The reactions of lithium trimethysilylmethyls with isocyanides; structures and reactions of the derived lithium 1-azaallyls, β-diketiminates and a 1-azabuta-1,3-dienyl-3-amide
Hitchcock, Peter B.; Lappert, Michael F.; Layh, Marcus; Journal of the Chemical Society, Dalton Transactions  (2001) 2409–; doi:10.1039/b103553n

data_7010780
_publ_section_title
;
 The reactions of lithium trimethysilylmethyls with isocyanides;
 structures and reactions of the derived lithium 1-azaallyls,
 \b-diketiminates and a 1-azabuta-1,3-dienyl-3-amide
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2409
_journal_paper_doi               10.1039/b103553n
_journal_year                    2001
_chemical_formula_structural     '[(tmeda)Li{PhCHC(SiMe3)NC6H3Me2}]'
_chemical_formula_sum            'C25 H40 Li N3 Si'
_chemical_formula_weight         417.63
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 113.77(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.900(7)
_cell_length_b                   8.553(2)
_cell_length_c                   19.852(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     5112(2)
_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
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_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_sigmaI/netI    0.1624
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4567
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    riding
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_refine_ls_number_reflns         4494
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_refine_ls_R_factor_all          0.1941
_refine_ls_R_factor_obs          0.0884
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+17.3952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2225
_refine_ls_wR_factor_obs         0.1695
_reflns_number_observed          2174
_reflns_number_total             4494
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b103553n.txt
_cod_data_source_block           mfl-6b-(jan1698)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+17.3952P] 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^)+(0.0581P)^2^+17.3952P] 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        5112.4(21)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7010780