraf-Nonius CAD4 software'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       'omega-2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0874
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11482
_diffrn_reflns_theta_max         21.98
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.121
_refine_ls_goodness_of_fit_obs   1.267
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         11478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_restrained_S_obs      1.267
_refine_ls_R_factor_all          0.1398
_refine_ls_R_factor_obs          0.1018
_refine_ls_shift/esd_max         0.009
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+47.2046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2984
_refine_ls_wR_factor_obs         0.2754
_reflns_number_observed          7900
_reflns_number_total             11482
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b002376k.txt
_cod_data_source_block           dec1597
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+47.2046P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+47.2046P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4701.2(32)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7009621