Tetrahedranyllithium: Synthesis, Characterization, and Reactivity
Akira Sekiguchi; Masanobu Tanaka; Journal of the American Chemical Society 125 (2003) 12684–12685; doi:10.1021/ja030476t

data_4114267
_publ_section_title
;
 Tetrahedranyllithium: Synthesis, Characterization, and Reactivity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12684
_journal_page_last               12685
_journal_paper_doi               10.1021/ja030476t
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C22 H51 Li N3 Si3'
_chemical_formula_weight         448.87
_chemical_name_systematic
; 
 Tris(trimethylsilyl)tetrahedranyllithium
 (N,N,N',N'-tetramethyletylenediamine)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.278(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1390(2)
_cell_length_b                   15.1390(5)
_cell_length_c                   22.1150(6)
_cell_measurement_reflns_used    30115
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.28
_cell_volume                     3051.20(15)
_computing_cell_refinement       'HKL scalepack'
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        Denzo
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'MacScience DIP2030 Image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            30115
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    0.977
_exptl_crystal_description       Plate
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0211(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         7253
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+0.6894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1054
_reflns_number_gt                6367
_reflns_number_total             7253
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja030476t.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4114267