Main Group Multiple C-H/N-H Bond Activation of a Diamine and Isolation of A Molecular Dilithium Zincate Hydride: Experimental and DFT Evidence for Alkali Metal-Zinc Synergistic Effects
Ross Campbell; Daniel Cannon; Pablo García-Álvarez; Alan R. Kennedy; Robert E. Mulvey; Stuart D. Robertson; Jörg Saßmannshausen; Tell Tuttle; Journal of the American Chemical Society 133 (2011) 13706–13717; doi:10.1021/ja205547h

data_4106678
_publ_section_title
;
 Main Group Multiple C-H/N-H Bond Activation of a Diamine and Isolation of
 A Molecular Dilithium Zincate Hydride: Experimental and DFT Evidence for
 Alkali Metal-Zinc Synergistic Effects
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13706
_journal_page_last               13717
_journal_paper_doi               10.1021/ja205547h
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C24 H49 N2 Na O3 Zn'
_chemical_formula_weight         502.01
_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                81.497(4)
_cell_angle_beta                 88.765(3)
_cell_angle_gamma                84.978(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6661(3)
_cell_length_b                   9.8248(5)
_cell_length_c                   15.2836(7)
_cell_measurement_reflns_used    13826
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      72.9858
_cell_measurement_theta_min      4.5542
_cell_volume                     1429.93(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.1020
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15955
_diffrn_reflns_theta_full        64.99
_diffrn_reflns_theta_max         64.99
_diffrn_reflns_theta_min         4.57
_exptl_absorpt_coefficient_mu    1.521
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_description       prism
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.357
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1433P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1663
_refine_ls_wR_factor_ref         0.1701
_reflns_number_gt                4393
_reflns_number_total             4793
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja205547h_si_002_5.cif
_cod_data_source_block           pgapga18
_cod_database_code               4106678