Alkali-Metal-Induced C‒C Bond Cleavage and CH4Elimination in the Amido →Aza-Allyl Transformation of the (S)-N-α-(Methylbenzyl)benzylamido Anion
Andrews, Philip C.; Blair, Victoria L.; Border, Emily C.; Peatt, Anna C.; MacLellan, Jonathan G.; Thompson, Christopher D.; Organometallics 32 (2013) 7509–; doi:10.1021/om400997b

data_4082184
_publ_section_title
;
 Alkali-Metal-Induced C--C Bond Cleavage and CH4Elimination in the Amido
 \\rightarrow Aza-Allyl Transformation of the
 (S)-N-\a-(Methylbenzyl)benzylamido Anion
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7509
_journal_paper_doi               10.1021/om400997b
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C21 H30 N3 Na'
_chemical_formula_sum            'C21 H30 N3 Na'
_chemical_formula_weight         347.47
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 93.79(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.165(3)
_cell_length_b                   9.6420(19)
_cell_length_c                   28.075(6)
_cell_measurement_reflns_used    15479
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.80
_cell_measurement_theta_min      2.85
_cell_volume                     4096.2(14)
_computing_cell_refinement       'DENZO-SMN (Otwinoski & Minor, 1997)'
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        'DENZO-SMN (Otwinoski & Minor, 1997)'
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  '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  0.0876
_diffrn_reflns_av_sigmaI/netI    0.0921
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            15479
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.85
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3610
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1288
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0770P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1547
_reflns_number_gt                1913
_reflns_number_total             3610
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400997b_si_002.cif
_cod_data_source_block           sambnatm
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4082184