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_4110653
_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         'C12 H26 Li N3'
_chemical_formula_sum            'C12 H26 Li N3'
_chemical_formula_weight         219.30
_chemical_name_systematic
;
  ?
;
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_cell_angle_beta                 102.21(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.582(1)
_cell_length_b                   8.878(1)
_cell_length_c                   18.408(2)
_cell_measurement_temperature    150(2)
_cell_volume                     1370.8(3)
_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      150(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  0.030
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
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_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.063
_exptl_crystal_description       chunk
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.064
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3138
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_restrained_S_obs      1.106
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          -0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+0.1769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.0988
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_reflns_number_total             3138
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja060272nsi20060113_045259.cif
_cod_data_source_block           Fraenkel1103
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4110653