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_4106675
_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            'C32 H70 Li2 N4 O2 Zn2'
_chemical_formula_weight         687.54
_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                82.577(5)
_cell_angle_beta                 78.661(6)
_cell_angle_gamma                81.212(6)
_cell_formula_units_Z            1
_cell_length_a                   8.7028(6)
_cell_length_b                   10.0294(7)
_cell_length_c                   11.2396(7)
_cell_measurement_reflns_used    5330
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.78
_cell_measurement_theta_min      2.62
_cell_volume                     945.60(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.979
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0803
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10295
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.299
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       plate
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.084
_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     234
_refine_ls_number_reflns         4928
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0391P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0834
_reflns_number_gt                3715
_reflns_number_total             4928
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja205547h_si_002_2.cif
_cod_data_source_block           pgaross19
_cod_database_code               4106675