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_7009625
_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_structural     '[{Li(thf)(Me3SiNCPhNCPhCHNSiMe3)}2]'
_chemical_formula_sum            'C50 H74 Li2 N4 O2 Si4'
_chemical_formula_weight         889.37
_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                94.22(7)
_cell_angle_beta                 93.81(7)
_cell_angle_gamma                110.94(8)
_cell_formula_units_Z            1
_cell_length_a                   11.075
_cell_length_b                   11.440(5)
_cell_length_c                   11.514(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     1352.0(12)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_molecular_graphics    'CAMERON (Watkin and Pearce,1993)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       ' Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_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    0.0970
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3289
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.149
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.991
_refine_ls_goodness_of_fit_obs   1.048
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_restrained_S_obs      1.048
_refine_ls_R_factor_all          0.1281
_refine_ls_R_factor_obs          0.0793
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1451P)^2^+0.7252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2341
_refine_ls_wR_factor_obs         0.1946
_reflns_number_observed          2096
_reflns_number_total             3289
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b002376k.txt
_cod_data_source_block           oct797
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1451P)^2^+0.7252P] 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^)+(0.1451P)^2^+0.7252P] 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        1352.0(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7009625