Organoaluminum Hydroxides Supported by β-Diketiminato Ligands: Synthesis, Structural Characterization, and Reactions
Yang, Ying; Schulz, Thomas; John, Michael; Yang, Zhi; Jiménez-Pérez, Victor Manuel; Roesky, Herbert W.; Gurubasavaraj, Prabhuodeyara M.; Stalke, Dietmar; Ye, Hongqi; Organometallics 27 (2008) 769–; doi:10.1021/om700969g

data_4070726
_publ_contact_author
'Prof. Dr. Dietmar Stalke, Prof. Dr. H. W. Roesky'
_publ_section_title
;
 Organoaluminum Hydroxides Supported by \b-Diketiminato Ligands:
 Synthesis, Structural Characterization, and Reactions
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              769
_journal_paper_doi               10.1021/om700969g
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C32 H38 Al N2 O'
_chemical_formula_weight         493.62
_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                93.6510(10)
_cell_angle_beta                 106.2490(10)
_cell_angle_gamma                114.6840(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4187(11)
_cell_length_b                   11.5317(11)
_cell_length_c                   12.1602(11)
_cell_measurement_reflns_used    8831
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.302
_cell_measurement_theta_min      2.2395
_cell_volume                     1366.6(2)
_computing_cell_refinement       'SAINT V7.23A'
_computing_data_collection       'APEX2 v2.1.0'
_computing_data_reduction        'SAINT V7.23A'
_computing_molecular_graphics    'XP in SHELXTL ver. 6.12'
_computing_publication_material  'XP in SHELXTL ver. 6.12'
_computing_structure_refinement  'SHELXL in SHELXTL ver. 6.12'
_computing_structure_solution    'SHELXS in SHELXTL ver. 6.12'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Bruker TXS-Mo rotating anode with APEX II detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC Helios mirror optics'
_diffrn_radiation_source         'Bruker TXS-Mo rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25588
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.786432
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2004/1
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             530
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5606
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0428P)^2^+0.7135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                4370
_reflns_number_total             5606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700969g-file002.cif
_cod_data_source_block           L1AlPh(OH)
_cod_original_cell_volume        1366.5(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4070726