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_4082182
_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         'C27 H38 N Na O3'
_chemical_formula_sum            'C27 H38 N Na O3'
_chemical_formula_weight         447.57
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.26(3)
_cell_angle_beta                 71.20(3)
_cell_angle_gamma                72.66(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3243(19)
_cell_length_b                   11.022(2)
_cell_length_c                   13.790(3)
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_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.41
_cell_volume                     1275.2(6)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        Nonius
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'Microsoft Office 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'psi 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  0.0716
_diffrn_reflns_av_sigmaI/netI    0.1131
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
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_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
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_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.41
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            'red green'
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
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_refine_diff_density_max         0.699
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         4467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1622
_refine_ls_R_factor_gt           0.0691
_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^)+(0.1050P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1691
_refine_ls_wR_factor_ref         0.2084
_reflns_number_gt                2097
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400997b_si_002.cif
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_cod_original_cell_volume        1275.3(6)
_cod_original_sg_symbol_H-M      P-1
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