Synthesis and Stability of Homoleptic Metal(III) Tetramethylaluminates
Giovanni Occhipinti; Christian Meermann; H. Martin Dietrich; Rannveig Litlabø; Florian Auras; Karl Wilhelm Törnroos; Cäcilia Maichle-Mössmer; Vidar R. Jensen; Reiner Anwander; Journal of the American Chemical Society 133 (2011) 6323–6337; doi:10.1021/ja2001049

data_4106031
_publ_contact_author_address
;
;
_publ_contact_author_email       wolfgang.scherer@physik.uni-augsburg.de
_publ_contact_author_name
;
  Prof. Dr. W. Scherer, wolfgang.scherer@physik.uni-augsburg.de
;
_publ_section_title
;
 Synthesis and Stability of Homoleptic Metal(III) Tetramethylaluminates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6323
_journal_page_last               6337
_journal_paper_doi               10.1021/ja2001049
_journal_volume                  133
_journal_year                    2011
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C12 H36 Al3 Ce'
_chemical_formula_sum            'C12 H36 Al3 Ce'
_chemical_formula_weight         401.47
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_date             'Mar 14 17:00:14 2010'
_audit_creation_method           'PLATON <TABLE ACC> option'
_audit_update_record
;
;
_cell_angle_alpha                90
_cell_angle_beta                 108.531(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.8247(13)
_cell_length_b                   18.2909(12)
_cell_length_c                   13.7888(10)
_cell_measurement_reflns_used    38473
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.46
_cell_measurement_theta_min      3.24
_cell_volume                     4262.5(5)
_computing_cell_refinement       'X-Area,   (STOE&Cie, 2006)'
_computing_data_collection       'X-Area,   (STOE&Cie, 2006)'
_computing_data_reduction        'SORTAV,   (Blessing 1995)'
_computing_molecular_graphics    'PLATON    (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92     (Altomare (1993)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56085
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0589
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23613
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        20.52
_diffrn_reflns_theta_max         20.52
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    1.190
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
A multi-scan absorption correction was performed using 'Sortav'
R. H. Blessing Acta Crystallogr. 1995, A51, 33-37.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         8456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
'w=1/sigma^2(Fo)^2 + (0.0434*P)^2 where P=(Max(Fo^2,0) + 2*Fc^2)/3'
;
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0952
_reflns_number_gt                6036
_reflns_number_total             8456
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja2001049_si_005.cif
_cod_data_source_block           Compound4a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4106031