Characterization of β-Amino Ester Enolates as Hexamers via 6Li NMR Spectroscopy
Anne J. McNeil; Gilman E. S. Toombes; Sithamalli V. Chandramouli; Benoit J. Vanasse; Timothy A. Ayers; Michael K. O'Brien; Emil Lobkovsky; Sol M. Gruner; John A. Marohn; David B. Collum; Journal of the American Chemical Society 126 (2004) 5938–5939; doi:10.1021/ja049245s

data_4112564
_publ_section_title
;
 Characterization of \b-Amino Ester Enolates as Hexamers via 6Li NMR
 Spectroscopy
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5938
_journal_page_last               5939
_journal_paper_doi               10.1021/ja049245s
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C15 H30 Li3 N3 O6'
_chemical_formula_weight         369.24
_chemical_name_systematic
;
 ?
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.83(3)
_cell_angle_beta                 104.60(2)
_cell_angle_gamma                111.29(3)
_cell_formula_units_Z            4
_cell_length_a                   13.423(11)
_cell_length_b                   13.495(12)
_cell_length_c                   13.817(12)
_cell_measurement_temperature    173(2)
_cell_volume                     2235(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker 1K CCD area detector'
_diffrn_measurement_method       '0.6 deg. 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  0.0575
_diffrn_reflns_av_sigmaI/netI    0.1165
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9964
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.9920
_exptl_absorpt_correction_T_min  0.9684
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_density_meas      0
_exptl_crystal_description       irregular
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         6120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1275
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          2.283
_refine_ls_shift/su_mean         0.100
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0939P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1793
_reflns_number_gt                3433
_reflns_number_total             6120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja049245ssi20040211_071635.cif
_cod_data_source_block           am1
_cod_database_code               4112564