Aluminum-Ligand Cooperative N-H Bond Activation and an Example of Dehydrogenative Coupling
Thomas W. Myers; Louise A. Berben; Journal of the American Chemical Society 135 (2013) 9988–9990; doi:10.1021/ja4032874

data_4120057
_publ_section_title
;
 Aluminum-Ligand Cooperative N-H Bond Activation and an Example of
 Dehydrogenative Coupling
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9988
_journal_page_last               9990
_journal_paper_doi               10.1021/ja4032874
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C55 H67 Al N4'
_chemical_formula_weight         811.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 113.3670(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.56300(10)
_cell_length_b                   26.0112(3)
_cell_length_c                   20.3273(2)
_cell_measurement_reflns_used    90
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.48
_cell_measurement_theta_min      2.84
_cell_volume                     4641.61(9)
_computing_cell_refinement       'Bruker Duo'
_computing_data_collection       'Bruker Duo'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Bruker Shelxtl'
_computing_publication_material  'Bruker Shelxtl'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'ccd area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17016
_diffrn_reflns_theta_full        68.72
_diffrn_reflns_theta_max         68.72
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  0.9578
_exptl_absorpt_correction_T_min  0.8857
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.187
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         8215
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0627
_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^)+(0.0805P)^2^+6.0842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.1675
_reflns_number_gt                7209
_reflns_number_total             8215
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4032874_si_002_2.cif
_cod_data_source_block           twm129
_cod_database_code               4120057