Synthesis and structures of lithium N-trimethylsilyl- and -neopentyl-anilides and their Et2O and tmen adducts; crystal structures of [(Li{μ-N(Ph)R}-trans)2(μ-tmen)]∞ (R = SiMe3 1 or CH2But 2) and [Li{μ-N(Ph)CH2But}(OEt2)]2 †
Bezombes, Jean Philippe; Hitchcock, Peter B.; Lappert, Michael F.; Merle, Philippe G.; Journal of the Chemical Society, Dalton Transactions  (2001) 816–; doi:10.1039/b009724l

data_7010493
_publ_section_title
;
 Synthesis and structures of lithium N-trimethylsilyl- and
 -neopentyl-anilides and their Et2O and tmen adducts; crystal
 structures of [(Li{\m-N(Ph)R}-trans)2(\m-tmen)]\\infty
 (R&#x2005;=&#x2005;SiMe3 1 or CH2But 2) and
 [Li{\m-N(Ph)CH2But}(OEt2)]2&#x200A;&#x2020;
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              816
_journal_paper_doi               10.1039/b009724l
_journal_year                    2001
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C30 H52 Li2 N2 O2'
_chemical_formula_structural     'C30 H52 LI2 N2 O2'
_chemical_formula_sum            'C30 H52 Li2 N2 O2'
_chemical_formula_weight         486.62
_chemical_name_common            '[{Li(OEt2)(PhNCH2tBu)}2]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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             1999-11-09T15:43:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 95.7960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9810(2)
_cell_length_b                   16.1914(4)
_cell_length_c                   19.2524(4)
_cell_measurement_reflns_used    14770
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      4.246
_cell_measurement_wavelength     0.71073
_cell_volume                     3095.40(12)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25409
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         4.33
_exptl_absorpt_coefficient_mu    0.063
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.044
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         7257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0897P)^2^+1.3997P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.1795
_reflns_number_gt                5366
_reflns_number_total             7257
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b009724l.txt
_cod_data_source_block           nov1399
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7010493