Perturbation of Conjugation in Internally Solvated Allylic Lithium Compounds: Variation of Ligand Structure. NMR and X-ray Crystallography
Gideon Fraenkel; Judith Gallucci; Hua Liu; Journal of the American Chemical Society 128 (2006) 8211–8216; doi:10.1021/ja060272n

data_4110654
_publ_section_title
;
 Perturbation of Conjugation in Internally Solvated Allylic Lithium
 Compounds: Variation of Ligand Structure. NMR and X-ray Crystallography
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8211
_journal_page_last               8216
_journal_paper_doi               10.1021/ja060272n
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C16 H32 Li2 N2 O2'
_chemical_formula_sum            'C16 H32 Li2 N2 O2'
_chemical_formula_weight         298.32
_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-93
_cell_angle_alpha                106.77(1)
_cell_angle_beta                 98.97(1)
_cell_angle_gamma                94.35(1)
_cell_formula_units_Z            1
_cell_length_a                   7.446(1)
_cell_length_b                   8.187(1)
_cell_length_c                   8.583(2)
_cell_measurement_temperature    200(2)
_cell_volume                     490.79(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega 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  0.023
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11734
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.009
_exptl_crystal_description       chunk
_exptl_crystal_F_000             164
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.157
_refine_diff_density_min         -0.132
_refine_diff_density_rms         0.027
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.046
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2231
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_restrained_S_obs      1.071
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          -0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+0.0784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1221
_refine_ls_wR_factor_ref         0.1168
_reflns_number_gt                1956
_reflns_number_total             2231
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja060272nsi20060113_045330.cif
_cod_data_source_block           Fraenkel1107
_cod_original_cell_volume        490.79(14)
_cod_database_code               4110654